xvEPA
United States
Environmental Protection
Agency
Off ice of
Solid Waste and
Emergency Response
Publication 9240.1 -05-01
EPA-540/R-94-013
PB94-963502
February 1994
Superiund
USEPA CONTRACT LABORATORY
PROGRAM NATIONAL FUNCTIONAL
GUIDELINES FOR INORGANIC DATA
REVIEW
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^ 9240.1-05-01
^ PB 94-963502
% EPA 540/R-94/013
^ February 1994
USEPA CONTRACT LABORATORY PROGRAM
NATIONAL FUNCTIONAL GUIDELINES
FOR
INORGANIC DATA REVIEW
Office of Emergency and Remedial Response
U.S. Environmental Protection Agency
Washington, DC 20460
U.S. Environment,--} Protection Agency
Region 5, Li^;. 1-12J)
77 West Jack-. ,
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NOTICE
The polices and procedures set forth here are intended as guidance to the
Agency and other governmental employees. They do not constitute
rulemaking by the agency, and may not be relied on to create a substantive or
procedural right enforceable by any other person. The Government may take
action that is at variance with the policies and procedures in this manual.
Additional copies of this document can be obtained from:
National Technical Information Service (NTIS)
U.S. Department of Commerce
5285 Port Royal Road
Springfield, VA 22161
(703) 487-4650
Document Number PB 94-963502
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TABLE OF CONTENTS
Page
INTRODUCTION 1
PRELIMINARY REVIEW 2
DATA QUALIFIER DEFINITIONS 4
INORGANIC DATA REVIEW 5
I. Holding Times 6
II. Calibration 8
III. Blanks 16
IV. ICP Interference Check Sample (ICS) 19
V. Laboratory Control Sample (LCS) 22
VI. Duplicate Sample Analysis 25
VII. Spike Sample Analysis 27
VIII. Graphite Furnace Atomic Absorption QC 30
IX. ICP Serial Dilution 33
X. Field Duplicates 35
XI. Overall Assessment 36
GLOSSARY A: Definition of Selected Terms 38
GLOSSARY B: Inorganic Regional Data Assessment Summary 41
in
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INTRODUCTION
This document is designed to offer guidance on EPA Contract Laboratory Program (CLP)
inorganic analytical data evaluation and review. In some applications it may be used as a Standard
Operating Procedure (SOP). In other, more subjective areas, only general guidance is offered due to
the complexities and uniqueness of data relative to specific samples. Those areas where specific SOPs
are possible are primarily areas in which definitive performance requirements are established. These
requirements are concerned with specifications that are not sample dependent; they specify certain
performance requirements on matters that should be fully under a laboratory's control. These specific
areas include blanks, calibration standards, calibration verification standards, laboratory control
standards, and interference check standards. In particular, mistakes such as calculation and
transcription errors must be rectified by resubmission of corrected data sheets.
These Guidelines include the requirements for the Inorganic Analysis Multi-media Multi-
Concentration method.
This document is intended to assist in the technical review of analytical data generated
through the CLP. Determining contract compliance is not the intended objective of these guidelines.
The data review process provides information on analytical limitations of data based on specific
quality control (QC) criteria. In order to provide more specific usability statements, the reviewer
must have a complete understanding of the intended use of the data. For this reason, it is
recommended that whenever possible the reviewer obtain usability issues from the user prior to
reviewing the data. When this is not possible, the user should be encouraged to communicate any
questions to the reviewer.
At times, there may be a need to use data which do not meet all contract requirements and
technical criteria. Use of these data does not constitute either a new requirement standard or full
acceptance of the data. Any decision to utilize data for which performance criteria have not been met
is strictly to facilitate the progress of projects requiring the availability of the data. A contract
laboratory submitting data which are out of specification may be required to rerun or resubmit data,
even if the previously submitted data have been utilized due to program needs. Data which do not
meet specified requirements are never fully acceptable. The only exception to this requirement is in
the area of requirements for individual sample analysis; if the nature of the sample itself limits the
attainment of specifications, appropriate allowances must be made.
All data reviews must have, as a cover sheet, the Inorganic Regional Data Assessment (IRDA)
form (a copy is attached at the end of this document). If actions are required, they should be
specifically noted on this form. In addition, this form is to be used to summarize overall deficiencies
requiring attention, as well as general laboratory performance and any discernible trends in the quality
of the data. (This form is not a replacement for the data review.) Sufficient supplementary
documentation must accompany the form to clearly identify the problems associated with a case. The
form and any attachments must be submitted to the Analytical Operations Branch Contract Laboratory
Program Quality Assurance Coordinator (CLP QAC), the Regional Technical Project Officer (TPO).
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PRELIMINARY REVIEW
In order to use this document effectively, the reviewer should have a general overview of the
sample delivery group (SDG) or sample case at hand. The exact number of samples, their assigned
numbers, their matrix, and the number of laboratories involved in their analysis are essential
information. Background information on the site is helpful but often this information is very difficult
to locate. The site manager is the best source for answers or further direction.
Sample cases (SDGs) routinely have unique samples which require special attention by the
reviewer. These include field blanks, field duplicates, and performance audit samples which need to
be identified. The sampling records should identify:
1. The Project Officer for site.
2. The Complete list of samples with notations on:
a) sample matrix,
b) blanks*,
c) field duplicates*,
d) field spikes*,
e) QC audit sample*,
f) shipping dates,
g) preservatives, and
h) labs involved
* If applicable
The chain-of-custody record includes sample descriptions and date(s) of sampling. The
reviewer must take into account lag times between sampling and start of analysis when assessing
technical sample holding times.
The laboratory's SDG Narrative is another source of general information. Notable problems
with matrices, insufficient sample volume for analysis or reanalysis, samples received in broken
containers, preservation, and unusual events should be found in the SDG Narrative.
The SDG Narrative for the sample data package must include a Laboratory Certification
Statement (exactly as written in the method), signed by the laboratory manager or his designee. This
statement authorizes the validation and release of the sample data results. In addition, the laboratory
must also provide comments in the SDG narrative describing in detail any problems encountered in
processing the samples in the data package.
For every data package, the reviewer must verify that the laboratory certification statement is
present, exactly stated as in the method (i.e., verbatim to the statement in the method), and signed by
the Laboratory Manager or designee. The reviewer must further verify that the data package is
consistent with the laboratory's certified narrative. Also, the reviewer should check the comments
provided in the narrative to determine if they are sufficient to describe and explain any associated
problem(s).
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The data review should include comments that clearly identify the problems associated with a
case or Sample Delivery Group (SDG) and to state the limitations of the data. Documentation should
include the sample number, analytical method, extent of the problem, and assigned qualifiers.
A data review narrative generally accompanies the laboratory data forwarded to the intended
data recipient (client) or user to promote communications. A copy of the data review narrative should
be submitted to the Regional CLP Technical Project Officer (TPO) assigned oversight responsibility
for the laboratory producing the data.
It is a responsibility to notify the appropriate Regional CLP TPO concerning problems and
deficiencies with regard to laboratory data. If there is an urgent requirement, the TPO may be
contacted by telephone to expedite corrective action. It is recommended that all items for TPO action
be presented at one time.
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DATA QUALIFIER DEFINITIONS
The following definitions provide brief explanations of the national qualifiers assigned to
results in the data review process. If the Regions choose to use additional qualifiers, a complete
explanation of those qualifiers should accompany the data review.
U - The material was analyzed for, but was not detected above the
level of the associated value. The associated value is either the
sample quantitation limit or the sample detection limit.
The associated value is an estimated quantity.
R - The data are unusable. (Note: Analyte may or may not be
present.)
UJ - The material was analyzed for, but was not detected. The
associated value is an estimate and may be inaccurate or
imprecise.
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INORGANIC DATA REVIEW
The inorganic data requirements to be checked during validation are listed below:
I. Holding Times (Method Holding Times)
II. Calibration
o Initial
o Initial and Continuing Calibration Verification
III. Blanks
IV. ICP Interference Check Sample
V. Laboratory Control Sample
VI. Duplicate Sample
VII. Spike Sample Analysis
VIII. Graphite Furnace Atomic Absorption QC
IX. ICP Serial Dilution
X. Field Duplicates
XI. Overall Assessment
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I. HOLDING TIMES
A. Review Items: Form I-IN, Form XIII-IN, EPA Sample Traffic Report and/or chain-of-
custody, raw data, and SDG Narrative.
B. Objective:
The objective is to ascertain the validity of results based on the holding time of the sample
from the time of collection to the time of analysis.
C. Criteria:
Technical requirements for sample holding times have only been established for water
matrices. The addition of Nitric Acid or Sodium Hydroxide to adjust the pH is only required
for aqueous samples.
The technical holding time criteria for water samples are as follows:
METALS: 180 days; preserved (with Nitric Acid) to pH < 2
MERCURY: 28 days; preserved (with Nitric Acid) to pH < 2
CYANIDE: 14 days; cooled @ 4°C _+ 2°C, preserved (with
Sodium Hydroxide) to pH > 12
The preservation for soil/sediment samples is maintenance at 4°C +_ 2°C until analysis.
NOTE; The technical holding time is based on the date of collection, rather than validated
time of sample receipt (VTSR), and date of analysis. The method maximum holding times
may differ from the technical holding times.
D. Evaluation:
Technical holding times are established by comparing the sampling date(s) on the EPA Sample
Traffic Report with the dates of analysis found on FORM 1-IN, and in the laboratory raw
data (instrument run logs). Information contained in the complete SDG file should also be
considered in the determination of holding times. Verify that the analysis dates on the Form
Is and the raw data/SDG file are identical. Review the SDG narrative to determine if the
samples were properly preserved. If there is no indication in the SDG narrative or the sample
records that there was a problem with the samples, then the integrity of samples can be
assumed to be good. If it is indicated that there were problems with the samples, then the
integrity of the sample may have been compromised and professional judgement should be
used to evaluate the effect of the problem on the sample results.
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E. Action:
1. If technical holding times and preservation requirements are not met, qualify all
results greater than the Instrument Detection Limit (IDL) as estimated (J), and results
less than the IDL as estimated (UJ).
2. If holding times are exceeded, the reviewer must use professional judgement to
determine the reliability of the data and the effects of additional storage on the sample
results. The expected bias would be low and the reviewer may determine that results
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II. CALIBRATION
A. Review Items: Form II-IN (Part A & B), Form XIII-IN, preparation logs, calibration
standard logs, instrument logs, instrument printouts, and raw data.
B. Objective:
Method requirements for satisfactory instrument calibration are established to ensure that the
instrument is capable of producing acceptable quantitative data for the metals and cyanide on
the Inorganic Target Analyte List (TAL). Initial calibration demonstrates that the instrument
is capable of acceptable performance at the beginning of the analytical run. Continuing
calibration verification establishes that the initial calibration is still valid by checking the
performance of the instrument on a continual basis.
C. Criteria:
1. Initial Calibration
The instruments must be successfully calibrated daily or once every 24 hours, and
each time the instrument is set up. The calibration date and time are to be included in
the raw data.
a. Inductively Coupled Plasma (ICP) Analysis
1) A blank and at least one calibration standard must be used in
establishing each analytical curve. All measurements must be within
the instrument linear working range where the interelement correction
factors are valid. A minimum of two replicate exposures are required
for standardization and all QC and sample analyses. The average
result of the multiple exposures for the standardization, QC, and
sample analyses must be used.
2) The instrumental calibration near the Contract Required Detection
Limit (CRDL) must be verified for each analyte. An ICP standard
solution (CRI) shall be prepared at two times the CRDL, or two times
the Instrument Detection Limit (IDL), whichever is greater. The CRI
shall be analyzed at the beginning and end of each sample analysis
run, or at a minimum of twice per 8 hour working shift, whichever is
more frequent, but not before Initial Calibration Verification.
3) The CRI shall be run by ICP for every wavelength used for analysis,
except those for Al, Ba, Ca, Fe, Mg, Na, and K. If the results for
the CRI did not fall within the fixed acceptance limits, the analysis
should have been terminated, the problem corrected, the instrument
recalibrated, and the new calibration then reverified.
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b. Graphite Furnace Atomic Absorption Analysis (GFAA)
1) Calibration standards are to be prepared fresh daily, or each time an
analysis is to be made, and discarded after use. The date and time of
standard preparation and analysis are to be recorded in the raw data.
2) A blank and at least three calibration standards must be used in
establishing each analytical curve, with the blank being analyzed first.
One of the calibration standards must be run at the CRDL.
3)
The linearity of the analytical curve must be verified near the CRDL
for Graphite Furnace AA (GFAA). A standard solution (CRA) shall
be prepared at the CRDL or at the IDL, whichever is greater. The
CRA shall be analyzed at the beginning of each sample analysis run,
but not before the Initial Calibration Verification.
4) All results and percent recoveries (%R) for the CRA are to be
reported on Form II (Part 2)-IN. If the results for the CRA did not
fall within the fixed acceptance limits, the analysis should have been
terminated, the problem corrected, the instrument recalibrated, and the
new calibration then reverified.
c. Cold Vapor Mercury Analysis
1) A blank and from five to eight calibration standards (depending on the
specific method being used) must be employed in establishing the
analytical curve, with the blank being analyzed first. One of the
calibration standards must be at the CRDL.
2) The linearity of the analytical curve must be verified near the CRDL.
A standard solution (CRA) shall be prepared at the CRDL or at the
IDL, whichever is greater. The CRA shall be analyzed at the
beginning of each sample analysis run, but not before the Initial
Calibration Verification.
3) Analysis of the CRA standard for mercury is required for both the
manual and automated cold vapor methods, and the results and %R
are to be reported on Form II(Part 2)-IN. However, no specific
acceptance criteria has been established by the EPA for mercury at
this time.
Note; The calibration curves for the AA metals (and Hg) should possess a
correlation coefficient of _>0.995, in order to ensure the linearity over the
calibrated range.
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d. Cyanide Analysis
1) A blank and at least three calibration standards, one of which must be
at the CRDL, must be used in establishing the analytical curve.
2) The standard curve must bracket the concentration of the samples.
3) At least one calibration standard (mid-level) must be distilled and
compared to similar values on the curve to ensure that the distillation
technique is reliable. The distilled standard must agree within ±1
of the undistilled standard.
2. Initial and Continuing Calibration Verification (ICV and CCV)
The acceptance criteria for the ICV and CCV standards is presented in the following table:
Analytical
Method
ICP/AA
Cold Vapor AA
Other
Inorganic
Species
Metals
Mercury
Cyanide
Low Limit
(% of true
value)
90
80
85
High Limit
(% of true
value)
110
120
115
a. Initial Calibration Verification (ICV)
1) Immediately after each ICP, AA, and cyanide system has been
calibrated, the accuracy of the initial calibration must be verified and
documented for every target analyte by the analysis of an Initial
Calibration Verification (ICV) solution(s),
2) If the ICV is not available from EPA, or where a certified solution of an
analyte is not available from any source, analyses shall be conducted on
an independent standard at a concentration level other than that used for
instrument calibration (or the CRI or CRA), but within the calibrated
range.
3) The ICV solution shall be run at each analytical wavelength used for
analysis.
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4) For cyanide analysis, the ICV standard solution shall be distilled with
each batch of samples analyzed. An ICV distilled with a particular set
of samples must be analyzed only with that sample set. Additionally, for
aqueous samples the ICV for cyanide can also be used as the Laboratory
Control Sample (LCS). However, a separate ICV is required for soil
cyanide samples.
b. Continuing Calibration Verification (CCV)
1) To ensure the accuracy during the course of each analytical run, the
CCV shall be analyzed and reported for each wavelength used for the
analysis of each analyte.
2) The CCV standard must be analyzed at a frequency of 10% or every two
hours during an analytical run, whichever is more frequent. The CCV
standard shall also be analyzed at the beginning of the run and after the
last analytical sample.
3) The analyte concentration(s) in the CCV standard(s) shall be different
than the concentration used for the initial calibration verification (ICV),
and shall be one of the following solutions at or near the mid-range
levels of the calibration curve:
a. EPA Solutions.
b. NIST Standards.
c. A Laboratory-prepared standard solution (self-prepared
or commercially available).
4) The same CCV standard solution shall be used throughout the analysis
runs for a case of samples received.
5) The CCV shall be analyzed in the same fashion as an actual sample.
Operations such as the number of replicate analysis, the number and
duration of the instrument rinses, etc., affect the measured CCV result
and are not to be applied to the CCV in a greater extent than they are
applied to the associated analytical samples.
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D. Evaluation:
a. ICP Analysis
1) Verify that the instrument was calibrated daily and each time the instrument was
set-up, utilizing a blank and at least one calibration standard.
2) Confirm that the measurements were within the documented linear working
range, and are the average result of at least two replicate exposures.
3) Evaluate the reported CRI standard to confirm that it analyzed at the proper
concentration, frequency, and location within the analytical run sequence. Verify
that acceptable %R results were obtained.
4) Verify that the ICV and CCV standards were analyzed for each analyte at the
proper frequency and at the appropriate concentration. Verify that acceptable
%R results were obtained.
5) Recalculate one or more of the ICV and CCV %R using the following equation
and verify that the recalculated value agrees with the laboratory reported values
on Form IIA. Due to possible rounding discrepancies, allow results to fall within
1% of the contract windows (e.g., for ICP 89-111%).
%R = Found x 100
True
Where: Found = Concentration (in ug/L) of each analyte measured in
the analysis of the ICV or CCV solution.
True = Concentration (in ug/L) of each analyte in the ICV or
CCV source.
b. Atomic Absorption (AA) and Cold Vapor Mercury Analysis
1) Verify the date and time the various calibration standards were prepared, and
their analytical use.
2) Verify that the instrument was calibrated daily for each analyte. For each time
that the instrument was set-up, confirm that a blank and the proper concentration
and number of calibration standards were utilized depending on the actual method
employed for the analysis (e.g., for AA a blank and at least three standards, and
for Hg a blank and from five to eight calibration standards, depending on the
method). Confirm that one of the calibration standards was analyzed at the
CRDL.
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3) Evaluate the reported CRA standard to confirm that it analyzed at the proper
frequency, concentration, and location within the analytical run sequence. Verify
that for AA CRA analysis, acceptable %R results were obtained.
4) Verify that the ICV and CCV standards were analyzed for each analyte at the
proper frequency and at the appropriate concentration. Verify that acceptable
%R results were obtained.
5) Recalculate one or more of the ICV and CCV %R using the following equation
and verify that the recalculated value agrees with the laboratory reported values
on Form IIA. Due to possible rounding discrepancies, allow results to fall within
1% of the contract windows (e.g., for AA 89-111%, and for Hg 79-121%).
%R = Found x 100
True
Where: Found = Concentration (in ug/L) of each analyte measured in the
analysis of the ICV or CCV solution.
True = Concentration (in ug/L) of each analyte in the ICV or CCV
source.
c. Cyanide Analysis
1) Verify that the instrument was calibrated daily and each time the instrument was
set-up, utilizing a blank and at least three calibration standards. Confirm that one
of the calibration standards was analyzed at the CRDL.
2) Check the distillation log and verify that the mid-level CN standard was distilled
and analyzed. Verify that the distilled mid-level CN standard agrees within
of the undistilled standard.
3) Verify that the ICV and CCV standards were analyzed at the proper frequency
and at the appropriate concentrations. Verify that acceptable %R results were
obtained.
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4) Recalculate one or more of the ICV and CCV %R using the following equation
and verify that the recalculated value agrees with the laboratory reported values
on Form HA. Due to possible rounding discrepancies, allow results to fall within
1% of the contract windows (e.g., for Cyanide 84-116%).
%R = Found x 100
True
Where: Found = Concentration (in ug/L) of each analyte measured in
the analysis of the ICV or CCV solution.
True = Concentration (in ug/L) of each analyte in the ICV or
CCV source.
E. Action:
1. If the minimum number of standards as defined in INORG Section II.B.I. above were
not used for initial calibration, or if the instrument was not calibrated daily and each time
the instrument was set up, qualify the data as unusable (R).
2. If the correlation coefficient is < 0.995 (AA and Cold Vapor Hg), qualify results greater
than the IDL as estimated (J), and results less than the IDL as estimated (UJ).
Depending on the degree of the deviation from linearity, further qualification of the data
may be required depending on the professional judgement of the reviewer (e.g, unusable
data (R)).
3. If one of the midrange CN standards was not distilled, analyzed, and shown to be in
agreement with the un-distilled standard, then qualify all associated sample results as
estimated (J).
4. If any CRA or CRI standards are outside the listed acceptance criteria:
a. Utilizing professional judgement, any potential effects on the data should be
noted in the data review narrative.
b. Extreme or repetitive failure should be noted for TPO action.
c. Professional judgement shall be used to determine if it is necessary to qualify
the data for any analyte.
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5. If the ICV or CCV %R falls outside the acceptance windows, use professional judgement
to qualify all associated data. If possible, indicate the bias in the review. The following
guidelines are recommended:
a. If the ICV or CCV %R falls outside the acceptance windows but within
the ranges of 75-89% or 111-125% (CN, 70-84% or 116-130%; Hg, 65-
79% or 121-135%), qualify results > IDL as estimated (J).
b. If the ICV or CCV %R is within the range of 111-125% (CN, 116-
130%; Hg, 121-135%), results < IDL are acceptable.
c. If the ICV or CCV %R is 75-89% (CN, 70-84%; Hg, 65-79%), qualify
results < IDL as estimated (UJ).
d. If the ICV or CCV %R is <75%, (CN, <70%; Hg, <65%), qualify
all positive results as unusable (R).
e. If the ICV or CCV %R is > 125%, (CN > 130%; Hg > 135%), qualify
results > IDL as unusable (R); results < IDL are acceptable.
6. If the laboratory has failed to provide adequate calibration information, the designated
representative should contact the laboratory and request the necessary information. If the
information is not available, the reviewer must then use professional judgement to assess
the data.
7. Whenever possible, the potential effects on the reported data due to exceeding the
calibration criteria should be noted in the data review narrative.
8. If calibration criteria are grossly exceeded, the specifics should be noted for TPO action.
Note: For truly critical samples, a further in-depth evaluation of the calibration curve may be
warranted to determine if additional qualification is necessary.
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III. BLANKS
A. Review Items: Form I-IN, Form III-IN, Form XIII-IN, Form XIV-IN, preparation logs,
calibration standard logs, instrument logs, and raw data.
B. Objective:
The assessment of blank analysis results is to determine the existence and magnitude of
contamination resulting from laboratory (or field) activities. The criteria for evaluation of blanks
applies to any blank associated with the samples (e.g., method blanks, calibration blanks, field
blanks, etc.). If problems with any blank exist, all associated data must be carefully evaluated
to determine whether or not there is an inherent variability in the data, or if the problem is an
isolated occurrence not affecting other data.
C. Criteria:
1. No contaminants should be found in the blank(s).
2. The initial calibration blank (ICB) is analyzed after the analytical standards, but not
before analysis of the ICV, during the initial calibration of the instrument, (see INORG
Section II.C.I. above).
3. A continuing calibration blank (CCB) must be analyzed at each wavelength used for the
analysis, immediately after every initial and continuing calibration verification. The CCB
shall be analyzed at a frequency of 10% or every two hours during the run, whichever
is more frequent. The CCB shall be analyzed at the beginning of the run, and after the
last CCV that was analyzed after the last analytical sample of the run. The CCB result
(absolute value) must not exceed the CRDL, for each analyte analyzed for.
4. At least one preparation blank (PB), must be prepared and analyzed for each matrix, with
every SDG, or with each batch of samples digested, whichever is more frequent. The
preparation blank consists of deionized distilled water processed through the appropriate
sample preparation and analysis procedure.
5. If any analyte concentration in the PB is above the CRDL, the lowest concentration of
that analyte in the associated samples must be 10 times the PB concentration. Otherwise,
all samples associated with that PB with the analyte's concentration less than 10 times the
PB concentration, and above the CRDL, should have been re-digested and re-analyzed
for that analyte (except for an identified aqueous soil field blank). The sample
concentration is not to be corrected for the blank value.
6. If the concentration of the PB for a certain analyte is below the negative CRDL, then all
samples reported below 10 times the CRDL (associated with that analyte in that blank),
should have been re-digested and re-analyzed.
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D. Evaluation:
1. Verify that an ICB was analyzed after the calibration, and that the CCB was analyzed at
the proper frequency and location during the run. PB's were prepared and analyzed as
appropriate for the SDG (e.g., total number of samples, various types of matrices
present, number of digestion batches, etc.).
2. Review the results reported on the Blank Summary (Form III-IN), as well as the raw data
(e.g., ICP printouts, strip charts, printer tapes, bench sheets, etc.), for all blanks and
verify that the results were accurately reported.
3. Evaluate all of the associated blanks for the presence of target analytes.
E. Action:
1. If the appropriate blanks were not analyzed with the correct frequency, then the data
reviewer should use professional judgement to determine if the associated sample data
should be qualified. The reviewer may need to obtain additional information from the
laboratory. The situation should then be recorded in the review narrative, and noted for
TPO action.
2. Action regarding unsuitable blank results depends on the circumstances and origin of the
blank. The reviewer should note that in instances where more than one blank is
associated with a given sample, qualification should be based upon a comparison with the
associated blank having the highest concentration of a contaminant. The results must not
be corrected by subtracting any blank value.
3. Some general "technical" review actions are as follows:
a. Actions in the case of unusable blank results depends on the circumstances and
origin of the blank in question. Sample results greater than the IDL but less than
5 times the amount found in any blank should be qualified as (U).
b. Any blank reported with a negative result whose absolute value is greater than
the IDL must be carefully evaluated to determine its effect on the sample data.
The reviewer shall then use professional judgement to asses the data.
c. The blank analyses may not involve the same weights, volumes, or dilution
factors as the associated samples. In particular, soil sample results reported on
Form I-IN will not be on the same basis (units, dilution) as the calibration blank
data reported on Form III-IN. The reviewer may find it easier to work from the
raw data when applying the 5X criteria to soil sample data, or calibration blank
data.
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4. Specific "method" actions are as follows:
a. If the magnitude (absolute value) of the CCB result exceeds the IDL, the result
shall be reported in ug/L on Form III-IN, otherwise report as "IDL-U".
b. If the absolute value of the CCB result exceeds the CRDL, the analysis should
have been terminated. This situation should be noted for TPO action, and
recorded in the data review narrative. The reviewer shall then use professional
judgement to asses the data.
c. If the absolute value of the concentration of the PB is less than or equal to the
CRDL, no correction of the sample results is performed.
d. If any analyte concentration in the PB is above the CRDL, the lowest
concentration of that analyte in the associated samples must be 10 times the PB
concentration. Otherwise, all samples associated with that blank should have
been redigested and reanalyzed. This situation should be noted for TPO action,
and recorded in the data review narrative. The reviewer shall then use
professional judgement to asses the data. The sample concentration is not to be
corrected for the blank value.
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IV. ICP INTERFERENCE CHECK SAMPLE flCS)
A. Review Items: Form IV-IN, Form XIV-IN, instrument printouts, raw data.
B. Objective:
The ICP Interference Check Sample (ICS) verifies the contract laboratory's interelement and
background correction factors.
C. Criteria:
1. The ICS consists of two solutions: Solution A and Solution AB. Solution A consists of
the interferents, and solution AB consists of the analytes mixed with the interferents. An
ICS analysis consists of analyzing both solutions consecutively, starting with solution A,
for all wavelengths used for each analyte reported by ICP.
2. An ICS must be run at the beginning and end of each sample analysis run (or a minimum
of twice per 8 hour working shift), whichever is more frequent. The ICS is not to be run
prior to the initial calibration verification.
3. Results for the ICP analysis of the ICS solution AB must fall within the control limits of
_+_ 20% of the true value for the analytes included in the solution. If true values for the
analytes are not supplied with the ICS, the mean shall be determined by initially
analyzing the ICS at least five times repetitively for the particular analytes. This mean
determination shall be made during an analytical run where the results for the previously
supplied EPA ICS solution met all contract specifications. Additionally, the results of
this initial mean determination shall be used as the true value until the solution is
exhausted.
4. The ICS should be obtained from EPA (EMSL-LV) if available and analyzed according
to the instructions supplied with the solutions. If the ICS is not available from EPA, then
an independent ICS solution shall be prepared with the interferant and analyte
concentrations at the levels specified in the method. The mean and standard deviation
of the prepared solution shall be established by initially analyzing the ICS at least five
times repetitively for each parameter on Form IV-IN. The mean and standard deviation
shall be reported in the raw data.
D. Evaluation:
1. Verify from the raw data (ICP instrumental printout) that the ICS was analyzed at the
proper frequency and location during the analytical run.
2. Evaluate the ICS raw data for results with an absolute value greater than the IDL for
those analytes which are not present in the ICS solution.
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3. If an ICS solution not obtained from EPA was used, investigate the raw data for the five
repetitive analyses. Check the calculations of the mean and standard deviation for the
ICS analytes.
4. Recalculate from the raw data one or more of the analyte percent recoveries (%R) using
the following equation, and verify that the recalculated value agrees with the laboratory
reported values on Form IV-IN.
ICS %R = Found Solution AB x 100
True Solution AB
Where:
Found Solution AB — concentration (in ug/L) of each analyte measured in the
analysis of solution AB.
True Solution AB = concentration (in ug/L) of each analyte in solution AB.
E. Action:
1. For samples with concentrations of Al, Ca, Fe, and Mg which are comparable to or
greater than their respective levels in the Interference Check Sample:
a. If the ICS recovery for an element is > 120% and the sample results are < IDL,
this data is acceptable for use.
b. If the ICS recovery for an element is > 120% and the sample results are > IDL,
qualify the affected data as estimated (J).
c. If the ICS recovery for an element falls between 50 and 79% and the sample
results are > IDL, qualify the affected data as estimated (J).
d. If sample results are < IDL, and the ICS recovery for that analyte falls within
the range of 50-79%, the possibility of false negatives may exist. Qualify the
data for these samples as estimated (UJ).
e. If ICS recovery results for an element fall <50%, qualify the affected data as
unusable (R).
Note; If possible, indicate the bias for the estimated results in the data review narrative.
2. If results > IDL are observed for elements which are not present in the ICS solution,
the possibility of false positives exists. An evaluation of the associated sample data for
the affected elements should be made. For samples with comparable or higher levels of
interferents and with analyte concentrations that approximate those levels found in the
ICS (false positives), qualify sample results > IDL as estimated (J).
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3. If negative results are observed for elements that are not present in the ICS solution, and
their absolute value is > IDL, the possibility of false negatives in the samples may exist.
If the absolute value of the negative results is > IDL, an evaluation of the associated
sample data should be made. For samples with comparable or higher levels of
interferents, qualify results for the affected analytes < IDL as estimated (UJ).
4. In general, the sample data can be accepted if the concentrations of Al, Ca, Fe and Mg
in the sample are found to be less than or equal to their respective concentrations in the
ICS. If these elements are present at concentrations greater than the level in the ICS, or
other elements are present in the sample at > 10 mg/L, the reviewer should investigate
the possibility of other interference effects as given in the ICP method. These analyte
concentration equivalents presented in the method should be considered only as estimated
values, since the exact value of any analytical system is instrument specific. Therefore,
estimate the concentration produced by an interfering element. If the estimate is greater
than 2X CRDL and also greater than 10% of the reported concentration of the affected
element, qualify the affected results as estimated (J).
5. Actions regarding the interpretation and/or the subsequent qualification of ICP data due
to the ICS analytical results can be extremely complex. The data reviewer should use
professional judgement to determine the need for the associated sample data to be
qualified. The reviewer may need to obtain additional information from the laboratory.
All interpretive situations should then be recorded in the data review narrative.
6. If the ICS acceptance criteria are grossly exceeded, the specifics should be noted for TPO
action.
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V. LABORATORY CONTROL SAMPLE (LCS\
A. Review Items: COVER PAGE-IN, Form VII-IN, Form XIII-IN, Form XIV-IN, preparation
logs, instrument printouts, raw data.
B. Objective:
The Laboratory Control Sample (LCS) serves as a monitor of the overall performance of each
step during the analysis, including the sample preparation.
C. Criteria:
1. Aqueous and solid Laboratory Control Samples shall be analyzed for each analyte
utilizing the same sample preparations, analytical methods, and QA/QC procedures as
employed for the samples. The aqueous LCS solution shall be obtained from EPA.
However, if the LCS is unavailable from EPA, the Initial Calibration Solutions may be
used.
2. One aqueous LCS must be prepared and analyzed for every group of aqueous samples
in an SDG, or with each batch of aqueous samples digested, whichever is more frequent.
Note; An aqueous LCS is not required for mercury. For cyanide, a distilled ICV is
used as the LCS (see INORG Section II.C.2.a.4. above).
3. All aqueous LCS results must fall within the control limits of 80-120%R, except for Sb
and Ag which have no fixed control limits. If the %R for the aqueous LCS falls outside
of the fixed control limits (except for Ag and Sb), the analyses should have been
terminated, the problem corrected, and the samples associated with that LCS redigested
and reanalyzed.
4. An EPA provided solid LCS shall be prepared and analyzed utilizing each of the
preparation and analytical procedures applied to the soil/sediment samples received, with
one exception: The percent solids determination is not required for the LCS. If the EPA
solid LCS is not available, other EPA Quality Assurance Check samples or other certified
materials may be used.
5. One solid LCS shall be prepared and analyzed for every group of soil/sediment samples
in an SDG, or for each batch of samples digested and/or distilled, whichever is more
frequent.
6. All solid LCS results must fall within the control limits established by EPA-EMSL/LV.
If the results for the solid LCS fall outside of the control limits, the analyses should have
been terminated, the problem corrected, and the samples associated with that LCS
redigested and reanalyzed.
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D. Evaluation:
1. Verify from the COVERPAGE-IN, Form XIII-IN, and the raw data that the appropriate
number of required Laboratory Control Samples were prepared and analyzed for the
SDG.
2. Evaluate Form VII-IN and verify that all results, for each analyte, fall within the
established control limits.
Note; Certain elements have only advisory limits for the LCS. Professional judgement
should be used when evaluating these elements.
3. Check the raw data (ICP printouts, strip charts, bench sheets) to verify that the reported
percent recoveries (%R) on Form VII-IN were accurately transcribed. Recalculate one
or more of the reported recoveries (%R) using the following equation:
LCS%R = LCS Found x 100
LCS True
Where:
LCS Found = concentration (in ug/L for aqueous; mg/kg for solid) of each analyte
measured in the analysis of LCS solution.
LCS True = concentration (in ug/L for aqueous; mg/kg for solid) of each analyte in
the LCS source.
E. Action:
If the LCS criteria are not met, then the laboratory performance and method accuracy are in
question. Professional judgement should be used to determine if the data should be qualified or
rejected. The following guidance is suggested for qualifying sample data for which the associated
LCS does not meet the required criteria.
1. Aqueous LCS:
a. If the LCS recovery for any analyte falls within the range of 50% - 79% or
> 120%, qualify results > IDL as estimated (J).
b. If the results are < IDL and the LCS recovery is greater than 120%, the data
are acceptable.
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c. If the results are < IDL and the LCS recovery falls within the range of 50-79%,
qualify the data for the affected analytes as estimated (UJ).
d. If LCS recovery results are <50%, qualify the data for these samples as
unusable (R).
2. Solid LCS:
a. If the solid LCS recovery for any analyte falls outside the EPA control limits,
qualify all sample results > IDL as estimated (J).
b. If the LCS results are higher than the control limits, and the sample results are
< IDL, the data are acceptable.
c. If the LCS results are lower than the control limits, then qualify all sample
results < IDL as estimated (UJ).
3. It should be noted for TPO action if a laboratory fails to analyze an LCS with each SDG,
or if a laboratory consistently fails to generate acceptable LCS recoveries.
4. Whenever possible, the potential effects on the data due to out-of-control LCS results
should be noted in the data review narrative.
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VI. DUPLICATE SAMPLE ANALYSIS
A. Review Items: Form I-IN, Form VI-IN, instrument printouts, raw data.
B. Objective:
Duplicate sample determinations are used to demonstrate acceptable method precision by the
laboratory at the time of analysis. Duplicate analyses are also performed to generate data in
order to determine the long-term precision of the analytical method on various matrices.
C. Criteria:
1. Samples identified as field blanks cannot be used for duplicate sample analysis.
2. One duplicate sample must be prepared and analyzed from each group of samples with
a similar matrix type (e.g., water, soil) and concentration (e.g., low, medium), or for
each SDG. Duplicates cannot be averaged for reporting on Form I-IN.
Note: Additional duplicate sample analyses may be required through Regional EPA or
Project Officer request. Alternately, EPA may require that a specific sample be used for
the duplicate sample analysis.
3. Duplicate sample analyses are required for percent solids determination.
4. If two analytical methods are used to obtain the reported values for the same element
within a SDG (e.g., ICP and GFAA, or a soil and a water method), duplicate samples
must be run by each method used.
5. A control limit of +. 20% for the Relative Percent Difference (RPD) shall be used for
original and duplicate sample values greater than or equal to 5x the CRDL. The absolute
value of the control limit (CRDL) shall be entered in the "Control Limit" column on
Form VI-IN.
6. A control limit of _+_ the CRDL shall be used if either the sample or duplicate value is
less than 5x CRDL. In the case where only one result is above the 5x the CRDL level
and the other is below, the +_ the CRDL criteria applies. If both samples values are less
than the IDL, the RPD is not calculated of Form VI-IN
Note; The control limits as specified above (±20% RPD and ± the CRDL) are method
requirements for duplicate samples, regardless of the sample matrix type. However, it
should be noted that laboratory variability arising from the sub-sampling of non-
homogeneous soil samples is a common occurrence. Therefore, for technical review
purposes only, Regional policy may allow the use of less restrictive criteria (e.g., _+
35% RPD, ±_ 2x the CRDL) to be assessed against duplicate soil samples.
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D. Evaluation:
1. Verify from the COVERPAGE-IN, Form VI-IN, and the raw data that the appropriate
number of required duplicate samples were prepared and analyzed for the SDG.
2. Evaluate Form VI-IN and the raw data to verify that all duplicate results, for each analyte
and method, fall within the established control limits.
3. Verify that the field blank was not used for duplicate analysis.
4. Check the raw data and recalculate one or more of the RPD values using the following
equation to verify that the results have been correctly reported on Form VI-IN.
RPD = !S-Di x 100
(S+D)/2
Where:
RPD = Relative Percent Difference
S = First Sample Value (original sample)
D = Second Sample Value (duplicate)
E. Action:
1. If the appropriate number of duplicate samples were not analyzed for each matrix, with
the correct frequency, then the data reviewer should use professional judgement to
determine if the associated sample data should be qualified. The reviewer may need to
obtain additional information from the laboratory. The situation should then be recorded
in the data review narrative, and noted for TPO action.
2. If the results from a duplicate analysis for a particular analyte fall outside the appropriate
fixed control windows, qualify the results for that analyte in all associated samples of the
same matrix as estimated (J).
3. It should be noted for TPO action if a laboratory uses a field blank for the duplicate
sample analysis. All of the other QC data must then be carefully checked, and
professional judgement exercised by the data reviewer when evaluating the data.
Note; This information must be included on the IRDA form.
4. Whenever possible, the potential effects on the data due to out-of-control duplicate
samples results should be noted in the data review narrative.
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VII. SPIKE SAMPLE ANALYSIS
A. Review Items: Form I-IN, Form V-IN (Part A & B), instrument printouts, raw data.
B. Objective:
The spiked sample analysis is designed to provide information about the effect of each sample
matrix on the sample preparation procedures and the measurement methodology. If the spike is
added to the sample prior to any distillation steps (cyanide), or before the digestion (e.g., prior
to the addition of other reagents), it is then referred to as a spiked sample, a pre-digestion/pre-
distillation spike, or a matrix spike. If the spike is added to the sample after the completion of
the distillation or digestion procedures, it is then referred to as a post-digestion/post-distillation
spike, or an analytical spike.
C. Criteria:
1. Samples identified as field blanks cannot be used for spiked sample analysis.
2. At least one spiked sample (pre-distillation/pre-digestion) must be prepared and analyzed
from each group of samples with a similar matrix type (e.g., water, soil) and
concentration (e.g., low, medium), or for each SDG.
3. For Flame AA, ICP, and CN analysis, when the pre-distillation/pre-digestion spike
recovery falls outside of the control limits and the sample result does not exceed 4x the
spike added, a post-digestion/post-distillation spike shall be performed for those elements
that do not meet the specified criteria. Spike an aliquot of the remaining unspiked sample
at 2x the indigenous level, or 2x the CRDL, whichever is greater.
Note: Post-digestion spikes are not required for Ag and Hg. Additional spiked sample
analyses may be required through Regional EPA or Project Officer request. Alternately,
EPA may require that a specific sample be used for the spiked sample analysis.
4. If two analytical methods are used to obtain the reported values for the same element
within a SDG (e.g., ICP and GFAA, or a soil and a water method), spiked samples must
be run by each method used.
5. The spike percent recovery (%R) must be within the established acceptance limits.
However, spike recovery limits do not apply when sample concentration exceeds the
spike concentration by a factor of 4 or greater. In such an event, the data shall be
reported unflagged even if the percent recovery does not meet the acceptance criteria.
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6. If the spiked sample analysis was performed on the same sample that was chosen for the
duplicate sample analysis, spike calculations shall be performed using the results of the
sample designated as the "original sample". The average of the duplicate results cannot
be used for the purpose of determining percent recovery.
Note; The final spike concentrations required for the various target analytes are
presented in the actual analytical methodologies.
D. Evaluation:
1. Verify from the COVERPAGE-IN, Form V-IN, and the raw data that the appropriate
number of required spiked samples were prepared and analyzed for the SDG.
2. Verify that the field blank was not used for the spiked sample analysis.
3. Evaluate Form V-IN and the raw data to verify that all pre-distillation/pre-digestion
spiked sample results, for each analyte and method, fall within the established control
limits. If not, verify that a post-digestion/post-distillation spike was prepared and
analyzed (see INORG Section VII.C.3. above).
4. Recalculate from the raw data one or more of the spiked sample percent recoveries (%R)
using the following equation, and verify that the recalculated value agrees with the
laboratory reported values on Form V-IN.
%R = (SSR-SR) x 100
SA
Where:
SSR = Spiked Sample Result
SR = Sample Result
SA = Spike Added
Note; When the sample concentration is less than the instrument detection level (IDL),
use SR=0 only for the purposes of calculating the %R. The actual spiked sample
results, sample results, and %R (positive or negative) still shall be reported on Form V-
IN for ICP, AA, and Cyanide analyses.
E. Action:
It should be noted for TPO action if a laboratory uses a field blank for the spiked sample
analysis. All of the other QC data must then be carefully checked, and professional
judgement exercised by the data reviewer when evaluating the data.
Note: This information must be included on the IRDA report form.
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2. In the instance where there is more than one spiked sample result per matrix and
concentration, per analytical method per SDG, if one spiked sample recovery is not
within contract criteria, flag all of the samples of the same matrix, level, and method in
the SDG.
3. If the pre-distillation/pre-digestion spike recovery does not meet criteria, a post-
distillation/post-digestion spike is required for all analytes (except Ag and Hg), and is
required for all methods (except furnace). The data from the post-spikes is not to be
used to qualify sample results.
Note; This information must be included in the IRDA report form.
4. If the spike recovery is > 125% and the reported sample results are < IDL, the data is
acceptable for use.
5. If the spike recovery is > 125% or < 75% and the sample results are > IDL, qualify the
data for these samples as estimated (J).
6. If the spike recovery falls within the range of 30-74% and the sample results are < IDL,
qualify the data for these samples as estimated (UJ).
7. If spike recovery results fall < 30% and the sample results are < IDL, qualify the data
for these samples as unusable (R).
8. Whenever possible, the potential effects on the data due to out-of-control spiked sample
results should be noted in the data review narrative.
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VIII. GRAPHITE FURNACE ATOMIC ABSORPTION PC
A. Review Items: Form I-IN, Form V-IN, Form VIII-IN, instrumental printouts, raw data.
B. Objective:
Because of the nature of the Graphite Furnace Atomic Absorption (GFAA) technique, special
analytical procedures are required for the quantitation of samples. The special QA/QC furnace
procedures are outlined in the method. Duplicate injections and multiple level furnace post
digestion spikes are used to establish the precision and accuracy of the individual analytical
determinations.
C. Criteria:
1. All GFAA analyses shall fall within the calibration range. In addition, all GFAA
analyses, except during full Methods of Standard Additions (MSA), require duplicate
injections. Average concentration values are used for reporting purposes.
2. The Furnace Atomic Absorption Analysis Scheme ("MSA Tree") must be followed as
described in the method.
3. A maximum of 10 full sample analyses to a maximum 20 injections may be performed
between each consecutive continuing calibration verification (CCV) and blank analysis.
4. For sample concentrations greater than the CRDL, the duplicate injection readings must
agree within 20% Relative Standard Deviation (RSD), or Coefficient of Variation (CV),
otherwise the analytical sample must be rerun once (e.g., at least two additional
injections).
5. The post-digestion (analytical) spike concentration must be at 2x the CRDL (except for
lead which must be at 20 ug/L). This requirement for an analytical spike will include
the LCS and the Preparation Blank (PB).
Note; The LCS shall be quantitated from the calibration curve and corrective action, if
needed, shall be taken accordingly. MSA is not to be performed on the LCS or the PB,
regardless of spike recovery results.
6. The analytical spike of a sample must be run immediately after that sample.
7. The spike percent recovery must be within the established acceptance limits of the
method, in order for the sample to be quantitated directly from the analytical calibration
curve.
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8. If the spiked sample's percent recovery is outside of the method acceptance limit criteria,
quantitation by MSA is then required.
9. The correlation coefficient for any MSA analysis shall be greater than or equal to 0.995.
If the correlation coefficient for a specific MSA is less than 0.995, then that MSA shall
be repeated at least once prior to reporting.
D. Evaluation:
1. Review the Furnace AA raw data to verify that the Furnace Atomic Absorption Scheme
has been followed.
2. Check the raw data and verify that duplicate injections agree within ±20% RSD (or CV)
for sample concentrations reported greater than the CRDL.
3. Recalculate the spike recovery results for the LCS and/or the PB. Verify that the spike
recovery results are within the established method acceptance window.
4. Recalculate from the raw data one or more of the MSA results (if MSA was performed),
and verify that the recalculated value(s) agrees with the laboratory reported value(s) on
Form VIII-IN.
5. Confirm that the MSA spikes have been performed at the appropriate concentration
levels.
E. Action:
1. If duplicate injections are outside the ±20% RSD (or CV) acceptance limit and the
sample has not been rerun once as required, qualify the associated data as estimated (J).
2. If the rerun sample results do not agree within +20% RSD (or CV), qualify the data as
estimated (J).
3. If the post-digestion spike recovery is:
a. Less than 40%, qualify results greater than the IDL as estimated (J).
b. Less than or equal to 10%, but <40%, qualify results less than the IDL as
estimated (UJ).
c. Less than 10%, qualify results less than the IDL as unusable (R).
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4. If sample absorbance is <50% of the post digestion spike absorbance then:
a. If the furnace post digestion spike recovery is not within the established method
acceptance limits, then qualify the sample results greater than the IDL as
estimated (J).
b. If the furnace post digestion spike recovery is not within the established method
acceptance limits, qualify the sample results less than the IDL as estimated (UJ).
5. If Method of Standard Additions (MSA) is required but has not been done, qualify the
data as estimated (J).
6. If any of the samples run by MSA have not been spiked at the appropriate levels, qualify
the data as estimated (J).
7. If the MSA correlation coefficient is less than 0.995, qualify the data as estimated (J).
8. Whenever possible, the potential effects on the reported data due to out-of-control spiked
Prep Blanks, spiked LCS, or MSAs should be noted in the data review narrative.
Professional judgement shall be exercised by the data reviewer when evaluating the data.
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IX. ICP SERIAL DILUTION
A. Review Items: Form I-IN, Form IX-IN, instrumental printouts, raw data.
B. Objective:
The serial dilution of samples quantitated by ICP determines whether or not significant physical
or chemical interferences exist due to sample matrix.
C. Criteria:
1. An ICP Serial Dilution analysis must be performed on a sample from each group of
samples with a similar matrix type (e.g., water, soil) and concentration (e.g., low,
medium), or for each Sample Delivery Group (SDG), whichever is more frequent.
2. Samples identified as field blanks cannot be used for the ICP serial dilution analysis.
3. If the analyte concentration is sufficiently high (concentration in the original sample is
minimally a factor of 50 above the IDL), the serial dilution analysis (a 5-fold dilution)
must then agree within a 10% Difference (%D) of the original determination after
correction for dilution.
D. Evaluation:
1. Check the raw data and recalculate the %D using the following equation. Verify that the
serial dilution analysis results, and the calculated %D results agree with the values
reported by the laboratory on Form IX.
%D = |I-S| x 100
I
Where:
I = Initial Sample Result
S = Serial Dilution Result (Instrument Reading x 5)
2. Check the raw data for any evidence of negative interference (results from the diluted
sample which are significantly higher than the original sample), possibly due to high
levels of dissolved solids in the sample, ionization effects, etc.
E. Action:
1. When the required 10% Difference criteria are not met, qualify the associated data as
estimated (J).
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2. If evidence of negative interference is found, professional judgement must be used to
qualify the associated sample data. The potential effects on the reported data should be
noted in the data review narrative.
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X. FIELD DUPLICATES
A. Review Items: Form I-IN, Instrumental printouts, raw data.
B. Objective:
Field duplicate samples may be taken and analyzed as an indication of overall precision. These
analyses measure both field and lab precision; therefore, the results may have more variability
than lab duplicates which measure only lab performance. It is also expected that soil duplicate
results will have a greater variance than water matrices due to difficulties associated with
collecting identical field samples.
C. Criteria:
There are no "required" review criteria for field duplicate analyses comparability.
D. Evaluation:
Samples which are field duplicates should be identified using EPA Sample Traffic Reports or
sample field sheets. The reviewer should compare the results reported for each sample and
calculate the Relative Percent Difference (RPD), if appropriate.
E. Action:
Any evaluation of the field duplicates should be provided within the data reviewer's narrative
comments.
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XI. OVERALL ASSESSMENT
A. Review Items: Entire data package, data review results, preparation logs, calibration standard
logs, instrument logs, instrumental printouts, and raw data.
B. Objective:
The objective is to ensure that the reported sample quantitation results are accurate. It is
appropriate for the data reviewer to make professional judgements and express concerns, as well
as to comment on the validity of the overall data for a Case. This is particularly appropriate
when there are several QC criteria out of specification. The additive nature of QC factors out
of specification is difficult to assess in an objective manner, but the reviewer has a responsibility
to inform the user concerning data quality and data limitations in order to assist that user in
avoiding inappropriate use of the data, while not precluding any consideration of the data at all.
If qualifiers other than those used in this document are necessary to describe or qualify the data,
it is necessary to thoroughly document/explain the additional qualifiers used. The data reviewer
would be greatly assisted in this endeavor if the data quality objectives were provided. The cover
form and supplementary documentation must be included with the review.
C. Criteria:
Assess the overall quality of the data.
Review all available materials to assess the overall quality of the data, keeping in mind the
additive nature of analytical problems.
Reported analyte concentrations must have been quantitated according to the appropriate analytical
method, as listed in the method.
D. Evaluation:
The raw data should be examined to verify that the correct calculation of the sample results was
reported by the laboratory. Digestion and distillation logs, instrument printouts, strip charts, etc.
should be compared to the reported sample results recorded on the Inorganic Forms.
1. Evaluate any technical problems not previously addressed.
2. Examine the raw data for any anomalies (i.e., baseline shifts, negative absorbance,
omissions, legibility, etc.).
3. Verify that there are no transcription or reduction errors (e.g., dilutions, percent solids,
sample weights) on one or more samples.
4. Verify that results fall within the linear range of the ICP (Form XIII) and within the
calibrated range for the non-ICP parameters.
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5. When the laboratory provides both ICP and furnace results for an analyte in a sample and
the concentration is > ICP IDL, the results can assist in identifying quantitation
problems.
6. If appropriate information is available, the reviewer may assess the useability of the data
to assist the data user in avoiding inappropriate use of the data. Review all available
information, including the QAPjP (specifically the Data Quality Objectives), SAP, and
communication with data user that concerns the intended use and desired quality of these
data.
E. Action
1. Use professional judgement to determine if there is any need to qualify data which were
not qualified based on the QC criteria previously discussed.
2. Write a brief narrative to give the user an indication of the analytical limitations of the
data. Any inconsistency of the data with the SDG narrative should be noted for TPO
action. If sufficient information on the intended use and required quality of the data are
available, the reviewer should include his/her assessment of the useability of the data
within the given context.
3. If there are any discrepancies found, the laboratory may be contacted by the designated
representative to obtain additional information that could resolve any differences. If a
discrepancy remains unresolved, the reviewer may determine qualification of the data is
warranted.
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GLOSSARY A;
Definition of Selected Terms
Associated Samples
AA
Calibration Curve
Case
CCB
CCS
CCV
CLP
CRDL
CV
EMSL/LV
Field Blank
Any sample related to a particular QC analysis.
For example:
- For ICV, all samples run under the same calibration curve.
- For duplicate RPD, all SDG samples digested/distilled of the
same matrix.
Atomic Absorption
A plot of absorbance versus concentration of standards
A finite, usually predetermined number of samples collected in
a given time period for a particular site. A Case consists of one
or more Sample Delivery Groups.
Continuing Calibration Blank - a deionized water sample run
every ten samples designed to detect any carryover
contamination.
Contract Compliance Screening - process in which SMO
inspects analytical data for contractual compliance and provides
EMSL/LV, laboratories, and the Regions with their findings.
Continuing Calibration Verification - a standard run every ten
samples designed to test instrument performance.
Contract Laboratory Program
Contract Required Detection Limit
Coefficient of Variation
Environmental Monitoring System Laboratory/Las Vegas (P.O.
Box 15027, Las Vegas, Nevada 89114)
Field blanks are intended to identify contaminants that may have
been introduced in the field. Examples are trip blanks, travel
blanks, rinsate blanks, and decontamination blanks.
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Field Duplicate
Holding Time
ICB
ICP
ICS
ICV
Initial Calibration
IRDA
LCS
MS
MSA
Post Digestion Spike
QAC
RPD
RSCC
RSD
Serial Dilution
A duplicate sample generated in the field, not in the laboratory.
The time from sample collection to laboratory analysis.
Initial Calibration Blank - first blank standard run to confirm the
calibration curve.
Inductively Coupled Plasma
Interference Check Sample
Initial Calibration Verification - first standard run to confirm the
calibration curve.
The establishment of a calibration curve with the appropriate
number of standards and concentration range. The calibration
curve plots absorbance or emission versus concentration of
standards.
Inorganic Regional Data Assessment
Laboratory Control Sample - supplied by EPA
Matrix Spike - introduction of a known concentration of analyte
into a sample to provide information about the effect of the
sample matrix on the digestion and measurement methodology.
Method of Standard Addition
The addition of a known amount of standard after digestion.
(Also identified as analytical spike, or spike, for furnace
analyses.)
Quality Assurance Coordinator
Relative Percent Difference
Regional Sample Control Center
Relative Standard Deviation
A sample run at a specific dilution to determine whether any
significant chemical or physical interferences exist due to sample
matrix effects. (ICP only)
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SDG Sample Delivery Group - defined by one of the following,
whichever occurs first:
- case of field samples
- each twenty field samples in a Case
- each 14-day calendar period during which field samples in
a Case are received, beginning with receipt of the first
sample in the SDG.
SMO Sample Management Office
SOP Standard Operating Procedure
SOW Statement of Work
TPO Technical Project Officer
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GLOSSARY B;
INORGANIC REGIONAL DATA ASSESSMENT
Region
CASENO. SITE
LABORATORY NO. OF SAMPLES/MATRIX
SDG# REVIEWER (IF NOT ESD)J
SOW#
REVIEWER'S NAME
TPO: ACTION FYI
COMPLETION DATE
1. HOLDING TIMES
2. CALIBRATIONS
3. BLANKS
4. ICS
5. LCS
6. DUPLICATE ANALYSIS
7. MATRIX SPIKE
8. MSA
9. SERIAL DILUTION
10. SAMPLE VERIFICATION
11. OTHER QC
DATA ASSESSMENT SUMMARY
ICP AA Hg CYANIDE
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12. OVERALL ASSESSMENT
O = Data had no problems/or qualified due to minor problems.
M = Data qualified due to major problems.
Z = Data unacceptable.
X = Problems, but do not affect data.
ACTION ITEMS:
AREAS OF CONCERN:
NOTABLE PERFORMANCE:
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