18R0004_Amend_2_Prior_Year_Lab_Analysis.pdf

Laboratory Case Narrative for Laboratory WorkOrder # 1706179

The samples were received and processed using normal regulatory and laboratory protocols. Unless noted in the Final

Report, there were no significant data anomalies or failures noted during data assessment and reporting. The results within this report relate only to the samples received and reported for this project and this report shall not be reproduced except in full, without the approval of Empirical Laboratories, LLC. The test results meet all requirements of NELAC unless otherwise noted. Data uncertainty is linked to the method and regulatory mandated quality control data associated with the sample.

Prior to accepting a Project, Empirical Laboratories, LLC verifies certification requirements and where applicable ensures that the requirements are in place prior to sample analysis. Many states do not carry matrix or program specific certifications. A listing of certifications held by Empirical Laboratories, LLC is included at the end of this report.

EMPIRICAL LABORATORIES, LLC Work Order: 1706179 Report Date: 07/18/2017

ResultAnalyte RL BatchAnalyzed Method Notes DilutionUnits

Client Sample ID: Lime Sludge

MDL

Lab Sample ID: 1706179-01

Sample Matrix: Solid

Sample Collection Date/Time: 06/26/2017 11:00

Sample Received Date/Time: 06/27/2017 08:50

Laboratory Analytical Results Report

Classical Chemistry Parameters

SM2540B36 7G0300507/05/17 15:05% 1% Solids 1.01.0

SW9045D10.2 7G1100607/11/17 13:55pH Units 1Laboratory pH 0.1000.100 H

Metals (Total) by ICP

SW6010C4430 7G0500507/10/17 21:13mg/Kg dry 2Aluminum 21754.1 D

ND SW6010C07/10/17 21:13mg/Kg dry 7G050052Arsenic 10.83.25 U

ND SW6010C07/10/17 21:13mg/Kg dry 7G050052Cadmium 5.412.17 MU

SW6010C2.23 7G0500507/10/17 21:13mg/Kg dry 2Chromium 10.82.17 DJ

ND SW6010C07/10/17 21:13mg/Kg dry 7G050052Copper 10.84.33 U

ND SW6010C07/10/17 21:13mg/Kg dry 7G050052Lead 5.411.62 U

ND SW6010C07/10/17 21:13mg/Kg dry 7G050052Molybdenum 21.75.41 U

ND SW6010C07/10/17 21:13mg/Kg dry 7G050052Nickel 10.83.25 U

ND SW6010C07/10/17 21:13mg/Kg dry 7G050052Selenium 10.83.25 U

SW6010C13.3 7G0500507/10/17 21:13mg/Kg dry 2Zinc 21.75.41 DJ

Mercury by CVAA

ND SW7471B07/07/17 14:36mg/Kg dry 7G050191Mercury 0.09290.0366 U

Result RL Units Level

Spike

Result

Source

%REC

%REC

Limits RPD

RPD

Limit Notes Analyte

Classical Chemistry Parameters - Quality Control

MDL

Batch 7G03005

Duplicate Prepared: 07/03/2017 Analyzed: 07/05/2017Source: 1706225-04

% Solids %83.29 1.0 85.16 202.221.0

Batch 7G11006

LCS Prepared & Analyzed: 07/11/2017

Laboratory pH pH Units6.080 0.100 6.630 80-12091.70.100

LCS Prepared & Analyzed: 07/11/2017

Laboratory pH pH Units6.090 0.100 6.630 80-12091.90.100

LCS Prepared & Analyzed: 07/11/2017

Laboratory pH pH Units6.090 0.100 6.630 80-12091.90.100

LCS Prepared & Analyzed: 07/11/2017

Laboratory pH pH Units6.100 0.100 6.630 80-12092.00.100

Duplicate Prepared & Analyzed: 07/11/2017Source: 1706141-01

Laboratory pH pH Units7.530 0.100 7.520 20 H0.1330.100

Result

Source

%REC

%REC

Limits RPD

RPD

Limit Notes Analyte

Metals (Total) by ICP - Quality Control

MDL

Batch 7G05005

Blank Prepared: 07/05/2017 Analyzed: 07/10/2017

Aluminum mg/Kg wet

ND 40.0 U10.0

Arsenic mg/Kg wet

ND 2.00 U0.600

Cadmium mg/Kg wet

ND 1.00 U0.200

Chromium mg/Kg wet

ND 2.00 U0.400

Copper mg/Kg wet

ND 2.00 U0.800

Lead mg/Kg wet

ND 1.00 U0.300

Molybdenum mg/Kg wet

ND 4.00 U1.00

Nickel mg/Kg wet

ND 2.00 U0.600

Selenium mg/Kg wet

ND 2.00 U0.600

Zinc mg/Kg wet

ND 4.00 U1.00

LCS Prepared: 07/05/2017 Analyzed: 07/10/2017

Aluminum mg/Kg wet

402.7 40.0 400.0 80-12010110.0

Arsenic mg/Kg wet

50.44 2.00 50.00 80-1201010.600

Cadmium mg/Kg wet

26.31 1.00 25.00 80-1201050.200

Chromium mg/Kg wet

39.72 2.00 40.00 80-12099.30.400

Copper mg/Kg wet

49.16 2.00 50.00 80-12098.30.800

Lead mg/Kg wet

49.96 1.00 50.00 80-12099.90.300

Molybdenum mg/Kg wet

206.6 4.00 200.0 80-1201031.00

Nickel mg/Kg wet

106.2 2.00 100.0 80-1201060.600

Selenium mg/Kg wet

49.70 2.00 50.00 80-12099.40.600

Zinc mg/Kg wet

103.2 4.00 100.0 80-1201031.00

Matrix Spike Prepared: 07/05/2017 Analyzed: 07/10/2017Source: 1706180-01

Aluminum mg/Kg dry

17240 435 2176 11820 D80-120249109

Arsenic mg/Kg dry

277.1 21.8 272.0 ND D80-1201026.53

Cadmium mg/Kg dry

153.3 10.9 136.0 12.14 D80-1201042.18

Chromium mg/Kg dry

286.1 21.8 217.6 68.41 D80-1201004.35

Result

Source

%REC

%REC

Limits RPD

RPD

Limit Notes Analyte

Metals (Total) by ICP - Quality Control

MDL

Batch 7G05005

Matrix Spike Prepared: 07/05/2017 Analyzed: 07/10/2017Source: 1706180-01

Copper mg/Kg dry

905.2 21.8 272.0 609.9 D80-1201098.70

Lead mg/Kg dry

301.9 10.9 272.0 36.80 D80-12097.53.26

Molybdenum mg/Kg dry

1114 43.5 1088 23.99 D80-12010010.9

Nickel mg/Kg dry

598.9 21.8 544.0 32.52 D80-1201046.53

Selenium mg/Kg dry

286.9 21.8 272.0 19.81 D80-12098.26.53

Zinc mg/Kg dry

2728 43.5 544.0 2122 D80-12011110.9

Matrix Spike Dup Prepared: 07/05/2017 Analyzed: 07/10/2017Source: 1706180-01

Aluminum mg/Kg dry

16710 444 2219 11820 20 D80-120220 3.09111

Arsenic mg/Kg dry

279.6 22.2 277.4 ND 20 D80-120101 0.8956.66

Cadmium mg/Kg dry

158.3 11.1 138.7 12.14 20 D80-120105 3.232.22

Chromium mg/Kg dry

290.3 22.2 221.9 68.41 20 D80-120100 1.464.44

Copper mg/Kg dry

884.5 22.2 277.4 609.9 20 D80-12099.0 2.318.88

Lead mg/Kg dry

311.2 11.1 277.4 36.80 20 D80-12098.9 3.033.33

Molybdenum mg/Kg dry

1151 44.4 1110 23.99 20 D80-120102 3.2611.1

Nickel mg/Kg dry

622.4 22.2 554.8 32.52 20 D80-120106 3.856.66

Selenium mg/Kg dry

296.0 22.2 277.4 19.81 20 D80-12099.6 3.126.66

Zinc mg/Kg dry

2646 44.4 554.8 2122 20 D80-12094.5 3.0411.1

Result

Source

%REC

%REC

Limits RPD

RPD

Limit Notes Analyte

Mercury by CVAA - Quality Control

MDL

Batch 7G05019

Blank Prepared: 07/05/2017 Analyzed: 07/07/2017

Mercury mg/Kg wet

ND 0.0330 U0.0130

LCS Prepared: 07/05/2017 Analyzed: 07/07/2017

Mercury mg/Kg wet

0.3764 0.0330 0.3333 80-1201130.0130

Matrix Spike Prepared: 07/05/2017 Analyzed: 07/07/2017Source: 1706214-08

Mercury mg/Kg wet

0.3734 0.0319 0.3226 ND 80-1201160.0126

Matrix Spike Prepared: 07/05/2017 Analyzed: 07/07/2017Source: 1706214-08

Mercury mg/Kg wet

0.3520 0.0300 0.3030 ND 80-1201160.0118

Matrix Spike Dup Prepared: 07/05/2017 Analyzed: 07/07/2017Source: 1706214-08

Mercury mg/Kg wet

0.2393 0.0319 0.3226 ND 2080-12074.2 43.80.0126

Matrix Spike Dup Prepared: 07/05/2017 Analyzed: 07/07/2017Source: 1706214-08

Mercury mg/Kg wet

0.3483 0.0300 0.3030 ND 2080-120115 1.040.0118

Data Qualifiers

As applicable and where required, the following general qualifiers are associated with the sample results. Additional qualifiers will be specified within the reporting sections of the data package or within the body of the Case Narrative.

Analytical Report Terms and Qualifiers

DL: The detection limit (DL) is defined as the minimum concentration of a substance that can be measured and reported with 99% confidence that the analyte concentration is greater than zero. The DL is supported by the method detection limit (MDL) which is determined from analysis of a sample containing the analyte in a given matrix.

The Limit of Detection is an estimate of the minimum amount of a substance that an analytical process can reliably detect. An LOD is analyte- and matrix-specific and may be laboratory-dependent. This definition is further clarified in the DoD QSM as the smallest amount or concentration of a substance that must be present in a sample in order to be detected at a high level of confidence (99%). At the LOD, the false negative rate ( Type II error) is 1%.

LOD:

The Limit of Quantitation is the minimum level, concentration, or quantity of a target variable (e.g., target analyte) that can be reported with a specified degree of confidence. This term is further clarified within the DoD QSM as the lowest concentration that produces a quantitative result within specified limits of precision and bias.

LOQ:

The presence of a "B" to the right of an analytical value indicates that this compound was also detected in the method blank and the data should be interpreted with caution. One should consider the possibility that the correct sample result might be less than the reported result and, perhaps, zero.

B:

Exceeding quality control criteria are associated with the reported result.*:

When a sample (or sample extract) is rerun diluted because one of the compound concentrations exceeded the highest concentration range for the standard curve, all of the values obtained in the dilution run will be flagged with a

"D".

D:

E: The concentration for any compound found which exceeds the highest concentration level on the standard curve for that compound will be flagged with an "E". Usually the sample will be rerun at a dilution to quantitate the flagged compound. For Metals, the qualifier indicates that the serial dilution was outside of the control limits and the compound should be considered estimated due to the presence of interference.

H1: The result was analyzed outside of the EPA recommended holding time.

The result was extracted outside of the EPA recommended holding time

The sample for this analyte was received outside of the EPA recommended holding time .

H2:

H3:

J: The presence of a "J" to the right of an analytical result indicates that the reported result is estimated. The mass spectral data pass the identification criteria showing that the compound is present, but the calculated result is less than the LOQ. One should feel confident that the result is greater than zero and less than the LOQ.

M: Indicates that the sample matrix interfered with the quantitation of the analyte. In dual column analysis the result is reported from the column with the lower concentration. In inorganics, it indicates that the parameters DL/LOD/LOQ have been raised.

N: The MS/MSD accuracy and/or precision are outside criteria. The predigested spike recovery is not within control limits for the associated parameter.

P: The associated numerical value is an estimated quantity. There is greater than a 40% difference between the two

GC columns for the detected concentrations. The higher of the two values is reported unless matrix interference is obvious or for HPLC analysis where the primary column is reported.

Q: The relative percent difference (RPD) and/or % recovery exceeded limits in the associated Quality Control Criteria

S: The associated internal standard exceeded criteria.

U: The presence of a "U" indicates that the analyte was analyzed for but was not detected or the concentration of the analyte quantitated below the DL.

X:

Y:

Z:

The parameter shows a potential positive bias on a reported concentration due to an ICV or CCV exceeding the upper control limit on the high side.

The parameter shows a potential negative bias on a reported concentration due to an ICV or CCV exceeding the lower control limit on the low side.

The parameter shows lack of confirmation/detection, which may be due to a negative bias in the ICV or CCV which exceeds the lower control limit.

B1 The BOD Blank concentration was non-detect but DO depletion exceeded the method specified concentration of 0.20 mg/L

ANALYTICAL REPORT

TestAmerica Laboratories, Inc.

TestAmerica Nashville 2960 Foster Creighton Drive Nashville, TN 37204 Tel: (615)726-0177

TestAmerica Job ID: 490-131844-1 Client Project/Site: 1706179

For:

Empirical Laboratories, LLC 621 Mainstream Drive - Suite 270 Nashville, Tennessee 37228

Attn: Teri L Horsley

Authorized for release by:

7/11/2017 1:14:08 PM

Jennifer Gambill, Project Manager I (615)301-5044 jennifer.gambill@testamericainc.com

The test results in this report meet all 2003 NELAC and 2009 TNI requirements for accredited parameters, exceptions are noted in this report. This report may not be reproduced except in full, and with written approval from the laboratory. For questions please contact the Project Manager at the e-mail address or telephone number listed on this page.

This report has been electronically signed and authorized by the signatory. Electronic signature is intended to be the legally binding equivalent of a traditionally handwritten signature.

Results relate only to the items tested and the sample(s) as received by the laboratory.

Table of Contents

Client: Empirical Laboratories, LLC Project/Site: 1706179

TestAmerica Job ID: 490-131844-1

TestAmerica Nashville

7/11/2017

Cover Page

Table of Contents

Sample Summary

Case Narrative

Definitions

Client Sample Results

QC Sample Results

QC Association

Chronicle

Method Summary

Certification Summary

Chain of Custody

Receipt Checklists

Sample Summary TestAmerica Job ID: 490-131844-1Client: Empirical Laboratories, LLC

Project/Site: 1706179

Lab Sample ID Client Sample ID ReceivedCollectedMatrix

490-131844-1 Lime Sludge 1706179-01 Solid 06/26/17 11:00 06/28/17 15:00

TestAmerica Nashville

Page 3 of 14 7/11/2017

Case Narrative Client: Empirical Laboratories, LLC TestAmerica Job ID: 490-131844-1

Project/Site: 1706179

Job ID: 490-131844-1

Laboratory: TestAmerica Nashville

Narrative

Job Narrative

490-131844-1

Comments

No additional comments.

Receipt

The sample was received on 6/28/2017 3:00 PM; the sample arrived in good condition, properly preserved and, where required, on ice.

The temperature of the cooler at receipt was 1.9º C.

General Chemistry

Method(s) 351.2: Due to the high concentration of TKN, the matrix spike / matrix spike duplicate (MS/MSD) for 442495 could not be evaluated for accuracy and precision. The associated laboratory control sample / laboratory control sample duplicate (LCS/LCSD) met acceptance criteria.

No additional analytical or quality issues were noted, other than those described above or in the Definitions/Glossary page.

TestAmerica Nashville Page 4 of 14 7/11/2017

Definitions/Glossary

Project/Site: 1706179

Qualifiers

General Chemistry

Qualifier DescriptionQualifier

Glossary

These commonly used abbreviations may or may not be present in this report.Abbreviation

DL

DLC

EDL Estimated Detection Limit (Dioxin)

MDA

MDC

MDL Method Detection Limit

ML Minimum Level (Dioxin)

NC Not Calculated

ND Not Detected at the reporting limit (or MDL or EDL if shown)

TestAmerica Nashville

Page 5 of 14 7/11/2017

Client Sample Results

Project/Site: 1706179

Lab Sample ID: 490-131844-1Client Sample ID: Lime Sludge 1706179-01 Matrix: SolidDate Collected: 06/26/17 11:00

Date Received: 06/28/17 15:00

General Chemistry

RL MDL

Kjeldahl Nitrogen as N 11600 ^ 400 208 mg/Kg 06/30/17 09:53 07/03/17 16:18 20

Analyte Dil FacAnalyzedPreparedUnit DResult Qualifier

TestAmerica Nashville

Page 6 of 14 7/11/2017

QC Sample Results

Project/Site: 1706179

Method: 351.2 - Nitrogen, Total Kjeldahl

Client Sample ID: Method BlankLab Sample ID: MB 490-441776/1-A

Matrix: Solid Prep Type: Total/NA

Analysis Batch: 442495 Prep Batch: 441776

RL MDL

Kjeldahl Nitrogen as N ND 25.0 13.0 mg/Kg 06/30/17 09:53 07/03/17 16:05 1

MB MB

Analyte Dil FacAnalyzedPreparedDUnitResult Qualifier

Client Sample ID: Lab Control SampleLab Sample ID: LCS 490-441776/2-A

Matrix: Solid Prep Type: Total/NA

Analysis Batch: 442495 Prep Batch: 441776

Kjeldahl Nitrogen as N 250 233.0 mg/Kg 93 80 120

Analyte

LCS LCS

DUnitResult Qualifier %Rec

Spike

Added

%Rec.

Limits

TestAmerica Nashville

Page 7 of 14 7/11/2017

QC Association Summary

Project/Site: 1706179

General Chemistry

Prep Batch: 441776

Lab Sample ID Client Sample ID Prep Type Matrix Method Prep Batch

Solid 351.2Total/NA

Solid 351.2Total/NA

Solid 351.2Lab Control Sample Total/NA

Analysis Batch: 442495

Lab Sample ID Client Sample ID Prep Type Matrix Method Prep Batch

Solid 351.2 441776Total/NA

Solid 351.2 441776Lab Control Sample Total/NA

Analysis Batch: 442496

Lab Sample ID Client Sample ID Prep Type Matrix Method Prep Batch

Solid 351.2 441776Total/NA

TestAmerica Nashville

Page 8 of 14 7/11/2017

Lab Chronicle Client: Empirical Laboratories, LLC TestAmerica Job ID: 490-131844-1

Project/Site: 1706179

Client Sample ID: Lime Sludge 1706179-01 Lab Sample ID: 490-131844-1 Matrix: SolidDate Collected: 06/26/17 11:00

Date Received: 06/28/17 15:00

Prep 351.2 LDT06/30/17 09:53441776

Type

Batch

Method

Batch

Prep Type LabAnalystRun

Prepared or Analyzed

Initial

Amount Amount

Final Batch

NumberFactor

Dil

Total/NA 0.25 g 20 mL

Analysis 351.2 20 442496 07/03/17 16:18Total/NA

Laboratory References:

TestAmerica Nashville

Page 9 of 14 7/11/2017

Method Summary

Project/Site: 1706179

Method Method Description LaboratoryProtocol

351.2 Nitrogen, Total Kjeldahl

Protocol References:

MCAWW = "Methods For Chemical Analysis Of Water And Wastes", EPA-600/4-79-020, March 1983 And Subsequent Revisions.

Laboratory References:

TAL NSH = TestAmerica Nashville, 2960 Foster Creighton Drive, Nashville, TN 37204, TEL (615)726-0177

TestAmerica Nashville

Page 10 of 14 7/11/2017

Page 13 of 14 7/11/2017

OFFICE OF THE MISSOURI STATE CHEMIST

June 30, 2017

Teri Horsley

Empirical Laboratories, LLC

621 Mainstream Drive, Suite 270

Nashville, TN 37228

Dear Ms. Horsley:

The following report includes the analyses on the sample submitted to the Experiment Station

Chemical Laboratories on June 27, 2017. The sample is reported on an as received basis.

A University of Missouri Invoice will be sent to you by the Accounting Department for payment for the analysis of this sample.

ESCL Sample No. 09522

Sample ID Lime sludge

Free water, w/w% 72.0

ENM*, #/ton 189

CCE**, w/w% 23.6

US Std. Sieve, retained weight

% +8 0.0

% -8 +40 0.0

% -40 + 60 0.0

% -60 100.0

Fineness Factor 100.0

Reference standards were performed with these analyses. The original results will be on file in our office and are available for review by you on request. We are glad that we have been able to perform these tests for you and we look forward to being of service to you again. Please contact us if you have any questions.

Sincerely, Paul K. Eggeman Dr. Thomas P. Mawhinney

Supervisor Fertilizer Laboratory Director *ENM - Effective Neutralizing Value **CCE - Calcium Carbonate Equivalence