CERTIFICATION AND SURVEILLANCE ASSESSMENT OF …...NOBLE GAS SAMPLE ANALYSIS This paper is a revised...

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CTBT/PTS/INF.96/Rev.9*

1 August 2012

ENGLISH ONLY

CERTIFICATION AND SURVEILLANCE ASSESSMENT OF

RADIONUCLIDE LABORATORIES FOR PARTICULATE AND

NOBLE GAS SAMPLE ANALYSIS

This paper is a revised version of the guidelines on certification of radionuclide

laboratories, and recommendations on the current paper from Working Group B are

welcome. The main revisions of CTBT/PTS/INF.96/Rev.81 to Rev.7 are updated

management requirements in Section 4 so that they correspond to the quality system

currently in use, categorization of noble gas samples were added in Section 5, a more

detailed description of evaluation of acceptability of analytical results in Section 6, general

requirements for optional noble gas samples analysis in Section 7 and an updated procedure

for the surveillance assessment of a certified radionuclide laboratory in Section 10. The

checklist for surveillance assessment of a certified laboratory is included in Appendix VI

and the certification checklists for noble gas sample analysis are presented in Appendix IX.

After Rev.8 was issued, a few changes were made as a result of additional feedback from

radionuclide laboratories and experts. The main revisions to CTBT/PTS/INF.96/Rev.8 are

the inclusion of an energy calibration linearity requirement for the gamma ray spectrometry

system, clarification of the minimum detectable activity (MDA) requirement for radioxenon

analysis and revisions in the surveillance assessment visit checklist.

Summary

This document describes the certification requirements and the process of certifying the

radionuclide laboratories which support the network of International Monitoring System

(IMS) radionuclide stations. It contains management and technical requirements for the

analysis of both particulate and noble gas samples from IMS radionuclide monitoring

stations. In terms of technique-specific procedures for the analysis of IMS particulate

samples, certification issues related to gamma ray spectrometric analysis only are addressed

at this stage. The procedure and checklist to be used during surveillance assessment of

certified laboratories for particulate samples analysis are also included.

1 *

Reissued for technical reasons.

CTBT/PTS/INF.96/Rev.9

Contents

1. ABBREVIATIONS AND DEFINITIONS .......................................................................................................... 5

1.1. Abbreviations ................................................................................................................................ 5 1.2. Definitions ..................................................................................................................................... 5 2. INTRODUCTION................................................................................................................................................ 9

2.1. Radionuclide Laboratory Network ................................................................................................ 9 2.2. Radionuclide Laboratory Quality Systems and Certification ....................................................... 9 2.3. Objectives of Radionuclide Laboratory Analyses ....................................................................... 10 2.4. Data Quality Objectives .............................................................................................................. 10 3. OPERATIONAL RESPONSIBILITIES ............................................................................................................ 10 4. MANAGEMENT REQUIREMENTS ............................................................................................................... 12

4.1. Organization ................................................................................................................................ 12 4.2. Quality System ............................................................................................................................ 12 4.3. Quality Manual ........................................................................................................................... 12 4.4. Technical Documentation ........................................................................................................... 13 4.5. Control of Records ...................................................................................................................... 13 4.6. Other Management Requirements ............................................................................................... 14 5. TECHNICAL REQUIREMENTS .................................................................................................................... 14

5.1. Preparedness................................................................................................................................ 14 5.2. Personnel ..................................................................................................................................... 15 5.3. Environmental Conditions .......................................................................................................... 15 5.4. Methods ....................................................................................................................................... 16

5.4.1. Selection of Methods ........................................................................................................ 16 5.4.2. Validation of Methods ...................................................................................................... 17 5.4.3. Uncertainty of Measurement ............................................................................................ 17

5.5. Equipment ................................................................................................................................... 17 5.5.1. General .............................................................................................................................. 17 5.5.2. Technique Specific Requirements for Equipment ............................................................ 18 5.5.3. Global Communications Infrastructure ............................................................................. 18

5.6. Measurement Traceability ........................................................................................................... 18 5.6.1. Calibration ........................................................................................................................ 18 5.6.2. Reference Standards and Materials ................................................................................... 19

5.7. Different IMS Sample Categories ............................................................................................... 19 5.7.1. Particulate Sample Categories .......................................................................................... 19 5.7.2. Noble Gas Sample Categories .......................................................................................... 20

5.8. Sample Management ................................................................................................................... 20 5.8.1. Receipt and Dispatch of Samples ..................................................................................... 20 5.8.2. Security of Samples .......................................................................................................... 21 5.8.3. Laboratory Sample Tracking ............................................................................................ 21 5.8.4. Handling of Samples ......................................................................................................... 21

5.9. Quality Assurance of Analysis Results and Data Verification.................................................... 22 5.9.1. Quality Assurance of Analysis Results ............................................................................. 22 5.9.2. Data Verification............................................................................................................... 22

5.10. Management of Analysis Data .................................................................................................... 22 5.11. Reporting ..................................................................................................................................... 22

5.11.1.Contents of the Report and Reporting Time .................................................................... 22 5.11.2. Data and Report Format .................................................................................................. 22 5.11.3. Data Authentication ........................................................................................................ 23

5.12. Messages ..................................................................................................................................... 23 5.12.1. Communication Protocols ............................................................................................... 23 5.12.2. Communication Software ................................................................................................ 23 5.12.3. Laboratory Message Format and Contents ...................................................................... 23

6. REQUIREMENTS FOR GAMMA SPECTROMETRIC ANALYSIS

OF PARTICULATE SAMPLES ....................................................................................................................... 23


6.1. Sample Preparation ..................................................................................................................... 23 6.2. Spectral Acquisition and Analysis .............................................................................................. 24 6.3. Detector Efficiency ..................................................................................................................... 24 6.4. Detector Calibration .................................................................................................................... 24 6.5. Minimum Detectable Activity..................................................................................................... 25 6.6. Energy Resolution and Peak Shape ............................................................................................. 26 6.7. Detector Background and Blank Measurements ......................................................................... 26 6.8. Sample Counting Geometry ........................................................................................................ 26 6.9. Uncertainty of Analytical Results ............................................................................................... 26 6.10. Reporting ..................................................................................................................................... 27

6.10.1. Reporting Schedules ........................................................................................................ 27 6.10.2. Report Content ................................................................................................................ 28 6.10.3. Report Format ................................................................................................................. 28

6.11. Acceptability of Analysis Results ............................................................................................... 28 7. REQUIREMENTS FOR NOBLE GAS SAMPLE ANALYSIS. ...................................................................... 29

7.1. General Requirements ................................................................................................................. 30 7.1.1. Minimum Detectable Activity .......................................................................................... 30 7.1.2. Sample Preparation ........................................................................................................... 30 7.1.3. Detector Background ........................................................................................................ 31 7.1.4. Blank Sample Measurement ............................................................................................. 31 7.1.5. Gas Background Measurement ......................................................................................... 31 7.1.6. Sample Counting Geometry .............................................................................................. 31 7.1.7. Measurement Cell ............................................................................................................. 31 7.1.8. Uncertainty of Analytical Results ..................................................................................... 31 7.1.9. Reporting .......................................................................................................................... 32 7.1.10. Auxiliary Measurements ................................................................................................. 32 7.1.11. Cross-Contamination ....................................................................................................... 32

7.2. Requirements for the Gas Quantification System ....................................................................... 33 7.2.1. Noble Gas Sample Transfer and Processing ..................................................................... 33 7.2.2. Optional Gas Composition Measurement ......................................................................... 33

7.3. Requirements for Spectrometric Analysis of Noble Gas Samples .............................................. 33 7.3.1. Spectral Acquisition and Analysis .................................................................................... 33 7.3.2. Detector Calibration .......................................................................................................... 33

8. CERTIFICATION PROCESS .......................................................................................................................... 34

9. CERTIFICATION PROCEDURES .................................................................................................................. 39

9.1. Formal Arrangement ................................................................................................................... 39 9.2. Acceptance of Documentation .................................................................................................... 39

9.2.1. Objective ........................................................................................................................... 39 9.2.2. Documents to be Reviewed .............................................................................................. 40 9.2.3. Procedure .......................................................................................................................... 40

9.3. Acceptance of the Quality of Analytical Results ........................................................................ 41 9.3.1. Objective ........................................................................................................................... 41 9.3.2. Procedure .......................................................................................................................... 41

9.4. Formats Check ............................................................................................................................ 42 9.4.1. Objective ........................................................................................................................... 42 9.4.2. Procedure .......................................................................................................................... 42

9.5. Communication Test ................................................................................................................... 42 9.5.1. Objective ........................................................................................................................... 42 9.5.2. Procedure .......................................................................................................................... 42

9.6. Authentication Test ..................................................................................................................... 42 9.6.1. Objective ........................................................................................................................... 42 9.6.2. Procedure .......................................................................................................................... 42

9.7. IMS Sample Analysis Test .......................................................................................................... 43 9.7.1. Objective ........................................................................................................................... 43

9.8. Certification Visit ........................................................................................................................ 43


9.8.1. Objective ........................................................................................................................... 43 9.8.2. Items to Be Evaluated ....................................................................................................... 43 9.8.3. Procedure .......................................................................................................................... 43

9.9. Formal Certification .................................................................................................................... 44 9.10. Certification of Additional Equipment ........................................................................................ 44 10. SURVEILLANCE ASSESSMENT OF A CERTIFIED LABORATORY ..................................................... 44

10.1. Objective ..................................................................................................................................... 44 10.2. Items to be Evaluated .................................................................................................................. 45

10.2.1. Intercomparison and Proficiency Test Programme ......................................................... 45 10.2.2. Performance in IMS Sample Analysis ............................................................................ 45 10.2.3. Changes at the Radionuclide Laboratory and in the Documentation .............................. 45

10.3. Procedure for Surveillance Assessment ...................................................................................... 45 11. TECHNIQUE SPECIFIC PROCEDURES ..................................................................................................... 46

11.1. Gamma Spectrometric Analysis .................................................................................................. 46 11.1.1. Radionuclide Detection Sensitivity ................................................................................. 46 11.1.2. Radionuclide Analysis Check ......................................................................................... 47

11.2. Certification of Additional Spectrometry Systems ..................................................................... 47 11.2.1. Objective ......................................................................................................................... 47 11.2.2. Items to be Evaluated ...................................................................................................... 47 11.2.3. Procedure ......................................................................................................................... 48

12. BIBLIOGRAPHY ............................................................................................................................................ 48

12.1. CTBT Related Documents .......................................................................................................... 48 12.2. Publications and Standards ......................................................................................................... 49

APPENDIX I: OVERVIEW OF MESSAGES RELATED TO ANALYSIS OF IMS

SAMPLES AT RADIONUCLIDE LABORATORIES ........................................................................................ 51

APPENDIX II: PROCEDURE FOR DETERMINING THE MINIMUM DETECTABLE

ACTIVITY ............................................................................................................................................................ 55 APPENDIX III: RECOMMENDED PROCEDURE TO ESTIMATE THE UNCERTAINTY OF

ANALYSIS RESULTS BY GAMMA RAY SPECTROMETRY ........................................................................ 57 APPENDIX IV: CONTENT OF REPORTS FOR GAMMA SPECTROMETRIC ANALYSIS

(PARTICULATES) .............................................................................................................................................. 60

APPENDIX V: CERTIFICATION CHECKLISTS (PARTICULATES) ............................................................ 82

APPENDIX VI: SURVEILLANCE ASSESSMENT PLAN AND CHECKLIST ............................................... 82

APPENDIX VII: IMS RADIONUCLIDE LABORATORY SET-UP INFORMATION ..................................... 88 APPENDIX VIII: CONTENT OF REPORTS FOR IMS XENON SAMPLE ANALYSIS FOR

NETWORK QUALITY ASSURANCE/QUALITY CONTROL PURPOSES .................................................... 93

APPENDIX IX: CERTIFICATION CHECKLISTS ( NOBLE GAS) .................................................................. 95

ANNEX I: GUIDANCE ON THE STRUCTURE AND CONTENT OF CTBT SPECIFIC

DOCUMENTATION FOR RADIONUCLIDE LABORATORIES ................................................................... 112


1. ABBREVIATIONS AND DEFINITIONS

1.1. Abbreviations

AWB airway bill

CTBT Comprehensive Nuclear-Test-Ban Treaty

CTBTO Comprehensive Nuclear-Test-Ban Treaty Organization

DSA digital signature algorithm

ETA estimated time of arrival

FWHM full width at half-maximum (of photopeak)

FWTM full width at tenth-maximum (of photopeak)

GCI Global Communications Infrastructure

HPGe

IDC

high purity germanium detector

International Data Centre

IMS

ISO

International Monitoring System

International Organization for Standardization

MDA minimum detectable activity

MDC minimum detectable concentration

PKI Public Key Infrastructure

PTS

PTE

Provisional Technical Secretariat

proficiency test exercise

QA quality assurance

QC quality control

RL

RLR

radionuclide laboratory

Radionuclide Laboratory Report

SRID sample reference identification

WGB Working Group B

1.2. Definitions

Certification The assessment of a radionuclide laboratory’s compliance

with the requirements described in this document. This

leads to formal acceptance of the radionuclide laboratory

by the PTS to support the network of IMS radionuclide

stations.

Combined standard uncertainty Standard uncertainty of the result of a measurement when

that result is obtained from the values of a number of other

quantities equal to the positive square root of a sum of

terms, the terms being the variances or covariances of

these other quantities weighted according to how the

measurement result varies with changes in these quantities.

Corrective action Action taken to eliminate the causes of an existing

nonconformity, defect or other undesirable situation in

order to prevent recurrence.

Coverage factor Numerical factor (k) used as a multiplier of the combined

standard uncertainty in order to obtain an expanded

uncertainty. Usually k = 2 or k = 3.


Document Any set of information or instructions, including paper

documents, computer files, software, etc.

Expanded uncertainty Quantity defining an interval about the result of a

measurement that may be expected to encompass a large

fraction of the distribution of values that could reasonably

be attributed to the measurand.

IMS sample analysis Process including sample management (receipt, security,

chain of custody, dispatch, preparation and storage),

measurement, analysis, data management, messages and

reports.

IMS particulate sample

categories

(A) Network quality control (QC) samples; (B) high

priority samples; (C) intercomparison or proficiency test

samples; (D) station backup samples; and (E) other

measurements as requested by the PTS. See Section 5.7.1

for details.

IMS noble gas sample

categories

(GA) Xenon network QC samples; (GX) radioactive xenon

spikes; (GC) intercomparison or proficiency test samples;

(GD) noble gas station backup samples; and (GE) other

measurements as requested by the PTS. See Section 5.7.2

for details.

Intercomparison exercise

An activity whose purpose is to find out if methods and

results produced by these methods at participating

laboratories agree with each other. One reference sample

or several very similar samples (as in the case of real

environmental samples collected at the same place at the

same time) are distributed and analysed. The radioactivity

content of the sample is determined based on the results of

the participants. The intercomparison exercises and

proficiency tests are used to determine the performance of

a laboratory against pre-established criteria.

Management review Formal evaluation by laboratory management of the status

and adequacy of the quality system in relation to quality

policy and objectives.

Measurand Particular quantity to be measured.

National Authority As required under Article III of the CTBT, the body

designated by a State Party to be the national focal point

for liaison with the CTBTO and with other States Parties.

Noble gas samples Gases collected from the air by the noble gas monitoring

systems at radionuclide stations in the IMS network.


Nonconformity Non-fulfilment of a specified requirement.

Operational Manual Operational Manual for Radionuclide Monitoring and the

International Exchange of Radionuclide Data. Official

document that defines quality, technical and operational

requirements for IMS radionuclide stations and

radionuclide laboratories. This document,

CTBT/PTS/INF.96, is based on the Operational Manual.

Particulate samples Airborne particles or aerosols that are collected on filters

by air samplers at the radionuclide stations in the IMS

network.

Preventive action Action taken to eliminate the causes of a potential

nonconformity, defect or other undesirable situation in

order to prevent occurrence.

Process Set of interrelated resources and activities which transform

inputs into outputs (resources may include personnel,

finances, facilities, equipment, techniques and methods).

Proficiency test Reference samples (proficiency test samples) with certified

radioactivity content are distributed to participants. The

samples may also be just spectra. The certified values are

unknown to the participating laboratories at the time of the

analysis. The purpose is to test the quality of analysis

results of the laboratories against the certified values.

Quality assurance (QA) All the planned and systematic activities implemented

within the quality system, and demonstrated as needed, to

provide adequate confidence that an entity will fulfil

requirements for quality. (In the context of this document,

entity refers to a radionuclide laboratory and requirements

are those related to the specific activities carried out for

IMS sample analysis.)

Quality management All activities of the overall management function that

determine the quality policy, objectives and

responsibilities, and implement them by means such as QA

and quality improvement within the quality system.

Quality manual Document stating the quality policy and describing the

quality system of an organization. (A quality manual will

normally contain or refer to, as a minimum: (a) quality

policy; (b) the responsibilities, authorities and

interrelationships of personnel who manage, perform,

verify or review work affecting quality; (c) the quality

system procedures and instructions; and (d) a statement for

reviewing, updating and controlling the manual.)

Quality policy Overall intentions and direction of an organization with


regard to quality as formally expressed by top

management.

Quality system Laboratory structure, processes, procedures and resources

needed to implement quality management.

Radionuclide laboratory One of the 16 laboratories in Table 2-B of Annex 1 to the

Protocol to the CTBT, certified by the PTS, or further

laboratories that may be designated in accordance with the

procedure described in paragraph 11 of the Protocol.

Radionuclide Laboratory Report

(RLR)

Measurement data, supporting data and analysis results

from an IMS sample analysis at radionuclide laboratories

in a predefined format. The report is produced by the

radionuclide laboratory and distributed by the PTS.

Sample reference identification

(SRID)

Unique identifier for an IMS radionuclide sample.

Standard uncertainty Uncertainty of the result of a measurement expressed as a

standard deviation.

Surveillance assessment Ongoing evaluation of the performance of a certified

laboratory to ensure that it continues to meet the

certification criteria.

Uncertainty (of measurement) Parameter associated with the result of a measurement that

characterizes the dispersion of the values that could

reasonably be attributed to the measurand.


2. INTRODUCTION

2.1. Radionuclide Laboratory Network

According to the Comprehensive Nuclear-Test-Ban Treaty (CTBT), as found in Part I.C,

paragraph 11, of the Protocol, the International Monitoring System (IMS) network of

radionuclide monitoring stations is to be supported by laboratories through the analysis of

samples from these stations. These radionuclide laboratories will be certified by the Technical

Secretariat in accordance with the relevant IMS operational manual, which, in its current draft

form, is entitled Operational Manual for Radionuclide Monitoring and the International

Exchange of Radionuclide Data (henceforth referred to as Operational Manual).

In addition to the analysis of the IMS particulate samples, some radionuclide laboratories may

also offer services for the analysis of noble gas samples from radionuclide monitoring

stations. The sections in this document apply to the analysis by radionuclide laboratories of

both particulate and noble gas samples unless explicitly indicated that the analysis was for

particulate samples only or noble gas samples only.

2.2. Radionuclide Laboratory Quality Systems and Certification

The purpose of certification by the PTS is to provide States Signatories and the Preparatory

Commission with confidence that the services provided by radionuclide laboratories meet the

standards required for the CTBT verification regime.

To serve this purpose, the radionuclide laboratory shall have a quality system, as well as

documentation and procedures for the process of IMS sample analysis.

For certification, the radionuclide laboratory shall provide documentation to demonstrate that

certification requirements are satisfied. All documentation that must be reviewed to assess

compliance with certification requirements shall be available in English.

This document includes certification requirements and a description of the certification

process and procedures. Requirements are divided into three sections: management

requirements, technical requirements and requirements for gamma spectrometric analysis of

particulate samples. Additionally, for the laboratories with noble gas analysis capabilities,

certain requirements have to be met for the analysis of noble gas samples to take place. The

sections on certification process and procedures include a description of the process in the

form of flow charts, and the Provisional Technical Secretariat (PTS) procedures to be

followed during the process. When the process is successfully completed, a confirmation

letter will be sent to the radionuclide laboratory by the PTS. Certification checklists are

included in Appendix V.

This document is subject to further revision to take into account the input from Working

Group B, new developments and experience gained in planning and implementation of

technical solutions and will be re-issued with the next consecutive revision number.

Terminology associated with quality management in this document has been adopted from

ISO/IEC 17025:2005, General Requirements for the Competence of Testing and Calibration

Laboratories, and from CTBT/PTS/INF.103/Rev.1, Quality Manual. Terminology associated

with uncertainty of a measurement result is largely adopted from the ISO Guide to the


Expression of Uncertainty in Measurement (ISO/IEC Guide 98-3:2008). The term PTS will

be used prior to entry into force of the Treaty and TS (Technical Secretariat) after that time.

2.3. Objectives of Radionuclide Laboratory Analyses

As defined under the Treaty, the main role of the radionuclide laboratories is to perform

analyses on samples from IMS radionuclide stations. The purposes of the analyses are given

in the Operational Manual:

(a) To corroborate the results of the routine analysis of a sample from an International

Monitoring System station, in particular to confirm the presence of fission

products and/or activation products;

(b) To provide more accurate and precise measurements;

(c) To clarify the presence or absence of fission products and/or activation products

in the case of a suspect or irregular analytical result from a particular station.

The Operational Manual also outlines the general quality criteria for IMS sample analysis at

the radionuclide laboratories. To achieve the stated objectives of analysis at the radionuclide

laboratories, the radionuclide laboratory shall be capable of reliably identifying the

radionuclides in the sample and determining their activities, and of providing an expert

assessment of the properties of the sample.

2.4. Data Quality Objectives

The general requirements in this document relating to data quality are intended to be

consistent with those of ISO/IEC 17025:2005. The objective of the certification process is to

assess that the laboratory is both technically competent to carry out IMS sample analysis and

has a quality system that is appropriate for CTBT functions. However, the process does not

constitute an assessment of direct compliance with the quality system requirements in

ISO/IEC 17025:2005.

In terms of data quality, the objective of the certification requirements is to ensure that the

IMS sample analyses are carried out and reported in a timely manner, and in accordance with

certified procedures and IMS formats. The certification process also must be able to provide

an assurance that the laboratory’s results are accurate and valid. This will be done through

proficiency test exercises involving samples with certified activity values against which the

laboratory’s results can be evaluated. Traceability of equipment calibration to national or

international standards through an unbroken chain of measurements is also assured during the

certification process.

3. OPERATIONAL RESPONSIBILITIES

The responsibilities described in this section are related to certified operations. The

certification process will assess the abilities of the radionuclide laboratory to meet these

responsibilities.

The radionuclide laboratories will be contracted by the PTS to perform analyses of IMS

samples on a fee-for-service basis. Within the terms of this contract, the radionuclide


laboratory shall be responsible for performing the requested analysis of IMS samples and for

providing an independent report on the analysis. As an essential component of the report, the

radionuclide laboratory shall be required by the PTS to provide an expert assessment of the

analytical results to meet the analysis objectives stated in Section 2.3.

The radionuclide laboratory shall demonstrate during the certification process its capability to

maintain a state of preparedness for receiving a high priority sample from an IMS

radionuclide station for analysis. This capability includes provision for personnel to be

reachable during weekends and holidays to avoid delays in the case of a sample requiring

urgent analysis. Operationally, this service will not be required until entry into force of the

CTBT or upon notification by the PTS in accordance with the decisions of the Preparatory

Commission.

The radionuclide laboratory shall facilitate the delivery and receipt of IMS samples at its

premises, including, if necessary, obtaining the relevant clearances. The radionuclide

laboratory shall also advise the PTS in advance of relevant local factors relating to sample

transportation.

The radionuclide laboratory shall participate regularly in intercomparison and proficiency test

exercises organized by the PTS.

The radionuclide laboratory may also be requested to carry out routine sample measurement

during a period of inoperability at an IMS radionuclide station. The provision of this type of

service shall only be required after the feasibility and the practicalities have been discussed

and agreed upon by both the PTS and the radionuclide laboratory as part of the contracting

process.

The radionuclide laboratory shall comply with certified procedures and formats for IMS

sample analysis, which include:

(a) Acknowledgement of messages

(b) Acknowledgement of sample receipt

(c) Sample chain of custody

(d) Sample and data security

(e) Sample preparation methods

(f) Measurement and analysis

(g) Data and report formats

(h) Reporting schedule

(i) Control of sample records.

The PTS will be responsible for notifying the radionuclide laboratory of sample dispatch for

laboratory analysis. The PTS shall also provide the radionuclide laboratory with relevant

transport information, estimated time of arrival and sample information, necessary for the

analysis. For particulate samples, the PTS will provide samples of certified IMS sample

geometries and materials, to facilitate calibrations of the measurement systems at the

radionuclide laboratories. For noble gas samples, the PTS will also provide all necessary


details on the noble gas archived samples including archive container properties and their

expected content.

4. MANAGEMENT REQUIREMENTS

4.1. Organization

The radionuclide laboratory shall define its organization and management structure, its place

in any parent organization and relevant organizational charts. A quality manager (however

named) having the responsibility and authority to ensure that the quality system is

implemented and followed, shall be appointed.

Definition of the organization (and its position and authorities relative to other parts of an

overarching parent organization, if that is the case) is required in order to identify who is

legally responsible for fulfilling the contract with the CTBTO. That definition will identify

the top management who take ultimate responsibility for providing and maintaining the

resources necessary to fulfil the contract and to maintain the viability of the operation and its

quality system. The description of the organization will identify inter-relationships within it

(and with its parent organization), key posts, post-holders and specify the duties and

authorities that key personnel and deputies have. An organizational chart is often beneficial

for this purpose. Policies and procedures that are in place to maintain the integrity,

independence and confidentiality of the operation should be well defined.

4.2. Quality System

The radionuclide laboratory shall establish and maintain a quality system. ISO/IEC

17025:2005 will be used as a guideline in evaluating the adequacy of the quality system.

Existing relevant accreditation may be used to demonstrate compliance with CTBTO

certification criteria.

The elements of the quality system shall be documented, made available to, understood and

implemented by the personnel.

4.3. Quality Manual

The quality manual, however named, shall state the organization’s quality policy and describe

the quality system. The manual shall incorporate a quality statement specifying the objectives

and commitments of the top management, to include:

(a) Managerial commitment to good laboratory practices and analysis quality;

(b) Management’s statement of the standard of service;

(c) Objectives and description of the quality system;

(d) Managerial commitment to ensure that all staff of the organization concerned with

activities related to the functions of the radionuclide laboratory comply with the

quality system.

The quality manual shall also include or make reference to:


(a) The responsibilities, authorities and interrelationships of personnel who manage,

perform, verify or review work affecting quality;

(b) Quality system procedures and instructions;

(c) A statement concerning control and maintenance of documentation, including the

quality manual.

The quality manual includes or makes reference to the technical documents described in

Section 4.4.

4.4. Technical Documentation

The radionuclide laboratory shall document, in detail, the whole process of IMS sample

analysis and all supporting activities carried out by the laboratory. The activities and

resources to be documented include:

(a) Preparedness to receive and analyse a high priority sample;

(b) Documentation on personnel authorized to have access to IMS samples and data;

(c) Environmental conditions that may affect the analysis results;

(d) Analysis methods and their validation;

(e) Procedures for calibration and maintenance of equipment;

(f) Records on measurement system(s) and other major equipment as well as

reference standards and materials used;

(g) Procedures for sample management (receipt and dispatch, security, tracking);

(h) QA of analytical results, through, for example, PTS organized intercomparison

exercises and proficiency tests, other intercomparison and proficiency testing

programmes, and use of reference standards and materials;

(i) Reporting results (management of data, formats and time requirements);

(j) Message traffic related to IMS sample analysis;

(k) Technique specific requirements for methods, equipment, analysis and reports.

4.5. Control of Records

The radionuclide laboratory shall have procedures in place for managing quality and technical

records. A record system shall be maintained that documents all laboratory activities carried

out within the process of IMS sample analysis. A laboratory information management system

should be implemented, in electronic or hard copy form, for the establishment and

maintenance of technical records for IMS sample analysis for a period to be defined by the

laboratory, but for not less than five years.

The radionuclide laboratory shall retain a record of the receipt and dispatch of samples, chain

of custody, sample handling, all original observations, measurements, calculations and

derived data, calibration records and analysis reports.

The record keeping system shall enable the historical reconstruction of activities that

produced the sample analytical data, as well as identification of factors affecting the analytical


uncertainties. Staff responsible for sample data entries shall be identified and a record of any

changes in the data shall be kept.

4.6. Other Management Requirements

In consistency with quality system requirements specified in ISO/IEC 17025:2005, the

radionuclide laboratory shall establish and maintain procedures and practices for:

(a) Document control;

(b) Review of terms of reference and contracts;

(c) Not subcontracting any part of the IMS sample analysis without the prior written

approval and clearance of the PTS, except for subcontracts for the provision of

utilities and/or non-technical maintenance work;

(d) Purchasing of supplies, ensuring that supplies that are purchased from outside the

radionuclide laboratory are subjected to the same degree of quality assessment

and control as any other product that is generated in-house;

(e) Maintenance of a good client service with the PTS;

(f) Resolution of complaints from the PTS;

(g) Control of nonconformity in work related to the provision of IMS sample

analyses;

(h) Measures that will be taken in order to effect continuous improvement of the

quality system;

(i) Implementation of corrective and preventive actions to ensure compliance with

the quality system and technical procedures;

(j) Internal auditing of activities related to IMS analyses;

(k) Periodic management reviews of the laboratory’s quality system and procedures

for IMS sample analyses.

5. TECHNICAL REQUIREMENTS

5.1. Preparedness

The radionuclide laboratory shall document procedures relating to their preparedness for the

receipt and expeditious analysis of samples from an IMS radionuclide station. Operational

preparedness shall be implemented only after the CTBT enters into force or upon notification

by the PTS in accordance with decisions by the Commission. Once preparedness is

implemented, laboratory personnel shall be reachable during weekends and holidays to avoid

excessive delays in the analysis of any samples designated by the PTS. Arrangements may be

based on the assumption that, outside of normal office hours, there will be a minimum of

12 hours between laboratory sample dispatch notification from the PTS and the anticipated

receipt of the sample by the radionuclide laboratory.


5.2. Personnel

The radionuclide laboratory shall authorize specific personnel to carry out the activities in

IMS sample analysis and only these personnel shall have access to IMS samples and IMS

sample data.

A record of personnel authorized for CTBT operations shall be maintained as part of the

laboratory specific operational manual. The PTS shall be notified of changes in authorized

personnel.

The management of the radionuclide laboratory shall ensure that the authorized personnel are

competent to carry out the activities for IMS sample analysis and maintain current job

descriptions. In case there are changes in authorized personnel who are directly involved in

sample analysis, the management shall ensure that the corresponding replacement(s) have the

required competence and training for IMS sample analysis. The PTS shall be notified of

changes in authorized personnel. Record of the qualifications, skills, training and experience

of the replacement will be sent to the PTS together with the notification. Authorized staff,

including those undergoing training, shall be appropriately supervised.

Training should include radiological health and safety measures such as, for example, the

screening of samples for activity level and contamination of the packaging, wearing of gloves

when handling the sample and keeping the analyzed samples in such a manner as to prevent

cross-contamination. The risk of potential exposure of personnel should be minimized using

the ALARA principle as guidance, i.e. exposures should be kept as low as reasonably

achievable, taking into account social and economic considerations.

Records shall be maintained of the qualifications, skills, training and experience of all

authorized technical staff.

5.3. Environmental Conditions

The radionuclide laboratory shall maintain the facilities in which IMS samples are processed

and analysed in such a way as to facilitate proper performance of analyses. These facilities

include laboratory accommodation, test areas, power sources, lighting, heating and

ventilation.

The quality of analysis results shall not be adversely affected by the environmental conditions

of the facilities where IMS samples are processed and analysed. The radionuclide laboratory

shall document and control any particular environmental factors pertaining to the laboratory’s

facilities that may significantly affect the performance of the measurement systems or other

aspects of data quality

The radionuclide laboratory shall monitor and control environmental conditions in the room

housing the measurement system that could affect the system performance, including

temperature and relative humidity.

All necessary precautions shall be taken to prevent radioactive cross-contamination between

IMS samples and other radioactive materials in the radionuclide laboratory. This includes, but

is not limited to, screening samples for external contamination upon receipt, separating work

areas for handling low and high activity samples, and routinely performing adequate

decontamination procedures and checks.


The radionuclide laboratory shall ensure that any non-IMS-related activities performed at the

same facilities do not compromise the integrity of IMS samples, influence IMS sample

management procedures or affect the quality of IMS sample analyses.

5.4. Methods

5.4.1. Selection of Methods

The radionuclide laboratory shall use methods and procedures that are appropriate for the

process of IMS sample analysis and that have been certified by the PTS. Where possible, the

laboratory should use methods published as international or national standards, in relevant

scientific journals or texts, or specified by the equipment manufacturer. Laboratory developed

methods, including software, shall be documented and validated.

The radionuclide laboratory shall not deviate from the use of certified methods without PTS

approval and any deviations shall be documented.

Any changes in the certified methods that could compromise the fulfilment of certification

requirements shall only be implemented with the approval of the PTS and such changes shall

be documented and technically justifiable.

Prior to adoption of any new method for IMS sample analysis, procedures should be

developed and contain the following information, in harmony with the requirements of

ISO/IEC 17025:2005:

(a) Appropriate identification of the method/procedure;

(b) Scope;

(c) Description of the type of item to be tested or calibrated;

(d) Parameters or quantities and ranges to be determined;

(e) Apparatus and equipment, including technical performance requirements;

(f) Reference standards and reference materials required;

(g) Environmental conditions required and any stabilization period needed;

(h) Description of the procedure, including:

(i) Affixing of identification marks, and handling, transporting, storing and

preparation of the samples;

(ii) Checks to be made before the work is started;

(iii) Checks that the equipment is working properly and, where required, calibration

and adjustment of the equipment before each use;

(iv) Method of recording the observations and results;

(v) Any safety measures to be observed;

(i) Criteria and/or requirements for approval/rejection;

(j) Data to be recorded and method of analysis and presentation;

(k) The uncertainty or the procedure for estimating the uncertainty.


5.4.2. Validation of Methods

The radionuclide laboratory shall ensure that the analytical methods used for IMS sample

analysis are valid for that purpose. Validation comprises assessment that the performance of

the method and the quality of the results are fit for the intended use.

The validation should include the following:

(a) Test method capability, including detection limits and performance range;

(b) Calibration with reference standards and materials;

(c) Factors affecting the result;

(d) Uncertainty in the result;

(e) Performance of algorithms to process raw data to final results;

(f) Appropriate environmental conditions for measurement systems.

The radionuclide laboratory shall participate in intercomparison exercises to test the validity

of its methods. In addition to other intercomparison programmes in which the radionuclide

laboratory participates, the quality of analytical results shall be demonstrated through

participation in intercomparison and proficiency test exercises organized by the PTS.

Satisfactory performance in these exercises is an essential requirement for the certification

and ongoing performance assessment of the radionuclide laboratory.

5.4.3. Uncertainty of Measurement

The radionuclide laboratory shall apply a documented procedure to estimate the uncertainty of

a measurement result. All factors affecting the uncertainty in the IMS sample analysis process

shall be identified and quantified to the extent possible. If a metrologically and statistically

valid calculation is not possible, the laboratory shall give a reasonable estimate for the

uncertainty and identify its components.

ISO/IEC Guide 98-3:2008 “Uncertainty of Measurement Part 3: Guide to the Expression of

Uncertainty in Measurement”, will be used as a guideline for determining and reporting the

combined standard uncertainty of a measurement result. Laboratories shall report their

uncertainty of measurement as combined standard uncertainty (k = 1), unless otherwise

specified by the PTS. In case an expanded uncertainty is reported, the coverage factor (e.g.

k = 2 or k = 3) that was used to obtain the expanded uncertainty and the corresponding

approximate level of confidence (e.g. 95% or 99%) shall be indicated.

5.5. Equipment

5.5.1. General

Only authorized personnel shall operate the equipment during IMS sample analysis. Current

operating instructions for all equipment used for all stages of the analysis shall be available.

Each item of equipment used for IMS sample analysis and that is significant to the result of

the analysis shall be uniquely identified. Records shall be maintained for these items of

equipment. These records shall include the following:

(a) Name of the item of equipment;


(b) Name of manufacturer;

(c) Type, identification and serial number or other unique identification;

(d) Date received and date placed in service (if available);

(e) Current location, where appropriate;

(f) Condition when received (e.g. new, used, reconditioned);

(g) Copy of manufacturer’s instructions, where available, or reference to its location;

(h) Dates and results of calibrations and/or verifications and date of the next

calibration and/or verification;

(i) Details of maintenance carried out to date and planned for the future;

(j) History of any damage, malfunctions, modification or repair.

All equipment shall be properly inspected and maintained. Maintenance procedures shall be

documented. The radionuclide laboratory shall have a process to ensure that all equipment is

calibrated, the calibration status is known and the equipment is functioning properly whenever

used.

5.5.2. Technique Specific Requirements for Equipment

Specific requirements for the measurement system for the analysis of IMS particulate samples

by high resolution gamma ray spectrometry are presented in Section 6. Specific requirements

for the analysis of IMS noble gas samples are presented in Section 7.

5.5.3. Global Communications Infrastructure

The radionuclide laboratory shall communicate with the PTS via the Global Communications

Infrastructure (GCI), the requirements for which are found in CTBT/PC/V/WGB/PTS/1,

Global Communications Infrastructure: Technical Specifications.

5.6. Measurement Traceability

5.6.1. Calibration

The radionuclide laboratory shall have an established programme for the calibration of all

items of equipment that have a significant effect on the accuracy or validity of the results of

IMS sample analyses. The programme shall include procedures and schedules for the initial

calibrations and regular verification of the calibration status of the equipment. It shall be

designed and conducted to ensure that measurements made by the radionuclide laboratory are

traceable to national or international standards.

The following shall be documented for calibration of equipment:

(a) Details of the procedures for the calibration, including calculation, integration and

acceptance criteria with associated statistics (these shall be included or referenced

in the test method);

(b) Sufficient raw data records to permit reconstruction of the calibration;

(c) Verification of initial instrument calibrations with a standard obtained from a

second source and traceable to a national (or international) standard;


(d) The uncertainty for calibrations.

Calibration certificates shall indicate the traceability of the calibration measurements to

national or international standards and shall provide the measurement results and associated

uncertainty. The radionuclide laboratory shall maintain records of all such certificates.

Calibration of the xenon volume measurement system has to be performed using certified gas

mixtures of sufficiently high purity and composition precision to meet the uncertainty

requirement specified in Table 2.

5.6.2. Reference Standards and Materials

The radionuclide laboratory shall have a process for maintaining confidence in the calibration

status of its reference standards and materials. Records shall be kept for reference standards

and materials as well as for their verifications. The radionuclide laboratory shall protect the

integrity of its reference standards and materials.

5.7. Different IMS Sample Categories

5.7.1. Particulate Sample Categories

There are, potentially, five categories of IMS samples that may require analysis at a

radionuclide laboratory. These categories are:

A. Network QC samples routine samples regularly sent from IMS radionuclide

stations to assess the performance of the network.

B. High priority samples samples categorized as Level 5 samples2 within the

International Data Centre (IDC) event categorization and screening process or

routine samples from stations exercised as high priority samples to maintain

preparedness and necessary procedures. They may also be samples on which

States Parties have requested additional analysis regardless of category.

C. Intercomparison or proficiency test samples distributed to radionuclide

laboratories as part of intercomparison exercises or proficiency tests.

D. Station backup samples during a period when the measurement system at an

IMS radionuclide station is inoperable, the routine filter samples may be sent to a

radionuclide laboratory for measurement if it is practical to do so. The laboratory

would only be required to transmit the unprocessed spectral data to the IDC,

where the data processing would take place.

E. Other samples for measurement agreed on between the radionuclide laboratory

and the PTS. This category may include blank filter materials, other samples

arising from station certification, and other samples for analysis required by the

PTS.

2 The definition for Level 5 samples from the Draft Working Text of the Operational Manual for the

International Data Centre (September 2000 Update), CTBT/WGB/TL-2/55, states: “Level 5 (Multiple

Anthropogenic). The spectrum contains multiple anomalous measurements of anthropogenic nuclides, which

are on the standard list of relevant nuclide[s].” The list refers to the Recommended Standard List of Relevant

Radionuclides for IDC Event Screening (CTBT/WGB/TL-2/40 and Corr.1).


Each category has different requirements for analysis and reporting times, the details of which

are presented in the technique specific sections (currently Sections 6 and 7). The general

requirements for sample and data security apply to samples from IMS stations only

(categories A, B, D and some category E samples). IMS samples that do not originate from

IMS stations and are not confidential may be treated according to the normal procedures at the

laboratory.

5.7.2. Noble Gas Sample Categories

There are five categories of IMS noble gas samples that may require analysis at a radionuclide

laboratory. These categories are:

GA. Xenon network QC samples routine samples regularly sent from IMS

radionuclide xenon stations to assess the performance of the network. The samples may

or may not contain radioxenons, depending on the radioxenon background patterns at

the site of the station.

GX. Radioactive xenon spikes a xenon spike with known isotopic composition

(including approximate activities) is introduced into the station system and measured.

The resulting archived sample is sent for analysis to a certified laboratory that will

analyse and report at a minimum: xenon activity concentrations, isotopic ratios, xenon

volume, archive bottle pressure and optionally, also gas composition other than xenon.

GC. Intercomparison or proficiency test samples distributed to radionuclide

laboratories as part of intercomparison exercises or proficiency tests.

GD. Station backup samples during a period when the measurement system at an

IMS radionuclide station is inoperable, the xenon gas sample may be sent to a

radionuclide laboratory for measurement if it is practical to do so. The laboratory would

be required to transmit the unprocessed spectral data to the IDC where the data

processing would take place.

GE. Other samples for measurement agreed on between the radionuclide laboratory

and the PTS. This category may include, for example, samples arising from station

certification.

5.8. Sample Management

The radionuclide laboratory shall have procedures for handling samples from receipt to

dispatch. Additionally, it shall maintain a record of all procedures to which a sample is

subjected while in the possession of the radionuclide laboratory (see Section 4.5, Control of

Records).

Each sample shall be tracked by referencing the sample reference identification (SRID) that is

assigned at the radionuclide station. The format of the SRID is found in IDC 3.4.1, Formats

and Protocols for Messages.

5.8.1. Receipt and Dispatch of Samples

The radionuclide laboratory shall have procedures for receiving and dispatching IMS samples,

and for notifying the PTS of sample receipt and dispatch. There shall be procedures for all

preparations necessary for sample receipt.


Upon receipt, the radionuclide laboratory shall record the condition of the sample and submit

a report to the PTS (a SAMACK message). A permanent chronological record (such as a

logbook or an electronic database) of IMS sample receipt and dispatch shall be kept,

containing the following information: date and time of receipt/dispatch, SRID, the

radionuclide laboratory’s own sample ID if applicable and the signature of the person

receiving/dispatching. When returning a particulate sample to the PTS or an empty archive

container to a noble gas station from where it originated, the package shall be shipped via

courier and should be registered with delivery receipt requested. The shipment of empty

archive containers should be declared appropriately in order to avoid delays owing to customs

formalities (e.g. return of empty sample containers). Receipts should be retained as part of the

chain of custody. Information about the record should be retrievable by the SRID.

The receipt procedure for the noble gas samples shall be designed to avoid unnecessary delay

in sample delivery within the premises of the parent organization of the laboratory. It shall

ensure that xenon samples will be delivered to the radionuclide laboratory on the day of

arrival (within 24 hours) within the restrictions of normal working times at the laboratory.

The time requirement for starting the measurement depends on the sample type: for routine

samples that contain radioxenons and for xenon spike samples, the measurement shall be

started within six working hours of sample receipt (during normal working times of the

laboratory). For routine samples that do not contain radioxenons, there is no specific time

requirement for the start of measurement. The PTS may request the laboratory to start as soon

as possible, for example in cases where the station appears not to meet its operational

specifications. The measurement time shall be optimized with regard to nuclide identification

and quantification.

5.8.2. Security of Samples

Procedures relating to laboratory and sample security shall be in place. Access to areas in

which IMS samples will be processed, measured and stored shall be controlled to prevent

inadvertent or malicious manipulation. The IMS samples shall be accessible only to

authorized laboratory personnel responsible for IMS sample handling. Bar code readers could

be used at appropriate locations to record the details of the chain of custody.

5.8.3. Laboratory Sample Tracking

Sample chain of custody shall be maintained and recorded for the entire period that an IMS

sample is under the jurisdiction of the radionuclide laboratory. Chain of custody records shall

establish a continuous record of the physical possession and storage of samples. These records

shall identify and include signatures of individuals who physically handled the samples.

5.8.4. Handling of Samples

Procedures for handling and storage of IMS samples shall provide the assurance that sample

deterioration by contamination, loss or damage is avoided. Additionally, procedures for

handling and storage of any radioactive materials within the radionuclide laboratory shall

provide the same assurance that cross-contamination of IMS samples are avoided.


5.9. Quality Assurance of Analysis Results and Data Verification

5.9.1. Quality Assurance of Analysis Results

QA/QC procedures for validity of results shall be documented and implemented at the

radionuclide laboratory. QA of results provided to the PTS should include:

(a) Internal QC procedures, including background measurements and calibration

checks using statistical techniques;

(b) Successful participation in proficiency tests and intercomparison exercises;

(c) Use of certified reference materials;

(d) Replicate tests and remeasurement of retained samples, if possible.

5.9.2. Data Verification

The radionuclide laboratory shall have a documented procedure to ensure that the reported

data are free from transcription and calculation errors. It shall establish a procedure to ensure

that the QC measures are implemented before any data are reported.

5.10. Management of Analysis Data

During certification the radionuclide laboratory shall demonstrate that its processes will fulfil

the following requirements:

(a) All data for IMS samples generated at the radionuclide laboratory, including

relevant calibration information, background measurements and information on

environmental conditions, shall be safely stored and archived until further

direction is given by the PTS;

(b) All the intermediate results shall be stored;

(c) There shall be a log, either automated or manual, for recording the steps taken by

the analyst during the analysis;

(d) Only authorized personnel listed in the radionuclide laboratory’s CTBT specific

documentation shall have access to the data;

(e) Documented procedures shall be implemented to ensure data confidentiality.

5.11. Reporting

5.11.1. Contents of the Report and Reporting Time

The radionuclide laboratory shall have procedures to meet the specific requirements of the

PTS for contents of reports and reporting time, as defined in the technique specific sections

(Section 6 and 7).

5.11.2. Data and Report Format

Analysis data and reports transmitted to the IDC shall be in the current IMS format and in

accordance with IDC 3.4.1, Formats and Protocols for Messages (current version).


5.11.3. Data Authentication

Internal procedures must ensure secure data transfer (either physical or electronic) from the

acquisition and analysis system to the point where the data are sent through the GCI. The

CTBT specific data authentication programme shall be implemented in accordance with the

requirements of the PTS. The basic requirement is to digitally sign and authenticate messages

via a hardware unit dedicated to the generation and verification of digital signatures. The unit

must support a digital signature algorithm (DSA) with a 1024 bit public key. Transmission of

messages must be compatible with the CTBTO Public Key Infrastructure (PKI).

5.12. Messages

5.12.1. Communication Protocols

Procedures for communications with the PTS via the GCI and Internet shall be documented

and in compliance with the message schedules specified in Appendix I.

5.12.2. Communication Software

Mail server software shall be installed for communication with the PTS, allowing data to be

transmitted and received as email.

5.12.3. Laboratory Message Format and Contents

The radionuclide laboratory shall be able to handle message types related to IMS sample

analysis. These message types are specified in IDC 3.4.1, Formats and Protocols for

Messages.

6. REQUIREMENTS FOR PARTICULATE SAMPLE ANALYSIS BY GAMMA

RAY SPECTROMETRY

A detailed description of the measurement equipment to be used for analysis of IMS samples

by gamma ray spectrometry shall be included in CTBT specific documentation of the

laboratory. Table 1 summarizes the technical specifications for the gamma ray spectrometry

system.

6.1. Sample Preparation

If any IMS samples require further preparation at the radionuclide laboratory prior to analysis

by gamma ray spectrometry, only a non-destructive method shall be used. Any gamma ray

spectrometry methods requiring sample pre-concentration, such as wet or dry ashing, or

radionuclide separation and radiochemical analysis, shall only be used with the approval of

the PTS. Such methods shall be documented and subject to certification. Risk of loss of

volatile elements during sample preparation and handling should be minimized.


Table 1. Summary of Minimum Technical Specifications for Gamma Analysis

Equipment

Property Requirement

Detector type High resolution HPGe

Detector relative efficiency 40 %

Calibration measurement range 46.5-1836 keV

Calibration range (extrapolated) 30-2700 keV

Channels in spectrum 8192

MDA for 140

Ba

With decay correction to start of spectral

acquisition, with acquisition time no

longer than 7 days

24 mBq

For a cylindrical sample geometry with

a diameter of 70 ± 0.5 mm, a height

of 6 ± 0.5 mm and a density of

0.7 ± 0.1 g/cm3

Energy calibration – maximum deviations

between actual and computed energies

(maximum order of fitting polynomial = 3)

± 0.6 keV

FWHM at 1332.5 keV 2.3 keV

FWHM at 122.1 keV 1.3 keV

FWTM/FWHM at 1332.5 keV 2.0

6.2. Spectral Acquisition and Analysis

The spectral acquisition software shall be capable of collecting and storing a full pulse height

gamma spectrum, in addition to all other key parameters associated with acquisition. At least

8192 channels shall be used.

The maximum spectral acquisition time is seven days. Intermediate spectra shall be recorded

at least every 24 hours for all IMS samples when possible. For station backup samples

measured at a radionuclide laboratory during a period of inoperability at a radionuclide

station, the measurement time shall be 20 hours (CTBT/PC/II/1/Add.2, p. 48), with an

intermediate spectrum recorded after the first four hours of acquisition.

Software and analysis tools used to collect, format, analyse and store sample spectra shall be

documented and validated. Relevant actions taken by the analyst during analysis shall be

recorded.

6.3. Detector Efficiency

The relative efficiency of any detector used for IMS sample analysis shall be greater than or

equal to 40%. In exceptional circumstances, for example if high radionuclide activity would

generate a problem involving a large dead time correction, a detector of lower efficiency may

be used if authorized by the PTS. However, the detector shall be certified prior to its use for

the IMS analysis and meet the other certification requirements.

6.4. Detector Calibration

Any detector that is used for IMS sample analysis shall be calibrated over the full range of

gamma energies of the key fission and activation products produced in a nuclear explosion as

presented in the IDC Operational Manual. To cover all relevant gamma lines of these


radionuclides, as well as the typical natural radionuclides in network QC samples, the

efficiency calibration range shall cover the energy range of 30 to 2700 keV3.

For empirical efficiency calibration methods, the radioactive source shall have the same

geometry and approximate density as the filter samples, and contain radionuclides that emit

gamma rays covering the energy range of 46.5 to 1836 keV. The radionuclide sources used

for detector efficiency calibration shall be traceable to standards provided by a recognized

national standards organization. Source certificates shall be appropriately stored and available

for review. The radionuclide laboratory shall ensure that true coincidence summing does not

distort the calibration.

If semi-empirical and mathematical methods are used for detector calibration, the relevant

software shall be appropriately validated. It shall be demonstrated and documented that the

calibration results agree with experimental data.

The radionuclide laboratory shall maintain calibrations for detector efficiencies for all

geometries used by the laboratory in the analysis of IMS samples. The PTS will provide

particulars of filter materials and geometries currently used at IMS radionuclide stations,

including examples of materials. If the IMS sample geometry is modified at the radionuclide

laboratory in order to provide optimal detection efficiency, detector calibration shall be

maintained for the modified geometry.

The analysis of calibration spectra shall be made using the same procedures used for sample

spectral analysis, namely peak search, peak area determination and error estimation.

Appropriate mathematical functions should be fitted to the calibration data, for example a low

degree polynomial for the energy calibration, a logarithm polynomial for efficiency

calibration and a square root polynomial for peak shape calibration.

6.5. Minimum Detectable Activity

Within the IMS technical specifications, the requirement for the baseline sensitivity of

radionuclide stations for particulate monitoring is expressed as a concentration range of 10 to

30 Bq m-3

for 140

Ba. In order to meet the objectives stated in Section 2.3, a greater analytical

sensitivity should be achievable at radionuclide laboratories. This requirement is expressed as

a minimum detectable activity (MDA) in lieu of the minimum detectable concentration

(MDC) given for radionuclide stations.

The measurement system at the radionuclide laboratory shall be capable of achieving an

MDA of 24 mBq for 140

Ba. For purposes of certification, this MDA must be achievable for

compressed cylindrical geometries of 70 ± 0.5 mm in diameter, 6 ± 0.5 mm in height and

0.7 ± 0.1 g/cm3 in density, and with an acquisition time of not more than 7 days.

The MDA of the measurement system shall be determined by analysis of a blank filter. The

method for determining the MDA is described in Appendix II.

3 The detector shall be reliably calibrated for the range of 30 to 2700 keV. Empirical calibration measurements

should range from 46.5 to 1836 keV. The validity of the extrapolation, especially at the low end, must be

verified.


6.6. Energy Resolution and Peak Shape

The energy resolution (FWHM for a photopeak with a certain energy) of the measurement

system is a key parameter for accurately and unambiguously identifying peaks with energies

close to one another. In order to improve upon the performance required of the stations, the

laboratories should achieve FWHM values of 2.3 keV at 1332.5 keV and 1.3 keV at

122.1 keV.

The environmental conditions in the room housing the detector and associated electronics

shall ensure that the stability of the detector resolution is not affected. In particular, the room

temperature shall be maintained within the operational temperature range of the measurement

equipment. Any variation in ambient temperature during a sample measurement should not

exceed 2C. If necessary a climate control system shall be installed in the room housing the

detector system.

To facilitate accurate resolving of multiple peaks, peak shape shall be optimized. The ratio of

FWTM to FWHM shall be 2.0 at 1332.5 keV.

6.7. Detector Background and Blank Measurements

To achieve the required data quality and MDA, the radionuclide laboratory shall implement

appropriate measures to control the detector background. A detector background measurement

shall be performed regularly, but in any case not less than annually as part of analytical

quality assurance to ensure there is no contamination. Blank measurements for the different

geometries shall also be performed regularly and the spectra provided to the PTS.

.

The radionuclide laboratory shall assess the effect of indoor radon concentration on its

analytical results and have in place control measures to prevent the indoor concentrations of

natural radionuclides from compromising the quality of results.

Radioactive sources shall be stored in such a way that there is no chance of gamma ray

interference during a sample measurement, which might lead to a false interpretation of the

spectral data.

6.8. Sample Counting Geometry

For each type of certified sample produced at IMS radionuclide stations, the sample to

detector geometry shall be well defined and reproducible. A non-compressed non-cylindrical

IMS sample must be brought to an optimal counting geometry by non-destructive methods at

the radionuclide laboratory.

6.9. Uncertainty of Analytical Results

A documented procedure shall be applied to estimate uncertainty of analytical results. All

factors affecting the uncertainty in the IMS sample analysis process shall be identified and

quantified. A combined standard uncertainty shall be reported for the radioactivity of each

radionuclide and shall include at a minimum the individual contributions of the sources of

uncertainty detailed in Appendix III.

Any uncertainties in the sample preparation, for example, weighing or sample splitting, are

also to be assessed. Uncertainties from sampling for particulate samples, e.g. in the volume


sampled, that contribute to the uncertainty of activity concentration will be provided by the

PTS.

6.10. Reporting

6.10.1. Reporting Schedules

The radionuclide laboratory shall have procedures to meet the following requirements for

reporting time, according to different types of IMS samples, as defined in the sections below.

6.10.1.1. Network Quality Control Samples (A)

For type A samples, the radionuclide laboratory shall submit the final report no later than

15 days after the receipt of the sample.

6.10.1.2. High Priority Samples (B)4

For type B samples, the radionuclide laboratory shall submit a preliminary report within four

hours of the receipt of the sample, including the results from the first one-hour spectrum; and

thereafter submit additional preliminary reports daily with intervals of 24 hours or less. As the

appropriate intervals for storing data and reporting results are likely to depend on the

concentrations and half-lives of the radionuclides in the sample, the radionuclide laboratory

shall use its judgment as to the most suitable intervals.

For type B samples, the radionuclide laboratory shall submit a final report to the PTS no later

than eight days after receipt of the sample or, alternatively, within 24 hours of the completion

of the measurement if the total acquisition time is less than seven days. This latter situation

could arise either as a result of a specific PTS request, or because the laboratory has

determined that an optimal measurement has been achieved.

6.10.1.3. Intercomparison or Proficiency Test Samples (C) or Other Measurements (E)

For sample type C the reporting time will be specified separately prior to the respective

exercise and for sample type E agreed between the radionuclide laboratory and the PTS.

6.10.1.4. Station Backup Samples (D)

For type D samples the radionuclide laboratory shall attempt to simulate the time schedule

that is required of the radionuclide stations, as specified in CTBT/PC/II/1/Add.2 on page 48.

This means that the laboratory shall only start the spectral acquisition after the minimum

decay time for the sample has passed and that the radionuclide laboratory shall, when

possible, transmit the final sample spectrum to the PTS within 72 hours of the start of sample

collection at the radionuclide station. However, the minimum count time of 20 hours has

precedence over this reporting time requirement. In cases when sample transport to the

laboratory has resulted in an overlong decay period, the laboratory shall adjust the transmittal

time of the final spectrum accordingly. In all cases the laboratory shall transmit a preliminary

sample spectrum to the PTS within four hours of the start of acquisition.

4 Until preparedness is required samples in this category are treated as Network QC Samples (A) with regard to

the reporting schedule.


6.10.2. Report Content

For sample types A and B, the radionuclide laboratory shall provide the information and data

specified in Appendix IV. In the case of preliminary reports (sample type B only) the level of

detail provided shall be subject to any time constraints and availability of information

imposed by the reporting schedule.

For the IMS sample type C, the content requirements in Appendix IV may be amended by the

PTS depending on the instructions for the particular intercomparison exercise or proficiency

test. For sample type E, the content requirements will be defined by the PTS depending on the

agreement or special instructions for the analysis of specific samples. For both types, the

laboratory will be advised in advance by the PTS of the specific requirements for the report

content.

For sample type D only spectra shall be transmitted.

6.10.3. Report Format

The radionuclide laboratory shall comply with the current IMS format for reports,

Radionuclide Laboratory Report (RLR), specified in IDC 3.4.1, Formats and Protocols for

Messages (current version). The transmitted spectra shall also be in the current IMS format.

6.11. Acceptability of Analysis Results

Analytical results are assessed in proficiency tests and intercomparisons for identification of

radionuclides, accuracy and precision of results.

With regard to identification, in each proficiency test, a number of nuclides should be defined

that is considered the minimum number of identifiable nuclides, and laboratories’ results

evaluated against that criterion.

For accuracy, the u-test (also called the zeta test) according to equation (1), will be applied.

The zeta test is one of the performance statistics recommended in ISO13528:2005, “Statistical

methods for use in proficiency testing by interlaboratory comparisons”.

322

assignedabl

assignedlab

uu

AA (1)

where:

Alab = activity reported by the radionuclide laboratory;

Aassigned = assigned value for the activity (e.g. from certified reference material);

ulab = combined standard uncertainty reported by the radionuclide laboratory (k = 1);

uassigned = combined standard uncertainty of the assigned value (k = 1).

For acceptable results, the score of the zeta test should be less than 3. Depending on the

sample and the radionuclide in question, a more strict (or a more relaxed) rule may be applied.

The reported combined uncertainty (k = 1) shall be as accurate as possible (not under- or

overestimated). A statistical test, e.g. inter-quartile range method, as appropriate, will be used

to determine outliers among uncertainties reported by laboratories for a given nuclide in an

exercise.


For estimating bias, the %deviation or %difference (%D) in the value reported by the

radionuclide laboratory from the assigned value will be determined by applying equation (2).

% Difference is among the performance statistics recommended in ISO 13528:2005 for

estimating bias.

100%

assigned

assignedlab

A

AAD (2)

For acceptable results, the value of %D should be less than 15. Depending on the sample and

the radionuclide in question, a more strict (or a more relaxed) rule may be applied.

A test will be applied for precision. It may be, for example, the ratio of the laboratory

uncertainty and the assigned value uncertainty. The test and its target value are proficiency-

test specific and will be determined on a case by case basis.

Evaluation of results of proficiency tests and consequent actions depending on the

performance of the laboratory in the proficiency test will be according to the most current

version of CTBT/WGB/TL-1/53. Other indicators maybe used by the PTS such as timeliness

of reporting and correct formatting of reports, which will be announced to the participants of

the proficiency test before the exercise.

The PTS records and evaluates the results of the radionuclide laboratory and the laboratory

shall respond to this evaluation with its comments and/or corrective actions report, as

necessary.

The laboratory shall implement its corrective actions within a specified period agreed with the

PTS. The PTS will verify if the corrective actions implemented are effective, either by

sending the laboratory a test sample for analysis or at the next proficiency test exercise or

during surveillance assessment.

7. REQUIREMENTS FOR NOBLE GAS SAMPLE ANALYSIS

The methods implemented for analysis of IMS xenon samples shall be fit for their purpose as

QA/QC support for the IMS noble gas station network, appropriate and effective for the

analysis of IMS xenon samples and shall comply with the requirements specified in this

document. Currently, radioxenon samples can be analysed using gamma spectrometric or

beta–gamma coincidence analysis. A laboratory may decide to offer its analytical services for

archive samples of specific xenon system(s).

A detailed description of the methods, analysis processes and procedures and the

measurement equipment to be used for analysis of IMS xenon samples shall be included in

the CTBT specific documentation of the laboratory. Table 2 summarizes the minimum

technical specifications for the measurements and related equipment.


Table 2. Summary of Minimum Technical Specifications for IMS Xenon Sample

Measurements and Related Equipment for Routine Measurements Measurement/Property Specification

Pressure in station archive container Combined standard uncertainty <0.5 kPa (5 mbar)

Memory effect, if applicable <5%

Xenon volume in the archive container Combined standard uncertainty <10%

Xenon volume in the measurement cell Combined standard uncertainty <10%

Xenon Activity and Activity Concentration

Isotopes Detection and analysis of all relevant isotopes,

Xe-131m, Xe-133m, Xe-133 and Xe-135

Minimum detectable activity for Xe-133 5 mBq, for a blank sample within a 3 day

measurement

Minimum detectable activity for Xe-131m and

Xe-133m

10 mBq for a blank sample within a 3 day

measurement

Minimum detectable activity for Xe-135 15 mBq, for a blank sample within a 3 day

measurement

Uncertainty for the measurement of activity

concentrations of Xe-131m, Xe-133, Xe-133m and

Xe-135

The uncertainty of the activity concentration

measurement shall not be larger than 15% for a

measurement with a statistical uncertainty of less

than 3% (combined standard uncertainty, k = 1)

Gas Composition (Optional)

List of gases to be determined N2, O2, CO2, Xe, Ar, and common carrier gases

such as He [alternative set, to be determined, N2,

CO2, Xe]

7.1. General Requirements

7.1.1. Minimum Detectable Activity

The detection limits specified in Table 2 shall be calculated with decay correction to the start

of spectral acquisition. The minimum MDA requirements specified in Table 2 are defined for

an acquisition time of not more than three days, including gas background measurement.

Noble gas samples for routine re-analysis, e.g. for QA/QC purposes, can be sent to

laboratories meeting these minimum MDA requirements. However, in case more in-depth

analysis is required by the PTS, the samples shall be sent only to laboratories which meet the

more rigid MDA requirements of 5 mBq for Xe-131m and Xe-133m for a blank sample

within a six day measurement and 15 mBq for Xe-135 for a blank sample within a two day

measurement.

The MDA of the measurement system shall be determined by the analysis of a blank

measurement. The method for determining the MDA is described in Appendix II.

7.1.2. Sample Preparation

The sample shall be transferred from the archive bottle into the measurement cell so that the

transfer losses are minimized. At least 50% of the sample in the archive shall be transferred to

the measurement cell.


7.1.3. Detector Background

The detector background is defined as the non-sample associated background.

The detector background measurement shall be acquired over a period of at least six days

prior to commencement of operations. The PTS will analyse, evaluate and document in detail

all sources present in the background spectrum which can affect the measurement of the

xenon isotopes of interest. For the detector background measurement any potential residual

activity in the measurement cell from previous measurements must have decayed completely.

The background measurement shall be carried out with the same settings as the sample

measurement. A new detector background measurement has to be carried out after the

replacement of components which may affect the detector background.

7.1.4. Blank Sample Measurement

The effect of the sample matrix, such as stable xenon or any other gases, on the activity

measurement shall be determined in a blank sample measurement, i.e. in a measurement of

the aforementioned matrix gases. The measurement shall be repeated as appropriate, e.g. after

changes to the measurement system.

7.1.5. Gas Background Measurement

If the system shows a memory effect greater than 0.3%, a gas background measurement shall

be carried out prior to the sample measurement under the same conditions in which the IMS

xenon sample is being measured. The acquisition time of the gas background measurement

shall be at least 12 hours, or equal to the acquisition time of the sample measurement if this is

shorter than 12 hours. The analysis results of the blank sample measurements and the

measurement data shall be transmitted to the PTS.

7.1.6. Sample Counting Geometry

To guarantee constant counting efficiency, the sample to detector geometry has to be well

defined, i.e. the sample should be always in the same position during measurement so that it is

reproducible for all samples, QC and calibration sources.

7.1.7. Measurement cell

The measurement cell should be leak tight and made of materials not easily susceptible to

deformation. Technical drawings with details of the specific material of the sample

measurement cell shall be provided to the PTS.

7.1.8. Uncertainty of Analytical Results

A documented procedure shall be applied to estimate uncertainty of analytical results. All

factors affecting the uncertainty in the IMS sample analysis process shall be identified and

quantified. A combined standard uncertainty (k = 1) shall be reported for the radioactivity of

each xenon isotope of interest and shall include the individual contributions of the sources of

uncertainty.


7.1.9. Reporting

Requirements for management of analysis data are described in Section 6.11.

7.1.9.1. Reporting Schedules

For IMS xenon sample categories GA and GX, the laboratory shall transmit the measurement

data and the final report on the IMS xenon sample analysis within 15 days of sample receipt,

and shall have in place the respective procedures to meet the reporting time requirement. For

sample categories GC and GE the reporting time will be specified separately prior to the

analysis, in connection with the analysis request, and as agreed on between the radionuclide

laboratory and the PTS. If not specified, the default reporting time is also within 15 days from

sample receipt. For sample category GD, the radionuclide laboratory shall attempt to simulate

the time schedule that is required of the radionuclide station, the laboratory shall, when

possible, transmit the final sample spectrum to the IDC within 48 hours of the start of sample

collection at the radionuclide station. However, the measurement acquisition time shall be not

shorter than the standard acquisition time of the sample measurement at the station for which

the laboratory is acting as a backup.

7.1.9.2. Report Content

In its analysis report for IMS xenon sample categories GA and GX, the laboratory shall

provide the information and data specified in Appendix VIII. The report contents for sample

categories GC and GE may be specified separately prior to the analysis, in connection with

the analysis request, and as agreed between the radionuclide laboratory and the PTS. For

sample category GD, the two hour preliminary and full sample spectra SAMPLEPHD shall be

sent to the IDC. Any other reporting requirements may be specified separately prior to the

analysis, in connection with the analysis request, and as agreed between the radionuclide

laboratory and the PTS.

7.1.9.3. Report Format

The radionuclide laboratory shall comply with the current formats for reports and data as

specified in the current version of IDC 3.4.1, Formats and Protocols for Messages.

7.1.9.4. Measurement Data

The radionuclide laboratory shall transmit, together with the analysis report, pertinent

measurement data, such as spectral data from the xenon activity measurement. The purpose of

this is to enable the PTS to verify compliance with requirements for data quality and

measurement system characteristics and to ensure the end users of the laboratory results of the

transparency of the laboratory analysis.

7.1.10. Auxiliary Measurements

Requirements on the pressure and temperature measurements used to calculate results are

presented in Table 2.

7.1.11. Cross-Contamination

The cross-contamination between two subsequent samples shall be less than 0.3%.


7.2. Requirements for the Gas Quantification System

The xenon volume measurement process shall ensure that the actual xenon volume from

which the xenon activity is measured is determined with sufficient accuracy and precision

(combined standard uncertainty <10%). The xenon volume shall be reported at standard

temperature and pressure (STP) conditions (273.15 K, 101.325 kPa).

7.2.1. Noble Gas Sample Transfer and Processing

The expected volume of the stable xenon in a station archive sample ranges from 0.3 to

10 cm3. At a minimum, the laboratory shall be able to process and measure samples with

xenon volumes between 0.3 and 3 cm3.

7.2.2. Optional Gas Composition Measurement

In order to provide as much quality control as feasible, a gas composition measurement

consisting of the following gases may be reported (listed according to relevance): xenon (Xe),

carbondioxide (CO2), nitrogen (N2), oxygen (O2), helium (He) and Argon (Ar). This provides

very basic quality control, such as determining whether an archive bottle has leaked or CO2

was not effectively removed, or that somehow carrier gas was in the detector at the station.

The gas analysis uncertainties should roughly match or be superior to, the field

measurements; thus a ±10% gas composition measurement is required. The gas composition

shall be reported as percentages and as absolute volumes (at STP).

7.3. Requirements for Spectrometric Analysis of Noble Gas Samples

7.3.1. Spectral Acquisition and Analysis

Software and analysis tools used to collect, format, analyse and store sample spectra shall be

documented and validated. Relevant actions taken by the analyst during analysis shall be

recorded. Intermediate spectra shall be recorded at least every two hours for all IMS samples.

7.3.2. Detector Calibration

For empirical efficiency calibration methods, the radioactive source shall have the same

geometry and approximate density as the samples.

For empirical calibration of HPGe detection systems, the calibration sources shall contain

radionuclides that emit gamma rays covering the energy range of 30 to 350 keV required for

analysis. The radionuclide sources used for detector efficiency calibration shall be traceable to

standards provided by a recognized national or international standards organization. Source

certificates shall be appropriately stored and available for review. The radionuclide laboratory

shall ensure that true coincidence summing and other interference factors are taken into

account and do not distort the calibration.

For empirical calibration of beta–gamma detectors, the calibration sources shall contain

radionuclides that emit gamma and beta rays covering the full energy range required for

analysis.


If semi-empirical and mathematical methods are used for detector calibration, the relevant

software shall be appropriately validated. It shall be demonstrated and documented that the

calibration results agree with experimental data.

The analysis of calibration spectra shall be made using the same procedures used for sample

spectral analysis.

For beta–gamma detectors, interference factors for all relevant interfering nuclides (i.e.

interference from 214

Pb and from radioxenon isotopes with each other) have to be determined

during the calibration.

The calibration shall also assess and take into account, if necessary, the loss due to self

absorption by stable xenon.

8. CERTIFICATION PROCESS

This section documents the certification process for the radionuclide laboratories and links it

to other relevant PTS documentation.

The certification process consists of a series of subprocesses or stages. These stages do not

necessarily have to be carried out chronologically in the order listed. The “Acceptance of the

quality of analytical results”, in particular, requires a record of the results gathered over a

period of time before the subprocess can be completed. Laboratories shall participate in the

intercomparison and proficiency test exercise programme to demonstrate their analytical

capabilities. Before acceptance by the PTS, there must be sufficient data for each

measurement system to be used for IMS sample analysis. This is expected to require

participation in several exercises prior to acceptance. Data provided by a radionuclide

laboratory from participation in relevant non-CTBT-related proficiency tests can also be used

for evaluation of the quality of analytical results.

The technical procedures necessary to conduct a certification are detailed in Section 9.

The checklists presented in Appendix IX are an integral part of the certification procedures

and are used to document the compliance of a radionuclide laboratory with the certification

criteria. The purpose of the checklist is to guide the review team and to document the review,

the comments of the team and the conclusions of the review. The items in the checklists are

based on the requirements presented in the relevant sections of this document.

Links between this document and other relevant PTS documentation are presented in

Figure 1. The requirement manuals constitute the highest level (below the Treaty), on which

this document is based. This document contains two levels of documentation linked to each

other: certification requirements; and operational processes and technical procedures.

Figure 2 presents an overview of the certification process by subprocesses or stages. The

subprocesses are not necessarily carried out chronologically in the order shown. The

scheduling of any stage will be based on the dependence, if any, on the outcome of the

previous stage or alternatively, will be arranged to ensure the efficiency of the whole

certification process. Once certified, the laboratory undergoes regular surveillance

assessments by the PTS to ensure that it continues to meet the certification criteria.


The certification process is presented in Figure 3 as a flow chart to indicate the various

actions and decision making steps that comprise the whole process.

REQUIREMENT

MANUALS

Quality Manual


Operational Manual for Radionuclide

Monitoring and the International

Exchange of Radionuclide Data

CTBT/WGB/TL-11/5/Rev.8

CERTIFICATION OF RADIONUCLIDE LABORATORIES

CTBT/PTS/INF.96

OPERATIONAL

PROCESSES

AND TECHNICAL

PROCEDURES

Certification process:

links, processes,

procedures, checklists

RESULTS

Certified

laboratories

CERTIFICATION

REQUIREMENTS

MANUAL Certification

requirements

Figure 1. Links between this document and other PTS documentation.


Figure 2. Overview of the subprocesses in the certification process.

1. Formal arrangement

2. Acceptance of documentation

3. Acceptance of the quality of analytical results

4. Data and report formats check

5. Communication test

6. Authentication test

7. IMS sample analysis test

8. Certification visit

9. Formal certification

10. Surveillance assessment of the certified radionuclide laboratory


1. Formal arrangement

State Party Laboratory

2. Acceptance of

documentation

PTS

Facility

Agreement

Accreditation

Quality manual

Technical documentation

Preparation of

documentation

yes

Documentation

checklist

OK?

New review

no Required

amendments

implemented

Acceptance of

documentation

3. Acceptance of the

quality of analytical

results

yesOK?

New review

no Required

amendments

implemented

Acceptance of

analytical results

Checklist for

analytical results

Programme of

intercomparison and

proficiency test exercises

Demonstration of the

quality of analytical

results: correctness,

sensitivity,

resolution…

Figure 3. Certification process as flow chart.


4. Data and report formats

check

5. Communication test

6. Authentication test

7. Sample transport test

Analysis

report

Message, received and sent through

the GCI

Message with signature

Sample received from station,

analysed, reported on, and sent

back to the PTS

Raw data

including

calibration

data

7. IMS sample analysis test

8. Certification visit

9. Formal certification

Certification report

Certification group

meeting

Confirmation

PTS Laboratory

yes

Certification visit

checklist

OK?

New review

no Required

amendments

implemented

10. Surveillance assessment of the radionuclide laboratory

Intercomparison and

proficiency test

exercises

IMS sample analysis

Substantial changes at

lab

Review and acceptance

Evaluation of

performance

Reporting on

surveillance

assessment

Figure 3 (cont.)


9. CERTIFICATION PROCEDURES

This section describes the procedures that will take place as part of the process for

certification of a radionuclide laboratory for IMS sample analysis. The procedures would not

necessarily be carried out chronologically in the order listed. The scheduling would depend

firstly on whether a procedure depends on the outcome of the previous step and secondly on

the need for the process to be completed in the most efficient way.

Some of the procedures are specific to a particular analytical technique. At this stage

documented procedures have been developed to certify laboratories for gamma spectrometric

analysis of IMS particulate samples. Procedures for other analytical techniques will be

established if and when required.

9.1. Formal Arrangement

The certification process includes the following formal actions. The actions will be

implemented on a case by case basis.

(a) A facility agreement is established between the Commission and the State

Signatory hosting the radionuclide laboratory and covers the IMS related

functions of the laboratory;

(b) The radionuclide laboratory takes into account any relevant requirements of the

State Signatory;

(c) The radionuclide laboratory advises the PTS that it is ready to commence the

certification process;

(d) The PTS and the radionuclide laboratory agree on the commencement date and

scheduling of the initial certification steps.

9.2. Acceptance of Documentation

9.2.1. Objective

The objective of the review of documentation provided by the radionuclide laboratory is to

confirm that:

(a) A documented quality system is in place and is relevant to the CTBT related

activities to be carried out at the laboratory;

(b) The quality system is consistent with the requirements of the current version of

the PTS certification document, CTBT/PTS/INF.96;

(c) Technical documentation for CTBT related activities is also consistent with the

current version of CTBT/PTS/INF.96.


9.2.2. Documents to be Reviewed

The following documentation is to be presented by the radionuclide laboratory to the PTS for

review:

(a) A completed radionuclide laboratory information form (see Appendix VII);

(b) Documentation on existing national accreditation, if applicable;

(c) Sections of the existing quality manual of the radionuclide laboratory that relate to

CTBT activities; or

(d) A specific quality manual covering CTBT activities;

(e) Documented operational procedures and work instructions for the process of IMS

sample analysis;

(f) A summary which cross references, item by item, sections of the documentation

with requirements contained within the current version of CTBT/PTS/INF.96;

(g) A manufacturer’s data sheet for all measurement systems to be certified.

9.2.3. Procedure

A review is carried out by the PTS of the documentation provided by the radionuclide

laboratory. The approach taken is to check for consistency with the general requirements of

ISO/IEC 17025:2005 and also for compliance with the specific requirements in this

document. The steps taken in this stage are presented as a checklist in Appendix V, Part 1

(Review of Documentation).

The following steps are carried out by the PTS certification team:

(a) The documentation checklist is completed by the PTS to ensure that all required

documentation has been received.

(b) A review of the laboratory documentation is carried out against ISO/IEC

17025:2005 and the current version of CTBT/PTS/INF.96 with reference to the

specific checklist items in Appendix V, Part 1. A checked box for the individual

item indicates that the documentation satisfactorily meets the requirements of the

ISO/IEC standard and CTBT/PTS/INF.96. The Part 1 checklist has two columns

of check boxes, labelled “Nat./Int. Accredit.” and “PTS review”. One of the two

columns is marked, depending on whether the confirmation of consistency is

based on national accreditation or solely on PTS review. For CTBT specific items

covered by this document only, the column marked “PTS review” is checked once

consistency is verified.

(c) Once the documentation is accepted, the relevant conclusions box is checked and

the checklist is signed and filed; or, alternatively.

(d) If there are required actions to be taken before acceptance of documentation, the

appropriate box is checked and the list is signed and filed.

(e) When the required actions have been taken and the documentation has been

amended, a further review is conducted (see Figure 3, subprocess 2).


9.3. Acceptance of the Quality of Analytical Results

As part of the certification process, the laboratory needs to demonstrate to the PTS that it is

capable of performing IMS sample analysis at a sufficient level of quality for CTBT purposes.

The means of providing this assurance is for the laboratory to participate in intercomparison

and proficiency test exercises organized by the PTS. The laboratory may also provide data

from other intercomparison or proficiency tests as additional evidence of the quality of its

analyses.

In order to provide sufficient data as evidence of its analytical capabilities, a laboratory

undergoing certification should obtain an overall grade of B or higher based substantially on

the grading scheme according to the most current version of CTBT/WGB/TL-1/53 in at least

two out of three PTEs or intercomparison exercises organized by the PTS in the years

immediately preceding certification. Furthermore, as part of the certification process,

proficiency test data must be provided for each measurement system which will be certified

for IMS sample analysis.

9.3.1. Objective

Results from the intercomparison and proficiency test exercises are reviewed in order to

confirm that the quality of the analytical results is acceptable, and as an additional

confirmation that the measurement systems meet PTS certification requirements.

Requirements for gamma spectrometric analysis are presented in Section 6 and further

summarized in the checklist in Appendix V, Part 2 (Review of the Quality of Analytical

Results and Measurement Systems).

9.3.2. Procedure

The procedure for the review is as follows:

(a) For each intercomparison or proficiency test exercise, the results are recorded on

the relevant checklist (as in Part 2 of Appendix V) by the review team.

(b) The results are evaluated in accordance with the acceptance criteria detailed in

Section 6.11.

(c) Timeliness of reporting of the results in accordance with the deadline specified by

the PTS is noted.

(d) The evaluation is sent to the laboratory for comments and/or for corrective actions

report, as necessary.

(e) The comments of the laboratory and corrective actions report are reviewed, if

applicable.

(f) If and when the quality of the analytical results is deemed to be acceptable

according to the criteria, the conclusions section of the checklist in Part 2 is

completed accordingly.


9.4. Formats Check

9.4.1. Objective

The objective of the following procedure is to verify that the radionuclide laboratory is able to

send pulse height data (PHD) and LABDATA messages in the required IMS formats.

9.4.2. Procedure

(a) The radionuclide laboratory provides the PTS with the information needed in

advance to set up the system at the IDC for receiving and processing messages.

For this purpose, the laboratory will use the IMS Radionuclide Laboratory Set-Up

form in Appendix VII.

(b) The laboratory sends PHD (DETBKPHD, BLANKPHD, CALIBPHD and

SAMPLEPHD) and LABDATA messages (MESACK, SAMACK, ADDINS,

FINRLR, TECSDN and MISC) to the PTS.

(c) The PTS confirms that the PHD and LABDATA messages from the laboratory can

be processed; or, if not,

(d) The PTS advises that the laboratory needs to modify its formats.

9.5. Communication Test

9.5.1. Objective

The objective of the following procedure is to confirm that the laboratory messages can be

sent through the GCI and received at the PTS.

9.5.2. Procedure

(a) The PTS sends a test message to the GCI address of the radionuclide laboratory;

(b) The radionuclide laboratory sends an acknowledgement of the test message to the

PTS;

(c) The radionuclide laboratory sends a test message to the PTS;

(d) The PTS confirms that messages from the radionuclide laboratory address can be

received.

9.6. Authentication Test

9.6.1. Objective

The objective of the following procedure is to verify that the radionuclide laboratory is able to

create appropriate signatures to attach to messages and reports.

9.6.2. Procedure

(a) The laboratory sends a signed message to the PTS through the GCI;

(b) The PTS verifies that the signature is acceptable.


9.7. IMS Sample Analysis Test

9.7.1. Objective

The objective of the following procedure is to test the whole IMS sample analysis process,

including the efficacy of sample transport, customs clearance, other local arrangements and

the receipt of samples by the radionuclide laboratory.

(a) The PTS arranges for a test sample to be dispatched by courier from an IMS

radionuclide station to the radionuclide laboratory.

(b) The radionuclide laboratory acknowledges receipt of the sample and follows the

procedure for IMS sample analysis.

(c) The PTS records the results of the test.

(d) With the assistance of the laboratory, the PTS establishes the reasons for any

delays in the sample transport, e.g. due to courier arrangements, problems with

customs clearances, other local transport issues or other reasons.

(e) The radionuclide laboratory and the PTS take appropriate action to resolve

identified problems in local arrangements, including those related to the import of

samples.

9.8. Certification Visit

9.8.1. Objective

The PTS certification team visits the radionuclide laboratory to evaluate the overall capacity

of the laboratory to carry out IMS sample analysis and to see that the facilities and

measurement systems are as described in the laboratory’s documentation. In addition, the

team visits to confirm that the documented quality system of the laboratory is implemented

for IMS sample analysis.

9.8.2. Items to Be Evaluated

The checklist of items to be evaluated during the visit is presented in Appendix V, Part 3

(Certification Visit). The checklist items are based on the requirements in this document.

9.8.3. Procedure

The visit by the PTS certification team to the radionuclide laboratory is conducted in

accordance with the following procedure:

(a) The PTS and the radionuclide laboratory agree on the date and duration of the

visit.

(b) The PTS prepares a draft agenda and schedule for the visit in collaboration with

the laboratory.

(c) The PTS sends a note verbale to the Permanent Mission of the relevant State

Singatory. The note verbale includes details regarding the date, purpose and

agenda of the visit, and lists the PTS personnel participating in the visit.

(d) The PTS sends the final agenda for the visit to the laboratory.


(e) The PTS certification team conducts the site visit and completes the certification

visit checklist (Appendix V, Part 3). If a specific requirement is met then the box

for that item is marked. The PTS team also completes the details in the checklist

on the schedules and minutes of meetings with laboratory staff held during the

visit, provides comments for specific items, and provides details of recommended

and required actions to be taken in order to fully comply with the certification

requirements.

(f) On completion of the visit the checklist is signed by the review team.

(g) A visit summary is agreed upon and signed by the review team and the

radionuclide laboratory. It includes the required and recommended actions

resulting from the visit, as well as the status of the other steps in the certification

process.

(h) The radionuclide laboratory carries out any required action specified in the

summary to the satisfaction of the PTS team.

(i) The PTS updates the certification visit checklist to document the completion of

that stage of the process.

9.9. Formal Certification

Once the PTS certification team is satisfied that the laboratory meets the certification

requirements, the process can be finalized in accordance with the following procedure:

(a) The PTS review team prepares a certification report following the completion of

the stages of the certification process and any required actions by the laboratory.

(b) The certification report is submitted to a meeting of the Certification Group of the

PTS.

(c) If the Certification Group accepts the report, a confirmation is sent to the

radionuclide laboratory.

9.10. Certification of Additional Equipment

Once a laboratory has been certified, any additional equipment procured by the laboratory for

use in CTBT analyses must be certified as well. The procedures required to certify additional

equipment are dependent upon the analysis technique and are found in Section 10.

10. SURVEILLANCE ASSESSMENT OF A CERTIFIED LABORATORY

10.1. Objective

The PTS will conduct an ongoing evaluation of the performance of a certified radionuclide

laboratory to ensure that the laboratory continues to fulfil the certification criteria. As part of

this ongoing evaluation, a surveillance assessment visit will be carried out every three years

by default. An assessment may be conducted by the PTS earlier than the default 3 years under

the following situations: (1) when the laboratory performs poorly in two successive PTEs; (2)

when there are recurrent operational non-conformances such as errors in reporting or message

formats, failure to meet sample analysis or reporting timelines (refer to Appendix 1), and

errors affecting data quality; and (3) when there are changes at the laboratory which can

affect IMS sample analysis, e.g., changes in detector system and components or authorized


personnel (analysts). If in the process of these assessments, serious non-conformances with

certification requirements (which may include technical procedures and the quality system of

the laboratory) is found, the laboratory will be subject to a revalidation of its performance in

accordance with the current version of CTBT/PTS/INF.934. When a laboratory fails to

maintain the certification criteria, it will not be allowed to analyse samples for Treaty

verification purposes until the criteria are met once again.

10.2. Items to Be Evaluated

10.2.1. Intercomparison and Proficiency Test Programme

The PTS will assess and maintain a record of the results of the radionuclide laboratory in the

intercomparison and proficiency test exercises. Items to be evaluated are presented in the

checklist in Appendix V, Part 2 (Review of the Quality of Analytical Results and

Measurement Systems).

10.2.2. Performance in IMS Sample Analysis

The PTS will evaluate the ongoing performance of the radionuclide laboratory in terms of

compliance with the technical requirements for IMS sample analysis. Particular attention will

be given to timeliness in the conduct and reporting of analyses, adherence to IMS message

formats and continued observance of certified procedures.

The radionuclide laboratory is required to provide the PTS with a report of its CTBT specific

activities on an agreed periodic basis. This report is sent via email as a laboratory operations

report.

10.2.3. Changes at the Radionuclide Laboratory and in the Documentation

The radionuclide laboratory is required to advise the PTS of any changes in the technical

status and conditions at the laboratory that may have a significant impact on the ability to

carry out IMS sample analyses in accordance with certification requirements. When a

measurement service, such as gamma spectrometric analysis, is temporarily unavailable, the

PTS will be notified by email with a laboratory outage notification. For items such as the need

to relocate facilities, a change in the measurement system, or changes in key personnel, the

PTS will be notified by email with a configuration change notification.

The radionuclide laboratory shall provide the PTS with the most recent version of its CTBT

related documentation when new revisions are made following periodic reviews of quality

and technical documentation at the radionuclide laboratory. The radionuclide laboratory shall

notify the PTS of the revision by a Configuration Change Notification and submit the new

version of documents by email.

10.3. Procedure for Surveillance Assessment

The PTS notifies the radionuclide laboratory of an upcoming surveillance assessment and the

PTS and the radionuclide laboratory agree on the scheduling of the assessment. The following

documents will be produced for and referred to in the assessment by the radionuclide

laboratory and by the PTS:


(a) A list of changes in the radionuclide laboratory and in its CTBT specific

documentation since the previous assessment or the initial certification

(radionuclide laboratory);

(b) Record of laboratory performance in the proficiency tests and intercomparisons

(PTS);

(c) Record of laboratory performance in IMS sample analysis (PTS).

In addition to a review of the above documents, the surveillance assessment includes a

concise on-site visit. The overall procedure is the same as for the initial certification visit (as

described in Section 8.8), and the respective on-site procedure and checklist are presented in

Appendix VI (Surveillance Assessment Plan and Checklist).

The surveillance assessment is completed as follows:

(a) The PTS review team prepares a surveillance assessment report following the

completion of the surveillance process and any required actions by the laboratory.

(b) The surveillance assessment report is submitted to the Certification Group of the

PTS for acceptance.

(c) Upon acceptance of the report, a confirmation is sent to the radionuclide

laboratory.

11. TECHNIQUE SPECIFIC PROCEDURES FOR PARTICULATE SAMPLES

This section describes the additional procedures to be carried out during the certification

process to assess the quality of IMS sample analyses performed by the laboratory.

At this stage, for particulate samples, the procedures apply to IMS sample analysis by gamma

ray spectrometry but would be expanded to cover other techniques if and when approved for

CTBT related purposes.

11.1. Gamma Spectrometric Analysis

The procedures outlined in this section are applicable to stages 8.3 and 8.10 of the

certification procedure (as referred to in Section 8).

11.1.1. Radionuclide Detection Sensitivity

The following procedure is used to assess the sensitivity, expressed as MDA, of those gamma

ray spectrometry systems to be used for IMS sample analysis at the laboratory.

(a) The PTS provides the laboratory with a sample of blank filter material

compressed into the geometry required for checking the MDA requirement. The

filter material is chosen specifically from material known to have negligible

natural radioactivity.

(b) The laboratory is required to carry out a measurement of the blank filter for a total

counting time of no more than seven days. The measurement is to be performed

on each gamma detector to be certified for CTBT related purposes.


(c) The PTS provides the laboratory with a certified sample of same filter material

and same geometry of the blank sample used for checking the MDA requirement.

The laboratory will measure this sample to verify the compliance of laboratory

results with certified results for this geometry.

(c) The laboratory calculates the MDA of the detection system for 140

Ba using the

nuclear data and the equations detailed in Appendix II.

11.1.2. Radionuclide Analysis Check

During the certification visit, the laboratory is required to demonstrate the operational

procedure by which IMS particulate samples would be analysed. The PTS certification team

will also use this measurement as an additional quality check on the analytical capabilities of

the laboratory. The following procedure would apply at the time of the visit.

(a) The PTS provides a reference source consisting of a filter sample, spiked with

radionuclides of accurately known activities, presented in a standard IMS

geometry. The source activities are certified by the provider of the source and

traceable to a national standard.

(b) The laboratory personnel perform a measurement of the reference source on a

gamma ray spectrometer to be certified for CTBT related purposes. The

acquisition time for the measurement should be no more than one day. The

activities of radionuclides in the source will be such that a one day count produces

a random measurement uncertainty for each radionuclide of no greater than 1%.

(c) The laboratory calculates and provides a report of the activity (in Bq) of each

radionuclide in the sample. The report is part of the documentation compiled by

the PTS team during the certification visit and the results are summarized in the

certification visit checklist (Appendix V, Part 3).

(d) The laboratory also reports the combined uncertainties in the measured activities

based on realistic estimations and shall take into account all sources of

uncertainties, including as a minimum those presented in Appendix III.

(e) The PTS evaluates the acceptability of the laboratory measurement by comparison

with the known radionuclide activities in the reference source. Criteria for the

acceptability of results in a proficiency test are given in Section 6.11.

11.2. Certification of Additional Spectrometry Systems

11.2.1 Objective

It will be necessary to certify additional gamma ray spectrometry systems as previously

certified systems are replaced or the capabilities of the laboratory are expanded. As the

procedures and documentation of existing systems have already been certified, the

requirements for certification of additional systems are reduced to those that are specific to

the system itself.

11.2.2. Items to Be Evaluated

The checklist of items to be evaluated for the certification of additional gamma ray

spectrometry systems is presented in Appendix V, Part 4 (Certification of Additional Gamma


ray Spectrometry Systems). The checklist items are based on the requirements in this

document.

11.2.3. Procedure

Once a laboratory notifies the PTS that it has one or more additional gamma ray spectrometry

systems that it wishes to have certified, the following is carried out for each system:

(a) The laboratory sends the PTS the spectrometer information required for

certification. This includes a copy of the manufacturer’s data sheet, a completed

laboratory data sheet for the spectrometry system, and spectra (DETBKPHD,

BLANKPHD, CALIBPHD and SAMPLEPHD).

(b) The PTS certification team assesses the gamma ray spectrometry system and

completes the certification checklist (Appendix V, Part 4). If a specific

requirement is met then the box for that item is marked. The PTS team also

provides details of recommended and required actions to be taken in order to fully

comply with the certification requirements.

(c) Upon completion of the assessment the checklist is signed by the review team and

the radionuclide laboratory and filed.

(d) The radionuclide laboratory carries out any required action specified in the

checklist to the satisfaction of the PTS team.

12. BIBLIOGRAPHY

12.1. CTBT Related Documents

CTBT/PC/II/1/Add.2 Report of Working Group B to the Second Session of the

Preparatory Commission for the Comprehensive Nuclear-

Test-Ban Treaty Organization (16 May 1997).(Table 6 lists

the minimum requirements for IMS radionuclide stations as

recommended by WGB and adopted by the Preparatory

Commission. These requirements lay down the basis for the

certification procedures and are independent of the method

used for certification. The ultimate criterion is that the WGB

requirements are fulfilled by the installed system under local

conditions.)

CTBT/PC/III/WGB/CRP.14 Draft Report of the Informal Workshop on Radionuclide IMS

Network, Certusa di Pontigueno, Italy, 22-26 June 1997

(Chapter 3, Quality Assurance; Chapter 8, IMS Radionuclide

Laboratories) (4 August 1997).

CTBT/PC/V/WGB/PTS/1 Global Communications Infrastructure: Technical

Specification (28 January 1998) (Section 4.1.1, GCI/IMS

Interface Protocol).

CTBT/WGB-6/PTS/CRP.13 Counting Geometry and Detector Selection (26 May 1998).

CTBT/WGB/TL-2/40 Recommended Standard List of Relevant Radionuclides For

IDC Event Screening (17-21 January 2000).


CTBT/WGB/TL-

11,17/18/Rev.4

Operational Manual for Radionuclide Monitoring and the

International Exchange of Radionuclide Data, Draft (8 Sept.

2010).

CTBT/WGB/TL-1/53 Proposal for Evaluation of Radionuclide Laboratory

Proficiency Test Exercise Results.

CTBT/PTS/INF.58/Rev.8 Certification of IMS Particulate Radionuclide Stations (With

Guidelines for Station Installation (3 January 2007).



Certification of Radionuclide Laboratories (2005).

Certification and Surveillance Assessment of Radionuclide

Laboratories for Particulate and Noble Gas Sample Analysis

(2011)

CTBT/PTS/INF.103/Rev.1 Quality Manual (4 May 2000).

CTBT/PTS/INF.921/Rev.3 Certification of Noble Gas Equipment at IMS Radionuclide

Stations (with Guidelines for Station Installation).

IDC 3.4.1 current version Formats and Protocols for Messages (currently Rev.6

(November 2004).

12.2. Publications and Standards

Brookes, C.J., Betteley, I.G., Loxston, S.M., Fundamentals of Mathematics and Statistics,

Wiley, New York, pp. 369-377 (1985).

CEI IEC 1452, International Standard, Nuclear Instrumentation Measurement of Gamma

ray Emission Rates of Radionuclides – Calibration and Use of Germanium Spectrometers

(1995).

Guide to the Expression of Uncertainty in Measurement, International Organization for

Standardization (1995).

Gilmore, G., Hemingway, J., Practical Gamma ray Spectrometry, Wiley, Chichester, pp. 170-

172 (1995).

ANSI N42.14-1999, American National Standard for Calibration and Use of Germanium

Spectrometers for the Measurement of Gamma ray Emissions Rates of Radionuclides (1999).

ISO 10013:1998, International Organization for Standardization. Guidelines for Developing

Quality Manuals (1998).

ISO/TR 10013:2001, International Organization for Standardization. Guidelines for Quality

Management System Documentation (2001).

ISO/IEC 17025:2005, International Organization for Standardization: General Requirements

for the Competence of Testing and Calibration Laboratories (2005).

ISO 13528:2005, International Organization for Standardization: Statistical Methods for Use

in Proficiency Testing by Interlaboratory Comparisons (2005).


ISO/IEC Guide 98-3:2008, International Organization for Standardization. Uncertainty of

Measurement -- Part 3: Guide to the Expression of Uncertainty in Measurement (GUM:1995)

(2008).


APPENDIX I

OVERVIEW OF MESSAGES RELATED TO ANALYSIS OF IMS SAMPLES

AT RADIONUCLIDE LABORATORIES

Table 3. Overview of Messages Related to IMS Sample Analysis at Laboratories

Data Type Contents and Comments

Fro

m

To

Time

Requirement

PRESDN Notification that a sample will be sent to laboratory from station.

PT

S

Lab

0

TECSDN Notification that a sample was sent from a laboratory

SRID

Courier company

AWB number

ETA

Lab

PT

S

<2 h from

dispatch

LABSDN Notification that a sample has been sent to the laboratory from a

station

ETA, AWB and additional transport tracking information as

necessary

Relevant sample collection data

Identification (includes station number, collection start time, and

collection end time), total air volume sampled, partial volume if the

sample was split, the IDC activity summary, and the IDC event

screening flags

Type of analysis required, quantities to be determined

Priority category of the sample

For type B samples automatic notification that a sample is in

transit should be sent to laboratory person on call.

PT

S

Lab

0

MESACK Acknowledgement that a message was received and read. This is

required for all messages regarding type B samples and for all

PRESDN messages regardless of type.

Lab

PT

S

Immediately

after the

message is

read

SAMACK Notification that a sample was received and an indication of its

condition.

Condition of package and seals, description of sample

Comparison of the SRID with the one in the LABSDN Lab

/PT

S

PT

S/L

ab <2 h from

sample

receipt

RLR

PREL

Preliminary Radionuclide Laboratory Report. This is for type B

samples only.

Lab

PT

S

<4 h from

sample

receipt, then

within every

24 hours

RLR

FIN

Final Radionuclide Laboratory Report for type B samples. <8 d from

sample

receipt

Final Radionuclide Laboratory Report for type A samples, default

for types C and E, if not otherwise specified.

<15 d from

sample

receipt


ADDINS Instructions for the laboratory to

Continue or stop measurement

Proceed with other analysis methods

Dispatch the sample to a destination indicated in the message

PT

S

Lab

Any time

Request for additional instructions from the PTS on whether to

Continue or stop measurement

Proceed with other analysis methods

Lab

PT

S Any time

DATREQ Request for

Analysis results (when reporting time is not met)

Any additional information as necessary PT

S

Lab

Any time

MISC Free format to cover any message that does not fit one of the other

types.

Really should only be used as a “last resort.”

PT

S/L

ab

Lab

/PT

S Any time

Notes: 1. For the LABSDN and TECSDN data types, the first three letters indicate who receives the message. 2. Until preparedness is required the category B samples are treated as category A samples with regard to

reporting schedule and types of report required.


PTS

select labs to

analyse

sample

PRESDN

sent to selected

labs by PTS

Labs

acknowledge

receipt ofPRESDN

MESACK

sent to PTS by

labs

Labs

acknowledge

receipt of

samples

SAMACK

sent to PTS by

labs

PTS

compile

sample

information

LABSDN

sent to labs by

PTS

Labs

acknowledge

receipt ofLABSDN

MESACK

sent to PTS by

labs

Labs

perform

sample

analysis

RLR (PREL) and

SAMPLEPHD

(PREL)

sent to PTS by labs

RLR (FIN) and

SAMPLEPHD

(FULL)

sent to PTS by labs

PTS LABSMESSAGES

Figure 4. Message traffic during the sample analysis process.


PTS

request

missing

reports/data

DATREQ

sent to labs by

PTS

Labs

send missing

reports/data

RLR (PREL) and

SAMPLEPHD

(PREL)

sent to PTS by labs

RLR (FIN) and

SAMPLEPHD

(FULL)

sent to PTS by labs

Labs

dispatch

samples to

PTS

TECSDN

sent to PTS by

labs

PTS

acknowledge

receipt of

samples

SAMACK

sent to labs by

PTS

PTS

provide

further

instuctions

ADDINS

sent to labs by

PTS or vice versa

Labs

request

further

instructions

PTS LABSMESSAGES

Figure 4 (cont.)


APPENDIX II

PROCEDURE FOR DETERMINING THE MINIMUM DETECTABLE ACTIVITY

The minimum detectable activity of the nuclear detection system is calculated according to

Table 4 and the equations below:

Table 4. Nuclear Data

Parameter Radionuclide

140Ba

131mXe

133Xe

133mXe

135Xe

Half-life (days) 12.75 11.84 5.243 2.19 0.38

Key line energy5 (keV) 537.3

Emission probability (%) 24.4

Calculation of MDA (Bq) for gamma ray spectrometry systems:

CKPST

LMDA D

(2 a)

Calculation of MDA (Bq) for beta–gamma systems:

CKPPT

LMDA D

(2b)

Detection limit LD:

B65.471.2 DL (3)

Standard deviation of the background, B :

ROI

icountsB (4)

Decay correction during acquisition time, KC:

Ci

t

Ct

eK

C

i1

(5)

where

LD lower limit of detection at the 95% confidence level;

B standard deviation of the background at the energy of interest (ROI is defined as

1.25 FWHM (3) on either side of the hypothetical peak centroid)5;

5 The factor 1.25 is used for the certification because the MDC specifications (minimum requirements for IMS

radionuclide monitoring stations) were calculated using this width. The analysis software at the IDC can apply

a different value if it becomes necessary to do so in the future. 5

For gamma ray spectrometry, key lines with highest emission probability are used for MDA calculation and for

beta–gamma coincidence measurement, isotope-relevant ROIs are used.


T acquisition live time (s);

attenuation corrected efficiency (counts per gamma) at the energy of interest;

attenuation corrected efficiency (counts per beta) at the energy of interest;

S correction for true coincidence summing;

P

P

gamma emission probability (gammas per decay);

electron or conversion electron emission probability

KC decay correction during acquisition time;

i decay constant for the isotope i (s-1

);

tC clock real time between start and end of acquisition (s).


APPENDIX III

RECOMMENDED PROCEDURE TO ESTIMATE THE UNCERTAINTY OF

ANALYSIS RESULTS BY GAMMA RAY SPECTROMETRY

A procedure shall exist and be applied to estimate the combined uncertainty of a measurement

result. All factors affecting the uncertainty in the IMS sample analysis process shall be

identified and quantified to the extent possible.

The sources of uncertainty are identified by the input quantities, used to convert count rate to

a radionuclide activity (equation (6)):

SP

DRA n (6)

where

A activity of the radionuclide (Bq),

D radioactive decay of the radionuclide,

detection efficiency,

P gamma ray emission probability,

S correction for true coincidence summing,

Rn the net count rate due to the radionuclide corrected for both spectrum and detector

background.

The uncertainties of the above input quantity estimates, at a minimum, shall be included in the

combined uncertainty (uc(A)) for the activity (A) of each radionuclide analysed by gamma ray

spectrometry (equation (7)).

22222)()()()()()(

S

Su

P

Puu

D

Du

R

Ru

A

Au

n

nc (7)

where

u(Rn) uncertainty in the net count rate, including the uncertainties of both spectrum and

detector background.

u(D) uncertainty in radioactive decay of the nuclide. This may become significant if the

decay time is large with respect to the half-life or if there is a large uncertainty in

the nuclide half-life.

u() uncertainty in detection efficiency. This has two main components. The first of

these is the certified uncertainty of the calibration source. The second component

arises from the curve fit of efficiency against energy for the detector. If semi-

empirical or purely mathematical calibration methods are used, the uncertainties

introduced into the efficiency by these methods are to be included.

u(P) uncertainty of the gamma ray emission probability.

u(S) uncertainty in the correction for true coincidence summing (if necessary).


Equations (6) and (7) are estimates applicable for single energy gamma ray emitting

radionuclides, and for multi-energy gamma ray emitters in the case where the activity

calculation is based on the primary gamma line only. For radionuclides exhibiting coincidence

summing, this equation requires an estimate for the uncertainty of the coincidence correction

factor. Ideally, for correlated input quantities the covariances should be taken into account in

the combined uncertainty.

When the activity is calculated from several gamma lines associated with a radionuclide (as a

mean, by least squares fit, etc.), the radionuclide laboratory shall have an estimate for the

combined uncertainty that is appropriate for the calculation method. If individual components

of the combined uncertainty cannot be quantified the laboratory shall at least identify them

and present estimates for the most significant sources of uncertainty.

The radionuclide laboratory shall determine if there are any uncertainties arising during

sample preparation, for example, during weighing or sample splitting, that should also be

included in the combined uncertainty. Uncertainties from sampling, e.g. in the volume

sampled, that contribute to the combined uncertainty of activity concentration will be

provided by the PTS.

The combined standard uncertainty shall be used. If an expanded uncertainty (U) is reported,

the coverage factor (k) shall be stated (e.g. k = 2, k = 3) with the corresponding approximate

level of confidence.

CORRELATIONS AND OTHER SOURCES OF UNCERTAINTY

At present, the following issues are still under consideration by expert groups and no

definitive advice is available yet. It is discussed here as something to be aware of.

In most cases, the sources of uncertainty identified in equation 7 are those which are likely to

have the largest contributions. There are, however, many (other) potential sources of error,

each of which will have an associated uncertainty. It is important that, before the analysis

method is introduced, these sources of error and their uncertainties are identified and

quantified in order to determine whether or not they can be ignored in the determination of the

overall combined uncertainty of the measurement result.

Of particular concern is the existence of correlations between input quantities. For example,

where a radionuclide is assayed on the basis of a single gamma line and the calibration

efficiency has been determined solely from a calibration using a reference source of the same

nuclide, it is likely that the same photon emission probability (and uncertainty) has been used

in both measurements. In this case, the P uncertainty should be excluded from the calibration

and the assay uncertainties. Somewhat similar considerations might need to be taken to

account for the half-life.

Where an assay is determined on the basis of an efficiency calibration curve, this curve will

often have been generated using a mixed radionuclide, multi-gamma source. The fitting

procedures generally do not take into account the correlations between the uncertainties

on the activity values of the individual radionuclides in the mixture, nor do they

consider the correlations between the various P uncertainties. Generally the P covariances

are not known. For the reference source activities, these will often be traceable to an


individual national metrology institute which has used the same basic standardisation

technique so that the individual radionuclide activities will be heavily correlated but to an

unknown level. The use of a curve fitting algorithm ignores this effect and results in an

efficiency curve where the uncertainties, u(), at individual energies can be significantly

underestimated. A reasonable approach might be to assume that the activity values are totally

correlated and, as such, their uncertainties should not be included in the curve fitting

procedure. The uncertainty at individual energies would then be the quadrature sum of the

efficiency curve uncertainty at that point and the activity uncertainty for the relevant

radionuclide reference. These uncertainty levels would then define an uncertainty envelope

for all other energy points. The “true” uncertainty would lie somewhere between u() and

[u2() + u

2(A)]

1/2. However, it seems reasonable to err on the side of caution and to use the

pessimistic assessment of uncertainty. It should be noted that, although this approach may

result in slightly larger uncertainties, it also increases the probability that comparison results

will not be discrepant.


APPENDIX IV

CONTENT OF REPORTS FOR GAMMA SPECTROMETRIC ANALYSIS

(PARTICULATES)

Table 5. Description of the Required Report Content for Gamma Spectrometric

Analysis (Particulates)

Item Information or data required Report

Type6

Included in7

1. Purpose of

analysis

(a) Type of analysis and other analytical requirements

requested by the PTS;

P, F RLR

(b) Sample category;

(c) Other specific instructions from the PTS.

2. Sample

information

(a) Sample reference identification (SRID); P, F RLR,

SAMPLEPHD

(b) Receipt information – date, time; P, F RLR

(c) Sample information provided by the PTS and

additional information provided by the laboratory.

P, F RLR

3. Description of

work carried out

(a) Sample handling and pre-treatment; P, F RLR

(b) Identity of laboratory personnel responsible for the

analysis;

(c) Sample geometry used;

(d) Details regarding any modification of the sample

geometry from that received;

(e) The detection system used, including the CTBT

detector code;

(f) Measurement times – acquisition start and stop dates

and times, total acquisition time.

4. Measurement

results

(a) Sample spectrum; P, F SAMPLEPHD

(b) Peak report; P, F RLR

(c) Radionuclide identification and peak association.

5. Supporting data (a) Detector background measurement identification

(detector code, date and time);

P, F SAMPLEPHD

(b) Calibration measurement identification (detector

code, date and time);

P, F RLR

(c) Reference to the source of nuclear data used;

(d) Relevant information on the detector calibration,

including energy, efficiency and peak shape

calibration equations;

(e) Description of any coincidence summing corrections;

6 P = Preliminary report, F = Final report.

7 RLR = Radionuclide Laboratory Report, SAMPLEPHD = Sample Plus Height Data.


Table 5 (cont.)

Item Information or data required Report

Type

Included in

(f) Uncertainty budget (contribution of any significant

factors to the combined uncertainty of the result)

with, at a minimum, those factors detailed in

Appendix III.

6. Data analysis (a) Activities of all radionuclides detected and identified,

decay corrected to the start of the acquisition of the

spectrum, with associated combined uncertainties

P,F RLR

(b) Activity concentrations decay corrected to sampling8

with associated combined uncertainties (only

applicable to sample categories A and B);

(c) MDA values for those fission and activation products

included in the Revised Standard Categorization List

for Particulate Samples for IDC event screening

(CTBT/WGB/TL-2/40), or a subset thereof, as

agreed;

(d) Any specified activity ratios or reference times.

7. Comments Any comments relevant to the data analysis, including

explanation for peak rejection, or non-association or non-

identification of certain peaks by automated analysis.

P, F RLR

8. Conclusions Expert assessment of the analysis results to meet the

objectives of analysis stated in Section 2.3.

F RLR

8 Taking into account decay during spectral acquisition, sampling and during the period between sampling and

acquisition. Assume constant concentration during sampling.


APPENDIX V

CERTIFICATION CHECKLISTS (PARTICULATES)

PART 1: REVIEW OF DOCUMENTATION

Laboratory NNLXX, City, Country

The CTBT related documentation of the laboratory has been reviewed by the PTS for

compliance with certification requirements. The requirements and review procedure are

documented in the respective sections of CTBT/PTS/INF.96, current version at the time of the

certification process of the laboratory.

The results of the review are annotated below. Actions to be performed are of two categories:

required and recommended. Required actions shall be taken in order to fulfil IMS

specifications for the laboratory certification, before certification is finalized. Recommended

actions can be performed at a later stage in consultation with the PTS. They should be

considered as guidelines.

1. DOCUMENTATION REVIEW TEAM

Name Organization Division/Section/Unit Remarks

2. TIME OF REVIEW

Complete set of documents received (date)

Review completed (date)

3. CONCLUSIONS

The documentation is accepted.

The documentation requires amendment, and will be reviewed again after the required

actions that are specified in the following sections have been taken.

4. SIGNATURE

Date Name

PTS Certification Team Leader


5. CHECKLIST

5.1. Review of Documentation for Compliance with the Management Requirements

Quality system documentation encompasses the following subjects

and is consistent with ISO/IEC 17025:2005 and CTBT/PTS/INF.96/

Rev.9

Nat./Int.

Accredit.9

PTS

review10

5.1.1. Quality System

(a) Quality system has been established and maintained that

covers CTBT related operations

(b) Quality system has been documented and is implemented by

the personnel

(c) Structure of the laboratory

(d) Commitment of the management, quality manager

5.1.2. Quality Manual

(a) Quality policy statement

(b) Description of the quality system

(c) Maintenance of quality documentation

(d) Reference to technical procedures

(e) Roles and responsibilities

5.1.3. Technical Documentation Exists for IMS Sample Analysis

Process

5.1.4. Control of Records

(a) Quality records: reports from internal audits and management

reviews and records of corrective and preventive actions

(b) Contents of technical records related to IMS sample analysis

(c) Storage of technical records

(d) Recording and alterations to records

5.1.5. Other Quality System Management Practices

(a) Document control

(b) Review of terms of reference and contracts

9 Consistency of quality system with ISO/IEC 17025:2005 is traceable through national/international

accreditation. 10

Consistency of quality system with ISO/IEC 17025:2005 has been verified by the PTS review team.


(c) Subcontracting

(d) Purchasing of services and supplies

(e) Service to the CTBTO

(f) Complaints

(g) Control of nonconformity

(h) Corrective action

(i) Preventive action

(j) Audits

(k) Reviews

Comments:

Required actions:

Recommended actions:

5.2. Review of Documentation for Compliance with Technical Requirements

Documentation encompasses the following subjects and is consistent

with ISO/IEC 17025:2005 and CTBT/PTS/INF.96/Rev.9

Nat./Int.

Accredit.8

PTS

review9

5.2.1. Preparedness11

(a) Sample receipt

(b) Start of analysis

(c) On-call system

(d) Messaging

5.2.2. Personnel

(a) Authorization of specific personnel10

(b) List of authorized personnel10

with access to IMS samples and

data

(c) Objectives for and assurance of competence

(d) Job descriptions/authorization for specific tasks

11

CTBT specific requirements are related to this item, beyond the scope of the ISO/IEC 17025:2005. The box in

the PTS column must be checked for the documentation to be accepted.


(e) Records

5.2.3. Environmental Conditions

(a) Appropriate facilities and maintenance

(b) Environmental monitoring and control

(c) Cross-contamination prevention

(d) General access control

5.2.4. Analysis Methods and Validation of Methods (Including Software)

(a) Appropriate methods for the needs of the CTBTO

(b) Documentation of methods

(c) Documentation of software

(d) Validation procedures for methods

5.2.5. Uncertainty of Measurement

5.2.6. Equipment

(a) Appropriate equipment for IMS sample analysis

(b) Authorized personnel to operate the equipment

(c) Equipment records

(d) Maintenance of equipment

(e) VSAT10

5.2.7. Measurement Traceability

(a) Calibration programme

(b) Reference standards and materials

5.2.8. Procedures Exist According to Sample Category10

5.2.9. Sample Management10

(a) Receipt and dispatch of samples

(b) Security of samples

(c) Laboratory sample tracking

(d) Handling of samples

5.2.10. Quality Assurance of Analysis Results and Data Verification

(a) Quality assurance of analysis results


(b) Data verification

5.2.11. Management of Analysis Data10

(a) All data for IMS samples generated at the laboratory are

safely stored

(b) All intermediate results are stored

(c) A log for recording steps taken by the analyst during the

analysis exists

(d) Access to IMS sample analysis data is restricted to authorized

personnel

(e) Data confidentiality procedures are implemented

5.2.12. Reporting10

(a) Management of analysis data

(b) Content of the report and reporting time

(c) Data and report format

(d) Data authentication

5.2.13. Messages10

(1) Communications protocols

(2) Communication software

(3) Laboratory message format and contents

Comments:

Required actions:


5.3. Technique Specific Checklist for Gamma Spectrometric Analysis and Measurement

Systems10

According to the documentation, the following items are in compliance with the

respective section of CTBT/PTS/INF.96/Rev.9

PTS

review

5.3.1. Sample Preparation Methods

5.3.2. Acquisition and Analysis Software

(a) Documentation and validation

(b) Channels in spectrum 8192

5.3.3. Calibration

(a) Calibration methods

(b) Detector is calibrated for range 30-2700 keV


(c) Energy calibration – maximum deviations between actual and computed

energies (maximum order of fitting polynomial = 3) are within 0.6 keV

(d) Calibration measurements range 46.5-1836 keV

(e) Empirical calibration sources: geometry, density

(f) Semi-empirical and mathematical calibration methods: evaluated software

5.3.4. Detector Type: High Resolution HPGe

5.3.5. Detector Relative Efficiency: 40 %

5.3.6. MDA for 140

Ba ≤ 24 mBq for Cylindrical Sample Geometry with a

Diameter of 70 ± 0.5 mm, Height of 6 ± 0.5 mm and Density of 0.7 ± 0.1

g/cm3, with an Acquisition Time not more than Seven Days

5.3.7. FWHM and Peak Shape

(a) FWHM at 1332.5 keV 2.3 keV

(b) FWHM at 122.1 keV 1.3 keV

(c) Peak shape: FWTM/FWHM at 1332.5 keV 2.0

5.3.8. Background

(a) Regular (at least annual) measurements, records of measurements

(b) Appropriate control measures

5.3.9. Sample Counting Geometry

5.3.10. Uncertainty Budget

5.3.11. Reporting

(a) Content of analysis report

(b) Reporting time

Comments:

Required actions:



APPENDIX V


PART 2: REVIEW OF THE QUALITY OF ANALYTICAL RESULTS AND

MEASUREMENT SYSTEMS


As one step of the certification process of a radionuclide laboratory, evidence for quality of

gamma analysis results has been reviewed by the PTS for compliance with certification

requirements. The requirements and review procedure are documented in the respective

sections of CTBT/PTS/INF.96, current version at the time of the certification process of the

laboratory.

The evidence is produced mainly by participating in CTBTO laboratory intercomparison and

proficiency test exercises. Other proficiency tests can be considered if practical. The results of

the review are annotated below. Actions to be performed are of two categories: required and

recommended. Required actions must be taken in order to fulfil IMS specifications for the

laboratory certification, before certification is finalized. Recommended actions can be

performed at a later stage in consultation with the PTS. They should be considered as

guidelines.

1. REVIEW TEAM


2. TIME OF REVIEW

Evidence completed by (date)


3. CONCLUSIONS

According to the results submitted by the laboratory, the quality of analysis results is

acceptable.

According to the results, the technical specifications for gamma spectrometric

measurement system are met.

Improvement is required, and evidence will be reviewed again after the required


4. SIGNATURE

Date Name



5. CHECKLIST

5.1. Basis for Evaluation: Participation in Intercomparison and Proficiency Test

Exercises

The table below lists the exercises the laboratory has participated in and the results of

which have been used for the evaluation

Exercise Date Ref. No.

Comments:

Required actions:



Systems

5.2.1. Detection Sensitivity: MDA Determination

(a) The MDA for 140

Ba has been determined according to the test procedure in


(b) Required value for the MDA is achieved within the limit for the acquisition

time (24 mBq for cylindrical geometry with a diameter of 70 ± 0.5 mm, height

of 6 ± 0.5 mm and density of 0.7 g/cm3, with an acquisition time of not more

than 7 days)

(c) Details of the sample geometry and measurement are given below

CTBTO

Detector ID

Sample

Geometry

Sample

Density

Sample

Material

Acquisition

Time (days)

MDA for 140

Ba

(mBq)

Ref. No.

Comments:

Required actions:



5.2.2. Gamma Detector: Type, Energy Resolution and Relative Efficiency

(a) Detector type is HPGe

(b) Resolution is acceptable (2.3 keV at 1332.5 keV, 1.3 keV at 122.1 keV)

(c) Peak shape is acceptable (FWTM/FWHM 2.0 at 1332.5 keV)

(d) Relative efficiency is acceptable (40%)

(e) Energy calibration – maximum deviations between actual and computed


(f) Details of the sample geometry and measurement are given below CTBTO

Detector ID Type

Resolution at

1332.5 keV

Resolution at

122.1 keV

Peak shape at

1332.5 keV

Relative

Efficiency Ref. No.

Comments:

Required actions:


5.2.3. Radionuclide Analysis Check

(a) The laboratory has provided its analysis results in the programme of exercises,

where certified reference samples have been analysed. The samples have

certificates that trace the activities of radionuclides to national or international

standards

(b) The laboratory’s results are acceptable

(c) Calibration range valid in analysis is at least 30-2700 keV (empirical

measurements from 46.5 keV to 1836 keV)

(d) Number of channels in the spectra is 8192

(e) Comparison with source certificates and laboratory results are recorded below

Nuclide

Certificate Laboratory % Dev. Zeta test

result

Comment

[Pass/Fail]

Ref. No. Activity

(Bq) uc (%)

Activity

(Bq) uc (%)

Comments:

Required actions:



APPENDIX V


PART 3: CERTIFICATION VISIT


As one step of the certification process of a radionuclide laboratory, the PTS certification

team has visited the laboratory to verify compliance to the certification requirements. The

requirements and visit procedure are described in the respective section of

CTBT/PTS/INF.96, current version at the time of the certification process of the laboratory.

The results of the visit are annotated below. Actions to be performed are of two categories.

Required actions must be taken in order to fulfil IMS specifications for the laboratory

certification, before certification is finalized. Recommended actions can be performed at a

later stage in consultations with the PTS. They should be considered as guidelines.

1. PTS CERTIFICATION TEAM

Name Organization Dates Remarks

2. LOCAL PERSONNEL PRESENT


3. TIME AND PLACE OF THE VISIT

Dates Place

4. CONCLUSIONS

The certification requirements assessed during the visit are fulfilled; there are no

required actions resulting from the visit.

Not all certification criteria assessed during the visit are fulfilled. The status will be

reviewed again after the required actions that are specified in the following sections

have been taken.

Note: Irrespective of the above, there may be required actions from other steps of the certification process, such

as review of documentation or review of the quality of the analytical results and measurement systems.

5. SIGNATURE

Date Name



6. VISIT OPENING MEETING

The purpose of the opening meeting is to introduce the PTS visit team to the laboratory

personnel involved with the visit and to review the visit schedule and planned activities

during the visit. The laboratory is invited to give a general presentation on its activities as

well as on its CTBT specific operations. Possible changes to laboratory operations between

the documentation review and the visit should be addressed.

Date Time Place

Persons present:

Minutes:

7. DAILY VISIT MEETINGS/FINDINGS OF THE DAY

Date Time Place

Persons present:

Minutes:

8. VISIT CLOSING MEETING

The purpose of the closing meeting is to present the PTS visit team’s observations and

conclusions, to review, agree on, and sign this checklist.

Date Time Place

Persons present:

Minutes:


9. CHECKLIST

The technique specific items in this checklist pertain to non-destructive gamma-spectrometric

analysis.

9.1. General Observations

1. Conditions at the laboratory correspond to the information provided. 2. Laboratory personnel are aware of what is included in IMS sample process (what to do,

when to do, messaging scheme) and they know where to get the necessary information

from (technical documentation, process flow charts, procedures).

Comments:

Required actions:


9.2. Operational Procedures for Maintenance of Necessary Laboratory Resources

9.2.1. Readiness for IMS Sample Analysis and Authorized Personnel

3. Laboratory resources and procedures are in place to ensure that the laboratory is

prepared to receive an IMS sample. There are plans and provisions to implement the

operational preparedness when requested

4. Record of personnel authorized for CTBT operations is up to date

Comments:

Required actions:


9.2.2. Documentation, Technical Records, Quality Assurance for Measurement Systems

5. Technical documentation for IMS sample analysis is in use

6. Quality manual or equivalent is available

7. System for control of records of all IMS sample data is in place 8. Records are maintained for different IMS sample geometries and materials in use at

certified stations

9. Records are kept for equipment, calibrations, background and blank measurements,

calibration sources and reference materials, reference data such as nuclear decay data,

etc.

10. Equipment records include appropriate information such as identification, manufacturer,

type, serial number, date of receipt, location, condition, maintenance record, history

11. Manuals and working instructions for equipment are available as necessary 12. Results of proficiency tests and intercomparisons are assessed and used to implement

preventive or corrective actions and to improve the quality of analytical results as

necessary

13. Control charts or other appropriate procedures are in place to monitor status and

performance of measurement systems (e.g. calibration checks, detector parameters such

as energy shifting, energy linearity, resolution and other quality parameters)

Comments:

Required actions:



9.2.3. Calibration of Equipment

14. Calibration procedures and records are in place to ensure that equipment is calibrated

and that the calibration status is known

15. Calibrations exist and are maintained for all certified IMS sample geometries 16. Details of calibration procedures and raw data are stored to allow reconstruction of

calibration afterwards

17. Established criteria are applied to acceptance of calibration 18. Check procedure to create calibration (same as for sample analysis for peak search, peak

areas, etc., corrections are made for geometry, materials and coincidence summing)

19. Check production of calibration pairs that will be included in a) the CALIBPHD, b) a

SAMPLEPHD, which the calibration is applicable to (efficiency pairs in SAMPLEPHD

should be the ones used for the sample, corrected for sample geometry, materials and

coincidence summing)

20. Empirical calibrations: geometry, density, materials and traceability of sources.

Mathematical methods: validation of methods and software

Comments:

Required actions:


9.2.4. Detector Background

21. Records are maintained on background measurements

22. Control measures are taken for natural radioactivity indoors as necessary

Comments:

Required actions:


9.2.5. Blank Sample Measurements

23. Records are maintained on blank sample measurements

24. Blanks are measured for all certified IMS sample geometries

Comments:

Required actions:


9.3. Record of the MDA Check

A blank IMS sample is sent to the laboratory prior to the visit or the laboratory measures an

IMS blank available at the laboratory. The measurement is completed during the visit and the

MDA is calculated. Record whether the MDA is determined according to the documentation

and certification requirements and record the MDA:

25. SRID

26. Agreed MDA formula is used

27. Detector code

28. Measurement ID (detector code and start of measurement)

29. Acquisition time (≤7 days)

30. Date of reporting

31. MDA achieved (≤24 mBq)

32. BLANKPHD sent to the PTS


Comments:

Required actions:


9.4. Process of IMS sample analysis 33. Follow through and discuss the sample analysis process from receipt through

preparation, measurement and analysis to reporting and dispatch

34. Take pictures of the whole chain of custody (receipt, preparation, measurement, storage,

dispatch)

Comments:

Required actions:


9.4.1. Sample Receipt

35. Appropriate procedures exist for sample receipt and they are followed

36. See how samples are received (bring or send a sample to be received, if practical)

37. Inspection criteria are applied for the condition of the sample

38. Sample chain of custody record is started upon receipt

39. SAMACK is sent to the PTS

Comments:

Required actions:


9.4.2. Sample Tracking and Security

40. Sample identification system is adequate

41. Records are maintained of sample chain of custody 42. System of tracking which analysis and preparation methods a particular sample has been

subjected to while at laboratory is in place

43. Sample information is retrievable by the SRID 44. Access is controlled to areas where IMS samples are processed (prepared, measured and

stored)

45. There are a fire alarm system and emergency procedures

Comments:

Required actions:



46. Observe and discuss the sample preparation process and how it is recorded during

sample preparation

47. Cross-contamination is prevented in the preparation process (different areas and/or

equipment for low and high activity samples, decontamination procedures)

48. Is loss of elements prevented during preparation?

49. Instructions exist for preparation of different IMS sample types 50. Feasibility and provisions for splitting samples (splitting is normally only necessary

when requested by the PTS in order to send the other half to another laboratory)


51. Compression or other ways used to bring the samples into good measurement geometry,

as necessary: practical demonstration, sample compression procedure and equipment

Comments:

Required actions:


9.4.4. Sample Measurement

52. Check detector(s): manufacturer, type, serial number, etc. Compare with documentation

(to include the checklist for analytical quality and measurement systems). Confirm the

assignment and use of CTBT detector codes (NNLxx_yyy).

CTBT

Detector ID Manufacturer Type

Model

Number

Serial

Number

Year of

Acquisition

53. If materials are used in measurement to cut off X rays, this corresponds to the technical

documentation provided to the PTS

54. Measurement and spectrum are appropriately identified, access to sample and

measurement data is restricted during measurement

55. Cumulative spectrum can be set to be recorded every 24 hours (or at user defined

intervals)

56. Discuss capabilities (and procedures) for defining optimum measurement times (for

cases where results are needed as soon as possible) and for intermediate analyses of

spectrum can be done for QC and to optimize results for mother-daughter pairs, short

lived nuclides, etc.

57. Environmental conditions in measurement rooms, temperature and humidity control

(temperature should preferably be below 27C and with a maximum variation of 2C

during measurement; humidity should preferably be below 80%). Check the hydro-

thermograph, if installed.

Comments:

Required actions:


9.4.5. Analysis

58. Observe the analysis of a SAMPLEPHD (of the analysis check source or other relevant

sample)

59. Corrections for sample geometry, materials and coincidence summing are applied when

necessary

60. Intermediate results are recorded and stored: peak search, peak areas, baseline, peak

association, and methods for these different steps in the analysis

61. A log is kept of the steps taken by the analyst during the analysis 62. Reference is recorded for sample spectrum, calibration, background/blank subtraction,

coincidence correction factors, nuclear decay data, decay corrections, reference date for

results, etc.

63. Assessment has been made of uncertainty components and the significant ones are

included in the combined uncertainty of activity and activity concentration

64. Analysis and measurement data is retrievable by the SRID

65. Observe the analysis of a DETBKPHD

66. Laboratory DETBKPHD is fully characterized and explained

67. SAMPLEPHD and DETBKPHD sent to the PTS

Comments:


Required actions:


9.4.6. Data Storage and Security

68. All data and reports related to IMS sample analysis are stored. It is possible to

reconstruct and examine the validity of the analysis according to the stored information

69. The computer(s) or laboratory computer network, network drives, folders and data

structures are protected with user specific access management, passwords and/or

physical security measures (such as security cards)

70. Data storage backup and/or archival system (CDs, etc.) and their access control is in

place

71. Access to IMS sample data and reports is restricted to authorized personnel

Comments:

Required actions:


9.4.7. Quality Assurance on Results, Data Verification and Signature

72. Procedure is in place to ensure the quality of the results 73. Procedure is in place to ensure that report contents are verified before sending 74. Hardware token for creating the signature for messages is in use (validity of signatures

is checked in the messages arriving at the IDC)

Comments:

Required actions:


9.4.8. Reporting

75. Procedure for generating an RLR according to the current format is in use 76. Reporting schedules (reporting time requirements) are known to the staff 77. RLR is generated from the observed sample analysis and sent to the PTS

Comments:

Required actions:


9.4.9. Sample Dispatch

78. Sample dispatch procedure is in place (Note: By default the samples are to be returned

to the PTS within approximately a month, but more than one can also be collected to the

same shipment, if preferred for practical reasons, and if not otherwise instructed.)

79. Delivery confirmation received 80. Use of seals, secure envelopes, etc.

81. TECSDN sent to the PTS

Comments:

Required actions:



9.5. Record of the Analysis Check

If feasible, a spiked reference sample in IMS geometry, sent to the laboratory prior to the

visit, is analysed during the visit. Use this sample to follow the analysis process as described

in the checklist. Record the analysis results (items 82-87 apply to the spiked reference sample

only): 82. SRID 83. Detector code 84. Measurement ID (detector code and start of measurement) 85. Date of reporting

86. SAMPLEPHD sent to the PTS

87. RLR sent to the PTS

RN00 Check Sample Nuclide IDC Laboratory

%-dev.

Zeta

test

score

Comment

[Pass/Fail]

Ref.

No. Activity

(Bq/m3)

uc Activity

(Bq) ucA

(%) (Bq) (%) (Bq)

Spiked Reference Sample

Nuclide

Certificate Laboratory

%-dev.

Zeta

test

score

Comment

[Pass/Fail]

Ref.

No. Activity

(Bq)

uc Activity

(Bq)

ucA

(%) (Bq) (Bq) (%)

Note: If the analysis check source cannot be arranged to arrive at the time of the visit, another sample can be

used to follow the analysis procedure. In that case the results of the analysis check source are recorded when

they are available. In cases where the laboratory has demonstrated satisfactory performance in the proficiency

tests this step does not necessarily have to be completed before formal certification.

Comments:

Required actions (see notes above):



APPENDIX V


PART 4: CERTIFICATION OF ADDITIONAL GAMMA RAY SPECTROMETRY

SYSTEMS


When a certified radionuclide laboratory for whatever reason wishes to have one or more

additional gamma spectrometric systems certified for use with IMS sample analyses, this

checklist is used. No additional certification visit is required; however, the laboratory is

bound by all requirements for detector systems used in IMS sample analyses, detailed in the

current version of CTBT/PTS/INF.96 and those of the contract for analysis of IMS samples at

certified laboratories, not only those found in this checklist.

1. REVIEW TEAM

Name Division/Section/Unit Remarks

2. REVIEW DATE

Required data provided on (date)

Review completed on (date)

3. CONCLUSIONS

The following detector(s) are certified for unrestricted use in IMS sample

analyses (list by CTBTO Detector ID):

The following detector(s) are certified for use in IMS sample analyses only with

the permission of the PTS (list by CTBTO Detector ID):

4. SIGNATURE

Date Name



1. CHECKLIST


Systems

5.1.1. Manufacturer’s Data Check

(a) Check detector(s): manufacturer, type, serial number, etc. Compare with

documentation. The assignment and use of CTBT detector codes (NNLxx_yyy)

must be confirmed.

CTBTO


Model

Number

Serial

Number

Year of

Acquisition

Comments:

Required actions:



(a) The MDA for 140

Ba has been determined according to the test procedure in


(b) Required value for the MDA is achieved within the limit for the acquisition time.

(24 mBq for a cylindrical sample geometry with a diameter of 70 ± 0.5 mm,

height of 6 ± 0.5 mm and density of 0.7 ± 0.1 g/, with an acquisition time of not

more than 7 days)

(c) Details of the sample geometry and measurement are given below:

CTBTO

Detector

ID

Sample

Geometry

Sample

Density

Sample

Material

Acquisition

Time (days)

MDA for 140

Ba

(mBq)

Ref. No.

Comments:

Required actions:


5.1.3. Gamma Detector: Type, Energy Resolution and Relative Efficiency

(a) Detector type is HPGe

(b) Resolution is acceptable (2.3 keV at 1332.5 keV, 1.3 keV at 122.1 keV)

(c) Peak shape is acceptable (FWTM/FWHM 2.0 at 1332.5 keV)

(d) Relative efficiency is acceptable (40%)

(e) Energy calibration – maximum deviations between actual and computed


(f) Details of the sample geometry and measurement are given below:

CTBTO

Detector

ID

Type

Resolution

at 1332.5

keV

Resolution

at 122.1

keV

Peak shape

at 1332.5

keV

Relative

Efficiency Ref. No.

Comments:

Required actions:



5.1.4. Spectra

(a) Calibration range valid in analysis is at least 30-2700 keV (empirical

measurements from 46.5 keV to 1836 keV)

(b) Number of channels in the spectra is 8192

Comments:

Required actions:



APPENDIX VI

SURVEILLANCE ASSESSMENT PLAN AND CHECKLIST

PART 1: SURVEILLANCE ASSESSMENT VISIT PLAN


1. INTRODUCTION

The visit is one step in the surveillance assessment process for radionuclide laboratories

supporting the IMS radionuclide station network. Prior to the visit, the quality documentation

and written procedures related to CTBT activities are reviewed along with any existing

national or international accreditation.

2. OBJECTIVES OF THE VISIT

The objectives of the visit are:

to determine whether the elements in the quality system and the functions of the laboratory

related to CTBT-activities continue to be effective and implemented in accordance with the

policies and procedures that formed the basis of the original certification;

to evaluate and discuss the laboratory’s CTBT specific operations in order to determine

whether desirable and practicable improvements can be identified;

to discuss and evaluate changes in CTBT-requirements and the resulting implications for the

laboratory’s quality system and procedures.

3. SCOPE OF THE VISIT

Subject to evaluation during the visit are the quality system elements and procedures as they

are followed in practice, physical laboratory facilities, sample and data management,

equipment and procedures for CTBT samples. Specific items are reviewed according to the

attached surveillance visit checklist.

4. REFERENCE DOCUMENTS

Protocol to the Comprehensive Nuclear-Test-Ban Treaty, Part I C, IMS Operational Manual

CTBT/WGB/TL-11, 17/18 (latest version),

ISO/IEC 17025:2005: This standard is used as a guideline for things to pay attention to in the

certification process and for development of the certification document,

Documents provided by the PTS: Certification document CTBT/PTS/INF.96 (latest revision),

model terms of reference for the post-certification laboratory contract

IDC-3.4.1 (latest revision), Formats and Protocols for Messages


Documents provided by the laboratory: copy of certificate of accreditation, the laboratory’s

quality manual or equivalent documentation, procedures for CTBT specific work, lab data

sheet, manufacturer’s data sheets for detectors.

5. VISIT SCHEDULE

Before the visit, the PTS will provide a proposed schedule to the laboratory to ensure

availability of laboratory personnel involved in the visit.

Notes

Vertical audit implies following a complete, identifiable sample analysis using either a new

sample (generally inappropriate because of the nature of the process) or a sample received

and processed since the last visit. This would begin e.g. with the initial message and sample

receipt through to issue of final report and disposal of sample. It would involve scrutiny of

both management and technical requirements as specific to that sample. For example, on

training, it would need to be shown that the personnel involved in the process were

adequately trained and that the relevant records exist and are up to date.

Horizontal audit implies scrutiny of a particular quality system element across a range of

activities (or sample analyses). In training for example, the team would ensure that the QS

procedures are consistently applied across all staff, regardless of whether they were involved

in the vertical sample analysis. Similarly document control would look at control of all

documents, technical records, forms, etc.

6. REPORT OF THE VISIT AND REMAINING STEPS IN THE SURVEILLANCE

PROCESS

The visit is documented in the surveillance visit checklist by the PTS team. Any comments by

the visit team and any recommended or required actions are recorded in the checklist and/or in

the visit summary. The surveillance visit summary contains a summary of all steps in the

surveillance and any open required actions from the surveillance process to date, including

those from the review of documentation, review of the quality of analytical results and

measurement systems, format checks and communication/authentication check. The summary

is signed by the laboratory and the PTS. When the remaining steps and required actions have

been taken, presented by the laboratory, and approved by the PTS, the surveillance process

can be concluded. The PTS surveillance assessment team will produce a surveillance report,

which documents the whole process including the final versions of the checklists as well as

the corrective actions as recorded by the laboratory. The approval of the Certification Group

constitutes a formal end to the surveillance assessment process cycle. The laboratory will be

notified of the decision and will receive a copy of the surveillance assessment report.


APPENDIX VI

SURVEILLANCE ASSESSMENT PLAN AND CHECKLIST

PART 2: SURVEILLANCE VISIT


As part of monitoring that a certified radionuclide laboratory continues to meet the PTS

management and technical requirements for certification, the PTS surveillance assessment

team has conducted a surveillance assessment visit to the laboratory. The requirements and

visit procedure are described in the respective section of CTBT/PTS/INF.96, current version

at the time of the visit of the laboratory.

The results of the visit are annotated below. Actions to be performed are of two categories.

Required actions must be taken in order to fulfil IMS specifications for laboratory

certification, before the surveillance process is concluded. Recommended actions can be


guidelines.

1. PTS SURVEILLANCE ASSESSMENT VISIT TEAM





Dates Place

4. CONCLUSIONS

The certification requirements assessed during the visit are fulfilled; there are no

required actions resulting from the visit.

Not all certification criteria assessed during the visit are fulfilled. The status will be

reviewed again after the required actions that are specified in the following sections

have been taken.

Note: Irrespective of the above, there may be required actions from other steps of the surveillance

process, such as review of documentation or review of the quality of the analytical results and

measurement systems.

5. SIGNATURE

Date Name

PTS Surveillance Team Leader


6. SURVEILLANCE CHECKLIST

6.1. Review of Compliance with the Management Requirements

Quality system documentation encompasses the following subjects

and is consistent with ISO/IEC 17025:2005 and


Areas

surveyed

Result of

PTS

review

6.1.1. Quality System

(a) Quality system has been established and maintained that

covers CTBT related operations

(b) Quality system has been documented and is implemented by

the personnel

(c) Structure of the laboratory

(d) Commitment of the management, quality manager

6.1.2. Quality manual

(a) Quality policy statement

(b) Description of the quality system

(c) Maintenance of quality documentation

(d) Reference to technical procedures

(e) Roles and responsibilities

6.1.3. Technical Documentation Exists for IMS Sample Analysis Process

6.1.4. Control of Records

(a) Quality records: reports from internal audits and management

reviews and records of corrective and preventive actions

(b) Contents of technical records related to IMS sample analysis

(c) Storage of technical records

(d) Recording and alterations to records

6.1.5. Other quality system management practices

(a) Document control

(b) Review of terms of reference and contracts

(c) Subcontracting

(d) Service to the CTBTO

(e) Complaints

(f) Control of nonconformity

(g) Corrective action

(h) Preventive action

(i) Audits

(j) Reviews

Comments:

Required actions:



6.2. Review of Compliance with Technical Requirements

Documentation encompasses the following subjects and is consistent

with ISO/IEC 17025:2005 and CTBT/PTS/INF.96/Rev.9

Areas

surveyed

Result of

PTS

review

6.2.1. Preparedness

(a) Sample receipt


(c) On-call system

(d) Messaging

6.2.2. Personnel

(a) Authorization of specific personnel

(b) List of authorized personnel with access to IMS samples and

data

(c) Objectives for and assurance of competence

(d) Job descriptions/authorization for specific tasks

(e) Records




(c) Cross-contamination prevention

(d) General access control






6.2.5. Equipment

(a) Appropriate equipment for IMS sample analysis

(b) Authorized personnel to operate the equipment

(c) Equipment records

(d) Maintenance of equipment

(e) VSAT



(b) Calibration methods

(c) Reference standards and materials


(a) QA of analysis results


6.2.8. Management of Analysis Data

(a) All data for IMS samples generated at the laboratory are

safely stored



analysis exists

(d) Access to IMS sample analysis data is restricted to authorized

personnel



6.2.9. Reporting





6.2.10. Messages

(1) Communications protocols

(2) Communication software

(3) Laboratory message format and contents

Comments:

Required actions:



Systems

According to the documentation, the following items are in

compliance with the respective section of


Areas surveyed Result of

PTS

review

6.3.1. Sample Receipt

(a) Appropriate procedures exist for sample receipt and

they are followed

(b) Inspection criteria are applied for the condition of

the sample

(c) Sample chain of custody record is started upon

receipt

(d) SAMACK is sent to the PTS within the required

timeline

6.3.2. Sample Handling

(a) Appropriate procedures for sample preparation are in

place

(b) Cross-contamination is prevented in the preparation

process (different areas and/or equipment for low

and high activity samples, contamination checks and

decontamination procedures)

(c) Loss of elements is prevented during preparation

(d) Up to date instructions exist for preparation of

different IMS sample types


(a) Sample identification system is adequate

(b) Records are maintained of sample chain of custody

(c) System of tracking which preparation steps and

analysis methods a particular sample has been

subjected to while at laboratory is in place

(d) Sample information is retrievable by the SRID

(e) Access is controlled to areas where IMS samples are

processed (prepared, measured and stored)


6.3.4. Measurement

(a) Sample measurement geometry is applied as

documented

(b) If materials are used in measurement to cut off

X rays, this corresponds to the technical

documentation provided to the PTS

(c) Cumulative spectrum is set to be recorded every 24

hours or at other appropriate user-defined intervals

(d) Capabilities (and procedures) exist for defining

optimum measurement times (for cases where results

are needed as soon as possible) and intermediate

analyses of spectrum can be done for quality control

and to optimize results for mother-daughter pairs,

short-lived nuclides, etc.

6.3.5. Measurement System

(a) Detector type: high resolution HPGe

(b) Detector relative efficiency: 40%

(c) MDA for 140

Ba ≤ 24 mBq for cylindrical sample

geometry with a diameter of 70 mm and height of up

to 6 mm with acquisition time not more than seven

days

(d) FWHM at 1332.5 keV 2.3 keV

(e) FWHM at 122.1 keV 1.3 keV

(f) Peak shape: FWTM/FWHM at 1332.5 keV 2.0

(g) Detector identification is in accordance with

certified documentation and subsequent updated

information

CTBT Detector ID Manufacturer Type Model

Number

Serial

Number

Year of

Acquisition

6.3.6. Detector Calibrations, Background and Blank Sample Measurements

(a) Channels in spectrum 8192

(b) Detector is calibrated for range 30-2700 keV

(c) Calibration measurements range 46.5-1836 keV

(d) Energy calibration – maximum deviations between

actual and computed energies (maximum order of

fitting polynomial = 3) are within 0.6 keV

(e) Empirical calibration sources for gamma ray

spectrometry have appropriate geometry, density,

materials and certificates

(f) Semi-empirical and mathematical calibration

methods comprise appropriately evaluated software

(g) Detector background measurements: regular

measurements performed according to programme,

records are kept of the


(h) Blank sample measurements performed for all IMS

sample types

6.3.7. Analysis

(a) Analysis procedure is in place for IMS sample

analysis and it is followed in practice

(b) A log is kept by the analyst for recording steps taken

during the analysis. Relevant analyst actions are

transferred to the RLR

(c) All intermediate data and results are stored

(d) Assessment has been made of uncertainty

components and the significant ones are included in

the combined uncertainty of activity and activity

concentration

(e) Analysis and measurement data is retrievable by the

SRID

(f) Detector backgrounds and blank sample

measurements are fully characterized and explained

6.3.8. QA on Results, Data Verification and Signature

Procedure is in place to ensure correctness of the

reported results

Procedure is in place to ensure that report contents

are verified before sending

Hardware token for creating the signature for

messages is in use (validity of signatures is checked

in the messages arriving at the IDC) and the

signatures are valid

6.3.9. Reporting

(a) Procedure for generating an RLR according to the

current format and content requirements is in use

(b) Reporting schedules (reporting time requirements)

are known to the staff and observed in practice

(c) RLR is generated from the observed sample analysis

according to the procedure


(a) All data and reports related to IMS sample analysis

are stored. It is possible to reconstruct and examine

the validity of the analysis according to the stored

information

(b) The computer(s) or laboratory computer network,

network drives, folders and data structures are

protected with user-specific access management,

passwords and/or physical security measures (such

as security cards)

(c) Data storage back-up and/or archival system (CDs,

etc.) and their access control is in place

(d) Access to IMS sample data and reports is restricted

to authorized personnel


6.3.11 Sample dispatch

(a) Appropriate sample dispatch procedure is in place

(Note: By default the samples should be returned to

the PTS on a quarterly basis if not otherwise

instructed.)

(b) TECSDN sent to the PTS upon dispatch

Comments:

Required actions:



APPENDIX VII

IMS RADIONUCLIDE LABORATORY SET-UP INFORMATION

To be able to set up a radionuclide laboratory at the PTS certain information is required.

Please complete this form and send it to [email protected].

Notes

1. Dimensions are to be given in mm, apart from the detector dead layers, which

should be in m.

2. Densities should be given in g/cm3.

3. The numbers in brackets refer to the figures at the end of this form.

4. If a material is not in the list, provide as much information as possible.

Station Information

Laboratory code

Point of Contact

Name

Telephone number

Address

Email address

Other information

Message System Configuration

Sender email address (the one that will appear on the FROM line)

Alternate email address (for resending of data in cases where it is not possible

to use the original address)

Receipt acknowledgement required? (if yes, provide email address)

Yes No

IMS Reporting System

Email address reports should be sent to

Email address(es) that should receive a copy


Detector Information

Detector system

Detector code

Number of channels 8192 16384

Detector type P-type N-type

Coaxial Planar

Detector manufacturer

Detector model

Detector serial number

Rated resolution (at 1332 keV)

Rated relative efficiency

Cooling method LN2 Electrical

Detector Calibration*

Energy range (min-max, keV)

Energy calibration reference lines (keV)

Resolution calibration reference lines (keV)

Efficiency calibration reference lines (keV)

Date of first calibration

* Default values (keV): 46.52, 59.54, 88.03, 122.06, 165.85, 391.69, 661.62, 898.04, 1173.24,

1332.50, 1836.06, and 2505.74.

Detector Dimensions

Crystal Material

Crystal

diameter (1) Crystal length (2)

Top edge radius of

curvature (3)

Hole

diameter (4) Hole depth (5)

Hole radius of curvature

(6)

Dead layer

top

(in m) (7)

Dead layer outside

(in m) (8)

Dead layer inside/bottom

(in m) (9)

Crystal Holder

Material Copper Thickness (10)

End Cap

Material Carbon fibre

Outer diameter (11) Thickness (13)

End Cap Window

Window Material Carbon fibre

Thickness (14) Distance to crystal

(15)

Diameter (16)


Shielding Information

Model

Inner diameter (33) Inner height (34)

First layer Thickness (35) Material

Second layer Thickness (36) Material

Third layer Thickness (37) Material

Fourth layer Thickness (38) Material

Assembling Dimensions

Distance between end cap window and shielding (40)

Distance between sample (container) and detector end cap

Detector Electronics

Detector electronics manufacturer

Detector electronics model

Detector electronics number

Materials

Material name Germanium Density 3.323 Formula Ge

Material name Copper Density 8.933 Formula Cu

Material name Aluminum Density 2.7 Formula Al

Material name Tin Density 7.287 Formula Sn

Material name Lead Density 11.342 Formula Pb

Material name Magnesium Density 1.74 Formula Mg

Material name Cadmium Density 8.69 Formula Cd

Material name Gold Density 19.282 Formula Au

Material name Boron Density 2.37 Formula B

Material name Stainless steel Density 7.5 Formula Fe68.2-Mn1.55-Cr17.7-

Ni11.2-Mo1.22-C0.0005

Material name 3M Filter 3M5379 Density 0.6 Formula

C85-H14.3-N0.3-Cl0.012-

Na0.0045-Al0.008-

Ti<0.001-Ca0.046-

K0.033-V0.0001-

Mg<0.01-Cu<0.001

Material name Camfil glass fibre

CS5.0 Density 0.14 Formula

O60.07-Si21.84-B6.06-

Na5.7-Al2.43-Ca1.64-

K1.12-Zn0.67-Ba0.48

Material name Carbon fibre Density 1.15 Formula C72.1-O21.9-H6

Material name Polyethylene Density 0.94 Formula C85.6 - H14.4

Material name Teflon Density 2.2 Formula F76 - C24

Material name Plexiglas Density 1.19 Formula C5O2H8

Material name PVC Density 1.3 Formula C2H3Cl

Material name Density Formula



















2

3

5

7

8

1

6

9

4

17

10

11

13

1614

15

Figure 5. Detector: Coaxial.


33

34

40

38

3635

37

Figure 6. Shielding.


APPENDIX VIII

CONTENT OF REPORTS FOR IMS XENON SAMPLE ANALYSIS FOR NETWORK

QUALITY ASSURANCE/QUALITY CONTROL PURPOSES

Item Information or data required Included in12

1. Purpose of

analysis

(a) Type of analysis and other analytical requirements

requested by the PTS

RLR

(b) Sample category

(c) Other specific instructions from the PTS

2. Sample

information

(a) Sample reference identification (SRID) RLR

(b) Receipt information – date, time

(c) Sample information provided by the PTS and

additional information provided by the laboratory.

Comments to transport, comments to sample and

sample container condition, comment to seal condition

if applicable, any additional relevant information

3. Description of

work carried out

and methods

applied

(a) Relevant information on calibrations of main

measurement equipment

RLR

(b) Sample handling, transfer and processing (including

details on any concentration and purification)

(c) Sample measurement and analysis

(d) Details regarding the measurement conditions

including environmental conditions during

measurements which may influence the result

(e) Measurement times (start, stop, live and real times, as

applicable to different measurements)

SAMPLEPHD

(f) Analysis software and description of algorithms RLR

(g) Comments relevant to the data analysis (including

analyst action regarding addition/rejection of peaks or

association of peaks in the spectra during xenon

activity analysis)

(h) Identity of laboratory personnel responsible for the

analysis

4. Measurement

data and

intermediate

results

(a) Such as critical limits in the xenon activity

measurement, signal significances in different

measurements as applicable

RLR

5. Supporting data (a) Detector background measurement identification

(detector code, date and time)

RLR

(b) Gas background measurement identification (detector

code, date and time)

12

RLR = contents and format to be specified for xenon sample analysis.


Item Information or data required Included in11

(c) Calibration measurement identifications (equipment

codes, dates and times)

(d) Sample measurement identification (measurement

system code, date and time)

(e) Blank MDAs for the four xenon isotopes

(f) Source of nuclear data and other reference data

(g) Corrections applied to measurement data and

intermediate results

(h) Uncertainty budget (contribution of any significant

factors to the combined uncertainty of the result) with,

at a minimum, those factors detailed in Appendix Y

6. Analysis results (a) Archive container pressure (Pa (at 273.15 K)) and its

combined uncertainty (%)

RLR

(b) Xenon volume in the archive container (cm3) and its

uncertainty (%)

(c) Xenon volume in the measurement cell (cm3) and its

uncertainty (%)

(d) Identity of the detected radioxenons

(e) Activity of each detected radioxenon isotope (Bq) and

its combined uncertainty, decay corrected to the start

of spectral acquisition

(f) Activity concentration (Bq/m3) of each detected

radioxenon isotope and its combined uncertainty (%),

decay corrected to the sampling time (assuming

constant concentration in the air and constant

collection)

(g) Reference time for activities and activity

concentrations (start of spectra acquisitions and sample

collection)

(h) MDAs for the four radioxenons of interest, decay

corrected to the start of spectral acquisition

(i) MDCs for the four radioxenons of interest, decay

corrected to the sampling time (assuming constant

concentration in the air and constant collection)

(j) Activity ratios (as applicable): Xe-135/Xe-133, Xe-

133m/Xe-133, Xe-133m/Xe-131m

(k) Reference time for activity ratios (sample collection

period)

7. Comments Any comments and additional information relevant to the

analysis

RLR

8. Conclusions Expert assessment of the analysis results to meet the

objectives of analysis

RLR

9. Completion of

analysis and report

transmission

Times of completion of the analysis and report

transmission.

RLR

Notes: All times shall be reported in UTC, all combined uncertainties shall be reported with k = 1.


APPENDIX IX

CERTIFICATION CHECKLISTS (NOBLE GAS)

PART 1: REVIEW OF DOCUMENTATION


The CTBT related documentation of the laboratory has been reviewed by the PTS for

compliance with certification requirements. The requirements and review procedure are

documented in the respective sections of CTBT/PTS/INF.96, current version at the time of the

certification process of the laboratory.

The results of the review are annotated below. Actions to be performed are of two categories:

required and recommended. Required actions shall be taken in order to fulfil IMS


actions can be performed at a later stage in consultation with the PTS. They should be


1. DOCUMENTATION REVIEW TEAM


2. TIME OF REVIEW

Complete set of documents received (date)


3. CONCLUSIONS

The documentation is accepted.

The documentation requires amendment, and will be reviewed again after the required


4. SIGNATURES

Laboratory Representative PTS Certification Team Leader


5. CHECKLIST

5.1. Review of Documentation for Compliance with Technical Requirements

Documentation encompasses the following subjects, is consistent with

ISO/IEC 17025:2005 and CTBT/PTS/INF.96/Rev 9:

Nat./Int.

Accredit.8

PTS

review9

5.1.1. Preparedness10

(a) Sample receipt


(d) Messaging

5.1.2. Personnel

(a) List of authorized personnel with access to IMS noble gas

samples and data

(b) Objectives for and assurance of competence

(c) Job descriptions/authorization for specific tasks

(d) Records




(d) Noble Gas Measurement Equipment room access control






5.1.5. Uncertainty of Analytical Results [7.1.7]

5.1.6. Equipment

(a) Appropriate equipment for noble gas analysis

(b) Equipment records including maintenance




(b) Reference standards and materials

5.1.8. Sample Management

(a) Receipt and dispatch of samples

(b) Security of samples

(c) Laboratory sample tracking

(d) Handling of samples


(a) QA of analysis results


5.1.10. Management of Analysis Data

(a) All data for IMS noble gas samples generated at the

laboratory are safely stored



analysis exists

(d) Access to IMS noble gas sample analysis data is restricted to

authorized personnel


5.1.11. Reporting





Comments:

Required actions:



5.2. Technique Specific Checklist for Noble Gas Analysis

According to the documentation, the following items are in compliance with the

respective section of CTBT/PTS/INF.96/Rev.9:

PTS

review

5.2.1. Analysis Software and Calibration

(a) Documentation and validation

(b) Capable of collecting SPHD spectrum every 2 hours

(c) Calibration procedures documented and validated

5.2.2. Radioactive Xenon Detector System

(a) Four isotopes detection capability (Xe-131m, Xe-133, Xe-133m, and

Xe-135)

(b) Uncertainty13

of Activity Measurement ≤15% if statistical uncertainty is

<3%

(c) For a blank sample within a 3 day measurement:

Minimum detectable activity (MDA) for Xe-133 is 5 mBq and

MDA for Xe-131m and Xe-133m is 10 mBq and

MDA for Xe-135 is 15 mBq

(d) MDA for Xe-131m, Xe-133 and Xe-133m is 5 mBq, for a blank sample

within a 6 day measurement and

MDA for Xe-135 is 15 mBq, for a blank sample within a 2 day

measurement

(e) Sample to the measurement cell transfer efficiency is better than 50%

(f) Gas background is performed if memory effect is greater than >0.3%

(g) Cross-contamination <0.3%

(h) Memory effect is <0.3%

5.2.3. Gas Quantification System

(a) Stable xenon volume reported in cm3 at STP

14

(b) Uncertainty of Xe volume in measurement cell <10%

(c) Uncertainty in pressure in station archive container <0.5 kPa

(d) Archive container volume information

(e) Measurement cell dead volume determined

13

All references to uncertainties imply combined standard uncertainty with the coverage factor k = 1. 14

STP – Standard Temperature and Pressure used in this document are referring to NIST definition:

temperature 0°C, pressure 101.325 kPa (1 bar).


APPENDIX IX


PART 2: REVIEW OF THE QUALITY OF ANALYTICAL RESULTS AND

MEASUREMENT SYSTEMS


As one step of the certification process of a radionuclide laboratory, evidence for quality of

gamma analysis results has been reviewed by the PTS for compliance with certification

requirements. The requirements and review procedure are documented in the respective

sections of CTBT/PTS/INF.96, current version at the time of the certification process of the

laboratory.

The evidence is produced mainly by participating in CTBTO laboratory intercomparison and

proficiency test exercises. Other proficiency tests can be considered if practical. The results of

the review are annotated below. Actions to be performed are of two categories: required and

recommended. Required actions must be taken in order to fulfil IMS specifications for the

laboratory certification, before certification is finalized. Recommended actions can be


guidelines.

1. REVIEW TEAM


2. TIME OF REVIEW

Evidence completed by (date)


3. CONCLUSIONS

According to the results submitted by the laboratory, the quality of analysis results is

acceptable.

According to the results, the technical specifications for gamma spectrometric

measurement system are met.

Improvement is required, and evidence will be reviewed again after the required


4. SIGNATURES



5. CHECKLIST

5.1. Basis for Evaluation: Participation in Intercomparison and Proficiency Test

Exercises

The table below lists the exercises the laboratory has participated in and the results of

which have been used for the evaluation

Exercise Date Ref. No.

Comments:

Required Actions:

Recommended Actions:

5.2. Technique Specific Checklist for Gamma Spectrometric Analysis and

Measurement Systems


The required MDA for Xe-133, Xe-133m, Xe-131m and Xe-135 for routine

measurements is achieved within the limit for the acquisition time

CTBTO

Detector

ID

Acquisition

Time (days)

Xe-131m

MDA

Xe-133m

MDA

Xe-133

MDA

Xe-135

MDA Ref. No

Comments:

Required Actions:



5.2.3. Radioxenon Analysis Check

(a) The laboratory has provided its analysis results in the programme of exercises,

where certified reference samples have been analysed. The samples have

certificates that trace the activities of radionuclides to national or international

standards

(b) The laboratory’s results are acceptable

(c) Calibration range is valid

(d) Detector(s) specs are within requirements

(e) Comparison with source certificates and laboratory results are recorded below

Nuclide

Certificate Laboratory % Dev. Zeta test

score

Comment

[Pass/Fail]

Ref. No. Activity

(Bq) uc (%)

Activity

(Bq) uc (%)

Comments:

Required Actions:



APPENDIX IX


PART 3: CERTIFICATION VISIT


As one step of the certification process of the noble gas measurement technique of a

radionuclide laboratory, the PTS certification team has visited the laboratory to verify

compliance to the certification requirements. The requirements and visit procedure are

described in the respective section of CTBT/PTS/INF.96, current version at the time of the

certification process of the laboratory. The results of the visit are annotated below. Actions to

be performed are of two categories. Required actions must be taken in order to fulfil IMS


actions can be performed at a later stage in consultations with the PTS. They should be


1. PTS CERTIFICATION TEAM





Dates Place

4. CONCLUSIONS

The equipment for the measurement of xenon samples from IMS stations and the

related operation and maintenance procedures are considered effective in meeting the

objectives and requirements set for noble gas analysis at IMS Laboratories.

Not all certification criteria are fulfilled. The status will be reviewed again after the

required actions that are specified in the following sections have been taken.

5. SIGNATURES



6. VISIT OPENING MEETING

The purpose of the opening meeting is to introduce the PTS visit team to the laboratory

personnel involved with the visit and to review the visit schedule and planned activities

during the visit. Possible changes to laboratory operations related to IMS xenon sample

analysis should be addressed.

Date Time Place

Persons present:

6.1. Minutes of the Meeting

7. DAILY VISIT MEETINGS

Date Time Place

Persons present:

7.1. Minutes of the Meetings

8. VISIT CLOSING MEETING

The purpose of the closing meeting is to present the PTS visit team’s observations and

conclusions, to review, agree on, and sign this checklist.

Date Time Place

Persons present:

8.1. Minutes of the Meeting


9. CHECKLIST

9.1. Use and Maintenance of Documentation and Technical Records

(a) Documentation of sample preparation, measurement and analysis methods for

noble gas IMS sample analysis are in use

(b) A system is in use for control of records of IMS noble gas sample data

(c) Records are kept for equipment, calibrations, background measurements,

maintenance, certificates for calibration and reference sources, nuclear data, etc.

Comments:

Required actions:


9.2. Physical Locations

(a) Follow through (discuss) the sample analysis process from receipt through

preparation, measurement and analysis to reporting and dispatch

(b) Walk the path of the sample and on the way inspect the facilities

(c) Take pictures of the whole chain of custody (receipt, preparation, measurement,

storage, dispatch of empty sample archive back to the station)

(d) Confirm that the conditions at the laboratory correspond to the information

provided

Comments:

Required actions:


9.3. Control of Environmental Conditions

(a) Temperature should always be preferably below 27C, with a maximum

variation of 2C during measurement. Humidity should be preferably below

80%.

Comments:

Required actions:


9.4. Sample Management

9.4.1. Receipt and Dispatch

(a) Check the sample receiving area

(b) See how samples are received (bring or send a sample to be received, if

practical)

(c) Check acknowledgement of receipt, inspection criteria for the condition of

sample

(d) Check empty archive container dispatch procedure

(e) Is a dispatch notification sent to the PTS?

Comments:

Required actions:




(a) Review sample identification system

(b) Review physical and/or electronic records of sample chain of custody

(c) Review system of tracking which analysis and preparation methods a particular

sample has been subjected to while at laboratory

(d) Is the sample information retrievable with the SRID?

(e) Verify that access control is implemented to areas where IMS samples are

measured

Comments:

Required actions:



(a) Inspect sample preparation process: sample shall be transferred from the archive

container into the measurement cell according to the documented procedures

(b) Is loss of sample prevented during preparation?

(c) Estimate the transfer efficiency by comparison of xenon concentration reported

by the laboratory and by the station. Taking into account potential losses of gas

prior to arrival of the sample at the laboratory, the transfer efficiency shall be at

least 50%

(d) Cross-contamination between two subsequent samples shall be less than 0.3%

Analyse the sample immediately after the sample containing a spike

Comments:

Required actions:


9.5. Equipment

9.5.1. Records of Noble Gas Measurement System

(a) Review physical and/or electronic records: identification, manufacturer, type,

serial number, date of receipt, location, condition

(b) Check availability of manuals, instructions, maintenance record, history

Comments:

Required actions:


9.5.2. Calibration of Equipment

(a) Review physical and/or electronic calibration records

(b) Are details of calibration procedures and raw data stored to allow reconstruction

of calibration afterwards?

(c) Observe, if practical, a calibration check measurement

(d) Are there established criteria for acceptance of calibration and are they

implemented?


(e) Check records and use of calibration standards and reference materials

(f) Review process to ensure that equipment is calibrated, calibration status is

known, and equipment is functioning properly

Comments:

Required actions:


9.6. Management of Analysis Data


(a) Check if all spectral data related to IMS sample analysis are stored, transmitted

to the PTS with the analysis report and archived.

(b) Check storage of auxiliary measurements (pressure and temperature) used to

calculate results.

(c) Check how the computer(s) are protected with passwords and/or physical

security measures, such as security cards

(d) Review data storage backup system (CDs, etc.) and their access control

Comments:

Required actions:


9.6.2. Data Verification and Signature

(a) Review the procedure to ensure that data quality is verified before reporting

(b) Check that the hardware token for creating the signature is in use. (Validity of

signatures has to be checked in the messages coming into the IDC)

Comments:

Required actions:


9.7. Stable Xenon Volume Measurement

The calibration and recalibration procedures for the stable Xenon measurement are

documented and approved by the PTS. The documentation demonstrates that the

uncertainty of the calibrated instrument is better than 10%

Check if calibration gases are provided with a certificate, issued by the supplier of the

gas, stating the concentration of each relevant gas constituent and its uncertainty

Check if measurements of the room temperature sensor used for stable gas analysis

compare well with those from the PTS Testo temperature sensor

Review the uncertainty budget for the stable gas measurement

Check if the range of stable Xenon volume measurement is from 0.3 cm3 to 10 cm

3.


9.8. Nuclear Detection System and Analysis

(a) Review and document the detection method used by the laboratory

(b) Check detector(s): manufacturer, type, serial number, etc. Compare with

documentation. The assignment and use of CTBT detector codes (NNLxx_yyy)

must be confirmed

CTBT


Model

Number Serial Number

Year of

Acquisition

9.8.1. Detector Calibration (Procedure, Source, Checks)

(a) Review the procedures, algorithm and software used for the detector calibration

9.8.2. Detector Background and Gas Background Measurements

(a) Check background measurement records: background shall be acquired over a

period of at least six days prior to commencement of operations, with the same

settings as the sample measurement

(b) Discuss control measures for natural radioactivity indoors

(c) Inspect storage of any radioactive sources

(d) If the system shows memory effect greater than 0.3%, a gas background

measurement shall be carried out prior to sample measurement and under the

same conditions, in particular the same acquisition time

Comments:

Required actions:


9.8.3. Sample Measurement

(a) Examine sample diameter versus detector diameter, if relevant (e.g. for HPGe

detectors)

(b) Examine detector to sample geometry: it shall be well defined, i.e. the sample

shall always be in the same position during measurement

(c) Is a cumulative spectrum recorded every 24 hours as a default?

(d) Memory effect is <0.3%

Comments:

Required actions:



9.8.4. MDA Check

MDA measurement shall be performed under the same conditions as a sample measurement

with at least 3 cm3 of stable xenon gas in the measurement cell. Record that the sample

analysis process is according to documentation and certification requirements

(a) Acquisition time

(b) MDA achieved for routine analysis

(c) MDA achieved for in-depth analysis also

(d) Detector code

Comments:

Required actions:


9.8.5. Analysis Check

A spiked reference sample sent to the laboratory prior to the visit, is analysed during the visit.

Record that the sample analysis process is according to documentation and certification

requirements. Record the analysis results

(a) Receipt, ID, sample tracking, chain of custody

(b) Detector code

(c) Results are recorded in the table below

Nuclide

Certificate Laboratory

% Dev.

Zeta test

score

Comment

[Pass/Fail] Ref. No. Activity

(Bq)

uc

(%)

Activity

(Bq) ucA

(%)

Comments:

Required actions:



ANNEX I

GUIDANCE ON THE STRUCTURE AND CONTENT OF CTBT SPECIFIC

DOCUMENTATION FOR RADIONUCLIDE LABORATORIES

1. INTRODUCTION

It is a certification requirement for radionuclide laboratories that a quality system is

established and maintained for CTBT specific activities. This is to assure the quality of the

results of IMS sample analysis and compliance with the other CTBT related conditions, such

as those for reporting, sample and data security and confidentiality. A key element of any

quality system is the need to document both the quality system and related technical

procedures.

The documentation of the radionuclide laboratory will be reviewed as part of the certification

process carried out by the PTS. This documentation shall include the evidence necessary to

demonstrate that the certification requirements are fulfilled. It shall comprise a quality manual

and technical documentation for the IMS sample analysis. The documentation shall include a

list of cross references between the documentation and the related certification requirements.

If national accreditation exists, a copy of the certificate should be included.

The following sections provide guidance on the preparation of a CTBT specific quality

manual and technical procedures that would meet the certification requirements.

2. GENERAL GUIDANCE

2.1. Format of Documentation

The approach taken here is to divide the documentation into two sections: a quality manual

and technical documentation. The quality manual consists of two parts: the quality policy and

the associated quality system practices. These can be presented in the form of statements and

descriptions. The technical documentation is comprised of a description of the processes and

operational procedures for the IMS sample analysis, supporting procedures, and the related

forms. These shall be presented in enough detail to demonstrate compliance with certification

requirements. Depending on the approach preferred by the laboratory, it might be practical to

include these details within the CTBT specific quality manual itself, in separate CTBT

specific technical documentation, or by reference to another existing laboratory manual.

Figure 5 presents the optional approaches to documentation of the laboratory quality

management system for CTBT specific activities, in particular IMS sample analysis, taking

into account the existing documentation for other services provided by the parent

organization. The parent organization is intended to mean the whole organization, or a unit

within the organization, of which the radionuclide laboratory is part.

The laboratory has the option of preparing a comprehensive CTBT specific quality manual

and associated technical documentation which is represented by Option II in Figure 5.

Alternatively, the laboratory may choose to cross-reference existing quality system or


technical documentation. Options I and III would apply in that case and are discussed further

in Section 2.2 in relation to national accreditation schemes.

In assessing the radionuclide laboratory’s compliance with the certification requirements, all

documentation that is reviewed shall be written in English.

Further general guidance on the preparation of quality documentation can be obtained either

in the publication, ISO/TR 10013:2001, from the International Standards Organization or

from national accreditation bodies. The International Laboratory Accreditation Cooperation

(ILAC) http://www.ilac.org/home.html. provides a detailed reference list of guidance

documents from national accreditation bodies.

2.2. Existing National Accreditation

If the radionuclide laboratory or its parent organization is accredited under a national

programme, it is sufficient for the CTBT specific documentation to contain a cross reference

to the relevant part of the accreditation documentation.

The extent to which this cross-referencing would be acceptable will depend on the particular

international standard upon which the national accreditation is based and whether CTBT

specific laboratory activities are covered by the national scheme.

For example, accreditation to the current international standard for testing laboratories,

ISO/IEC 17025:2005, upon which the certification requirements are based, would imply

compliance with most or all management requirements. In addition, it would imply

compliance with a considerable portion of the technical requirements, with the exception,

perhaps, of those relating specifically to IMS sample analysis. Consequently, the

corresponding laboratory documentation would already exist and would not have to be

duplicated. Option III in Figure 5 is representative of this situation.

In the case of accreditation to ISO 9001, some parts of the documentation for general quality

management may also be applicable for the CTBT specific quality manual, even though this

standard does not encompass all the technical requirements for testing laboratories. Option I

in Figure 5 would most closely represent this particular case.

http://www.ilac.org/home.html


Figure 7. Approaches for radionuclide laboratory documentation for CTBT specific activities.

PO Quality Manual

Quality System Policy, Objectives,

Commitments

Quality System Generic Procedures

PO Quality Manual

Quality System Policy, Objectives,

Commitments


OPTION I OPTION III OPTION II

PARENT ORGANIZATION (PO) LEVEL

PO Operational Manual

Links to PO Quality Manual

Operational Procedures

RL CTBT SPECIFIC DOCUMENTATION


Links to PO Operational Manual

IMS Sample Analysis Description of

Processes; Operational Procedures

IMS Sample Analysis Forms and Records







Quality System Policy, Objectives and

Commitments





RADIONUCLIDE LABORATORY (RL) ORGANIZATION LEVEL

CTBT SPECIFIC OPERATIONS


3. GUIDANCE ON THE STRUCTURE AND CONTENTS OF THE CTBT

SPECIFIC QUALITY MANUAL

Section and Description of Contents

References

INF.96/

Rev.9

ISO/IEC

17025:

2005

3.1. Organization and Management Structure of the

Laboratory 4.1 4.2

3.1.1. Organizational Chart and Description, Place in any Parent

Organization 4.1 4.1.5

The overall structure of the laboratory to be presented in the

form of an organizational chart. Additional charts may need to

be provided to show the relationships between the CTBT

specific activities, other technical operations, the quality

management, support services and parent organization.

3.1.2. Responsibilities and Authorities 4.1, 5.2 4.1.5,

4.2.4

A statement of the responsibilities and authorities of key

personnel involved in CTBT specific work including the

identity of the staff member assigned to ensure compliance

with CTBT specific quality requirements (the quality

manager).

3.2. Scope of the Quality System 4.2 4.2

A statement of what activities the quality system pertains to;

Reference to any national or international accreditation for

services that the laboratory provides and links to the relevant

documentation for that accreditation;

Reference to the certificate of the national or international

accreditation.

3.3. Quality Policy Statement 4.3 4.2.2

A quality policy statement for CTBT specific activities issued

with the authority of the chief executive of the parent

organization:

The laboratory management’s commitment to quality of

service and to good scientific practice.

A statement of the laboratory’s standard of service.

A statement of the objectives of the quality system and a

description of how the laboratory will achieve these objectives

in terms of the policy, structure and overall procedures.

A description of the quality system in regard to the policies,

systems, programmes and procedures in place to assure the

quality of CTBT specific services and analyses.

A statement giving a commitment that all personnel involved

with CTBT specific activities are familiar with and implement

the quality system, as described in the quality manual.


3.4. References to Technical Documentation 4.4 –

An outline of the structure of the CTBT specific technical

documentation including reference to the procedures for IMS

sample analysis and associated forms and records. These

procedures may form part of the CTBT specific quality

manual or exist as a separate technical documentation.

3.5. Quality System Practices and Instructions 4.2-4.6 4.2.3

In this section, where a description of the procedures is called

for, the level of detail provided should be sufficient to enable

a clear understanding of the process, who is responsible, how

and when it is done, and the link or interface to other related

activities or procedures. Reference should be made to existing

documentation, where appropriate, to avoid duplication and

reduce complexity. It is not necessary to provide a

comprehensive procedure so long as the activity can be

adequately described in the statement. A flow chart of the

process may be a good alternative in some cases.

3.5.1. Control of Records 4.5 4.12

3.5.1.1. Quality System Records

The procedures for establishing and maintaining quality

system records, such as the findings and results of internal

audits and management reviews, the records of control of non-

conformance, and corrective and preventive actions. These

procedures include identification of records, collection,

indexing, access, filing, storage, disposal and maintenance of

security and confidentiality.

3.5.1.2. Technical Records Related to IMS Sample Analysis

Details of the procedures in place to maintain the technical

records arising from IMS sample analysis including sample

receipt, chain of custody, sample measurements, data

processing and analytical reports and communications with

the PTS. These records should include any significant

observations during each stage, the original and derived data,

calibration records, and copies of reports, staff records and

identity of personnel responsible for each stage of the process

or responsible for checking results and reports.

3.5.1.3. Storage of Technical Records

Details of the location, method of storage and retrieval of

technical records, evidence that the security and physical

integrity of records can be maintained over the required period

of time.

3.5.1.4. Recording and Alterations to Records

Details of procedures to ensure that observations, data and

calculations are recorded at the time they are made and can be

related to a specific task and to a particular member of staff.

The means by which changes or mistakes to records are

identified and corrected.


3.5.2. Document Control 4.5 4.3.1 –

4.3.3

A description of the processes or procedures for approval,

issue, availability, identification, review, changes or

amendments and removal of invalid or obsolete documents.

This description includes the control of documents maintained

electronically.

3.5.3. Review of Terms and Reference and Contracts 4.6 4.4.1 –

4.4.5

Description of the procedures for the review of contracts

related to CTBT activities, to ensure that there is an

understanding and documentation of the client’s requirements,

the laboratory’s resources are available and that the

appropriate methods are to be used. The means of recording

the contract reviews and the method for implementing

changes to a contract and notifying the client of any deviation

from a contract.

3.5.4. Policy of Subcontracting 4.6 4.5.1 –

4.5.4

A statement not to subcontract any parts of the IMS sample

analysis without the prior and written approval of the PTS,

with an additional statement to ensure that, if permitted, any

subcontractor used would have to meet the certification

requirements and that the laboratory would be responsible for

any subcontracted work.

3.5.5. Purchasing of Services and Supplies 4.6 4.6.1 –

4.6.3

A statement regarding the policy and procedures for the

selection, purchasing, receipt and storage of services and

supplies related to IMS sample analysis. Reference to

procedures to verify that all materials that affect the data

quality comply with specifications, prior to their use and that

technical data and information in documents accompanying

supplies are reviewed and approved for use.

3.5.6. Service to the CTBTO 4.6 4.7

A statement that the laboratory shall cooperate with the PTS

to clarify requests and allow the monitoring of the

laboratory’s performance, and in addition will maintain good

communications with the PTS regarding IMS sample analysis

and related CTBT specific activities.

A further statement that policies and procedures are in place

to avoid participation in activities that, potentially, might

conflict with CTBT functions or would diminish the

laboratory’s technical competence, impartiality, scientific

judgement and integrity.


3.5.7. Resolution of Complaints 4.6 4.8

Statement regarding the policy and procedures in place to

resolve complaints from the PTS and other parties regarding

work carried out under IMS contracts and to ensure that

records of complaints and their resolution are maintained.

3.5.8. Control of Nonconformity 4.6 4.9

A statement regarding the policy and procedures that are

implemented when work or results do not comply with the

established procedures or the requirements of the PTS. This

should include a definition of responsibilities, an evaluation of

the significance of the nonconformity, the decision process

and the initiation of corrective actions, and notification of the

PTS.

3.5.9. Corrective Action 4.6 4.10

A statement on the policy and procedures in place to

implement corrective action, including:

the process to determine the cause of any problem;

the selection and implementation of corrective actions;

monitoring the outcomes to ensure effectiveness of the

actions;

auditing of the areas affected to ensure compliance with the

established quality system.

3.5.10. Preventive Action 4.6 4.11

A statement regarding the planning process for initiating

improvements, for identifying potential problems and for the

development and implementation of action plans to reduce the

likelihood of problems.

3.5.11. Internal Audits 4.6 4.13

A description of the internal process for regular auditing of

the on-going compliance of activities associated with IMS

analyses with the quality system and established procedures.

The description shall include identification of the staff

members responsible for planning and conduct of the audit,

corrective actions to be taken, audit record-keeping and

process for the conduct of follow-up audits.

3.5.12. Management Reviews 4.6 4.14

A description of the procedure for the review of the

laboratory’s quality system, and technical procedures for IMS

sample analysis, by management, to ensure the effectiveness

of the system and identify the need for improvements. The

scheduling, and objectives and contents of the review shall be

identified in the statement, as well as the process for recording

and implementing actions arising from the review.


4. GUIDANCE ON THE STRUCTURE AND CONTENTS OF THE CTBT

SPECIFIC TECHNICAL DOCUMENTATION

This section deals with technical documentation requirements for certification. The technical

documentation includes a description of the processes involved in IMS sample analysis and

related CTBT specific activities, information on personnel, laboratory facilities and

infrastructure, specific operational procedures where relevant, or references to existing

documented procedures.

Section and Description of Contents

References

INF.96/

Rev.9

ISO/IEC

17025:

2005

4.1. Preparedness 5.1 –

A description of the processes in place to ensure the

preparedness of the laboratory to receive and expedite the

analysis of IMS samples to meet the CTBT specific analytical

and reporting requirements. The following items are to be

covered in the statement:

the steps taken to ensure the sample receipt;

the commencement of analysis within the time frame

required;

a description of the on-call system in place for the relevant

laboratory personnel;

the messaging system in place to notify staff of the sample

dispatch;

the system in place to send the appropriate messages to the

PTS.

A link to specific operational procedures, forms and records

should be provided where appropriate.

4.2. Personnel 5.2 5.2

4.2.1. Authorization 5.2 5.2.5

A statement that management has authorized certain

laboratory personnel to perform specific activities related to

the CTBT specific services, including sample handling and

preparation, operation of particular types of equipment,

issuing of reports and messages and provision of

interpretations and expert opinions.

The statement should identify any potential conflicts of

interest with other laboratory functions for these personnel

and how these conflicts of interest would be avoided.

4.2.2. List of Personnel 5.2 5.2.3

A list should be provided of the names, qualifications and

experience of authorized personnel carrying out specific

CTBT related activities or having access to IMS samples and

data.


4.2.3. Objectives for and Assurance of Competence 5.2 5.2.2

A statement that the authorized personnel are familiar with

and have the appropriate level of competence to carry out the

various procedures for CTBT related services.

A description of the policy and procedures that are

implemented:

to identify training needs;

to conduct a training programme to maintain the level of

competence of personnel to carry out CTBT services;

to provide proper training of new personnel in CTBT specific

procedures.

4.2.4. Job Descriptions and Authorizations 5.2 5.2.4

A list of individual job descriptions for personnel involved in

CTBT analytical services.

A description of the appropriate level of supervision of

personnel for the performance of CTBT specific activities.

4.2.5. Job Records 5.2 5.2.5

A description of the record system for qualifications, skills,

training and experience of authorized personnel.

4.3. Environmental Conditions 5.3 5.3

4.3.1. Appropriate Facilities and Maintenance

A description of the laboratory areas that house equipment

and facilities for the processing and measurement of IMS

samples, together with the associated infrastructure such as

power, light, local communications and safety features. An

assurance should be given either that key aspects of these

facilities do not compromise the quality of the analytical

results, or measures are in place to overcome any deficiencies.

4.3.2. Environmental Monitoring and Control

A description of the monitoring, control and recording of

environmental conditions and an assurance that the ambient

conditions will not jeopardize the quality of the analytical

results or the performance of equipment. Reference should be

made to specific operational procedures and records.

4.3.3. Prevention of Cross-Contamination

An assurance that other activities carried out by the

organization will not compromise the integrity of IMS

samples, influence IMS sample management or affect

analytical quality. A statement that the location of facilities

and the conduct of procedures ensure that the use of

radioactive sources cannot lead to cross-contamination with

IMS samples.


4.4. Analysis Methods and Validation of Methods 5.4 5.4

4.4.1. Appropriate Methods 5.4.1 5.4.1 –

5.4.2

A statement to provide assurance that all operational

procedures for calibration and sample analyses are appropriate

for IMS samples. An assurance that the methods are based on

either the latest international or national standards, where

available. If laboratory developed or non-standard methods

are used, they should be properly validated.

4.4.2. Documentation of Methods 5.4.1 5.4.1. –

5.4.2.

A statement that all operational procedures and instructions in

use for CTBT related activities are documented and that the

current versions are available to relevant personnel.

4.4.3. Documentation of Software 5.4.1 5.4.1 –

5.4.2

A statement that software in use for sample analysis is

appropriately documented either by laboratory or

manufacturers’ documentation and that only the current

version is made available for use.

4.4.4. Validation Procedures for Methods 5.4.2 5.4.5

A description of the validation process for non-standard or

laboratory designed methods. Reference should be made to

the specific validation procedure and the laboratory records

detailing the results and conclusions of the validation tests.

4.5. Uncertainty of Measurement 5.4.3 5.4.6

A description of the process for estimating the combined

uncertainty of an analytical result that ensures that all

significant components of the measurement uncertainty are

taken into account in the overall estimate. The description

should include a reference to the relevant operational

procedures.

4.6. Equipment 5.5 5.5

4.6.1. Appropriate for IMS Sample Analysis 5.5.1 5.5.1 –

5.5.2

A statement that all equipment used for IMS sample analysis

is appropriate for the purpose. Reference to the detailed list of

equipment, including manufacturer specifications.

4.6.2. Authorized Personnel 5.5.1 5.5.3

A statement that only authorized personnel will operate

equipment for IMS sample analysis, together with an

assurance that only current versions of instructions on the use

and maintenance of equipment are available to the appropriate

personnel.

4.6.3. Equipment Records 5.5.1 5.5.4 –

5.5.5

A description of the maintenance of records for the specific

items of equipment used for IMS sample analysis. This

description should include reference to specific procedures

and forms for maintenance of equipment records.


4.6.4. Maintenance of Equipment 5.5.1 5.5.6 –

5.5.7

A description, including reference to specific operational

procedures, for the routine and unscheduled maintenance of

equipment. This description should also include the process

for scheduling and keeping records of maintenance

performed, with reference to specific procedures.

4.6.5. VSAT 5.5.3 –

A description of the interface with the GCI. Reference should

be made to the specific operational procedures. Information

should also be provided on the procedures in the case of

VSAT failure.

4.7. Measurement Traceability 5.6 5.6

4.7.1. Calibration Programme 5.6.1 5.6.1

A description of the programme for the calibration of

equipment before being put into service and for the regular

verification of the calibration status. This description is to

include details of the scheduling, maintenance of calibration

records, traceability of measurements and uncertainty of

calibration results. Specific operational procedures and forms

for maintenance of calibration records should be cross-

referenced.

4.7.2. Reference Standards and Materials 5.6.2 5.6.2

A description of the program to maintain the calibration of

reference standards and materials, including details of the

traceability of the primary and working standards and

reference materials and schedules for intermediate checks of

these sources. Reference to relevant operational procedures

and forms for record keeping.

4.8. Procedures for each IMS Sample Category 5.7 5.4.1 –

5.4.3

A statement that operational procedures are provided for the

processing and analysis of each sample type in the IMS

categories identified in document CTBT/PTS/INF.96.

4.9. Sample Management 5.8 5.8

4.9.1. Receipt and Dispatch 5.8.1 5.8.1 –

5.8.4

A description of the processes in place for the receipt and

dispatch of IMS samples, including on-call arrangements and

the transfer of responsibilities, and the messaging

requirements. Reference to specific operational procedures.

4.9.2. Security 5.8.2 5.8.1 –

5.8.4

A description of the processes, including references to

relevant operational procedures, to ensure the integrity of the

sample and to control access to areas where samples are

received, processed and stored.


4.9.3. Laboratory Sample Tracking 5.8.3 5.8.1 –

5.8.4

A description of the process to establish and maintain the

sample chain of custody, and to record and track samples

throughout the IMS analysis. Reference is to be provided to

relevant operational procedures and forms for sample

tracking.

4.9.4. Handling of Samples 5.8.4 5.8.1 –

5.8.4

A description of the processes in place to handle and prepare

IMS samples for analysis, with reference to the relevant

operational procedures.

4.10. Quality Assurance and Data Verification 5.9 5.9

4.10.1. Quality Assurance of Analysis Results 5.9.1 5.9

A description of the programme in place for assuring the

quality of results, which includes the following actions:

Background and blank measurements

Calibration checks

Participation in intercomparison and proficiency test exercises

Analysis of certified reference materials

Re-testing of samples

The description of the programme should include the

recording of QA results and review of QA data by trend

analysis and other relevant statistical tests.

Reference should be provided to the documented operational

procedures and associated forms, along with reference to

procedures for the establishment and maintenance of QA

records.

4.10.2. Data Verification 5.9.2 4.12.2,

5.4.7

A description of the process for the review of data entry,

transcription and other recording actions to check for errors

prior to reporting. Relevant operational procedures should be

referenced.

4.11. Management of Analysis Data 5.10 5.4.7

A statement providing an assurance that all data from IMS

sample analysis are stored securely, that the confidentiality of

the CTBTO is assured, with access to data records restricted

to authorized personnel. A description of the process to

maintain a log of the steps taken by relevant personnel during

the analysis. Reference should be made to the relevant

procedures.

4.12. Reporting 5.11 5.10

4.12.1. Contents of the Report and Reporting Time 5.11.1 5.10.1

A description of the process for the preparation of reports with

the contents and scheduling required by the PTS. Reference to

relevant operational procedures and report specifications is to


be provided.

4.12.2. Data and Report Formats 5.11.2 –

A description of the formatting of messages generated for data

and reports transmitted to the PTS, including reference to

specific operational procedures and formats.

4.12.3. Data Authentication 5.11.3 –

A statement that data authentication is implemented in

accordance with the certification requirements and the

security of data transfer from the measurement systems to the

GCI is assured. Reference to relevant operational procedures.

4.13. Messages 5.12 –

4.13.1. Communications Protocols 5.12.1 –

A description of the procedures for communication with the

PTS, including confirmation that the protocol requirements

are met.

4.13.2. Communication Software 5.12.2 –

A statement regarding the mail server software used for

communication with the PTS by email for both data

transmission and receipt.

4.13.3. Laboratory Message Format and Content 5.12.3 –

Statement that the laboratory can handle the message types

specified by the PTS for IMS sample analysis.

5. EXAMPLE OF THE FORMAT AND CONTENT FOR OPERATIONAL

PROCEDURES

5.1. Introduction

In general, an operational procedure is a description of the manner in which an activity is

carried out and will contain statements and/or instructions on:

What is to be done?

Why it is to be done?

Who is responsible for getting it done?

How, when and where it is done?

What resources in terms of facilities, equipment, etc. are to be used?

What links exist to other activities?

Any other information required to carry out the activity?

One objective of a procedure is to describe how the quality system is implemented within the

organization and therefore will be related to items or commitments outlined in the quality

manual. Alternatively, a procedure will be the documented basis upon which the laboratory

performs its testing and analytical activities. In this case, the procedure will take the form of

an analytical method and describe in working detail how a particular sample analysis is

carried out.


5.2. Typical Structure of a Procedure

The structure and actual content of the documentation of operational procedures will depend

on each laboratory’s needs and particular circumstances. The example given here is intended

to give a guide to the main components and it may not be necessary to include all these

components for each activity.

The degree of detail will depend on the experience, skill level and training of the particular

person required to perform the activity. As a general rule, operational procedures and methods

should be documented in sufficient detail that a person with a level of technical training and

experience appropriate to the task can carry out the procedure without having to rely on

additional instruction or help. In any case the level of detail shall be such as to provide the

PTS documentation review team with confidence that certification requirements are fulfilled.

The documentation should also give confidence in the reproducibility of the method and the

traceability of the results.

5.2.1. Identification

The procedure should be given a brief title that will indicate its purpose and uniquely identify

its place in the laboratory documentation. The identification should include the following

pieces of information:

Title

Reference No. for document control

Version

Issue date

Signature of authorized staff member responsible for maintaining quality

documentation.

5.2.2. Purpose of the Procedure

A brief statement of the purpose of the procedure should be provided, but this may not be

necessary if the procedure is simple and the purpose is obvious from the title or the other

sections.

5.2.3. Scope

The scope of application of the procedure should be given, indicating the sections, personnel

or the part of the process to which the procedure applies. Again this section may not be

necessary for less complex procedures and could be incorporated in the title.

5.2.4. Referenced Documents Relevant to the Procedure

Reference can be made to other documents that are linked to, or otherwise relate to, this

procedure. This could include:

Cross-references to other quality manual procedures, work instructions or test methods

ISO and other quality procedures


National or international standards

Technical references applicable to the procedure

Software documentation

Manufacturer’s instructions.

5.2.5. Specific Definitions and Abbreviations

It may be useful to define a word that has a special meaning, a technical term or an activity to

provide a clearer understanding for the reader.

5.2.6. Responsibilities

This section can be used to identify, by job title or description, the person responsible for

implementing the procedure or parts of it. An alternative is to identify the areas of

responsibility within the stepwise procedure itself.

5.2.7. List of Equipment and Other Materials to be Used

For certain procedures and methods it would be appropriate to provide a list of equipment and

specific materials, etc., to be used in the procedure.

5.2.8. Stepwise Procedure

This section is the most important as it describes actions and activities to be performed. The

instructions should provide a clear, stepwise account of the activity at each stage.

5.2.9. Forms and Records to Be Used in the Procedure

A list should be given of all forms and records to be used or generated in the procedure. These

include forms, log sheets, checklists, report sheets, data sheets etc., as well as those forms and

records retained as electronic versions. Generally, it is preferable that copies of all forms and

records that relate to a particular procedure should be attached as an appendix to that

procedure. However, in some instances, it may be more convenient to group all forms as an

appendix to the technical documentation.

5.2.10. Report Format

For those procedures that generate an analysis report, the format of the report should be given

in this section.

6. IMS SAMPLE ANALYSIS: REQUIRED PROCEDURES

The analysis of IMS samples by high resolution gamma ray spectrometry requires

documented procedures to describe the various activities in several stages:

Sample management

Sample preparation

Sample measurement


Data analysis

Reporting

QA

Messaging.

The flow chart in Figure 6 presents the various procedures for the analysis of IMS samples by

gamma ray spectrometry and the associated links between the procedures.

Table 6 lists the documented procedures that are required specifically for IMS sample

analysis. Depending on the particular laboratory and the activity, it may be more practical to

combine several related procedures into a single documented operational procedure.


Figure 8. Schematic representation of the process of IMS sample analysis.

Prepare

sample

Sample

preparation

necessary?

Quality

assurance

PTS notifies

laboratory of sample

dispatch

Receive

sample at

laboratory

Measure

sample

Analyse data

Prepare for

sample receipt

Complete

sample receipt

logs

Analysis

report (RLR)

Measurement

traceability

Prepare

report

YES

NO

Measure

intercomparison

samples

Verify data

entries

Calibrate

detector

Measure

reference

standards

Advise PTS of

sample receipt

Transmit

report to

PTS


Table 6. Specific Operational Procedures Required for IMS Sample Analysis

Analysis Stage CTBT/

PTS/

INF.96/

Rev.9

Reference

Specific Procedure

Sample Management

Preparedness 5.1 Notification of staff for sample dispatch

Receipt and dispatch 5.8.1 Sample receipt at laboratory

Sample dispatch to PTS

Sample security 5.8.2 Maintenance of sample security

Chain of custody 5.8.3 Recording and tracking samples

Sample handling 5.8.4 Preliminary monitoring of sample activity

Sample Preparation

Sample preparation 6.1 Sample splitting

Sample preparation for measurement

Sample Measurement

Spectral acquisition 6.2 Gamma ray spectrometry acquisition

Background 6.7 Measurement of detector background

Measurement of blank filters

Measurement

traceability

5.6.1,

5.6.2, 6.4

Calibration of detectors for efficiency and energy

Maintenance of calibration standards

Preparation of standard sources

Detector performance evaluation

Data Analysis

MDA calculation 6.5 Calculation of Ba-140 MDA

Data management 5.10 Maintenance of analytical data records

Uncertainty 6.9 Estimation of uncertainties in analysis results

Reporting

Report preparation 5.10, 5.11,

6.10.2

Preparation of analysis reports

Report transmission 5.11.2,

5.11.3,

6.10.1

Transmission of reports to PTS

Data authentication

Quality Assurance

QA of analysis data 5.9.1 Performance of intercomparison and proficiency test

exercises

Analysis of certified reference materials

Record maintenance 5.9.1 Maintenance of QA records

Data verification 5.9.2 Review of data entry, transcription and reporting

Communications

Communication

protocols

5.12.1 Communication with PTS

Messaging 5.12.3 Formatting of messages

Related Operations

Method selection and

validation

5.4 Validation of non-standard methods


Table 6 (cont.)

Analysis Stage CTBT/

PTS/

INF.96/

Rev.9

Reference

Specific Procedure

Facility operations 5.3 Monitoring of environmental conditions

Record maintenance

Cross-contamination control

Access control

General occupational health and safety

Equipment operations 5.5.1 Purchasing

Consumables storage

State of health monitoring

Equipment acceptance testing

Equipment functionality testing

Record keeping

Equipment

maintenance

5.5.1,

5.5.3

Routine equipment maintenance

Unscheduled maintenance

Spare part storage and records

Maintenance record keeping

VSAT and GCI interface maintenance

7. FORMS AND RECORDS FOR IMS SAMPLE ANALYSIS

Forms and records are an integral part of the documentation of the quality system. These may

be maintained as a hard copy or on electronic media. Items typically belonging to this

category are forms for data recording or sample chain of custody, equipment maintenance

records, certificates, general work sheets, description of algorithms, message formats,

reference lists and data sources.

Normally these items would be directly related to a specific operational procedure, and should

be integrated with that particular procedure. Otherwise, they should be clearly referenced

within the procedure.

Forms need to be uniquely identified and controlled in the same way as other quality system

documentation. The term record refers to a completed form, which then becomes a quality

record, or a technical record relating to a particular analysis. These records, therefore, must be

stored and maintained in accordance with quality system requirements. Records are an

important part of internal auditing and necessary to reconstruct the processing of a particular

sample analysis.

The list in Table 7 provides an indication of the forms, records and technical information that

should be provided in the documentation for IMS sample analysis. This list is additional to the

forms and records related to particular generic procedures required in the CTBT specific

quality manual, such as document control, audit schedules and reports and organizational

charts.


Table 7. Forms, Records and Technical Specifications to be Provided in the CTBT

Specific Technical Documentation

Analysis Stage CTBT/PTS/

INF.96/

Rev.9

Requirement

CTBT/PTS/

INF.96/

Rev.9

Reference

Forms and Records

Sample

management

Preparedness 5.1 Notification of staff for sample

dispatch

Staff roster for IMS analysis

Staff contact details for sample

receipt/dispatch

Receipt and

dispatch

5.8.1 Logs for sample receipt at laboratory

Logs for sample dispatch for return to

PTS

Sample

security

5.8.2 Sample security records

Chain of

custody

5.8.3 Sample recording and tracking

Sample

handling

5.8.4 Preliminary monitoring of sample

activity

Sample preparation Sample

preparation

6.1 Sample splitting forms

Sample preparation forms

Sample

measurement

Spectral

acquisition

6.2 Gamma ray spectrometry acquisition

log

Nuclear data lists

Spectral file formats

Spectral analysis software description

Background 6.7 Measurement records for detector

background

Measurement records for blank filters

Measurement

traceability

5.6.1, 5.6.2,

6.4

Calibration source certificates

Maintenance of calibration standards

Preparation of standard sources

Record of detector performance and

state of health results

Data analysis MDA

calculation

6.5 Algorithms for calculation of Ba-140

MDA

Data

management

5.10 Analytical data records

Uncertainty 6.9 Algorithms for the estimation of

uncertainties in analysis results

Reporting Report

preparation

5.10, 5.11,

6.10.2

Analysis report formats

Report

transmission

5.11.2,

5.11.3, 6.10.1

Transmission of reports to PTS


Table 7 (cont.)


INF.96/

Rev.9

Requirement

CTBT/PTS/

INF.96/

Rev.9

Reference

Forms and Records

Quality assurance QA of analysis

data

5.9.1 Report forms for intercomparison and

proficiency test exercises

Schedules for analysis of certified

reference materials

Reference material certificates

Record

maintenance

5.9.1 QA records for detector system, for

other equipment, performance charts,

etc.

Data

verification

5.9.2 Forms for review of data entry,

transcription and reporting

Method

selection and

validation

5.4 Validation test results

Communications Communica-

tion protocols

5.12.1 Communication with PTS

Messaging 5.12.3 Message formats

Related operations

and specifications

General CTBT

specific

operations

5.2 List of key staff with contact details

List of all procedures and related

forms for CTBT specific activities

Facility

operations

5.3 Forms for monitoring of

environmental conditions

Access control records

General occupational health and

safety forms

Laboratory floor plan for areas used

for CTBT specific activities

Equipment

operations

5.5.1 Purchasing forms

List of suppliers

List of consumables in storage

State of health monitoring report

forms

Equipment acceptance test report

forms

Equipment functionality schedules

and test results

Equipment

maintenance

5.5.1,5.5.3 Routine equipment maintenance

report forms

Unscheduled maintenance report

forms

Spare part storage and records

Maintenance schedules and record

keeping

VSAT and GCI interface maintenance

schedules and records


Table 7 (cont.)


INF.96/

Rev.9

Requirement

CTBT/PTS/

INF.96/

Rev.9

Reference

Forms and Records

Equipment

specifications

5.5.1 Inventory of equipment, including

specifications, manufacturer’s details,

including:

Name of the item of equipment

Manufacturer

Type, ID and serial number, other

identification

Dates received and placed into service

Current location

Condition when received (e.g. new,

used, reconditioned)

Copy of manufacturer’s instructions,

or reference to their location

Dates and results of calibrations

and/or verifications, and dates of next

calibration or verification

Details of maintenance performed to

date and planned for future

History of any damage, malfunctions,

modification or repair

Detector specifications (both

manufacturer’s and measured) –

CTBTO detector code, detector type,

efficiency, energy resolution at

reference energies, peak shape at

reference energies, etc.

Software specifications

Staffing Staff records – position,

qualifications, experience,

authorizations

Staff training records and reports

Bibliography Bibliography and general reference

list of literature used for IMS sample

analysis


8. REFERENCES AND BIBLIOGRAPHY FOR ANNEX I

European Standards Institution. General Criteria for the Operation of Testing Laboratories.

European Standard EN 45001, 1989.

International Organization for Standardization. General Requirements for the Competence of

Testing and Calibration Laboratories. ISO/IEC Guide 25:1990.

International Laboratory Accreditation Cooperation: Guidance Documents Available from

Accreditation Bodies for the Preparation of Laboratory Quality Manuals. ILAC-14, 1996

(http://www.ilac.org).

International Organization for Standardization: General Requirements for the Competence of

Testing and Calibration Laboratories. ISO/IEC 17025:1999.

International Organization for Standardization. Guidelines for Developing Quality Manuals.

ISO 10013:1998.

Preparatory Commission for the Comprehensive Nuclear-Test-Ban Treaty Organization.

Certification of Radionuclide Laboratories. CTBT/PTS/INF.96/Rev.3, 2001.

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