Final Checklist July 9, 2010 

### Steam Study Data Review Checklist Standard Operating Procedure (SOP) for Inductively Coupled Plasma Mass Spectrometry for Trace Element Analysis in Flue Gas

Desulfurization Wastewaters

SECTION A

- 1. Sample Identifiers

Laboratory Name:

Sampling Episode : Sample Numbers or Range: Data Reviewer signature: Date:

Instructions: Complete this checklist electronically or using a ballpoint pen.

Record reviewer comments in the Reviewer Comment section.

Record detailed information in the Comments in the “Overa ll Assessment”

section for each criterion not (“N”) met. Note: Requirements with a * are project requirements not specific to The Standard Operating Procedures (SOP) for Inductively Coupled Plasma Mass Spectrometry for Trace Element Analysis in Flue Gas Desulfurization (FGD) Wastewaters (FGD SOP).

Note: The FGD SOP is based on EPA Method 200.8 and 1638, but optimized for FGD wastewater. Some r equirements listed in 200.8 are still required even if they are not explicitly stated in the FGD

SOP. These requirements are indicated with a **

.



### SECTION A

- 2. OVERALL ASSESSMENT OF THE QUALITY OF THE DATA

General Comment Checklist

Deliverable Requirement Review

Level Require d Present Comments

Copies of Shipping Documents (Fed

- Ex Airbills) 1, 2, 3

Case Narrative 1, 2, 3

Table of Contents 3

Cross reference of Field Sample No., Lab Sample No., and Analytical Batch 1, 2, 3

Traffic Report Form (including Sample Receipt Checklist) 1, 2, 3

Sample Calculation (usually just a page copied

from S OW) 3

Results Summary for Each Sample and Blank 1, 2, 3

Method Detection Limit Study 3Steam Study Data Review C hecklist Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters Page 2 of 9

Final Checklist July 9, 2010 

### SECTION A

- 2. OVERALL ASSESSMENT OF THE QUALITY OF THE DATA

General Comment Checklist

Deliverable Requirement Review

Level Require d Present Comments
Instrument Detection Limit Study 3

Linear Range Study Results (if reported) 3

Initial and On

- going Demonstration of Capability 3

Instrument Tuning Res ults ( including mass calibration and mass resolution checks) 3

Mass 75 Interference Check Results 3

Initial Calibration Results 3

Initial Calibration Verification 3

Initial Calibration Blank 3

Reporting Limit Verification Standard Results 3

Laboratory Reagent Blank (LRB) Results 2, 3

Laboratory Fortified Blank Results 2, 3

Individual Interference Check Solution Results (if reported) 2, 3

Synthetic FGD Interference Check Solution 2, 3

Laboratory Fortified Synthetic FGD Solution 2, 3

Matrix Spike/Matrix Spike Duplicate Results 2, 3

Internal Standardization Results 2, 3

Continuing Calibration Verification Standard

Results 3

Continuing Calibration Blank (CCB) Results 3

Field Duplicate Results 2, 3

Data for all Mass es Monitored (e.g. all relevant isotopes) (if reported) 3

Quantitation List 3

Copies of Sample Preparation Work Sheets 3

Copies of Run Logs 3

Level 1 : Review of traffic reports, sample handling, and proper sample preparation

Level 2: Level 1 re view plus review of QA/QC results

Level 3: Level 2 review plus review of instrument performance

Level 4: Level 3 review plus analysis of raw data such as chromatograms or primary instrument

outputSteam Study Data Review C hecklist Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters Page 3 of 9

Final Checklist July 9, 2010



### FGD SOP / EPA METH OD 200.8 REQUIREMENT Reviewer Comment Cr iterion

met

Y N


### SECTION B. SAMPLE RECEIPT

1. Reviewed Sample Collection Record:

**•** Signatures?

**•** Completed?

**•** Sample ID numbers checked?

**•** Preservations? pH? Volume?

**•** Any anomalies reported?

2. Reviewed Lab Sample Receipt Record :

**•** Date received?

**•** Lab ID number c hecked?

**•** Lab ID number referenced to Sample ID

n umbers ?

**•** Preservation checked by lab? pH? Temp?

Volume?

**•** Sample c onditions

**•** Sample hold time

**•** Any anomalies reported by lab ?


### SECTION C . SAMPLE PREPARATION/EXTRACT HANDLING

INFORMATION

1. Reviewed Standard Pre lo gs:

**•** Standard expiration date:

**•** Concentrations prepared?

2. Reviewed Sample Prep Logs:

**•** Sample extraction date :

**•** Sample process or run date:

3. *Field Duplicates: Was a field duplicate collected and analyzed as part of the sampling episode?

Indicate the re lative percent difference.Steam Study Data Review C hecklist Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters Page 4 of 9

Final Checklist July 9, 2010



### FGD SOP / EPA METH OD 200.8 REQUIREMENT Reviewer Comment Cr iterion

met

Y N


### SECTION D

- 1. QC INFORMATION

– Method Performance

1. Review Lab’s Instrument Run Log Report: Were calibrations, QC samples and samples included in a batch of 20 samples?

2. Method Detect ion Limit Study (MDL): For each analyte of interest, were seven samples containing a

concentration of 3

- 5 times the MDL prepared using the synthetic FGD wastewater matrix and analyzed according to the methods in Section 10 of the FGD

SOP? Was an MDL study conducted before samples were analyzed, and repeated every year? (FGD SOP/12.1) What were the MDLs reported by the lab?

3. Instrument Detection Limit Study: For each mass used during the analysis, was an IDL study conducted q uarterly? During the IDL study was the analysis of 10 blanks run on three non

- consecutive days used to calculate the IDL? (FGD SOP/12.3) What were the IDLs reported?

4. Demon stration of Capabilities: Was an initial demonstration of proficiency (IDOC) performed prior to analysis of samples and was on

- going proficiency demonstrated annually? (FGD SOP/12.5) What were IDOCs reported by the lab?

Date IDOCs were done?


### SECTION D

- 2. QC INFORMATION

– Instrument Calibration

1. Instrument: Was an Inductively Coupled Plasma Spectrometer (ICP/MS) capable of providing th e resolution characteristics specified in Section 6.1 of the FGD SOP used for analysis? Was the ICP/MS used in the analysis equipped with a collision cell, a discrete sample introduction system, and an autosampler? (FGD SOP/6.1)Steam Study Data Review C hecklist Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters Page 5 of 9

Final Checklist July 9, 2010



### FGD SOP / EPA METH OD 200.8 REQUIREMENT Reviewer Comment Cr iterion

met

Y N

2. Instrument Tuning/Mass Calibration: Was the instrument tuned using a solution containing elements that represented all mass regions of

interest? Was the tuning solution used to run mass calibration and mass resolution checks at the beginning of every day?

Were the relative stan dard deviations less than 5% for at least four integrations of the tuning solution? (FGD SOP/10.3.2)

Were the mass calibration check results within 0.1 amu of the true value? (FGD SOP/10.3.2)

Were the mass resolution check results less than 0.9

amu full w idth at 10% peak height? (FGD SOP/10.3.2)

What were the elements and concentration of the tuning solution? If reported where was it p urchased

from? What were the reported results for instrument tuning? What was the lab’s reported results for mass

calibration check and mass resolution check?

3. Mass 75 Interference check: Were the counts per

second for mass 75 less than 10 when the blank matrix was infused? (FGD SOP/10.3.3)

4. Initial Calibration: Was the ICP/MS calibrated daily with a calibration blank and 3 calibration standards? (FGD SOP/10.3.4)

Indicate the true and analyzed concentration s of the

3 calibration standards us ed by lab

. If reported, w hat type of curve fit was used?Steam Study Data Review C hecklist Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters Page 6 of 9

Final Checklist July 9, 2010



### FGD SOP / EPA METH OD 200.8 REQUIREMENT Reviewer Comment Cr iterion

met

Y N

5. Initial Calibration Verification (ICV): Was an ICV standard (i.e., a standard from a different

vendor than the calibration stand ards) analyzed after

initial calibration? Was the percent recovery of the ICV sample within

90

- 110%? (FGD SOP/10.3.5) Note: The ICV standard satisfies the Quality Check Standard (QCS) requirement in 200.8.

What was the true concentration of the ICV

stand ard?

What w ere the reported results and % recovery ? If reported, indicate w here the ICV was purchased

from and the date purchased?

6. Initial Calibration Blank (ICB): After the ICV, was the ICB analyzed and were the results less than

the reporting limit (RL)? (FGD SOP/10.3.6) Indicate the concentration in the ICB, the RL, and

note any contamination reported by the lab.

7. Reporting Limit Verification Standard: After the ICB, was a RL verification standard analyzed and

were the resu lts within 50% of the expected value? If not, was the associated data qualified? (FGD SOP/10.3.7)

What was the result of the RL verification standard analyzed?

What was the percent recovery of the RL ?


### SECTION D

- 3 . QC INFORMATION

– Blanks

1. Method Blank/Laboratory Reagent Blank (MB/LRB): Was a MB/LRB containing reagent water processed in the same way as the samples and analyzed wit h each batch of 20 samples ? For all analytes of interest, was the concentration in

the blank < RL ? (FGD SOP/ 9.6) Indicate the concentration in the MB/LRB, the RL,

and note a ny contamination reported by the lab

.Steam Study Data Review C hecklist Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters Page 7 of 9

Final Checklist July 9, 2010



### FGD SOP / EPA METH OD 200.8 REQUIREMENT Reviewer Comment Cr iterion

met

Y N

2. Laboratory Control Sample/Laboratory Fortified Blank (LCS/LFB): Was a LCS/LFB containing all analytes of interest analyzed with each batch and was the percent recovery for all analytes within the

control limits of 85

- 115%? (FGD SOP/ 9.7) (200.8/7.9/9.3. 2)

What were the concentrations of all analytes in the LCS reported by the lab?

What were the % recover ies of all the analytes?


### SECTION D

- 4 . QC INFORMATION

- Instrument Per formance Checks

1. Synthetic FGD Interference Check Solution: Before initiating analysis and immediately after

calibration , was the synthetic FGD matrix solution specified in Section 7.2.7 of the FGD SOP analyzed?

Were all results for elements of interest < the RL unless the presence of an element can be confirmed

and in this case was the result < 5 times the RL? If dilution was required to analyze the synthetic

FGD solution , were all samples and QC samples diluted by the same factor? (FGD SOP/ 9.4)

2. Lab oratory Fortified Synthetic FGD Solution: Following the analysis of the synthetic FGD matrix, was a synthetic FGD solution spiked with each analyte of interest analyzed? Was the percent recovery between 70

– 130% of the

true value? Indicate the percent re covery for all analytes. If dilution was required to analyze the laboratory fortified synthetic FGD solution, were all samples and QC samples diluted by the same factor? (FGD

SOP/ 9.4 .1 )

3. Analytical Run Sequence: Was the following analytical run sequenc e used: instrument initialization, warm

- up, instrument tuning, mass calibration check, mass resolution check, tuning criteria validation, calibration blank, calibration standard, ICV, ICB, RL verification standard, CCV, CCB, 10 samples, CCV, and CCB. (FGD SOP/10.4.5)Steam Study Data Review C hecklist Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters Page 8 of 9

Final Checklist July 9, 2010



### FGD SOP / EPA METH OD 200.8 REQUIREMENT Reviewer Comment Cr iterion

met

Y N

4. Matrix Spike/Matrix Spike Duplicate/Laboratory Fortified Sample Matrix /Laboratory Fortified Sample Matrix Duplicate (MS/MSD/LFM/LFMD): Was one MS/MSD pair analyzed for every 10 samples? (FGD SOP/ 9.8) *Was a MS/MSD sample analyzed for ea ch midpoint and effluent point in a sampling episode? Was the percent recovery of the MS/MSD for all analytes within the control limits of 70

- 130% and

was the RPD ≤ 20%? (FGD SOP/9.8)

What were the % recover ies for all analytes? What were the RPDs reported by the lab?

5. Internal Standardization: Were responses from internal standards evaluated throughout each set of samples? (200.8/9.4.5)

Were results for all internal standards within 60

- 125% of the intensity in the calibration blank and if not, was the calibration blank reanalyzed? If the

results for the second calibration blank met the required QC criteria, was the sample diluted by a factor of 2 and rerun? (FGD SOP/ 9.9)

6. Continuing Calib ration Verification (CCV)

Standard: Was a 50 μg/L CCV standard tested at the beginning and end of each run and after the analysis of 10 samples and was the percent recovery

within 85

- 11 5 %? (FGD SOP/10.3.8) What were results reported fo r the CCV and the

percent recovery ?

7. Continuing Calibration Blank (CCB): Was a CCB analyzed after each CCV and were results less than the RL? (FGD SOP/10.3.6) Indicate the result for the CCB, the RL, and any contamination noted by the lab.


### SECTION E

. DATA REVIEW

– Sample Results

1. Calculations: Were all percent recoveries and relative percent differences for QC samples calculated according to the formulas presented in

Section 11.0 in the FGD SOP. Was the final concentration of an aqueous and digested solid sample calculated based on the formulas presented in Section 11.5 and 11.6 respectively of the FGD SOP?Steam Study Data Review C hecklist Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters Page 9 of 9

Final Checklist July 9, 2010



### FGD SOP / EPA METH OD 200.8 REQUIREMENT Reviewer Comment Cr iterion

met

Y N

2. Sample Results Reporting: For each field and QC sample analyzed, was the average of at least three integrations reported? (FGD SOP/10.4.1)

**W ere results reported in units of mic rograms per liter (μg/L)? **Were analyte concentrations below the MDL not reported? (200.8/12.1)

3. Dilutions: If the concentration of an analyte was above the linear range, was the sample diluted and reanalyzed? Was dilution not used for samples contai ning an analyte concentration < 5 times the RL? (FGD SOP/10.4.4)

4. Analysis of Interferences: Were interferences not removed by the collision cell evaluated? Were corrections applied to the data and if problems remained were they flagged? Were the

recomm ended elemental equations in Attachment 1

of the FGD SOP used and was internal standardization implemented to correct for both positive and negative interferences caused by the sample matrix? (FGD SOP/2.4/4.0)