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 “Overall 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 requirements 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

Required 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 SOW)

3

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

Method Detection Limit Study 3
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Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters 

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Final Checklist July 9, 2010

SECTION A-2. OVERALL ASSESSMENT OF THE QUALITY OF THE DATA

General Comment Checklist

Deliverable Requirement

Review 

Level

Required Present Comments

Instrument Detection Limit Study 3

Linear Range Study Results (if reported) 3

Initial and On-going Demonstration of Capability 3

Instrument Tuning Results (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 Masses 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 review 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 

output
Steam Study Data Review Checklist

Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters 

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Final Checklist July 9, 2010

FGD SOP/EPA METHOD 200.8

REQUIREMENT Reviewer Comment

Criterion

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 checked?

• Lab ID number referenced to Sample ID 

numbers?

• Preservation checked by lab? pH? Temp? 

Volume?

• Sample conditions

• Sample hold time

• Any anomalies reported by lab?

SECTION C. SAMPLE PREPARATION/EXTRACT HANDLING 

INFORMATION

1. Reviewed Standard Pre logs: 

• 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 relative percent difference.
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Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters 

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Final Checklist July 9, 2010

FGD SOP/EPA METHOD 200.8

REQUIREMENT Reviewer Comment

Criterion

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 Detection 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 quarterly? 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. Demonstration 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 the 

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)
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Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters 

Page 5 of 9

Final Checklist July 9, 2010

FGD SOP/EPA METHOD 200.8

REQUIREMENT Reviewer Comment

Criterion

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 standard 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 width at 10% peak height? (FGD 

SOP/10.3.2)

What were the elements and concentration of the 

tuning solution? If reported where was it purchased 

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 concentrations of the 

3 calibration standards used by lab. 

 If reported, what type of curve fit was used? 
Steam Study Data Review Checklist

Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters 

Page 6 of 9

Final Checklist July 9, 2010

FGD SOP/EPA METHOD 200.8

REQUIREMENT Reviewer Comment

Criterion

met

Y N

5. Initial Calibration Verification (ICV): Was an 

ICV standard (i.e., a standard from a different 

vendor than the calibration standards) 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 

standard? 

What were the reported results and % recovery? 

If reported, indicate where 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 results 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 with 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 any contamination reported by the lab.
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Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters 

Page 7 of 9

Final Checklist July 9, 2010

FGD SOP/EPA METHOD 200.8

REQUIREMENT Reviewer Comment

Criterion

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 % recoveries of all the analytes?

SECTION D-4. QC INFORMATION - Instrument Performance 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. Laboratory 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 recovery 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 sequence 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)
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Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters 

Page 8 of 9

Final Checklist July 9, 2010

FGD SOP/EPA METHOD 200.8

REQUIREMENT Reviewer Comment

Criterion

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 each 

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 % recoveries 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 Calibration 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 85-115%? (FGD SOP/10.3.8) 

What were results reported for 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 Checklist

Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters 

Page 9 of 9

Final Checklist July 9, 2010

FGD SOP/EPA METHOD 200.8

REQUIREMENT Reviewer Comment

Criterion

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)

**Were results reported in units of micrograms 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 containing 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 

recommended 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)