Prepared by: Pace Analytical Services Pace Project No ...

51
Analytical Data Package Prepared by: Pace Analytical Services Pace Project No.: 50231942

Transcript of Prepared by: Pace Analytical Services Pace Project No ...

Page 1: Prepared by: Pace Analytical Services Pace Project No ...

Analytical Data Package

Prepared by:

Pace Analytical Services

Pace Project No.: 50231942

Page 2: Prepared by: Pace Analytical Services Pace Project No ...

Table Of Contents

Project OverviewFinal Report with COC/SCUR 1

Certifications 2

Sample Summary 3

Sample Analyte Count 4

Analytical Results 5

Quality Control Data 6

Qualifiers 8

Quality Control Data Cross Reference Table 9

Chain of Custody 10

SDG Narrative 13

TCEQ Checklist and ER 14

InOrganicICP

Initial & Continuing Calibration Verification (Form 2A-IN) 20

CRDL Check Standard (Form 2B-IN) 22

Blanks (Form 3-IN) 23

Interference Check Sample (Form 4A-IN) 25

Matrix Spike Recovery (Form 5A-IN) 26

Post Digestion Spike Recovery (Form 5B-IN) 28

Duplicates (Form 6-IN) 29

Laboratory Control Spike (Form 7-IN) 30

Serial Dilution (Form 8-IN) 31

Linear Ranges (Form 11-IN) 32

Preparation Log (Form 12-IN) 33

Analysis Run Log (Form 13-IN) 34

ICPMSInitial & Continuing Calibration Verification (Form 2A-IN) 35

CRDL Check Standard (Form 2B-IN) 37

Blanks (Form 3-IN) 39

Interference Check Sample (Form 4B-IN) 40

Matrix Spike Recovery (Form 5A-IN) 41

Post Digestion Spike Recovery (Form 5B-IN) 43

Duplicates (Form 6-IN) 44

Laboratory Control Spike (Form 7-IN) 45

Serial Dilution (Form 8-IN) 46

Linear Ranges (Form 11-IN) 47

Preparation Log (Form 12-IN) 48

Analysis Run Log (Form 13-IN) 49

Page 3: Prepared by: Pace Analytical Services Pace Project No ...

#=CL#

August 02, 2019

LIMS USE: FR - ENVIRONMENTALLIMS OBJECT ID: 50231942

50231942Project:Pace Project No.:

RE:

Environmental ManagerRepublic Services, Inc. - Blue Ridge Landfill2200 FM 521Fresno, TX 77545

Blue Ridge LF VRS MW-9

Dear Environmental Manager:Enclosed are the analytical results for sample(s) received by the laboratory on July 18, 2019. Theresults relate only to the samples included in this report. Results reported herein conform to the mostcurrent, applicable TNI/NELAC standards and the laboratory's Quality Assurance Manual, whereapplicable, unless otherwise noted in the body of the report.

If you have any questions concerning this report, please feel free to contact me.

Sincerely,

Chris [email protected]

Project Manager(317)228-3100

Enclosures

cc: Trihydro, Trihydro

REPORT OF LABORATORY ANALYSISThis report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, LLC.

Pace Analytical Services, LLC7726 Moller Road

Indianapolis, IN 46268(317)228-3100

Page 1 of 12

1 of 49

Page 4: Prepared by: Pace Analytical Services Pace Project No ...

#=CP#

CERTIFICATIONS

Pace Project No.:Project:

50231942Blue Ridge LF VRS MW-9

Indiana Certification IDs7726 Moller Road, Indianapolis, IN 46268Illinois Certification #: 200074Indiana Certification #: C-49-06Kansas/NELAP Certification #: E-10177Kentucky UST Certification #: 80226Kentucky WW Certification #: 98019Michigan Department of Environmental Quality, Laboratory#9050

Ohio VAP Certification #: CL0065Oklahoma Certification #: 2018-101Texas Certification #: T104704355West Virginia Certification #: 330Wisconsin Certification #: 999788130USDA Soil Permit #: P330-16-00257

REPORT OF LABORATORY ANALYSISThis report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, LLC.

Pace Analytical Services, LLC7726 Moller Road

Indianapolis, IN 46268(317)228-3100

Page 2 of 12

2 of 49

Page 5: Prepared by: Pace Analytical Services Pace Project No ...

#=SS#

SAMPLE SUMMARY

Pace Project No.:Project:

50231942Blue Ridge LF VRS MW-9

Lab ID Sample ID Matrix Date Collected Date Received

50230716004 MW-9 Water 07/15/19 15:25 07/18/19 09:00

REPORT OF LABORATORY ANALYSISThis report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, LLC.

Pace Analytical Services, LLC7726 Moller Road

Indianapolis, IN 46268(317)228-3100

Page 3 of 12

3 of 49

Page 6: Prepared by: Pace Analytical Services Pace Project No ...

#=SA#

SAMPLE ANALYTE COUNT

Pace Project No.:Project:

50231942Blue Ridge LF VRS MW-9

Lab ID Sample ID MethodAnalytesReportedAnalysts

50230716004 MW-9 EPA 6010 1KJE

EPA 6020 1DMT

REPORT OF LABORATORY ANALYSISThis report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, LLC.

Pace Analytical Services, LLC7726 Moller Road

Indianapolis, IN 46268(317)228-3100

Page 4 of 12

4 of 49

Page 7: Prepared by: Pace Analytical Services Pace Project No ...

#=AR#

ANALYTICAL RESULTS

Pace Project No.:Project:

50231942Blue Ridge LF VRS MW-9

Sample: MW-9 Lab ID: 50230716004 Collected: 07/15/19 15:25 Received: 07/18/19 09:00 Matrix: Water

Parameters Results Units DF Prepared Analyzed CAS No. QualReport Limit

Analytical Method: EPA 6010 Preparation Method: EPA 30106010 MET ICP

Barium 87.2 ug/L 07/31/19 12:39 7440-39-307/30/19 06:0810.0 1

Analytical Method: EPA 6020 Preparation Method: EPA 200.26020 MET ICPMS

Vanadium ND ug/L 07/25/19 06:43 7440-62-207/24/19 09:0710.0 5

REPORT OF LABORATORY ANALYSISThis report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, LLC.Date: 08/02/2019 02:42 PM

Pace Analytical Services, LLC7726 Moller Road

Indianapolis, IN 46268(317)228-3100

Page 5 of 12

5 of 49

Page 8: Prepared by: Pace Analytical Services Pace Project No ...

#=QC#

QUALITY CONTROL DATA

Pace Project No.:Project:

50231942Blue Ridge LF VRS MW-9

Results presented on this page are in the units indicated by the "Units" column except where an alternate unit is presented to the right of the result.

QC Batch:QC Batch Method:

Analysis Method:Analysis Description:

511879EPA 3010

EPA 60106010 MET

Associated Lab Samples: 50230716004

Parameter UnitsBlankResult

ReportingLimit Qualifiers

METHOD BLANK: 2361432Associated Lab Samples: 50230716004

Matrix: Water

Analyzed

Barium ug/L ND 10.0 07/31/19 12:15

Parameter UnitsLCS

Result% RecLimits Qualifiers% RecConc.

2361433LABORATORY CONTROL SAMPLE:LCSSpike

Barium ug/L 10301000 103 80-120

Parameter UnitsMS

Result% RecLimits Qual% RecConc.

2361434MATRIX SPIKE & MATRIX SPIKE DUPLICATE:

MSSpikeResult

50230716003

2361435

MSDResult

MSD% Rec RPD RPD

MaxMSDMSSpikeConc.

Barium ug/L 1000 98 75-125100 1 201000345 1330 1350

REPORT OF LABORATORY ANALYSISThis report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, LLC.Date: 08/02/2019 02:42 PM

Pace Analytical Services, LLC7726 Moller Road

Indianapolis, IN 46268(317)228-3100

Page 6 of 12

6 of 49

Page 9: Prepared by: Pace Analytical Services Pace Project No ...

#=QC#

QUALITY CONTROL DATA

Pace Project No.:Project:

50231942Blue Ridge LF VRS MW-9

Results presented on this page are in the units indicated by the "Units" column except where an alternate unit is presented to the right of the result.

QC Batch:QC Batch Method:

Analysis Method:Analysis Description:

512433EPA 200.2

EPA 60206020 MET

Associated Lab Samples: 50230716004

Parameter UnitsBlankResult

ReportingLimit Qualifiers

METHOD BLANK: 2364011Associated Lab Samples: 50230716004

Matrix: Water

Analyzed

Vanadium ug/L ND 2.0 07/25/19 06:12

Parameter UnitsLCS

Result% RecLimits Qualifiers% RecConc.

2364012LABORATORY CONTROL SAMPLE:LCSSpike

Vanadium ug/L 40.340 101 80-120

Parameter UnitsMS

Result% RecLimits Qual% RecConc.

2364013MATRIX SPIKE & MATRIX SPIKE DUPLICATE:

MSSpikeResult

50230716002

2364014

MSDResult

MSD% Rec RPD RPD

MaxMSDMSSpikeConc.

Vanadium ug/L 40 100 75-12599 1 2040ND 42.6 42.4

REPORT OF LABORATORY ANALYSISThis report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, LLC.Date: 08/02/2019 02:42 PM

Pace Analytical Services, LLC7726 Moller Road

Indianapolis, IN 46268(317)228-3100

Page 7 of 12

7 of 49

Page 10: Prepared by: Pace Analytical Services Pace Project No ...

#=QL#

QUALIFIERS

Pace Project No.:Project:

50231942Blue Ridge LF VRS MW-9

DEFINITIONS

DF - Dilution Factor, if reported, represents the factor applied to the reported data due to dilution of the sample aliquot.ND - Not Detected at or above adjusted reporting limit.TNTC - Too Numerous To CountJ - Estimated concentration above the adjusted method detection limit and below the adjusted reporting limit.MDL - Adjusted Method Detection Limit.PQL - Practical Quantitation Limit.RL - Reporting Limit - The lowest concentration value that meets project requirements for quantitative data with known precision andbias for a specific analyte in a specific matrix.S - Surrogate1,2-Diphenylhydrazine decomposes to and cannot be separated from Azobenzene using Method 8270. The result for each analyte isa combined concentration.Consistent with EPA guidelines, unrounded data are displayed and have been used to calculate % recovery and RPD values.LCS(D) - Laboratory Control Sample (Duplicate)MS(D) - Matrix Spike (Duplicate)DUP - Sample DuplicateRPD - Relative Percent DifferenceNC - Not Calculable.SG - Silica Gel - Clean-UpU - Indicates the compound was analyzed for, but not detected.N-Nitrosodiphenylamine decomposes and cannot be separated from Diphenylamine using Method 8270. The result reported foreach analyte is a combined concentration.Pace Analytical is TNI accredited. Contact your Pace PM for the current list of accredited analytes.TNI - The NELAC Institute.

REPORT OF LABORATORY ANALYSISThis report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, LLC.Date: 08/02/2019 02:42 PM

Pace Analytical Services, LLC7726 Moller Road

Indianapolis, IN 46268(317)228-3100

Page 8 of 12

8 of 49

Page 11: Prepared by: Pace Analytical Services Pace Project No ...

#=CR#

QUALITY CONTROL DATA CROSS REFERENCE TABLE

Pace Project No.:Project:

50231942Blue Ridge LF VRS MW-9

Lab ID Sample ID QC Batch Method QC Batch Analytical MethodAnalyticalBatch

50230716004 511879 513910MW-9 EPA 3010 EPA 6010

50230716004 512433 512794MW-9 EPA 200.2 EPA 6020

REPORT OF LABORATORY ANALYSISThis report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, LLC.Date: 08/02/2019 02:42 PM

Pace Analytical Services, LLC7726 Moller Road

Indianapolis, IN 46268(317)228-3100

Page 9 of 12

9 of 49

Page 12: Prepared by: Pace Analytical Services Pace Project No ...

Page 10 of 12

10 of 49

Page 13: Prepared by: Pace Analytical Services Pace Project No ...

Page 11 of 12

11 of 49

Page 14: Prepared by: Pace Analytical Services Pace Project No ...

Page 12 of 12

12 of 49

Page 15: Prepared by: Pace Analytical Services Pace Project No ...

Page 1 of 1

08/02/2019

LABORATORY CASE NARRATIVE

BLUE RIDGE LANDFILL

VERIFICATION SAMPLING JULY 2019

1 GROUNDWATER

#50231942

General Reporting Comments

The project samples were analyzed for Verification Total Metals. Pace Analytical Services located in

Indianapolis, Indiana performed all sample analysis. No sample analysis was subcontracted. Total Metals

PQL (Practical Quanitation Limit) used were the Texas MSW-Final Benchmark PQLs dated 03-25-2010.

Please note, Exceptions Reports have been included for checklist items R6 line 1, R3 line2. These items

have been checked “yes” on the Laboratory Checklist, as Pace Analytical meets the criteria except in those

cases where it is not applicable (ICP, ICP/MS, multi- analyte analysis, etc.), as noted in the referenced

NELAC standards.

Sample Receiving

Any discrepancies concerning sample receipt or sample transfer were noted on the Sample Condition Upon

Receipt Form.

The case samples were analyzed within the method specified holding times for the requested parameters.

The case samples were analyzed in accordance with NELAC requirements. No anomalies or deviations

from these requirements were noted.

Christine Sarkan Project Manager

Pace Analytical Services

706-453-7203

[email protected]

13 of 49

Page 16: Prepared by: Pace Analytical Services Pace Project No ...

Appendix ALABORATORY DATA PACKAGE COVER PAGE

This data package is for Job No. 50231942 and consists of:

This signature page, the laboratory review checklist, and the following reportable data:

R1 - Field chain-of-custody documentation;X

X R2 - Sample identification cross-reference;

X R3 - Test reports (analytical data sheets) for each environmental sample that includes:

a. Items consistent with NELAC Chapter 5,

b. Dilution factors,

c. Preparation methods,

d. Cleanup methods, and

e. If required for the project, tentatively identified compounds (TICs).

X R4 - Surrogate recovery data including:

b. The laboratory's surrogate QC limits.

a. Calculated recovery (%R), and

X R5 - Test reports/summary forms for blank samples;

X R6 - Test reports/summary forms for laboratory control samples (LCSs) including:

c. The laboratory's LCS QC limits.

b. Calculated %R for each analyte, and

a. LCS spiking amounts,

R7 - Test reports/summary forms for matrix spike/matrix spike duplicates (MS/MSDs) including:X

a. Samples associated with the MS/MSD clearly identified,

c. Concentration of each MS/MSD analyte measured in the parent and spiked samples,

b. MS/MSD spiking amounts,

e. The laboratory's MS/MSD QC limits.

d. Calculated %Rs and relative percent differences, and

X R8 - Laboratory analytical duplicate (if applicable) recovery and precision:

c. The laboratory's QC limits for analytical duplicated.

a. The amount of analyte measured in the duplicate,

b. The calculated RPD, and,

X R9 - List of method quantitation limits (MQLs) and detectability check sample results for each analyte and

X R10 - Other problems or anomalies.

The exception Report for each "No" or "Not Reviewed (NR) " item in the Laboratory Review Checklist and for eachanalyte, matrix, and method for which the laboratory does not hold NELAC accredidation under the TexasLaboratory Accreditation Program.

Release Statement: I am responsible for the release of this laboratory data package. This laboratory is NELACaccredited under the Texas Laboratory Accreditation Program for all the methods, analytes, and matrices reported inthis data package except as noted in the Exception Reports. The data have been reviewed and are technicallycompliant with the requirements of the methods used, except where noted by the laboratory in the Exception Reports.By my signature below, I affirm to the best of my knowledge all problems/anomalies observed by the laboratory havebeen identified in the Laboratory Review Checklist, and no information affecting the quality of the data has beenknowingly withheld.

Check, if applicable: [ ] This laboratory meets an exception under 30 TAC §25.6 and was last inspected by [ ] TCEQ

Any findings affecting the data in this laboratory data package are noted in the Exception Reports herin. The officialsigning the cover page of the report in which these data are used is responsible for releasing this data package and isby signature affirming the above release statement is true.

Name (Printed)Chris Sarkan

Signature Official Title (Printed) Date08/02/2019Project Manager

14 of 49

Page 17: Prepared by: Pace Analytical Services Pace Project No ...

Table 1. Reportable Data.

Laboratory Name:

Project Name:

Reviewer Name:

LRC Date:

Laboratory Job Number:

Prep Batch Number(s):

Item0F

1 Analytes1F

2 Description Result

(Yes, No, NA, NR)2F

3

Exception Report

No.3F

4

R1 O, I Chain-of-custody (COC) Did samples meet the laboratory’s standard conditions of sample acceptability upon receipt? Were all departures from standard conditions described in an exception report?

R2 O, I Sample and quality control (QC) identification Are all field sample ID numbers cross-referenced to the laboratory ID numbers? Are all laboratory ID numbers cross-referenced to the corresponding QC data?

R3 O, I Test reports Were all samples prepared and analyzed within holding times? Other than those results < MQL, were all other raw values bracketed by calibration standards? Were calculations checked by a peer or supervisor? Were all analyte identifications checked by a peer or supervisor? Were sample quantitation limits reported for all analytes not detected? Were all results for soil and sediment samples reported on a dry weight basis? Was % moisture (or solids) reported for all soil and sediment samples? If required for the project, TICs reported?

R4 O Surrogate recovery data Were surrogates added prior to extraction? Were surrogate percent recoveries in all samples within the laboratory QC limits?

R5 O, I Test reports/summary forms for blank samples Were appropriate type(s) of blanks analyzed? Were blanks analyzed at the appropriate frequency?

Municipal Solid Waste Laboratory Review Checklist (rev. 08/19/11)

Pace Analytical Services, LLC

BLUE RIDGE LF LANDFILL VRS JULY 2019

Christine Sarkan

08/02/2019 50231942

Yes

Yes

Yes

Yes

Yes

Yes

Yes

Yes

NA

NA

NA

NA

NA

Yes Yes

1

Yes

15 of 49

Page 18: Prepared by: Pace Analytical Services Pace Project No ...

Item0F

1 Analytes1F

2 Description Result

(Yes, No, NA, NR)2F

3

Exception Report

No.3F

4

Were method blanks taken through the entire analytical process, including preparation and, if applicable, cleanup procedures? Were blank concentrations < MQL?

R6 O, I Laboratory control samples (LCS): Were all COCs included in the LCS? Was each LCS taken through the entire analytical procedure, including prep and cleanup steps? Were LCSs analyzed at the required frequency? Were LCS (and LCSD, if applicable) %Rs within the laboratory QC limits? Does the detectability data document the laboratory’s capability to detect the COCs at the MDL used to calculate the SQLs? Was the LCSD RPD within QC limits?

R7 O, I Matrix spike (MS) and matrix spike duplicate (MSD) data Were the project/method specified analytes included in the MS and MSD? Were MS/MSD analyzed at the appropriate frequency? Were MS (and MSD, if applicable) %Rs within the laboratory QC limits? Were MS/MSD RPDs within laboratory QC limits?

R8 O, I Analytical duplicate data Were appropriate analytical duplicates analyzed for each matrix? Were analytical duplicates analyzed at the appropriate frequency? Were RPDs or relative standard deviations within the laboratory QC limits?

R9 O, I Method quantitation limits (MQLs): Are the MQLs for each method analyte included in the laboratory data package? Do the MQLs correspond to the concentration of the lowest non-zero calibration standard? Are unadjusted MQLs included in the laboratory data package?

R10 O, I Other problems/anomalies Are all known problems/anomalies/special conditions noted in this LRC and ER? Were all necessary corrective actions performed for the reported data? Was applicable and available technology used to lower the SQL minimize the matrix interference affects on the sample results?

Municipal Solid Waste Laboratory Review Checklist (rev. 08/19/11)

Yes

Yes

Yes

Yes

Yes

Yes

Yes

NA

Yes

Yes

Yes

Yes

Yes

Yes

Yes

Yes

Yes

Yes

Yes

Yes

Yes

1

16 of 49

Page 19: Prepared by: Pace Analytical Services Pace Project No ...

Table 2. Supporting Data.

Laboratory Name:

Project Name:

Reviewer Name:

LRC Date:

Laboratory Job Number:

Prep Batch Number(s):

Item1 Analytes2 Description

Result (Yes,

No, NA, NR)3

Exception Report

No.4

S1 O, I Initial calibration (ICAL) Were response factors and/or relative response factors for each analyte within QC limits? Were percent RSDs or correlation coefficient criteria met? Was the number of standards recommended in the method used for all analytes? Were all points generated between the lowest and highest standard used to calculate the curve? Are ICAL data available for all instruments used? Has the initial calibration curve been verified using an appropriate second source standard?

S2 O, I Initial and continuing calibration verification (ICCV and CCV) and continuing calibration blank (CCB): Was the CCV analyzed at the method-required frequency? Were percent differences for each analyte within the method-required QC limits? Was the ICAL curve verified for each analyte? Was the absolute value of the analyte concentration in the inorganic CCB < MDL?

S3 O Mass spectral tuning: Was the appropriate compound for the method used for tuning? Were ion abundance data within the method-required QC limits?

S4 O Internal standards (IS): Were IS area counts and retention times within the method-required QC limits?

S5 O, I Raw data (NELAC section 1 appendix A glossary, and section 5.) Were the raw data (for example, chromatograms, spectral data) reviewed by an analyst? Were data associated with manual integrations flagged on the raw data?

Municipal Solid Waste Laboratory Review Checklist (rev. 08/19/11)

Pace Analytical Services, LLC

BLUE RIDGE LANDFILL JULY VRS 2019

Christine Sarkan

08/02/2019

50231942

Yes

Yes

Yes

Yes

Yes

Yes

Yes

Yes

Yes

Yes

NA

NA

NA

Yes

Yes

17 of 49

Page 20: Prepared by: Pace Analytical Services Pace Project No ...

Item1 Analytes2 Description

Result (Yes,

No, NA, NR)3

Exception Report

No.4

S6 O Dual column confirmation Did dual column confirmation results meet the method-required QC?

S7 O Tentatively identified compounds (TICs): If TICs were requested, were the mass spectra and TIC data subject to appropriate checks?

S8 I Interference Check Sample (ICS) results: Were percent recoveries within method QC limits?

S9 I Serial dilutions, post digestion spikes, and method of standard additions Were percent differences, recoveries, and the linearity within the QC limits specified in the method?

S10 O, I Method detection limit (MDL) studies Was a MDL study performed for each reported analyte? Is the MDL either adjusted or supported by the analysis of DCSs?

S11 O, I Proficiency test reports: Was the laboratory's performance acceptable on the applicable proficiency tests or evaluation studies?

S12 O, I Standards documentation Are all standards used in the analyses NIST-traceable or obtained from other appropriate sources?

S13 O, I Compound/analyte identification procedures Are the procedures for compound/analyte identification documented?

S14 O, I Demonstration of analyst competency (DOC) Was DOC conducted consistent with NELAC Chapter 5C? Is documentation of the analyst’s competency up-to-date and on file?

S15 O, I Verification/validation documentation for methods (NELAC Chap 5n 5) Are all the methods used to generate the data documented, verified, and validated, where applicable?

S16 O, I Laboratory standard operating procedures (SOPs): Are laboratory SOPs current and on file for each method performed?

Municipal Solid Waste Laboratory Review Checklist (rev. 08/19/11)

NA

NA

Yes

Yes

Yes

Yes

Yes

Yes

Yes

Yes

Yes

Yes

Yes

2

18 of 49

Page 21: Prepared by: Pace Analytical Services Pace Project No ...

Table 3. Exception Reports.

Laboratory Name:

Project Name:

Reviewer Name:

LRC Date:

Laboratory Job Number:

Prep Batch Number(s):

Exception Report No.

Description

1 Items identified by the letter “R” must be available as a hard copy or as a .pdf file. Items identified by the letter “S” should be retained and made available upon request for the appropriate retention period.

2 O - organic analyses; I - inorganic analyses (including general chemistry constituents, when applicable). 3 NA - Not applicable; NR - Not reviewed. 4 Exception Report identification number; an Exception Report should be completed for an item if the result is “No” or “NR.”

Municipal Solid Waste Laboratory Review Checklist (rev. 08/19/11)

Pace Analytical Services, LLC

BLUE RIDE LANDFILL VRS JULY 2019

Christine Sarkan

08/02/2019

50231942

1-R3,R9 NELAC EL-V1M4-2011 pg 79 of 136 h) The following shall occur for instrument technology(such as ICP or

ICP/MS) with validated techniques from manufacturers or methods employing standardizations with zero

point and single point calibration standard:

ii. A zero point and single point calibration standard shall be analyzed with each analytical batch.

iii. A standard corresponding to the limit of quantitation shall be analyzed with each analytical batch and

meet acceptance criteria.

iv. The linearity is verified at the frequency established by the method and/or manufacturer

2-S­10

MDL studies are per 40CFR136 and the 2017 Method Update Rule. These rules require the anlaysis of

prepped samples at or near the MDL at a minimum of 2 per quarter per instrument for all analyses. The

samples in this package are reported under 30TAC 330 and are reported according to the Guidelines

for Quantitation Limits letter dated May 25, 2010. The project samples were not reported to the MDL.

19 of 49

Page 22: Prepared by: Pace Analytical Services Pace Project No ...

FORM II INORGANIC-1

INITIAL AND CONTINUING CALIBRATION VERIFICATION

Pace Analytical - Indiana 50231942 Blue Ridge LF VRS MW-9

216663

216662

ug/L 50ICP4

Lab Name:

Initial Calibration Verification Source:

Continuing Calibration Verification Source:

Concentration Units: Instrument ID:

SDG No. : Contract:

Analyte

07/31/2019 07:59

True %RFound

Initial CalibrationVerification

ControlLimit

Barium 1000 1010 100.8 90-110

07/31/2019 08:32

True %RFound

07/31/2019 12:02

True %RFoundControlLimit

1000 1020 101.9 1000 1030 103.4 90-110

Continuing Calibration Verification

08/02/2019 13:4720 of 49

Page 23: Prepared by: Pace Analytical Services Pace Project No ...

FORM II INORGANIC-2

INITIAL AND CONTINUING CALIBRATION VERIFICATION

Pace Analytical - Indiana 50231942 Blue Ridge LF VRS MW-9

216663

ug/L 50ICP4

Lab Name:

Initial Calibration Verification Source:

Continuing Calibration Verification Source:

Concentration Units: Instrument ID:

SDG No. : Contract:

Continuing Calibration Verification

Analyte

07/31/2019 12:28

True Found %R

07/31/2019 13:27

True Found %RControlLimit

Barium 1000 1030 103.1 1000 1010 100.9 90-110

08/02/2019 13:4721 of 49

Page 24: Prepared by: Pace Analytical Services Pace Project No ...

FORM II INORGANIC-1

CRDL CHECK STANDARD

Lab Name: Pace Analytical - Indiana Contract:SDG No. : 50231942 Blue Ridge LF VRS MW-9

CRDL Check Standard Source: 216443

Concentration Units: ug/L

Analysis Date/Time: 07/31/2019 08:03

True Found %RControl Limit

%RBarium 10.0 10.4 103.6 50-150

AnalyteCRDL Check Standard

08/02/2019 13:4722 of 49

Page 25: Prepared by: Pace Analytical Services Pace Project No ...

FORM III INORGANIC-1

BLANKS

Lab Name: Pace Analytical - Indiana SDG No. : Blue Ridge LF VRS MW-950231942 Contract :

Method Blank Matrix:

Method Blank Concentration Units:

Water

ug/L

Instrument ID: 50ICP4

Analyte

InitialCalibration

Blank (ug/L)

07/31/2019C

08:01Barium 5.0 U

07/31/2019C

08:3407/31/2019

C12:04

07/31/2019C

12:30

5.0 U 5.0 U 5.0 U

Continuing Calibration Blank (ug/L) Method Blank

2361432 C

ND U

08/02/2019 13:4723 of 49

Page 26: Prepared by: Pace Analytical Services Pace Project No ...

FORM III INORGANIC-2

BLANKS

Lab Name: Pace Analytical - Indiana SDG No. : Blue Ridge LF VRS MW-950231942 Contract :

Method Blank Matrix:

Method Blank Concentration Units:

Instrument ID: 50ICP4

Analyte

InitialCalibration

Blank

C

Barium

07/31/2019C

12:57C C

5.0 U

Continuing Calibration Blank (ug/L)

08/02/2019 13:4724 of 49

Page 27: Prepared by: Pace Analytical Services Pace Project No ...

Sol. A %R Sol. AB %R Limits

477400 95.5 478100 95.6 80-120

0.8169 497.1 99.4 80-120

449400 89.9 446600 89.3 80-120

187800 93.9 188400 94.2 80-120

495700 99.1 496300 99.3 80-120

Sol. A Sol. AB

Aluminum 500000 500000

Barium 500

Calcium 500000 500000

Iron 200000 200000

Magnesium 500000 500000

Analyte

FoundTrue

FORM IV INORGANIC-1

INTERFERENCE CHECK SAMPLE

Lab Name: Pace Analytical - Indiana SDG No. : 50231942 Contract: Blue Ridge LF VRS MW-9

Instrument ID:

ICS Source:

Concentration Units:

50ICP4

ug/L

216594,216526

07/31/2019 08:06

07/31/2019 08:08

Solution A Run Date:

Solution AB Run Date:

08/02/2019 13:4725 of 49

Page 28: Prepared by: Pace Analytical Services Pace Project No ...

FORM V INORGANIC-1

MATRIX SPIKE SAMPLE RECOVERY

Lab Name: Pace Analytical - Indiana SDG No. : Blue Ridge LF VRS MW-950231942 Contract:

Matrix: Water

Percent Moisture:

Basis: Wet

SAMPLE NO.

2361434MS

Parent Sample ID: 50230716003

AnalyteControlLimit%R

Spiked SampleResult (SSR)

SampleResult (SR)

SpikeAdded (SA)

%RUnits

Barium 1000 981330 34575-125ug/L

08/02/2019 13:4726 of 49

Page 29: Prepared by: Pace Analytical Services Pace Project No ...

FORM V INORGANIC-2

MATRIX SPIKE SAMPLE RECOVERY

Lab Name: Pace Analytical - Indiana SDG No. : Blue Ridge LF VRS MW-950231942 Contract:

Matrix: Water

Percent Moisture:

Basis: Wet

SAMPLE NO.

2361435MSD

Parent Sample ID: 50230716003

AnalyteControlLimit%R

Spiked SampleResult (SSR)

SampleResult (SR)

SpikeAdded (SA)

%RUnits

Barium 1000 1001350 34575-125ug/L

08/02/2019 13:4727 of 49

Page 30: Prepared by: Pace Analytical Services Pace Project No ...

FORM V INORGANIC-1

POST-DIGESTION SPIKE SAMPLE RECOVERY

Lab Name: Pace Analytical - Indiana SDG No. : Blue Ridge LF VRS MW-950231942 Contract:

Matrix: Water

SAMPLE NO.

2370523PDS

50230716003Parent Sample ID:

AnalyteControlLimit%R

Spiked SampleResult (SSR)

SampleResult (SR)

SpikeAdded (SA)

%RUnits DF DF

Barium 1000 99.31340 34575-125ug/L 1 1

08/02/2019 13:4728 of 49

Page 31: Prepared by: Pace Analytical Services Pace Project No ...

FORM VI INORGANIC-1

DUPLICATES

Lab Name: Pace Analytical - Indiana SDG No. : Blue Ridge LF VRS MW-950231942 Contract:

Matrix: Water

Percent Moisture:

Concentration Units: ug/L

Basis: Wet

SAMPLE NO.

2361435MSD

AnalyteControlLimit

Sample Duplicate RPD

Barium 11330 135020

08/02/2019 13:4729 of 49

Page 32: Prepared by: Pace Analytical Services Pace Project No ...

FORM VII INORGANIC-1

LABORATORY CONTROL SAMPLE

Lab Name: Pace Analytical - Indiana SDG No. : Blue Ridge LF VRS MW-950231942 Contract:

Matrix: Water

SAMPLE NO.

2361433LCS

Analyte True Found %R LimitsUnits

Barium 1031000 1030 12080ug/L

08/02/2019 13:4730 of 49

Page 33: Prepared by: Pace Analytical Services Pace Project No ...

FORM VIII INORGANIC-1

SERIAL DILUTIONS

Lab Name: Pace Analytical - Indiana SDG No. : Blue Ridge LF VRS MW-950231942 Contract:

Matrix: Water

SAMPLE NO.

2370524SD

50230716003Parent Sample ID:

AnalyteInitial

SampleResult

SerialDilutionResult

%Difference

ControlLimit%D

Units

Barium 351 1.7345 10ug/L

08/02/2019 13:47

* Indicates that the % Difference exceeds the control limit.No difference is calculated if either result is a non-detect.

31 of 49

Page 34: Prepared by: Pace Analytical Services Pace Project No ...

FORM XI - INORGANIC-1

LINEAR DYNAMIC RANGES

Pace Analytical - Indiana 50231942 Contract :SDG No. : Blue Ridge LF VRS MW-9

50ICP4 Effective Date:09/29/2016

Lab Name:

Instrument ID:

Analyte Concentration(ug/L)

25000Barium

08/02/2019 13:47

32 of 49

Page 35: Prepared by: Pace Analytical Services Pace Project No ...

FORM XII INORGANIC-1

PREPARATION LOG

Contract:50231942Pace Analytical - IndianaLab Name: SDG No. : Blue Ridge LF VRS MW-9

Preparation Method: EPA 3010 Batch: MPRP 36714

Sample Name Preparation Date Initial Volume(mL)

Final Volume(mL)Lab Sample ID

2361432BLANK 07/30/2019 50 502361432

2361433LCS 07/30/2019 25 252361433

2361434MS 07/30/2019 25 252361434

2361435MSD 07/30/2019 25 252361435

MW-9 07/30/2019 50 5050230716004

08/02/2019 13:47

33 of 49

Page 36: Prepared by: Pace Analytical Services Pace Project No ...

FORM XIII INORGANIC-1

ANALYSIS RUN LOG

Lab Name: Pace Analytical - Indiana SDG No. : 50231942 Contract: Blue Ridge LF VRS MW-9

Instrument ID: 50ICP4 Analysis Method: EPA 6010

Start Date: 07/31/2019 07:41 End Date: 07/31/2019 13:27

Sample Name Date TimeD/FLab Sample IDBa

15486086CAL0 15486086CAL0 1 07/31/2019 07:41 X

15486088CAL2 15486088CAL2 1 07/31/2019 07:46 X

15486094ICV 15486094ICV 1 07/31/2019 07:59 X

15486095ICB 15486095ICB 1 07/31/2019 08:01 X

15486096CRDL 15486096CRDL 1 07/31/2019 08:03 X

15486097ICSA 15486097ICSA 1 07/31/2019 08:06 X

15486098ICSAB 15486098ICSAB 1 07/31/2019 08:08 X

15486099CCV 15486099CCV 1 07/31/2019 08:32 X

15486100CCB 15486100CCB 1 07/31/2019 08:34 X

15490551CCV 15490551CCV 1 07/31/2019 12:02 X

15490552CCB 15490552CCB 1 07/31/2019 12:04 X

2361432BLANK 2361432 1 07/31/2019 12:15 X

2361433LCS 2361433 1 07/31/2019 12:17 X

50230716003 50230716003 1 07/31/2019 12:24

2361434MS 2361434 1 07/31/2019 12:26 X

15490554CCV 15490554CCV 1 07/31/2019 12:28 X

15490555CCB 15490555CCB 1 07/31/2019 12:30 X

2361435MSD 2361435 1 07/31/2019 12:32 X

2370523PDS 2370523 1 07/31/2019 12:34 X

2370524SD 2370524 1 07/31/2019 12:37 X

MW-9 50230716004 1 07/31/2019 12:39 X

15490556CCB 15490556CCB 1 07/31/2019 12:57 X

15490557CCV 15490557CCV 1 07/31/2019 13:27 X

08/02/2019 13:4734 of 49

Page 37: Prepared by: Pace Analytical Services Pace Project No ...

FORM II INORGANIC-1

INITIAL AND CONTINUING CALIBRATION VERIFICATION

Pace Analytical - Indiana 50231942 Blue Ridge LF VRS MW-9

215957

215959

ug/L 50ICM2

Lab Name:

Initial Calibration Verification Source:

Continuing Calibration Verification Source:

Concentration Units: Instrument ID:

SDG No. : Contract:

Analyte

07/25/2019 04:17

True %RFound

Initial CalibrationVerification

ControlLimit

Vanadium 50 48.3 96.5 90-110

07/25/2019 04:40

True %RFound

07/25/2019 05:58

True %RFoundControlLimit

20 19.4 97.1 20 19.2 95.8 90-110

Continuing Calibration Verification

08/02/2019 13:4735 of 49

Page 38: Prepared by: Pace Analytical Services Pace Project No ...

FORM II INORGANIC-2

INITIAL AND CONTINUING CALIBRATION VERIFICATION

Pace Analytical - Indiana 50231942 Blue Ridge LF VRS MW-9

215957

ug/L 50ICM2

Lab Name:

Initial Calibration Verification Source:

Continuing Calibration Verification Source:

Concentration Units: Instrument ID:

SDG No. : Contract:

Continuing Calibration Verification

Analyte

07/25/2019 06:48

True Found %RControlLimit

Vanadium 20 19.4 97.1 90-110

08/02/2019 13:4736 of 49

Page 39: Prepared by: Pace Analytical Services Pace Project No ...

FORM II INORGANIC-1

CRDL CHECK STANDARD

Lab Name: Pace Analytical - Indiana Contract:SDG No. : 50231942 Blue Ridge LF VRS MW-9

CRDL Check Standard Source: 215960

Concentration Units: ug/L

Analysis Date/Time: 07/25/2019 04:26

True Found %RControl Limit

%RVanadium 1.0 0.98 97.5 50-150

AnalyteCRDL Check Standard

08/02/2019 13:4737 of 49

Page 40: Prepared by: Pace Analytical Services Pace Project No ...

FORM II INORGANIC-1

CRDL CHECK STANDARD

Lab Name: Pace Analytical - Indiana Contract:SDG No. : 50231942 Blue Ridge LF VRS MW-9

CRDL Check Standard Source: 215960

Concentration Units: ug/L

Analysis Date/Time: 07/25/2019 06:07

True Found %RControl Limit

%RVanadium 1.0 0.92 91.5 50-150

AnalyteCRDL Check Standard

08/02/2019 13:4738 of 49

Page 41: Prepared by: Pace Analytical Services Pace Project No ...

FORM III INORGANIC-1

BLANKS

Lab Name: Pace Analytical - Indiana SDG No. : Blue Ridge LF VRS MW-950231942 Contract :

Method Blank Matrix:

Method Blank Concentration Units:

Water

ug/L

Instrument ID: 50ICM2

Analyte

InitialCalibration

Blank (ug/L)

07/25/2019C

04:21Vanadium 0.50 U

07/25/2019C

04:4407/25/2019

C06:02

07/25/2019C

06:53

0.50 U 0.50 U 0.50 U

Continuing Calibration Blank (ug/L) Method Blank

2364011 C

ND U

08/02/2019 13:4739 of 49

Page 42: Prepared by: Pace Analytical Services Pace Project No ...

Sol. A %R Sol. AB %R Limits

19235.226 96.2 19037.501 91.5 80-120

397.08 99.3 400.531 98.2 80-120

449.016 112.3 451.551 110.7 80-120

0.015 7.817 97.7 80-120

Sol. A Sol. AB

Aluminum 20000 20800

Molybdenum 400 408

Titanium 400 408

Vanadium 8

Analyte

FoundTrue

FORM IV INORGANIC-1

INTERFERENCE CHECK SAMPLE

Lab Name: Pace Analytical - Indiana SDG No. : 50231942 Contract: Blue Ridge LF VRS MW-9

Instrument ID:

ICS Source:

Concentration Units:

50ICM2

ug/L

215961,215962

07/25/2019 04:31

07/25/2019 04:35

Solution A Run Date:

Solution AB Run Date:

08/02/2019 13:4740 of 49

Page 43: Prepared by: Pace Analytical Services Pace Project No ...

FORM V INORGANIC-1

MATRIX SPIKE SAMPLE RECOVERY

Lab Name: Pace Analytical - Indiana SDG No. : Blue Ridge LF VRS MW-950231942 Contract:

Matrix: Water

Percent Moisture:

Basis: Wet

SAMPLE NO.

2364013MS

Parent Sample ID: 50230716002

AnalyteControlLimit%R

Spiked SampleResult (SSR)

SampleResult (SR)

SpikeAdded (SA)

%RUnits

Vanadium 40.0 10042.6 ND75-125ug/L

08/02/2019 13:4741 of 49

Page 44: Prepared by: Pace Analytical Services Pace Project No ...

FORM V INORGANIC-2

MATRIX SPIKE SAMPLE RECOVERY

Lab Name: Pace Analytical - Indiana SDG No. : Blue Ridge LF VRS MW-950231942 Contract:

Matrix: Water

Percent Moisture:

Basis: Wet

SAMPLE NO.

2364014MSD

Parent Sample ID: 50230716002

AnalyteControlLimit%R

Spiked SampleResult (SSR)

SampleResult (SR)

SpikeAdded (SA)

%RUnits

Vanadium 40.0 9942.4 ND75-125ug/L

08/02/2019 13:4742 of 49

Page 45: Prepared by: Pace Analytical Services Pace Project No ...

FORM V INORGANIC-1

POST-DIGESTION SPIKE SAMPLE RECOVERY

Lab Name: Pace Analytical - Indiana SDG No. : Blue Ridge LF VRS MW-950231942 Contract:

Matrix: Water

SAMPLE NO.

2365513PDS

50230716002Parent Sample ID:

AnalyteControlLimit%R

Spiked SampleResult (SSR)

SampleResult (SR)

SpikeAdded (SA)

%RUnits DF DF

Vanadium 20 97.220.0 0.54J75-125ug/L 5 5

08/02/2019 13:4743 of 49

Page 46: Prepared by: Pace Analytical Services Pace Project No ...

FORM VI INORGANIC-1

DUPLICATES

Lab Name: Pace Analytical - Indiana SDG No. : Blue Ridge LF VRS MW-950231942 Contract:

Matrix: Water

Percent Moisture:

Concentration Units: ug/L

Basis: Wet

SAMPLE NO.

2364014MSD

AnalyteControlLimit

Sample Duplicate RPD

Vanadium 142.6 42.420

08/02/2019 13:4744 of 49

Page 47: Prepared by: Pace Analytical Services Pace Project No ...

FORM VII INORGANIC-1

LABORATORY CONTROL SAMPLE

Lab Name: Pace Analytical - Indiana SDG No. : Blue Ridge LF VRS MW-950231942 Contract:

Matrix: Water

SAMPLE NO.

2364012LCS

Analyte True Found %R LimitsUnits

Vanadium 10140.0 40.3 12080ug/L

08/02/2019 13:4745 of 49

Page 48: Prepared by: Pace Analytical Services Pace Project No ...

FORM VIII INORGANIC-1

SERIAL DILUTIONS

Lab Name: Pace Analytical - Indiana SDG No. : Blue Ridge LF VRS MW-950231942 Contract:

Matrix: Water

SAMPLE NO.

2365514SD

50230716002Parent Sample ID:

AnalyteInitial

SampleResult

SerialDilutionResult

%Difference

ControlLimit%D

Units

Vanadium 0.96U0.54J 10ug/L

08/02/2019 13:47

* Indicates that the % Difference exceeds the control limit.No difference is calculated if either result is a non-detect.

46 of 49

Page 49: Prepared by: Pace Analytical Services Pace Project No ...

FORM XI - INORGANIC-1

LINEAR DYNAMIC RANGES

Pace Analytical - Indiana 50231942 Contract :SDG No. : Blue Ridge LF VRS MW-9

50ICM2 Effective Date:12/05/2014

Lab Name:

Instrument ID:

Analyte Concentration(ug/L)

200Vanadium

08/02/2019 13:47

47 of 49

Page 50: Prepared by: Pace Analytical Services Pace Project No ...

FORM XII INORGANIC-1

PREPARATION LOG

Contract:50231942Pace Analytical - IndianaLab Name: SDG No. : Blue Ridge LF VRS MW-9

Preparation Method: EPA 200.2 Batch: MPRP 36768

Sample Name Preparation Date Initial Volume(mL)

Final Volume(mL)Lab Sample ID

2364011BLANK 07/24/2019 50 502364011

2364012LCS 07/24/2019 50 502364012

2364013MS 07/24/2019 50 502364013

2364014MSD 07/24/2019 50 502364014

MW-9 07/24/2019 50 5050230716004

08/02/2019 13:47

48 of 49

Page 51: Prepared by: Pace Analytical Services Pace Project No ...

FORM XIII INORGANIC-1

ANALYSIS RUN LOG

Lab Name: Pace Analytical - Indiana SDG No. : 50231942 Contract: Blue Ridge LF VRS MW-9

Instrument ID: 50ICM2 Analysis Method: EPA 6020

Start Date: 07/25/2019 03:54 End Date: 07/25/2019 06:53

Sample Name Date TimeD/FLab Sample IDV

15455130CAL0 15455130CAL0 1 07/25/2019 03:54 X

15455131CAL1 15455131CAL1 1 07/25/2019 03:59 X

15455132CAL2 15455132CAL2 1 07/25/2019 04:03 X

15455133CAL3 15455133CAL3 1 07/25/2019 04:08 X

15455134ICV 15455134ICV 1 07/25/2019 04:17 X

15455135ICB 15455135ICB 1 07/25/2019 04:21 X

15455136CRDL 15455136CRDL 1 07/25/2019 04:26 X

15455137ICSA 15455137ICSA 1 07/25/2019 04:31 X

15455138ICSAB 15455138ICSAB 1 07/25/2019 04:35 X

15455139CCV 15455139CCV 1 07/25/2019 04:40 X

15455140CCB 15455140CCB 1 07/25/2019 04:44 X

15463631CCV 15463631CCV 1 07/25/2019 05:58 X

15463632CCB 15463632CCB 1 07/25/2019 06:02 X

15463633CRDL 15463633CRDL 1 07/25/2019 06:07 X

2364011BLANK 2364011 1 07/25/2019 06:12 X

2364012LCS 2364012 1 07/25/2019 06:16 X

50230716002 50230716002 5 07/25/2019 06:21 X

2364013MS 2364013 5 07/25/2019 06:25 X

2364014MSD 2364014 5 07/25/2019 06:30 X

2365513PDS 2365513 5 07/25/2019 06:34 X

2365514SD 2365514 25 07/25/2019 06:39 X

MW-9 50230716004 5 07/25/2019 06:43 X

15463634CCV 15463634CCV 1 07/25/2019 06:48 X

15463635CCB 15463635CCB 1 07/25/2019 06:53 X

08/02/2019 13:4749 of 49