UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
REGION IX
75 Hawthorne Street
San Francisco, Ca. 94105
LABORATORY DOCUMENTATION REQUIREMENTS
FOR DATA VALIDATION
Document Control Number 9QA-07-90
January. 1990
Quality Assurance Management Section
DSEPA Region 9
San Francisco, California
Prepared by:
Santiago M. Lee
ESAT/ICF Technology Incorporated
San Francisco. CA
-------
TABLE OF CONTENTS
Introduce ion
Z . Organic
I. A.
I.B.
i.e.
Z.D.
I.E.
I.F.
i.e.
Analyses
Case Narrative
Summary of Environmental Results
Summary of QA/QC Results
I.E.I. Instrument Calibration
I.E. 2. Method Blank Analysis
I.E. 3. Surrogate Standard Recovery...
I. E.4. Precision and Accuracy
I.E. 5. Other QC Analyses
I.F.I. CC Analyses
I.F. 2. CC/MS Analyses
Summary of Documentation Requirements . .
XI. Inorganic Analyses
II. A.
II. B.
II. C.
II. D.
II. E.
II. F.
II. C.
Documentation
Case Narrative
Chain -of -Custody Documentation
Summary of Environmental Results
Summary of QA/QC Results
II. E.I. Instrument Calibration
II. E. 2. Method Blank Analysis
II. E. 3. ICP Interference Check Sample.
II. E. 4. Precision and Accuracy
II. E. 5. Other QC Analyses
Rav Data
Summary of Documentation Requirements..
Page
1
2
2
2
2
3
3
3
A
tt
h
5
5
5
6
7
6
8
8
8
9
9
9
10
10
10
11
12
13
Rev.
0
0
•o
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
Date
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
9/89
-------
Page Rev. Date
III. QA/QC Requirements Summaries 1* 0 9/89
III.A. CC/HS Organics Analyses 14 0 9/89
XXI.B. Pesticides and FCBs 16 0 9/89
IIX.C. Furgeables by GC 16 0 9/89
XXX.D. Metals Analyses 20 0 9/89
Li
-------
Section No.:
Revision No.: 1
Dace: 1/9/90
Page:_L_ of 21
INTRODUCTION
In all hazardous site investigations, it is essential to know the quality of
the data used for decision-making purposes. The process of generating data of
known quality begins in the planning stages when data quality objectives
(DQOs) are established, continues during sample collection activities and
laboratory analysis, and is completed by validating the analytical data. This
document was created to identify the specific laboratory documentation
requirements necessary for data validation.
Validation of data requires that appropriate QA/QC and documentation steps be
performed in both the lab and the field. Professionals trained in data
validation procedures review this information, "flag" data with qualifiers
when QA/QC criteria are not met, and prepare the data validation report.
The "P.K. Memo" and ICF/ESAT documents, which have previously addressed non-
CLP documentation requirements, have been incorporated into this document.
The general requirements are discussed here, but for ease of use it has been
formatted into two (2) sections, pertaining to the organic and inorganic
analyses. In addition to the documentation requirements, a new and separate
section for non-CLP QA/QC requirements was created.
The documentation provided by the laboratory in conjunction with the sample
results, allows for the evaluation of the following indicators of data
quality:
• Integrity and stability of the samples
• Instrument performance during sample analysis
• Possibility of sample contamination
• Identification and quantitation of analytes
• Precision
• Accuracy of the analytical results
-------
THIS IS A BLANK PAGE
-------
Section No. :
Revision No.: r>
Dace: 9/29/89
Page:_2_ of 21
I. ORGANIC ANALYSES
I. A. Documentation
The data package submitted for EPA data validation will consist of
five (5) sections:
• Case narrative
• Chain-of-Custody documentation
• Summary of results for environmental samples
(including quantitation limits)
• Summary of QA/QC results
• Raw data
I.B. Case Narrative
The case narrative will be written on laboratory letterhead and the
release of data will be authorized by the laboratory manager or
his/her designee. The Case Narrative will consist of the following
information:
• Client's sample identification and the corresponding laboratory
identification
• Parameters analyzed for each sample and the methodology used: vhen
applicable, cite EPA method numbers
• Whether the holding times were met or exceeded
• Detailed description of all problems encountered
• Discussion of possible reasons for any QA/QC criteria outside
acceptance limits
• Observations regarding any occurrences which may affect sample
integrity or data quality
I.C. Chain-of-Custody Documentation
Legible copies of Chain-of-Custody forms for. each sample shall be
submitted in the data package. The date of receipt and the observed
sample condition at the time of receipt must be described on the
Chain-of-Custody form. Any internal laboratory tracking document
should be included.
-------
Section So.: I
Revision .So. : Q_
Dace: 9/29/89
Page:_3_ of 21
I.D. Summary of Environmental Results
The following information is to be included in the summary of results
for each environmental sample. The summary should follow the CLP
format if possible, but ocher formats are acceptable provided thac all
necessary information is included.
• Client's sample identification and the corresponding laboratory
identification
• Sample matrix
• Date of sample extraction, as applicable
• Date and time of analysis
• Identification of the instrument used for analysis
• GC column and detector specifications
• Weight or volume of sample used for analysis/extraction
• Dilution or concentration factor for the samples
• Percentage of moisture in Che soil samples
• Method detection limits (MDL) or sample quantitation limits
• Definitions for any data qualifiers used
• Analytical results
I.E. Summary of QA/QC Results
The following QA/QC results will be presented in a summary. These
summaries should follow the CLP format, if possible. Other formats
may be acceptable provided that all necessary information is included
and the summary is easy to follow. These summaries will require to
have all the information stated in Section I.D.
I.E.I. Instrument Calibration (for each instrument used)
Initial Calibration
Report the concentrations of the initial calibration
standards and the date and time of analysis. List the
response factor (RF), percent relative standard deviation
(%RSD). and retention time (for GC analyses) for each
analyte.
-------
Section No.:
Revision No.:
Dace: 9/29/89
Page:Ji_ of 21
Daily Calibration and Kid-level Standard
Report the concentration of che calibration standard used for
the daily calibration and for the mid-level standard, and the
date and time of analysis. List che response factor (RF).
percent difference (%D). and retention time (for GC analyses)
for each analyte.
I.E.2. Method Blank Analysis
List the environmental samples and QC analyses associated
with each method blank. Report the concentrations of any
analytes found in the method blanks.
I.E.3. Surrogate Standard Recovery
Report the name and concentration of each surrogate compound
added. List the percent recoveries of all surrogates in the
samples, method blanks, matrix spike/matrix spike duplicates
and other QC analyses.
I.E.4. Precision and Accuracy
• Matrix spike/matrix spike duplicate (MS/MSD) analysis
Report the name and concentration of each spiking compound.
Samples are to be spiked with all specified compounds of
interest. List the sample results, spiked sample results.
percent recovery and the relative percent difference (RPD)
• Laboratory duplicate analysis, as applicable.
Report the relative percent difference (RPD) between
duplicate analyses.
• Laboratory QC check sample analysis
Report the percent recovery for each analyte in the
laboratory QC check sample. List the acceptable control
limits.
-------
Seccion No.:
Revision No.:
Date: 9/29/89
Page: 5 of 21
I.E.5. Other QC Criteria
• Retention time windows determination (GC)
Report the retention time window for each analyte. for both
primary and confirmation analyses.
Retention time windows are established by performing 3 .
analyses of standards for all analytes being measured
throughout the course of a 72-hour period. The retention
time window is defined as plus or minus 3 times the standard
deviation of the absolute retention time. Retention time
windows are to be updated daily.
• Compound identification (CC)
Report the retention times and the concentrations of each
analyte detected in the samples for both primary and
confirmation analyses.
• Method detection limits (HDL) determination
List the method detection limits.
Method detection limits are determined by performing at least
7 analyses of standards for all analytes measured at 2-5
times the required detection limit concentrations. The
method detection limits are calculated as 3 times the
standard deviation of the measured values. Refer to &0 CFR
Part 136 Appendix B.
I.F. Raw Data
Z.F.I. GC Analyses
This section shall include legible copies of the raw data for
the following:
• Environmental samples (arranged in increasing client's
sample number order).
The raw data for both the primary and confirmation analyses
are to be included.
• Instrument calibrations
• QC analyses
-------
Seccion No.:
Revision No.: 0
Dace: 9/29/89
Page:_6_ of 21
• Sample extraction and clean-up logs
• Instrument analysis logs for each instrument used
• GC/KS confirmation, as applicable
The rav data for each analysis shall include the following:
• Chromatograms (label all analyte peaks, internal standards
and surrogate standards with chemical names)
• Area print-outs or quantitation reports
I.F.2. GC/XS Analyses
This section shall include legible copies of the raw dacs for
the following:
• Environmental samples (arranged in increasing client's
sample number order)
• Mass and spectrometer tuning and mass calibration (BFfi:
DFTPP)
• Initial and continuing instrument calibrations
• QC analyses
• Sample extraction and clean-up logs
• Instrument analysis logs for each instrument used
The raw data for each analysis shall include the following:
• Chromatograms (label all analyte peaks, internal standards
and surrogate standards with chemical names)
• Enhanced spectra of target analytes and tentatively
identified compounds (TICs). with the associated best-
match spectra
• Quantitation reports
Legible copies of the raw data shall be organized systematically, and
each page shall be numbered. The raw data for compound identification
and quantitation must be sufficient to verify each result presented in
Sections I.D. and I.E.
-------
THIS IS A BLANK FACE
-------
Section No.:
Revision No.:
Dace: 9/29/89
Pa§c:_2_ of 21
I.C. SUMMARY OF DOCUMENTATION REQUIREMENTS
Organic Data
Seccion I. Case Narracive
Section II. Chain-of-Custody Documentation
1. Chain-of-Custody forms
2. Internal tracking documents, as applicable
Seccion III. Summary of Results - Forms for the following:
1. Environmental samples, with quantitation limits
(include dilutions and re-analyses)
Section IV. QA/QC Results Summaries
1. Initial calibration
2. Continuing calibration
3. Method blanks
6. Surrogate recoveries
5. Matrix spike (MS)
6. Laboratory duplicate or matrix spike duplicate (MSD)
7. Laboratory QC check sample, if applicable
8. Retention time windows
9. Method detection limits (MDL)
Seccion V. Raw Data - chromacograms and area/quantization reports
1. Environmental samples (include dilutions and re-analyses)
2. Instrument tuning, for mass spectrometry (GC/MS) analyses
3. Initial calibration
&. Continuing calibration
5. Method blanks
6. Surrogate recoveries
7. Matrix spike (MS)
8. Laboratory duplicate or matrix spike duplicate (MSD)
9. Laboratory QC check sample, as applicable
10. Retention time windows
11. Percent moisture for soil samples
12. Sample extraction and clean-up logs
13. Instrument analysis log for each instrument used
-------
THIS IS A BLANK PAGE
-------
Section No.:
Revision No.:
Date: 9/29/89
Page:_8_ of 21
II. INORGANIC ANALYSES
II.A. Documentation
The data package submitted for EPA data validation will consist of
five (5) sections:
• Case narrative
• Chain-of-Custody documentation
• Summary of results for environmental samples
(including quantitation limits)
• Summary of QA/QC results
• Raw data
II.B. Case Narrative
The case narrative will be written on laboratory letterhead and the
release of data will be authorized by the laboratory manager or
his/her designee. The Case Narrative will consist of the following
information:
• Client's sample identification and the corresponding
laboratory identification
• Parameters analyzed for each sample and the methodology used:
when applicable, cite EPA method numbers
• Whether the holding times were met or exceeded
• Detailed description of all problems encountered
• Discussion of possible reasons for any QA/QC criteria outside
acceptance limits
• Observations regarding any occurrences which may affect
sample integrity or data quality
II.C. Chain-of-Custody Documentation
Legible copies of Chain-of-Custody forms for each sample shall be
submitted in the data package. The date of receipt and the observed
sample condition at the time of receipt must be described on the
Chain-of-Custody form.
-------
Section No.:
Revision No.: 0
Date: 9/29/89
Page:_9_ of 21
II.D. Summary of Environmental Results
The following information is to be included in the summary of results
for each environmental sample. The summary should follow the CLP
format if possible, but other formats are acceptable provided that all
necessary information is included.
• Client's sample identification and the corresponding
laboratory identification
• Sample matrix
• Date of sample digestion, as applicable
• Date and time of analysis
• Identification of the instrument used for analysis
• Instrument specifications
• Weight or volume of sample used for analysis/digestion
• Dilution or concentration factor for the samples
• Percentage of moisture in the soil samples
• Instrument detection limits (IDL) or method detection limits
(MDL)
• Definitions for any data qualifiers used
• Analytical results
II.E. Summary of QA/QC Results
The following QA/QC results will be presented in a summary. These
summaries should follow the CLP format, if possible. Other formats
are acceptable provided that all necessary information is included and
the summary is easy to follow. These summaries will require to have
all information stated in Section II.D.
II.E.I. Instrument Calibration
The order of reporting of calibrations for each analyte muse
follow the temporal order in which the standards were
analyzed.
-------
Section No.:
Revision No.: 0_
Date: 9/29/89
Page: 10 of 21
Initial Calibration Verification
Report the source for the calibrations standards. Report the
concentration for the true value, the concentration found,
and the percent recovery for each element analyzed. Record
the date and time of analysis.
Continuing Calibration Verification
Report the source for the calibrations standards. Report the
concentration for the true value, the concentration found.
and the percent recovery for each element analyzed. Record
the date and time analysis.
Report results for (low-level) standards used to verify
instrument sensitivity (that the reported detection limits
can be achieved) in the manner described for continuing
calibration verification.
II.E.2. Method Blank Analysis
Report analyte concentrations found in the initial
calibration blank (ICB). the continuing calibration blank
(CCB). and in the preparation blank. Record the date and
time of analysis.
The order of reporting ICB and CCB for each analyte must
follow the temporal order in which the blanks were analyzed.
II.E.3. ICF Interference Check Sample
Identify the source for the interference check sample.
Report the true value, the initial and final results and the
calculated percent recovery.
II.E.4. Precision and Accuracy
• Matrix spike (MS) analysis
Report the concentration of the spiked sample result, the
sample result and the spiking solution added for each element
in the predigestion spike. Calculate and report the percent
recovery and list the control limits.
• Post Digest Spike
In addition to matrix spikes, post-digest spikes are analyzed
during furnace analysis. Report the concentration of the
spiked sample result, the sample result, and the spiking
-------
Section No.: II
Revision No.: 0
Date: 9/29/89
Page:_ll_ of _21_
solution added for each element. Calculate and report the
percent recovery and list the control limits.
• Laboratory Duplicate Analysis
Report the original concentration, duplicate concentration
and relative percent difference (RPD). List the control
limits.
• Laboratory Control Sample
Identify the source for the laboratory control sample.
Report the concentration of the spiked sample result, the
sample results and the spiking solution added for each
element analyzed. Calculate and report the percent recovery
and list the control limits.
The laboratory control check sample is prepared in the same
way as the analytical samples.
II.E.S. Other QC Criteria
• Method of Standard Additions (MSA)
This summary must be included when MSA analyses are required.
Report the absorbance values with corresponding concentration
values. Report the final analyte concentration and list the
correlation coefficient.
• ICP serial dilution
Report the initial and serial dilution results and the
percent difference.
• ICP Linear Ranges
For each instrument and wavelength used, report the date on
which the linear ranges were established, the integration
time, and the upper limit concentration.
• ICP Interelement Correction Factors
For each instrument and wavelength used, report the date-on
which the correction factors were determined. List the
interelement correction factors for Al, Ca, Fe. Mg and any
other element and the analytes to which they are applied.
-------
THIS IS A BLANK FACE
-------
Section No.:
Revision No.:
Date: 9/29/89
of
• Instrument detection limits (IDL) determination
List the instrument detection limits.
Instrument detection limits are determined by multiplying by
3. the-average of the standard deviations obtained on three
nonconsecutive days from the analysis of a standard solution
at a concentration 3-5 times the required detection limit
concentrations, with 7 consecutive measurements per day.
Refer to the 40 CFR Part 136 Appendix B.
II.F. Raw data
This section shall include legible copies of the raw data for the
following:
• Environmental samples (arranged in increasing client's sample
number order)
• Instrument calibrations
• QC analyses
• Sample preparation and digestion logs
• Instrument analysis logs for each instrument used
• Percent moisture in the soil samples
The raw data for each analysis shall include the following:
• Measurement print-outs and quantitation reports for each instrument
used
• Absorbance, titrimetric, or other measurements for wet chemical
analysis
Legible copies of the raw data shall be organized systematically, and
each page shall be numbered. The raw data for compound identification
and quantitation must be sufficient to verify each result presented in
Sections II.D. and II.E.
-------
Section No.:
Revision No.:
Dace: 1/9/90
Page:_JJ_ of 21
II.C. SUMMARY OF DOCUMENTATION REQUIREMENTS
Inorganic Data
Section I. Case Narrative
Section II. Chain-of-Custody Documentation
1. Chain-of-Custody forms
2. Internal tracking documents, as applicalbe
Section III. Summary of Results - Forms for the following:
1. Environmental samples, with quantitation limits
(include dilutions and re-analyses)
Section IV.
Section V.
QA/QC Result Summaries
1. Initial and continuing calibrations
2. Method blanks, continuing calibration blanks, and prep
blanks
3. ICP interference check sample
4. Matrix spike
5. Laboratory duplicate
6. Laboratory control sample
7. Method of standard additions
8. ICP serial dilution
9. Instrument detection limits
10. ICP linear range
Raw Data - sequential measurement readout records for ICP,
graphite furnace AA, flame AA, cold vapor mercury, cyanide,
and/or other inorganic analyses.
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
Environmental samples (including dilutions and reanalyses)
Initial and continuing calibrations
Continuing calibration and Preparation blanks
Matrix spikes
Post digest spikes
Method of standard additions, when applicable
Laboratory duplicate or matrix spike duplicates
ICP Serial Dilution
Laboratory control samples, when applicable
Percent moisture for soil samples
Sample digestion and/or sample preparation logs
Instrument analysis log, for each instrument used
Instrument tuning for ICP-MS, when applicable
-------
THIS IS A BLANK FACE
-------
Section No.: Ill
Revision No.: 0
Date: 9/29/B9
Page:_U_ of 21
III. QC REQUIREMENTS SUMMARY
III.A. CC/MS Organic Analyses
QC limits, unless specified below, shall be according to the analytical
methods. When QC limits are not specified in the methods, good laboratory
practices (GLF) are to be followed. Re-analyses nay be necessary when QC
limits are not met.
1. Instrument Tuning
• At the beginning of each day that samples are analyzed
2. Initial Calibration
• At the beginning of the QC program
• Whenever percent difference (%D) of the response factors for
specified compounds of interest or calibration check compounds
(CCC; a minimum of 5 compounds total) between continuing
calibration and initial calibration exceeds ±25%
• Whenever the response factors for specified compounds of
interest or system performance check compounds (SFCC; a minimum
of 5 compounds total) are less than 0.300 (0.250 for bromoform)
for volatiles or less than 0.050 for semi-volatiles analyses
• After installation of a new column or after maintenance
service/repair of the gas chromacography/mass spectromecry
(GC/MS)
3. Continuing Calibration
• Prior to the analysis of environmental samples, on each 12-hour
shift that samples are analyzed
4. Method Blank
• Volatiles: After each continuing calibration analysis and after
the analyses of unusually concentrated samples, to demonstrate
that the system is free of contamination.
• Semi-volatiles: One for each extraction batch of 20 or fewer
samples, for each sample matrix. Analyze method blanks on all
instruments used for sample analysis.
-------
Section No.: Ill
Revision No.: 0
Date: 9/29/89
Page: 15 of 21
Method blanks should not contain any analytcs of interest and
are to be free of interfering peaks.•
5. Calibration Range
• For samples containing one or more analytes at concentrations
above the initial calibration range, the samples are to be
diluted and re-analyzed.
6. Surrogate Standard
• Surrogate standards (3 for volatiles; 3 phenolic and 3 neutral
compounds for semi-volatiles) are to be added to the calibration
standards, method blanks, environmental samples and QC samples.
7. Internal Standard
• Internal standards (3 for volatiles and 6 for semi-volatiles)
are to be added to the calibration standards, method blanks.
environmental samples and QC samples.
• If the extracted ion chromatogram profile (EICP) area for any of
the internal standards changes by a factor of two (-50% to
+100%) from the last continuing calibration, re-analysis of the
samples is required after corrective action.
8. Matrix Spike (MS) Analysis
• For each extraction/analysis batch of 20 or fever samples, for
each sample matrix
• MS solutions are to contain all specified compounds of interest.
9. Sample Duplicate or Matrix Spike Duplicate (MSD) Analysis
• For each extraction/analysis batch of 20 or fewer samples, for
each sample matrix
10. Laboratory QC Check Sample
• At the beginning of the QC program and as needed
11. Method Detection Limits Determination
• At the beginning of the QC program and as needed
-------
Section No.: Ill
Revision No.: 0
Dace: 9/29/89
Page: 16 of 21
III. QC REQUIREMENTS SUMMARY
III.B. Pesticides/PCBs
QC limits, unless specified below, shall be according Co the analytical
methods. When QC limits are not specified in the methods, good laboratory
practices (GLP) are to be followed. Re-analyses nay be necessary when QC
limits are not met.
1. Initial Calibration
• At beginning of the QC program
• Whenever the percent difference (%D) in calibration factors
(CF) between continuing calibration and initial calibration
exceeds ±15%
• After installation of a. new column or after maintenance
service/repair of the gas chromatography (GC)
2. Daily Calibration
• Prior to the analysis of environmental samples, on each day
that samples are analyzed
3. Mid-level Standard
• After each group of 10 samples
• Report the percent breakdown for 4,4'-DDT and for endrin.
A. Method Blank
• For each extraction batch of 20 or fewer samples, for each
sample matrix. Analyze method blanks on all instruments used
for sample analysis.
• Method blanks must demonstrate that the analytical system is
free of contaminants and interfering peaks.
5. Calibration Range
• For samples containing one or more analytes at concentrations
above the initial calibration range, the samples are to be
diluted and re-analyzed.
-------
Section No.:
Revision No.: _
Date: 9/29/89
Page:JL2_ of
6. Surrogate Standard
• Surrogate standards are to be added to the calibration
standards, method blanks, environmental samples and QC samples.
7. Matrix Spike (MS) Analysis
• For each extraction batch of 20 or fewer samples, for each
sample matrix
• MS solutions are to contain all specified compounds of
interest.
8. Sample Duplicate or Matrix Spike Duplicate (MSD) Analysis
• For each extraction batch of 20 or fewer samples, for each
sample matrix
9. Laboratory QC Check Sample
• At beginning of the QC program and as needed
10. Retention Time Vindovs Determination
• For each GC column, to be updated daily
11. Method Detection Limits Determination
• At beginning of the QC program and as needed
-------
Section No.: Ill
Revision No.: 0
Date: 9/29/89
Page: 18 of 21
III. QC REQUIREMENTS SUMMARY
III.C. Furgeable Organics by GC
QC limits, unless specified below, shall be according to the analytical
methods. When QC limits are not specified in the methods, good laboratory
practices (CLP) are to be followed. Re -analyses may be necessary when QC
limits are not met.
1. Initial Calibration
• At beginning of the QC program
• Whenever the percent difference (%D) in calibration factors
(CF) between continuing calibration and initial calibration
exceeds
• After installation of a new column or after maintenance
service/repair of Che gas chromatography (GC)
2. Daily Calibration
• Prior to the analysis of environmental samples, on each day
that samples are analyzed
3. Mid- level Standard
• After each group of 10 samples
4. Method Blank
• After each daily calibration and mid- level standard analysis
and after the analyses of unusually concentrated samples, to
demonstrate that the system is free of contamination.
• Method blanks should not contain any analytes of interest and
are to be free of interfering peaks.
5. Calibration Range
• For samples containing one or more analytes at concentrations
above the initial calibration range, the samples are to be
diluted and re -analyzed.
-------
Section No.: Ill
Revision No.: 0
Dace: 9/29/89
Page:_li_ of 21
6. Surrogate Standard
• Surrogate standards are to be added to the calibration
standards, method blanks, environmental samples and QC samples.
7. Matrix Spike (MS) Analysis
• For each analysis batch of 20 or fewer samples, for each sample
matrix
• MS solutions are to contain all specified compounds of
interest.
8. Sample Duplicate or Matrix Spike Duplicate (MSD) Analysis
• For each analysis batch of 20 or fewer samples, for each sample
matrix
9. Laboratory QC Check Sample
• At beginning of the QC program and as needed
10. Retention Time tfindows Determination
• For each GC column, to be updated daily
11. Method Detection Limits Determination
• At beginning of the QC program and as needed
-------
Section No.: Ill
Revision No.: 0
Date: 9/29/89
Page: 20 of 21
III. QC REQUIREMENTS SUMMARY
III.D. Metals Analyses
QC limits, unless specified below, shall be according to the analytical
methods. When QC limits are not specified in the methods, good laboratory
practices (CLP) are to be followed. Re-analyses nay be necessary when QC
limits are not net.
1. Initial Calibration
• Daily and each time the instrument is set up
• Whenever the percent difference between the initial calibration
and the continuing calibration exceeds 10% (20% for mercury)
• whenever the percent difference between either of the ICP
interference check samples and Che true value exceeds 20% •
• Blank standard required as part of initial calibration
2. Continuing Calibration Verification Standard
• After every ten or fewer samples
• Analyses are required to have calibrations with acceptable
recoveries (the percent difference between the initial
calibration and the continuing calibration less than 10« [20%
for mercury]) before and after the sample analysis.
3. Blanks
• Continuing calibration blank run immediately following
continuing calibration verification standard
• Method blank for each preparation batch of 20 or fewer samples.
for each sample matrix
4. ICP Interference Check Sample
• At the beginning and at the end of the analytical run
• ICP analyses are required to have both ICP interference check
samples with acceptable recoveries (the percent difference
between the true value and the ICP interference check sample
less than 20%).
-------
Section No.: Ill
Revision No.: 0
Date: 9/29/B9
Page:_21_ of
5. Calibration Range
ce)
• For samples containing one or more analytes at concentrations
above the initial calibration range, the samples'iarei to be
diluted and re-analyzed.
6. Matrix Spike (MS) Analysis
• For each preparation batch of 20 or fewer sampllS* fo* tfdfltfir- .
sample matrix
• MS solutions are to contain all specified compounds of
interest.
7. Sample Duplicate Analysis
• For each preparation batch of 20 or fewer samples, for each
sample matrix
8. Laboratory Control Sample (LCS)
• For each preparation batch of 20 or fewer samples, for each
sample matrix
• Analyses are required to have the laboratory cKeck sample with
acceptable recoveries (the percent difference between the true
value and the laboratory check sample less thfeSf 20%7?crunen"
• Laboratory control samples are not required fbWhercury or
cyanide determinations.
9. Graphite Furnace Post Digest QC
• A post digest spike at 10 to 20 ug/L is required for all
furnace analyses. If the result is greater than or equal to 10
ug/L in the digestate and the recovery of the :s$5Lke is -riot'
within 85% to 115%, the method of standard additions'is
required to be used.
• If the method of standard additions correlatioif fcoefficient is
less than 0.995, the method of standard addiC&fcs'-'ttrialysis is
required to be repeated once.
10. ICP Serial Dilution
• For each preparation batch of 20 or fewer samples, for each
sample matrix, dilute the digestate by five and re-analyze.
------- |