1Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 1

Calibration and Measurement Capability of Gas Analysis

Calibration and Measurement Calibration and Measurement Capability of Gas AnalysisCapability of Gas Analysis

ByBy

Ratirat Ratirat SinweeruthaiSinweeruthai

Gas Analysis Laboratory

Department of Chemical Metrology and Biometry

National Institute of Metrology (Thailand)

May 25, 2009

NIMT, Thailand

Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 2

Gas Analysis LaboratoryGas Analysis LaboratoryGas Analysis Laboratory

As of May 2009

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Gas Analysis SectionGas Analysis SectionGas Analysis Section

GC : TCD, FID

SO2 Analyzer

FT-IR

Nox Analyzer

O2 Analyzer

CO Analyzer

ND-IR Analyzer

Micro GC

Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 4

Gas Weighing SectionGas Weighing SectionGas Weighing Section

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Gas Filling SectionGas Filling SectionGas Filling Section

Cleaning System for Gas CylinderCleaning System for Gas Cylinder Gas Filling System Gas Filling System

Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 6

11stst stage of traceability scheme on calibration at NIMTstage of traceability scheme on calibration at NIMTSI

CERI

Japan Gas

Company

NIMT

JapaneseUsers

Thai Gas Companiesor Users

NMIJ

primary

Secondary

calibration

calibration

Certification(Relative Uncertainty1%2%)

Transfer

Secondary

Working

High-purity gasCRM

comparison

(Firstly, for O2/N2 mixtures around 20% and CO/N2 mixtures 5 ppm 100 ppm)

jcss Certification, within 1%

JCSS Certification, 1%2% Working

calibration

Accreditation of ISO/IEC 17025

Secondary

Working

Working

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Certified Standard Gas and CalibrationCertified Standard Gas and CalibrationCertified Standard Gas and Calibration

Uncertainty : within 1%

CR

M

WR

M

WR

M

RM

O2 Analyzer

CO Analyzer

High Accuracy Low Accuracy

Uncertainty : within 1%

It is developing the method for reducing the uncertainty

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Method for Certified Standard GasMethod for Certified Standard GasMethod for Certified Standard Gas

Uncertainty : within 1%

CR

M

QC

cyl

ind

er

WR

M(s

am

ple

)

QC

cyl

ind

er

QC

cyl

ind

er

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Accreditation ScopeFor Certify and Calibration

Accreditation ScopeAccreditation ScopeFor Certify and CalibrationFor Certify and Calibration

Calibration O2 Analyzer and Certified O2 in N2

Range: 0.05 - 0.30 mol/mol

Uncertainty (k=2) : 0.25 % relative

WR

M

N2

99

.99

5%

O2 Analyzer

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Accreditation ScopeFor Certify and Calibration

Accreditation ScopeAccreditation ScopeFor Certify and CalibrationFor Certify and Calibration

Calibration CO Analyzer and Certified CO in N2

Range: 5 - 25 mol/molUncertainty (k=2) : 0.80 % relative

Range: 25 - 100 mol/molUncertainty (k=2) : 0.45 % relative

WR

M

N2

99

.99

5%

CO Analyzer

6Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 11

Quality Systems that need to be fulfilled according to Gas Analysis Laboratory

Quality Systems that need to be fulfilled Quality Systems that need to be fulfilled according to Gas Analysis Laboratoryaccording to Gas Analysis Laboratory

Quality System ISO/IEC 17025:2005

Gas Analysis Production according to ISO 6143

Analysis SectionAnalysis SectionAnalysis Section

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Service Route for O2 in N2 Service Route for OService Route for O22 in Nin N2 2

First Stage:First Stage:Service Type: Calibration and Certified Gas Mixture (CRM)Range: 0.05 mol/mol to 0.30 mol/mol Analysis Technique: Paramagnetic Oxygen AnalyzerService Time: April 2008Certified Reference Materials: CERI (u(x)= 0.2%rel)Bilateral Comparison: NMIJ, August 2008 (Draft B)Accreditation Body: IA Japan (In Process)

Degrees of equivalence plot

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Service Route for O2 in N2Service Route for OService Route for O22 in Nin N22Second Stage:Second Stage:

Service Type: Preparation Primary Reference Mixture (PRM)Certified Gas Mixture (CRM)Calibration

Range: 100 mol/mol to 0.30 mol/molAnalysis Technique: GC-TCD & Paramagnetic Oxygen AnalyzerService Time: within 2009

Third Stage:Third Stage:Service Type: Preparation Primary Reference Mixture (PRM)

Certified Gas Mixture (CRM)Calibration

Range: 1 mol/mol to 100 mol/mol Analysis Technique: GC-PDHIDComparison : NMiService Time: May 2010

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Service Route for CO2 in N2 Service Route for COService Route for CO22 in Nin N2 2 First Stage:First Stage:

Service Type: Preparation Primary Reference Mixture (PRM)Certified Gas Mixture (CRM) Calibration

Range: 100 mol/mol to 0.14 mol/mol Analysis Technique: GC-FID with MethanizerService Time: 2010

Second Stage:Second Stage:Service Type: Preparation Primary Reference Mixture (PRM)

Certified Gas Mixture (CRM)Calibration

Range: 1 mol/mol to 100 mol/mol Analysis Technique: GC-FID with MethanizerComparison : NMiService Time: 2011

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Service Route for CO in N2Service Route for CO in NService Route for CO in N22 First Stage:

Service Type: Calibration and Certified Gas Mixture (CRM)Range: 5 mol/mol to 100 mol/molAnalysis Technique: ND-IR & GC-FID with MethanizerService Time: April 2008Inter-comparison: CCQM

Second Stage:Service Type : Preparation Primary Reference Mixture (PRM)

Certified Gas Mixture (CRM)Calibration

Range: 100 mol/mol to 0.14 mol/mol Analysis Technique: ND-IR & GC-FID with MethanizerBilateral Comparison: NMiService: 2011

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First Stage: Inter-comparison CO in N2

Range: 5 mol/molAnalysis Technique: ND-IR Period: May 2008Certified Reference Material: CERIOrganization: CCQM Status: Draft AAccreditation Body: IA Japan Status: In Process

NIMT

Degrees of equivalence plotGC-FID ND-IR FT-IR

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Calibration ServicesCalibration Services CO AnalyzerCO Analyzer OO22 AnalyzerAnalyzer

Certified Reference MaterialsCertified Reference Materials CO in NCO in N22 OO2 2 in Nin N22

Training CourseTraining Course Planning to open in 2009Planning to open in 2009

Calibration, Certification and TrainingCalibration, Certification and TrainingCalibration, Certification and Training

Primary reference materials Primary reference materials O2 in N2 in range of 1 % to 25 % O2 in N2 in range of 1 % to 25 %

Planning to sell within 2009Planning to sell within 2009

Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 18

22ndnd stage of traceability scheme on calibration at NIMTstage of traceability scheme on calibration at NIMT(planned)(planned)SI

Japan Gas

Company

NIMT

JapaneseUsers

Thai Users

NMIJ

Preparation/Calibration

Secondary

Secondary

Working

High-purityCRM

Thai Gas

Company

Working

Primary Gas prepared by NIMT

calibration

CERI primary

Secondary

calibrationcomparison

jcss Certification, within 1%

JCSS Certification, 1%2%

Secondary

NIMT Certification

Gas Manufacture Certification

Transfer

calibration

Accreditation of ISO Guide 34

WorkingWorking

comparison

NMIs

10

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GAS Reference MaterialsGAS Reference MaterialsGAS Reference Materials

Vehicle emission gas

Stack emission gas

Plan to produce in 2009-2012

Natural Gas

Ethanol in N2

Plan to produce in 201x

Plan to produce in 2011-201x

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Quality Systems that need to be fulfilled according to Gas Analysis Laboratory

Quality Systems that need to be fulfilled Quality Systems that need to be fulfilled according to Gas Analysis Laboratoryaccording to Gas Analysis Laboratory

Quality System ISO/IEC 17025:2005

Gas Analysis Production according to ISO 6142 and ISO 6143

Production of Reference Material according to ISO Guide 34

11

Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 21

33rdrd stage of traceability scheme on calibration at NIMTstage of traceability scheme on calibration at NIMT(planned)(planned)SI

CERI

Japanese Gas

Company

NIMT

JapaneseUsers

Thai Users

NMIJ

primary

Secondary

calibration

Secondary

Secondary

Working

High-purity gasCRM

Thai Gas

CompanyWorking

primary

calibration

SI

High-purity gas, the purity (impurities) is determined by NIMT

comparison

comparison

jcss Certification, within 1%

JCSS Certification, 1%2%

NIMT Certification

Gas Manufacture Certification

calibration

Preparation/Calibration

Accreditation of ISO Guide 34

WorkingWorking

Secondary

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Mile-stoneMileMile--stonestone

-2008 ?Calibration using jcss secondary mixturesCertify Working standard gas (ISO/IEC 17025)

-2010 ?Accreditation of ISO Guide 34Preparation of Primary/Secondary gas mixtures by NIMT

-201x ? NIMT prepare High-purity gas, Primary/Secondary gas mixtures.

1st stage

2nd stage

3rd stage

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AcknowledgementAcknowledgementAcknowledgement

How to certified gases accurately.

How to calibrate gas analyzers accurately

How to prepare PRM by using gravimetric method for binary mixture.

How to estimate uncertainty following ISO 6143

How to manage the quality system ISO/IEC 17025

National Metrology Institute of Japan (NMIJ)

National Metrology Institute of Japan National Metrology Institute of Japan (NMIJ)(NMIJ)

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NMIJ FacilitiesNMIJ FacilitiesNMIJ Facilities

Gravimetric Method

( ISO 6142 )

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AcknowledgementAcknowledgementAcknowledgement

How to prepare PRM by using gravimetric method (ISO 6142). Binary Mixture Multi component mixture

Natural gas mixture Emission gas mixture

Ethanol gas mixture How to analysis impurity in purity gases or reagent.

FT-IR GC-PDHID Moisture Analyzer (Cavity ring down technique) Karl Ficher

Safety principle for preparing PRM Principle for dynamic dilution mixing ISO 6145

Dutch Metrology Institute (VSL)Dutch Metrology Institute (VSL)Dutch Metrology Institute (VSL)

14

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PRM by VSLPRM by VSLPRM by VSL

15

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VSL FacilitiesVSL FacilitiesVSL Facilities

Gravimetric Method

( ISO 6142 )

Dynamic Volumetric Method

( ISO 6145 )