NCD003200383_19930917_Koppers Co. Inc._FRBCERCLA SAP QAPP_QAPP Manual - Replacement Pages Appendix A-2-OCR

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KIJPPERS COMPANY. INC. NPL SITE LAB QUALITY ASSURANCE MANUAL -ATT. A MARDI 1993
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Vj =
=
DF =
The aliquot size (such as injection amount) of the - -
prepared sample, taken for analysis, in units of mL
The total final v_olume of the prepared sample ( extract
volume, digest volume, etc.) in units of mL
The amount of sa:f'e taken for preparation. For
liquid samples, use ; for solid samples use the weight
in kg. If the results are to be determined on the basis of
dry weight, use the following to determine the sample
size:
As (dry) = As (wet) x %solids
100
Dilution factor. The dilution factor is 1 for samples that
are prepared exactly as prescribed in the protocol. If
the extract or digestate require dilution, then the
dilution factor differ from unity. For example, if an
extract is diluted from 1 mL to 100 mL the dilution
factor becomes 100. If an extract is concentrated from
10 mL to 1 mL the dilution factor becomes 0.1.
In many methods, the data reduction is computerized, alleviating the need for
extensive manual reduction of the results. , However, the analyst must review the
data, relating it back to the fundamental measurements on which the analyses are
based. Thus, in chromatographic techniques, the analyst will compare area counts
of peaks with those of the corresponding standard, and verify that the data were in
fact correctly reduced. It is also the responsibility of the analyst to verify the
identification of parameters.
6.3 Data Validation
Data validation within each analytical group has been discussed previously. It is not
the responsibility of the QA/QC personnel to check and verify every value
generated and reported by the laboratory; however, the QA/QC Section will
function in a reviewing capacity to assure that the data validation process remains
reliable and is performed according to laboratory policy.
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These items must be verified during the data validation process:
a. Is the batch complete?
b.
c.
d.
e.
f.
g.
h.
i.
J.
Have all the analyses been performed within holding times, and if not
is there an acceptable explanation for deviations from the holding
times?
Is there a valid continuing calibration associated with the runs for
each parameter of the individual samples within the batch?
Is the sample sequence proper for the method (i.e., are there regular
blanks run when necessary, are there standards run for methods
requiring periodic standards, are there laboratory blank spikes, mati-ix
spikes, and laboratory duplicates)?
If surrogates are required by the method, are recoveries within the
control limits in the spiked blank?
Are surrogate recoveries within control limits in the samples?
Is the recovery of spiked compounds in the laboratory spiked blank
acceptable?
Is the recovery of spiked compounds in the spiked sample acceptable?
Do duplicate analyses in the run sequence exhibit precision within the
control limits?
Is the documentation in order?
If the answers to all the questions above are "yes", the data will be released and
reported .
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If the· answer to··· any of · the questions is '· negative, ··corrective · action will be
undertaken and reported to the QA/QC Section and the Project Manager. A
Corrective Action Notice (Figure 5-2) will ·be generated and submitted to the
QA/QC Section by the Group Leader, thus documenting the source of the problem
and its resolution. Data Validation is a check of the batch for completeness,
ac=acy and precision. If all criteria are met, ,the batch is released. If some are not
met, the batch may still be released, depending upon what criteria are not met and
what is the explanation for not meeting the criteria. There are certain
circumstances when the release of the data is not allowed regardless of the rationale
for the lack of acceptability. These are:
a.
b.
C.
Continuing calibration was either not performed as required,
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Laboratory control standards (spiked blanks) were not run or did not meet
acceptance criteria
Data sets are not complete
Corrective action for these situations will be discussed in Section 7.0.
If certain aspects of the data do not meet acceptance criteria, but consultation with
the project manager or the Group Leader res\ilted in a decision to release the data,
the Quality Assurance Manager will annotate on the Corrective Action (Figure 5-2)
the shortcomings_ of the data, the decision to :proceed with reporting the data, and
the person with whom that decision had been:reached. The QA Manager will then
submit the form to the Information Services Section so that the final report can be
prepared.
If the decision has been made not to release the data, the form will be marked "DO
NOT RELEASE DATA" and submitted to the Information Services Section.
In addition to validating the data, it is also necessary to validate specific jobs before
they are released. Specifically, releasing a job consists of insuring that all required
parameters have been analyzed and are reported. The result for each parameter
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·· · · must have been acceptably validated through approval of the individual batches that·
make up all of the parameters associated with the job. It is the responsibility of the
Information Services .Section in conjunction with the Project Manager to assure that
all data are validated and entered and that the documentation is complete before
the final report is generated. The QA/QC Section will only spot check the final
reports.
6.4 Data Compilation
Information Services personnel will review the job file to confirm that all the data
are in .the file and references are made to those items which are associated with the
job but are present in other files.
The data will then be entered in standardized forms, and the report printed out .
6.5 Final Review
When the final report has been printed, the Project Manager will proof the report
against the raw data in the file. If all the data are properly entered, the report will
be reviewed by the Lab Director and approved before it is sent to the client. A copy
of the report will be placed in the job file, and the file will be transferred to the
' central file storage for completed jobs.
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7.0 · CORRECTIVE ACTION .
There are many areas of the laboratory functions which may require corrective
action. The decision to undertake corrective action, and the ensuing action must be
documented so that traceability can be maintained. The point or originating the
corrective action varies, depending upon the mode of detecting that such action is
necessary. It is, however, frequently the role of the QA/QC Section to initiate such
action, simply because it is this section whic~ is most exposed to the malfunctions of
the laboratory as they reflect upon the data produced. Those actions that affect the
quality of the data will be recorded and the record maintained by the QA/QC
Section.
7.1 Identification of Potential Problem
Identification of sources of problems is not always an easy matter. It is not expected
that the QA/QC Section will be able to trace the source of every problem identified.
However, the QA/QC Section will be responsible for informing the Section
Manager or Group Leader and the Laboratory Director when a problem exists in a
particular analysis. In this case, data for that type of analysis will not be accepted
until the problem is isolated and corrected. It will be the responsibility of the Group
Leader to address the identification of the source of the problem, and the
responsibility of the Laboratory Director to assure that the Group Leader is acting
upon the need for corrective action.
In some situations, the need to correct an operation is apparent to the analyst. For
example, instrument failures are detected by 'the analyst and the corrective action is
taken in the form of repairing the instrument either through a service call or using
laboratory personnel. Such action must be recorded in the instrument maintenance
log and close scrutiny will be paid to the analyses just preceding the instrument
failure. If these analyses meet the required acceptance criteria, no further action
will be taken relative to that data.
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In other situations, the time of data validation is the more logical time to isolate a
potential problem. For example, if a systematic drift occurs due to chromatographic
column contamination, it is easier to identify at the time of validating the data and
comparing the results with historically available information.
7.2 Problems and Actions
7.2.1 Continuing Calibration Outside Acceptance Range
When the continuing calibration is outside the acceptance range, the problem
should be identified by the analyst and corrected before further sample processing is
undertaken. However, the acceptability of the continuing calibration is also subject
to review at all later checks in the data validation process.
The data on all samples that have been analyzed following the last time that the
calibration was within specification will be rejected. (If data have been released to
Information Services, the QA/QC Section will be notified i=ediately using the
Form shown in Figure 5-2.) The affected samples will be reanalyzed after the new
initial calibration curve has been constructed.
7.2.2 Calibration Standards Exceeding the Permitted Holding Time
If calibrations s~andards have been continuously used beyond their permitted shelf-
life, the group responsible for the analysis will be notified, and a Corrective Action
Notice (Figure 5-2) will be generated. The group will then be responsible for
preparing fresh calibration standards, and the instrument calibration will be checked
against the new standards. If the previous runs, performed with the expired
standards meet the acceptance criteria based on the new standard, the data
generated will be considered valid, in spite of the use of an expired calibration
standard.
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If the calibrations performed with the expiriid standard do.not meedhe acceptance -
criteria when measured against the new standards, the_ samples that have been
analyzed against the expired standard will be reanalyzed and quantified using the
freshly prepared standards.
7.2.3 Laboratory Method Blanks Exceed Method Detection Limit
but are Below Quantitation Limit
When laboratory blanks exhibit the presence: of target analytes at a level exceeding
the method detection limit, but still below the quantitation limit, the responsible
group will be notified.
The.responsible section will check the reagent blanks that have been retained at the
time o_f use of the reagents in order to determine if contamination or interferences
are due to impurities in the reagents. If this' is the case, the reagent batch will be
discarded, and new reagents will be used .
If the reagents appear to be sufficiently 'pure, the cleanliness in laboratory
procedures will be reviewed to establish if the source of problems may have been
contamination of the apparatus.
7.2.4 Laboratory Method Blank Exceeds the Quantitation Limit
When the laboratory method blank exceeds the quantitation limit, the Group
responsible for the analysis will be notified. As discussed in Section 7.2.3, the
analysts will check for potential contamination of reagents and apparatus. If the
reagents are contaminated, the existing reagent batch will be discarded and a fresh
batch from new containers will be prepared.
If the problem arose from the apparatus or glassware, the problem will be corrected
within the analytical group, and the correction documented before any further
analyses can be undertaken. Notification of the corrective action will be submitted
by the Group Leader to the QA/QC Section.
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Toe data associated with the failed method blank will not be accepted. Toe samples
will be reanalyzed to produce acceptable data.
7.2.5 Laboratory Control Standard Exhibits Recoveries Outside the
Acceptance Criteria
When the laboratory control standard (spiked blank) does not meet the acceptance
criteria, the batch of samples associated with the laboratory control standard will be
reanalyzed if determinative methods call for this as corrective action. Where, as in
many organic methods, a check sample is analyzed only for failed spiked sample
components, then reanalysis of the batch will also be necessary, but only for the
failed-components. In methods that require the use of a laboratory control standard
at frequent intervals through the day, only those samples analyzed since the last
acceptable laboratory control standard analysis will require repeating. Data
originating from batch analyses preceding the failed QC check will be rejected .
Before repeating a whole set of preparations of samples, the calibration of the
instrument or method shall be checked. If the instrument is within calibration, the
samples will require repreparation. If the instrument calibration has drifted, the
prepared samples from the initial preparation can be reanalyzed after the
instrument has been recalibrated.
7.2.6 Surrogates and Sample Spikes Exhibit Recoveries Outside the
Acceptance Limits
When recoveries from spiked samples are outside the acceptance limits, but the
laboratory spiked blank is within the acceptance criteria, the poor recovery or
enhanced apparent recovery may be due to matrix effect. One such sample from the
batch will be reprepared and reanalyzed. If, the same phenomenon is observed, it
will be assumed that the failure to meet recovery criteria was, in fact, a matrix effect.
This information will be included in the report to the client; however, the original
data will be accepted.
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7.2. 7 Control Chart Exhibits a Regular Trend
By their very nature,. the individual points that make up the control chart for any
analyte vary randomly about a mean value. The control chart is used to assess the
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· acceptability of recovery data on the basis of historical data. The control chart is
also used to warn the analyst that some consistent problem or deviation in the
method may be occurring.
When five successive points on the control chart form a steady pattern, either
regularly increasing or regularly decreasing, they imply that some change is
occurring in the analytical scheme. Even if all the points are within the control
limits_, a warning will be issued by the QA/QC Section to the responsible group to
investigate the cause of the pattern. If, in fact, a change has occurred in the method,
and if ·the change indicates an improvement in recoveries (an improvement is
defined as approaching complete recovery, not necessarily an upward trend), then a
new control chart will be established, and sub'sequent data will be compared to the
new control chart limits. If a change has occurred that worsens the recovery, it will
be the responsibility of the Group Leader to assure that a return to the previously
used technique is made in his section.
7.2.8 Internal and External Audits and Corrective Actions
Internal system ~udits are quarterly samples issued by the QA/QC Section, using
known spiked solutions to determine the acceptability of performance in every
group of the laboratory. External performance evaluation is either done through a
contract required performance audit, or though voluntary participation in
interlaboratory studies.
7.2.8.1 Evaluation of System Audits
When the achieved results on these audits fall below acceptable standards, as
defined on the basis of historical recovery data, a thorough review of the system will
be initiated. The QA/QC Section is responsible for the initiation of the process.
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. The first steiwill consist of complete review of the correctness of the documenting
of the job and the calculations of the results. This process will be performed by the
personnel of the QA/QC Section. When the results of the review are complete, .a
memo will be issued to the responsible group of the laboratory, itemizing the
deficiencies that have been identified. If no deficiencies have been identified, the
difficulty may be with the performance of the analyst, the analytical method, or
incorrect preparation of the audit sample.
7.2.8.2 Corrective Action and Feedback
The gr.oup leaders will be responsible for investigating problem areas identified by
the QA/QC Section. A written report of the findings and corrective action taken
will be submitted to the QA/QC Section within one week of the beginning of the
Group· Leader's investigation into the problem. If the source of the problem has not
been located at this point, the QA/QC Section will issue a repeat performance
evaluation audit sample. It will be assumed that the problem was with the original
audit sample itself if the repeat evaluation sample is successfully analyzed within
acceptance limits. Otherwise, the process outlined. above will continue until the
manager of the QA/QC Section determines •that the problem has been corrected
and notifies the Group Leader of the successful resolution.
7.2.8.3 Documentation of Corrective Action
When the cause for failed internal or external audit samples has been identified and
corrective action implemented, the QA/QC Section will document the resolution of
the problem in a brief report to laboratory management. The QA/QC Section will
also maintain a file of corrective actions which were necessary to remedy
performance deficiencies which have arisen.
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5.11 Development of New or Modified Methods
There are occasions when it is necessary in the laboratory either to devise a new
approach to analysis or modify an existing method. The former may be needed for
analytes for which proven methods do not exist, or if they do, they are not applicable
to the matrix being handled. The latter case is frequently the· situation that arises
because of unusual matrix interferences. It is not the intent of this manual to prescribe
analytical approaches to analytes for which methods do not yet exist. . However, in
order that the laboratory may use the methods with any reliance on the data, the new
method must be subjected to the repetitive analyses of a spiked matrix in order to
ascertain method precision and accuracy. No method will be employed by the
laboratory without the establishment of precision, accuracy, and detection limits.
When a method is being modified, or a new method is being devised and tested for
anaiytes for which an existing approved method is available, a new or modified method
will be subjected to equivalency testing. In performing the equivalency testing, the
analytes will be subjected to seven replicate analyses in parallel by the existing method
and the new method. To be acceptable, the new method must produce results that are
statistically equivalent or are better than the old method. In addition, sufficient
replicate analyses will be performed to assure that acceptance criteria may be
established. The new or modified method will then be written, the method with the
supporting data and documentation will be reviewed by the Section Manager for the
section in which the analyses will be performed and by the QA/QC Manager. When
approved, the method may become part of the repertoire of the laboratory for clients
whose work does not require method approval by EPA or other regulatory agencies.
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6.0 DATA HAi-..DLING
The data produced by the various groups of the laboratory are ultimately the
product which the laboratory offers. Hence, not only is it necessary to produce
results with accuracy and precision, but it is also necessary to be able to maintain
the traceability of the data and the association of sets of data with each other. The
responsibilities to the production of accurate and precise data are with the
individual analysts. They are, after all, the producers of the data. No amount of
supervision and validation can correct for mistakes or omissions occurring at the
bench. At best, supervision and validation can cull the unsupported data.
Tracea~ility of the data, however, pertains to the manner in which the records are
kept within the laboratory as a whole. Because of this, record keeping in the
laboratory, will be addressed first. This will be followed by a brief discussion of data
reduction, data validation, data review and release, and reporting.
6.1 Data Recording
The modes of maintaining data in the various groups will differ with the methods of
analysis. Certain aspects of record keeping have been addressed in the section
pertaining to the sample log in and distribution of the information through the
laboratory. The traveller and the sample transfer forms constitute the first step in
the generation of data for any set of samples. Samples in the laboratory, however,
are analyzed in batches. On large jobs, a batch may constitute just a portion of the
total number of samples in the job. For small job, a batch may consist of samples
from several travellers handled together. Thus, the maintenance or records in the
laboratory must also provide for cross-referencing batches and travellers.
6.1.1 Notebooks
Certain records are maintained in notebooks by the analysts. These records may
pertain to methods that are entirely manual, such as many of the methods in wet
chemistry, or they may be used to record unusual observations during the
performance of preparation and analyses of instrumental techniques. These
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notebooks become a permanent record of laboratory work, and they must be
traceable.
Bound hardcover notebooks, with prenumbered pages, will be numbered and issued
by the QA/QC section. The QA/QC section will number the notebook, and record
in its own notebook log the date of issuance and the laboratory section to which the ·
notebook has been issued. When the notebook has been filled, it will be maintained
in the analytical section for permanent archiving.
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Users of the notebooks will maintain good laboratory practices in their use. No
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pages will be tom out of the notebook; corrections will be done by single line-out
erasure·s, followed by initialling and dating the correction; and each page of the
notebook will be signed and dated by the analyst at the time entries are made on the
page. The use of correction tape, liquid paper, erasures, or other means to make
corrections is not permitted .
6.1.2 Record Keeping in Sample Preparation·
All records for routine sample preparation wiU be kept on standardized forms. The
forms will be filled by the person preparing the samples. The forms will be filled in
ink, with no erasures.
If an error occurs, the preparer will line out the erroneous entry once, and enter the
correct entry. The preparer will then initial and date the correction.
The following information must be entered:
a.
b.
C.
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The analysis type for which the samples are prepared (usually the
heading of the sheet)
The date of preparation, and the name of the preparer
The QC batch identification
6-2
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-d. ----A listing of the samples being prepared, using the laboratory's sample .
identification
e.
f.
g.
h.
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· For each sample listed, the quantity of sample taken, including the
units of measurement (for solid samples, use the wet weight)
If the method calls for the addition of surrogates, then for each
sample the surrogate mixture identification and the quantity,
including units
For any sample that is spiked, the identification of the spiking mixture
and the quantity, including units
The identification of the medium of the prepared sample (i.e., the
solvent for organic extraction, the acid for metal preparation, etc.)
and the lot numbers of the reagent media
The final volume of each prepared sample, including units
Any unusual observations. If these are recorded in a notebook, the
notebook and page numbers must be entered on the form.
In addition to filling the form, the preparer must also label the prepared samples.
As a minimum, the label will identify the sample and the QC batch in which the
sample has been prepared.
When the preparation is complete, the form will be checked for completeness by the
Group Leader .and initialed and dated. The preparer will make as many copies of
the filled form as there are different jobs in the batch. The original of the form will
be maintained in the file of the preparing section. The preparer will then transfer
the prepared samples with the accompanying copies of the preparation records to
the section responsible for the analysis of the prepared samples.
Examples of standard forms for maintaining the records in the sample preparation
areas are shown in Figures 6-1 and 6-2.
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I FIGURE6-1
CONTINUOUS EXTRACTION BENCH SHEET
l=xtracted by:
~eter _________ _
IJate Extraction Began. _______ _ Date Completed. _______ _
length of Extraction
~olvent, _____ _ Lot# __________ _ Manufacturer ___ --'------
Surrogate Matrix Spike
Lot# Lot#
Sample Sample Extract
Work Order Number Source pH Volume Amount Added Amount Added
'
tnalyst: ____________ _ Date:
•• wed by: ___________ _ Date:
I 6-3a
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a,
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O"
Case Number (CLP only)
SDG Number (CLP only)
Work Order Sample
Number Number
-
Lot Numbers:
-------
-------
Sample
Source
H202
--I --FIGURE 6-2
CHESTER LABNET-MONROEVILLE
AQUEOUS SAMPLE METALS DIGESTION
Date of Dlgesllon -----
Time of Dlgesllon -----
lnllial Vol. Final Vol. Color Color
(mis) (mis) Before After
.
HCI HNO3 ----------
Page N -----
Technician __________ _
Dlgesllon for (ICP/GFAA) ______ _
Clarlly Clarlly
Before After Comments
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6.1.3 Record Keeping for Instrument Analysis
Many instrument m~thods of analysis produce printed traces, charts, or tables.
Some of the information specified below is entered through a data system before
samples are analyzed. Clearly, those items of information need not be reentered
manually.
For every technique, however, a run log must be maintained. The following
information must be entered in the run log by the analyst.
a. Identification of the analysis (usually this will be the heading of the log)
b. Identification of the instrument
c. Date of analysis, and identification of the analyst
d.
e.
f.
g.
Identification of the QC batch
Sequential listing of samples (including tuning, initial calibration or continuing calibration, blanks, spiked blanks, samples, duplicate samples, spiked samples, etc). This listing must be accurate and sequential, and the run number (where applicable) must be included.
Aliquot of prepared sample that is taken for analysis, including units
Any unusual observations. If these are entered in a notebook, they need only be summarized on the form, and the notebook and page numbers entered for further identification of the comments.
' Where printouts for each sample are obtained separately, the printout must include
the identification of the method of analysis, date of analysis, identification of the
' analyst, identification of the run, identification of the QC batch, and the aliquot of
sample that was used.
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Before·transferring the data further, the analyst must"confirm that··the results,-as----
they appear on the printout, are correct. If the results are incorrect, the analyst will
line them out once, enter the correct val1;1e manually, and initial and date the
change. These corrections will be done in ink. When the analyst is finished with the
batch of samples, including the review of the data, he will initial the run log and
transfer the run log with the data to the Group Leader.
The Group Leader will review the run log to verify that the sample sequence has
been properly followed as required by the specific method. Next, the Group Leader
will check the QC data pertaining to the batch and verify that the instrument was
performing within the required specificatiotjs. The Group Leader also reviews any
dilutions to make sure that they are appropriate, assures that calculations are
accurate, and verifies that reporting units are proper. The QA/QC Section will spot
check ·data and provide guidance for data validation to the Group Leader.
When the Group Leader is satisfied that the data are valid (see Section 6.3, Data
Validation), he will initial the run log and date it. He will have as many copies
made of the run log as there are jobs represented in the batch that has been
analyzed. He will then transfer the sample data to Information Services. Together
with the data, the Group Leader will transfer the copies of the records from the
preparation group to the Information Servic,es Section. The original run log will be
maintained in the files and records of the section responsible for the analysis.
For instrument methods which do not produce the identifying code of the run on the
permanent records, for example, methods that employ a strip chart as the
instrumental output, the individual traces will be identified manually by the run
number, and the identification of the parameters associated with the run will be
recorded manually on the run log.
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6.1.4 . Record Keeping· in Noninstrument Analyses-. -...
'
Raw data from these analyses will be kept in permanently bound, sequentially
paginated notebooks and will include all the information discussed above in
reference to automated printouts. Copies of this data will be submitted to the
Information Services Section, and the original data will remain in the laboratory
notebooks.
6.2 Data Reduction
ReduciJ;lg the raw data to a presentable forin is the responsibility of the analyst
performing the analysis. In reducing data,, the analyst must take into account
whether the sample is aqueous or solid, the sample size, and whether or not the data
are to be presented in the form of wet weight or dry weight. All final values must be
accompanied with the units of the value. The following equation applies to the
calculation for concentration of an analyte in most analytical techniques employed
in the laboratory.
Where:
WB3.17n. 03('13
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RF
=
=
=
Concentration of the analyte in the sample, in
appropriate units [ng/L (ppt), ug/L (ppb), mg/L (ppm);
ng/kg (ppt), ug/kg (ppb), mg/kg (ppm)]
Signal size, in units appropriate to the method
The response factor, as defined in Section 5.6.1, in units
of signal size per unit weight of the analyte. This
response factor is essentially a mean response factor,
determined through regression of the initial calibration
data. If is not possible to use the mean response factor
( usually because of instrumental software limitations),
then the response factor from the run that corresponds
to the midpoint of the linear range is used, as long as
this response factor does not differ from the mean by
more than 10%. · The response factor to be used is
always taken from the initial calibration .
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5.8.2 Spiked Blank
The spiked blank, or laboratory control sample, serves as a measure of accuracy of the
analytical procedure in the laboratory. ni,e spiked blank is prepared by adding
prescribed amounts of specific analytes to laboratory reagent water prior to preparation
of the water for analysis. For inorganic parameters, a spiked blank is prepared for
each batch of twenty or fewer samples that are prepared at the same time. Water is
spiked for certain analytes of interest for the inorganic parameters.
For organic parameters, a spiked blank is pre~ared for every batch of 20 samples that is
subjected to sample preparation. The spike contains only selected analytes which are
specified in the pertinent methods of analysis in the Standard Operating Procedures.
Preparation of the spiking mixture is done in the same manner as the preparation of
standard solutions for calibration. The spiking mixture is also assigned an identifying
code, which is recorded at the time of preparil).g the spiked blank.
The spiked blank is carried through the entire analytical procedure, and the
concentrations of the spiked analytes determined. These values are accumulated by the
QA/QC Section to update acceptance criteria! and to validate data. The spiked blank
forms the backbone of the determination of the reproducibility of data in the laboratory,
I since it is based on a well-characterized matrix (water) and is designed to be essentially
free of matrix effects. If the spiked blank does not meet established acceptance
I criteria, the requirements of the analytical °;lethod will be relied upon to determine
whether the sample failing the acceptance criteria will be reprepared and reanalyzed.
5.8.3 Spiked Sample
Spiked samples serve to confirm that the sample matrix is causing certain effects which
I preclude the ability to recover analytes using the prescribed method. Thus, the spiked
sample is used only to determine matrix effects.
One sample per batch of twenty or fewer samples, of the same apparent matrix, will be
spiked with a spiking solution in the same manner as the spiked blank. The spiked
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sample will be processed through the entire analytical scheme, and the recovery of the
spiked analytes will be determined.
In utilizing spiked sample information, great care should be taken because deviations
from acceptability may be due either to procedure or to matrix effects. Generally, if
the spiked blank associated with the batch exhibits acceptable recoveries, it can be
assumed that the sample preparation and analysis have been performed correctly.
Since sample spiking is performed before the sample is initially analyzed, it is possible
that for some parameters the analyte level in the sample is so high that the spiked
amount is insignificant. Under those circumstances, the analyte spike recovery will be
meaningless and need not be calculated.
In selecting a sample for spiking, every effort ,will be made to choose a field sample,
and not one of the field or trip blanks. This ca~ be accomplished only if the identity of
the field and trip blanks is known in advance. If those samples are submitted entirely
' as blind samples, then the selection of the sample to be spiked will be random.
5.8.4 Sample Duplicate
Either sample or spiked sample duplicates are run to assess precision of the laboratory
work. One in a batch of 20 or fewer samples of the same matrix will be prepared and
analyzed as a sample or spiked sample duplicate.
The precision exhibited by the analyses of sample or spiked sample duplicates may vary
due to the effect of the matrix on the analyses. If that is the case, the related batch
samples will not be reanalyzed unless the approved method calls for such action.
As in the case of the spiked sample analysis, the choice of sample for sample or spiked
sample duplicate analysis will be limited to actual field samples, excluding blanks,
unless the identity of the blanks is not known. In that case, the selection will be
random.
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5.8.5 External Quality Control Audit
An external quality control audit will be performed periodically by submitting for
analysis known standard materials from a source other than that from which the
calibration standards are prepared. These quality control audit samples will be I
submitted for analysis by the QNQC Section, and they will be analyzed by the same
procedures as are used for the analyses of samples.
The external quality control audit will be performed on a quarterly basis. If there are
projects in the laboratory which have these audit samples submitted by the project, and
where the results are made known to the laboratory, then the QNQC Section will not
submit the external quality control audit samples for those parameters which are
includ_ed in project audit samples.
5.8.6 Record Keeping on Analysis of QC Samples
The results of the analyses of the QC samples may pertain to more than one project,
since the sample preparation area batches samples from potentially several sources to
' provide for efficient operation. Hence, the retrieval of the QC data may be necessary
for several different projects. The QC data is identified by the batching identification
provided upon the preparation of the samples. Hence, the retrieval of the data can be
readily achieved by identification of the preparation batch.
For every batch of samples, the identification of the batch will be entered at the
preparation stage on the appropriate forms. Sufficient number of copies of the forms
will be made to file with every project associated with the batch. The results of the
analysis of the QC samples will be filed sequenti_ally by the QC batch number and will
be retrieved through the batch number system whenever it is necessary to retrieve these
data.
The QC approval of an analyzed batch will be. based on the acceptance of the QC
samples associated with the batch. Once the QC samples are determined to be within
acceptable limits, the entire batch of samples will be released and the analytical data for
each sample will be recorded with the appropriate project.
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5.9 Use of Surrogates
The use of surrogates in orgarnc analysis serves as an additional measure of the
acceptability of the results. The significant advantage of the use of surrogates is in
measuring recovery against a historically established acceptance range in the
performance of each analysis. Thus, the data do not depend solely on the spiked blank
to assess the quality of each run.
Surrogates are compounds that are expected to behave analytically in a manner similar
to the target analytes. The surrogates are added into the sample before the preparation
stage is initiated, and their recovery is a measure of the efficiency of the extraction.
The fqllowing surrogates have been used at CHESTER LabNet and are recommended
for use in the approved methodology.
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TABLES-3
SURROGATE COMPOUNDS AND TYPICAL RECOVERIES
EPA METHOD
501/601/8010
502/602/8020
604/8040
605/8050
606/8060
608/8080
609/8090
610/8310
611/8110
612/8120
615/8150
COMPOUND
Bromochloromethane
2-Bromo-1-chloropropane
1,4-Dichlorobutane
Benzotrifluoride
2-Fluorophenol
2,4,6-Tribromophenol
1-Naphthylamine
Dibutylchlorendate
Dibutylchlorendate
2, 4 ,5 ,6-Tetrachloro-m-xylene
2-Fluorobiphenyl
Benzo( e )pyrene
2-Fluorobiphenyl
Isodrin
Dibutylchlorendate
2,4-DB
RECOVERY RANGE
70 · 120
70 · 120
70 · 120
. 80. 120
21 • 100
10 · 123
10 · 94
24 • 154
24 · 154
25 · 125
43 -116
15 -113
40 · 116
33 · 141
24 · 154
40 -140
For GC/MS, standard EPA surrogate compounds will be used for all analyses.
5.10 Establishment of Acceptance Criteria
Establishment of acceptance criteria is necessary in order to be able to determine
whether or not quantitative data generated by the laboratory are within the control
limits. The principal criteria that are used to measure the quality of the data are
accuracy and precision.
The initial determination of acceptance criteria hinges upon repetitive measurements of
prepared spiked solutions and determination of spike recovery. Twenty samples of
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laboratory reagent water are spiked with the analytes of interest at a concentration of
approximately twice the quantitation limit. Where applicable, the water is also spiked ' with surrogates and internal standards. The samples are then prepared for analysis
following the appropriate protocol, and the concentrations of the analytes are
determined. From these values, the mean and the standard deviation for the recovery
of each analyte are determined. The deviation of the mean from the known spiked
amount is a measure of the accuracy of the method. The standard deviation of the
series of measurements is a measure of the precision of the method.
The percent recovery is calculated as follows:
R = 100 X
Where: R = Percent recovery of the ana!yte.
Cm = The measured concentration of the analyte
C1 = The native concentration of the analyte in the sample
(C1 = 0 for blank spike).
Cs = The amount of analyte spiked into the sample.
The accepted recoveries of the analytes must be, within three standard deviations of the
mean. It should be emphasized that recoveries are dependent upon both the method of
sample preparation and the sample matrix. Thus, recoveries from soil are not expected
to be within the acceptance limits as determined for water. Similarly, extraction by
sonication may ·not show the same recovery as would an extraction via a Soxhlet
extractor. Thus, acceptance criteria must be determined matrix by matrix, and method
by method.
Frequently, samples are spiked at the time of sample preparation, without knowing if
the analytes that are being spiked into the sample are present or not, and without
knowing if these analytes are at levels that would make the spike amount insignificant.
The analyst is cautioned that recoveries of spikes should not be calculated if the amount
in the sample is greater than 5 times the spike_. For most applications, if the ratio
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C1/Cs is equal to or greater than 5, the spike recovery should not be calculated, since
the uncertainty in the native concentration is sufficient to cause greater uncertainties in
the spike recovery.
The acceptable prec_ision range is defined in a similar manner. The precision is a
measure of the deviations from the mean of repetitive measurements. Thus, standard
deviation can be used as a measure of precision. More frequently, the relative percent
deviation will be used because, at best, measurements are performed in duplicate.
The relative percent deviation is determined by the equation:
Xl -x2 %RPD= 100 X ' X m
· Where: x1 = High value for the_ analyte
x2 = Low value for the analyte
Xm = mean value for the. analyte
x1 + x2
=
2
The results of the determination of recoveries and relative percent deviations will be ' plotted, indicating the upper and lower limits of acceptance, and the upper and lower
warning limits. Future data will be considered acceptable if recoveries of spikes and
relative deviations of duplicates fall within the acceptance criteria. The control charts
will be updated regularly, generally requiring 20 data points to obtain a· valid control
chart. The QC Section will maintain the control charts and update them regularly,
when sufficient data are collected. Whenever the control charts are updated and the
acceptance limits modified, the QC Section will issue the new limits to the analytical
section of the laboratory in which the analyses are performed. It is the responsibility of
the Group Leader to assure that data within their section are within the acceptance
limits. If they are not, corrective action must be initiated immediately by the Group
Leader of the appropriate section.
If five successive measurements, while falling within the control limits, appear on the
same side of the mean, the analyst will stop to investigate if the trend indicates that a
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change in methodology has occurred. Such· successive points may indicate a pattern,
and it would be necessary to institute a return to preexisting conditions to avoid the
possibility that out of controfsituations may arise.
It is not feasible, in organic analysis, to obtain control charts for every analyte. Thus,
while initial control charts are constructed for all the parameters that are being
analyzed, continuous verification of the control is obtained through the use of surrogate
compounds and the spiked blank analysis. All other analytes in the organic analysis
will be assumed to be within control if their relative response to the internal standards
and surrogate have remained constant.
While accuracy and precision form the backbone of the acceptability of quantitative
data, _9ualitative identification is more difficult to cast into quantitative measures. In
organic analysis, the principal criterion for chromatographic analysis is the retention
time, or relative retention time. Relative retention time is used with those methods
employing internal standards. It is the more reliable measure because it is less
dependent on such physical parameters as the length of the column. In all cases, the
retention time for each analyte, or the relative retention time for the analyte, will be
based on the data obtained from the nearest standard.
To determine the acceptance windows for retention times, the continuing calibration
data will be employed. For each compound, the retention times obtained in performing
the continuing calibrations during the period of one week will be averaged and their
standard deviation determined. The acceptance window will consist of three standard
deviations from. the mean retention time for each compound. The retention time
acceptance window will be redetermined whenever the chromatographic column is
changed or the chromatographic conditions altered. It is the responsibility of the
analyst to maintain the records for retention time criteria. Copies of the established
acceptance windows will be available to the QC Section for reference in reviewing
work. In mass spectrometric analysis, in addition to the retention time, the mass
spectral match of the compound to the standard will be used to verify its identity.
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g. The name of the analyst preparing the standard
A sample logbook page is shown in Figure 5-3, however, Group Leaders may use
another format as long as the listed information is recorded.
In preparing the diluted working standards, it is the analyst's responsibility to make
sure that the stock standard is of valid vintage. The preparation of all working
standards is also recorded in the logbook. The following information is recorded in the
logbook:
a. Date of preparation and expiration date
b. Identification number of the stock standard solution
C. Volume of stock standard solution taken
d. Final volume of the diluted standard solution
e. Concentration of each parameter in the diluted standard
f. Identification number for the diluted standard
g. Name of the analyst preparing the diluted standards
All stock and working standard solutions will be labelled with ID number, composition
and concentration, date of preparation, initials· of the responsible individual, and
expiration date. The ID number assigned in the logbook is used for labelling. It
consists of: logbook number, page number, and item or line number identifier (e.g.,
1 -

2

-

3

is the ID number assigned to the solution found in logbook 1 on page 2 as
item 3).
The working standards for organic analysis will be stored in a freezer in the work area.
No other samples or extracts will be stored in the same freezer. The working standards
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-.-
SOLUTION
ID. NO.
---
PREP.
DATE BY 1-UMEl
-
--• --
STOCK IDENTIFICATION COMPOUND
PLfE STOCI CONG.STOCK EXP.
COM'. S01."N SOL'N. uglml DATE
. --
.
FIGURE 5-3
STANDARD PREPARATION LOG
-- ---•
QUANTITY TAKEN FINAL FIIIAL
VOL. CONC.
ml ug/ml
AMOUNl 9 mg ul mL
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for metals will be stored in the work area in a cabinet or shelf designated for standards
only. These do not need to be refrigerated. For other parameters, the working
standards will be maintained in either a refrigerator or at room temperature in the work
area on specifically designated cabinets or shelves where no other materials are being
stored.
5.5 Determination of Detection and Quantitation Limits
For many projects, knowledge of detection limits is essential in order to be able to
bracket analytical results that are obtained. Several such limits exist, and different
experts define these limits differently. For this reason the definition and determination
used by CHESTER LabNet is given below.
5.5.1 Instrument Detection Limit
In simple terms, the instrument detection limit is the smallest quantity of material that
the instrument can detect. It has been defined in the past as a certain value of the
signal-to-noise ratio. Many modern instruments, however, are designed to self
compensate for noise, so that the measurement of the signal-to-noise ratio is not a
simple matter.
For the purpose of work at CHESTER LabNet, the instrument detection limit is defined
as three times the standard deviation from the mean of seven replicate measurements of
a low concentration standard that produces a definite, measurable signal. The signal
may be an area count, a peak height, an absorbance reading, or electric measures (such
as voltage, current, resistance). The nature of the signal is
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dictated by the instrument and detector that are used. The instrument detection limit is
calculated from the following equation.
Where: IDL =
s =
RF =
The calculation of the
procedures are discussed.
Where: x· 1 =
Xm =
n =
= IDL
3S
RF
Instrument detection limit, in weight units (ng, mg) for those parameters where the signal depends on an absolute quantity (such as chromatographic methods), and in concentration units for those parameters that are concentration dependent
Standard deviation of the seven replicate readings, in units of the reading (i.e., area count, peak height, etc.)
Response factor, in units of signal reading/unit weight, or concentration, depending upon the units used for ID L
response factor is shown in Section 5 .6 where calibration
The calculation of th!! standard deviation is shown below.
s =
n ( -Xm)Z . E xi
I = 1
(n -1)
The value of the i'th reading of the set of replicates
The mean value ofthe replicates
The number of replicate measurements
The mean, Xm, is determined as follows:
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In order for the results to be useful, the standard chosen to obtain the detection limit
should be such that the mean of its readings, Xm, is slightly greater than 3S. This
may require some trial and error initially when a new instrument is installed.
Records of the instrument detection limit determination will be kept in the instrument
log, and the values of the instrument detection limit will be updated in the working
SOP' s at each time that the instrument detection limits are determined.
5.5.2 Method Detection Limit
The method detection limit is obtained in a manner very similar to that of the
instrument detection limit. The principal difference is that in determining the method
detection limit (MDL), the analytes are subjected to the entire analytical protocol for
the specific method that is being employed. Ideally, the method detection limit should
be determined for every matrix that is being analyzed. Unfortunately, obtaining
reproducible, well characterized matrices for media other than water is not yet feasible.
Hence, method detection limits will be determined for water only .
To determine the method detection limit, seven replicates of laboratory pure water are
each spiked with a known amount of the analyte. The amount that is being added is the
same for all seven replicates, and should be 2 -

3

times greater than the previously
determined instrument detection limit. The seven replicates are subjected to the same
analytical procedures as a sample would be, and the concentrations of the analytes of
interest are measured. The method detection limit, as was the instrument detection
limit, is definec! as three times the standard deviation of the seven readings. The
calculation of the method detection limit should be done in units of weight of the
analyte. In this fashion, such variables as injection volume in chromatographic
techniques or pathlength in spectrophotometric t,echniques are eliminated.
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The equations that apply to the calculations of method detection limits are identical to
those used for the instrument detection limit.
Where: MDL=
=
RF =
MDL =
RF
Method detection limit, in units of weight (ng,ug) for those methods that depend upon an absolute quantity, and in concentration units for those methods that depend upon concentration.
The standard deviation of the seven readings from the mean, in units of signal size (area, height, etc.)
The response factor of the instrument to the analyte, in units of signal size/unit weight or concentration,
depending upon the MDL units.
The standard deviation, sm,is determined just as before from the equation:
Where: Yi =
n =
n Yn/ E (Y; -i = 1 Sm = (n -1)
The instrument reading the i' th sample that has gone through the entire preparation procedure.
The mean value of the replicate readings.
The number of replicates that have been run.
The mean value is determined as follows:
n
E -
i = 1 n
The method detection limit will be determined· for all analytes associated with the
method on an annual basis.
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A method detection limit srudy will . also be performed whenever the instrument
undergoes major repair or modification, if the measurement of the instrument detection
limit shows a significant departure from the previously determined instrument detection
limit. If the instrum_ent detection limit has remained substantially unchanged after the
repair or the modification, there is no need to run the method detection limit again.
Additionally, a method detection limit srudy must be performed whenever the sample
preparation mode is modified.
5.5.3 Quantitation Limits
The q1:1antitation limit is determined at the same time as the method detection limit and
from the same runs. The quantitation limit (QL) is defined as five times the standard
devfation that has been measured in determining the method detection limit. Thus:
QL =
RF
' where the symbols have the same meaning as above.
5.5.4 Conversion of Detection Limits to J\,linimum Detectable
Concentration
The conversion. of the detection limit (MDL and QL) to a minimum detectable
concentration in a sample is done as follows:
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Where: DLS =
DL
V· I
V· J
s
=
=
=
=
DLS =
DL Vj
V· I
X s
Detection limit in sample in units of weight per unit weight or per unit volume.
Either the MDL or the QL as defined in the preceding sections.
Volume of prepared sample taken for analysis (such as the volume of extract injected into a GC), in mL.
The volume of the prepared sample (such as the final volume of an extract), in mL.
The sample size that was taken to produce the prepared sample of volume Vj. Sample size is normally measured in liters for aqueous samples and in grams, dry weight, for solid samples.
5.5.5 Documentation or Detection Limits
Whenever instrument detection limits, method detection limits, and quantitation limits
are determined, the results will be copied to the QA/QC Section. The results must
identify the type of detection limits and include both the value in terms of weight
(absolute quantity) and concentration. In reporting the concentration units, standard
sample sizes and aliquots will be reported.
5.5.6 Application or Limits in Data Reporting
In reporting data, the following rules pertaining to detection limits shall apply:
a. Results which are equal to or greater than the value of DLS that has been
calculated on the basis of Q L will be reported with the concentrations
found, without any qualifiers.
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b. Results below the value of D LS, calculated on the basis of the MDL,
will be reported as not detected at the DLS value.
Exceptions to these rules will be applied only for contracts and projects which specify
their detection limits, and whose detection limits exceed the value of QL. Also,
exceptions will be applied when a prepared sample requires very high dilution in order
to have the analyte of the highest concentration within the linear range of the method.
5.6 Instrument and Equipment Calibration
Instrument and equipment calibration must be rigorously and routinely performed m
order to provide reasonable assurance that the data generated are valid and acceptable.
Two principal types of calibration are performed. The first is an initial calibration,
which consist of determining the linear range of the instrument and its response factor.
The second is a verification calibration, which serves, during the course of running
samples, to ascertain that the instrument calibration has not drifted unacceptably. The
frequencies of performing the different types of calibrations are shown in Table 5-2 .
5.6.1 Initial Calibration
All instrumental methods of analysis are subjected to an initial calibration, consisting of
the measurements of responses to various concentration levels of the analytes of
interest. The standard solution of the lowest concentration should have a concentration
of the analytes of interest approximately 2-5 times the concentration that corresponds to
the Instrument Detection Limit; and the standard solution of the highest concentration
should have a concentration of the analytes of interest at or near the upper end of the
linear range of the method.
In performing the analyses of the standards to determine the response factor and the
linear range, the standard solution is prepared. as discussed in Section 5.4, and
surrogates and internal standards are added as required. The identification of the
working standard solution and the date of performing the calibration are entered on the
records of the run by the analyst.
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When the calibration is completed, the responses are fitted to a straight line of the
form:
y=ax+b
Where: y = The measured response
X = The known amount of the analyte
a = The response factor
b = They-intercept
In addition to determining the values of a and b, the correlation coefficient is
determined. The latter is a measure of how closely the five points were to the straight
line. The correlation coefficient is determined from the following equation:
n n n n I: X;Y; -I: X, I: Y; i = 1 ' i = l i = l T =
J
n -2 [i ~ I X;J 2 J n
[~ I Y; J 2 n I: XI -n I: Yl -i = l i = 1
Where: r = Correlation coefficient
x· I = The known amount.of the analyte in the i'th standard run
Yi = The measured response to the i' th standard
n = The number of standards run to obtain the calibration
curve
In order for the calibration curve to be valid, the correlation coefficient must be 0.995
or higher, and the ratio b/a must be no greater than the method detection limit (MDL).
If the correlation coefficient is not met, it usually implies that either the lowest or the
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highest concentration of standard is outside the linear range. To correct for this, the
analyst should rerun the highest standard, and also run a high standard somewhat more
dilute than the initially used highest concentration. Similarly, the analyst should
examine the effect of increasing slightly the concentration of the lowest standard.
If the ratio b/a criterion is not met, the problem may be with contamination in the
system or change in the noise level of the instrument. To correct for this, the
instrument detection limit should be first checked. If it has in fact changed, the ratio
should be compared to the newly determined noise level, in order to see if the criterion
is met.
While, as much as possible, certified standards are used in the preparation of solutions
for ca!ibration, it is always possible that the manufacturer has made a mistake. To
circumvent the possibility of error due to a mistake in the manufactured primary
standard, a calibration check sample will be analyzed whenever an initial calibration
curve is constructed. The calibration check sample will consist of a solution of the
analytes of interest, and at known concentration, but obtained and prepared by a
different source than the manufacturer of the calibration standards. When the analyte
concentrations in the check sample are calculated, they should differ by no more than
15 % from the known concentration. If the discrepancy is greater than 15 % , a
determination of the source of inaccuracy will be performed.
Once the initial calibration curve has been determined and verified, a table is prepared
with the response factors for all the analytes. The table also includes the identification
of all the standards used in generating the data, and the date of running the initial
calibration. A copy of the calibration curve is: maintained in the work area for ready
reference on a daily basis and is available for review by the QA/QC Section. Another
copy will be submitted with the sample data to the Information Services Section.
5.6.2 Continuing Calibration
Continuing calibrations, sometimes also called verification calibrations, serve to insure
that the instrument, during the course of running samples, is remaining sufficiently
stable so that the response factor calculated in the initial calibration remains valid.
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In performing a continuing calibration, the analyst analyzes a midrange standard
containing all the analytes of interest and internal standards and surrogate compounds if
applicable. The response factor is determined for each analyte by dividing the signal
by the known concentration of the analyte. If the response factor is sufficiently
representative of the originally determined response factor as specified by the
acceptance criteria for the relevant method, then the instrument is considered to be
within calibration. Analysis may continue without performing the initial calibration
procedure again. If the response factor is determined to be outside the acceptance
range, then the instrument will be recalibrated using the initial calibration process.
Samples that have been analyzed since the last acceptable calibration will also require
reanalysis after the instrument has been recalibrated.
In recording the information on continuing calibrations, the analyst will enter the
identification of the initial calibration to which .the cortinuing calibration relates. Copy
or copies will be submitted to the Information Services Section for inclusion in the file
of the project from which samples have been analyzed .
At no time should the response factor be corrected on the basis of the continuing
calibration. Until such time as it is necessary ·to reestablish the initial calibration, the
response factors determined in the initial calibration will be adhered to.
5.6.3 Calibration Frequency
Instruments have widely variable stabilities, requiring variable frequencies of
calibration. Table 5-2 summarizes the frequencies of such calibrations. It should be
emphasized that these frequencies are based. on instruments that are performing
normally. It is obvious that after change in instrument parameters or after repair the
initial calibration must be repeated and the cycle started over again. Thus, the
frequencies included in the table are minimum requirements.
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INSTRUMENT
GC/MS
GC/MS
GC
GC
HPLC
IC
Autoanalyzer
W83, 1236 -03193
TABLE 5-2
CALIBRATIONS FREQUENCIES
APPLICATION
Volatiles
Semi-Volatiles
Volatiles by
Purge-
and-Trap
Extracts
Extracts
Solutions
Solutions
INITIAL
CALIBRATION
As Needed
As Needed
Every Three
Weeks
Every Three
Weeks
Every Four
Weeks '
Every Three
Days
Daily
5 -18
CONTINUING
CALIBRATION
Every twelve hours and at the end
of a sample sequence, if the
instrument is about to be idle.
Every twelve hours and at the end
of a sample sequence, if the
instrument is about to be idle.
After every ten samples, and at
the end of a sample sequence.
After every ten samples, and at
the end of a sample sequence.
After every ten samples, and at
the end of a sample sequence.
After every ten samples, and at
the end of a sample sequence.
After every ten samples, and at the
end of a sample sequence.
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INSTRUMENT
ICP
AA
Mercury Analyzer
TOC Analyzer
TOX Analyzer
IR
UV/Vis
Spectrophoto-
meter
pH Meter
Analytical
Balance
Thermometers
TABLE 5-2
CALIBRATIONS FREQUENCIES
(CONTINUED)
APPLICATION
Digests
Digests
Digests
Solutions
Solutions
Solutions for
O&GorTPH
Solutions
Aqueous
Solutions
Solids
Temperature
INITIAL
CALIBRATION
Daily
Daily
Daily
Daily
Daily
Daily
Daily
Daily1
Annual2
Semi-Annual3
CONTINUING
CALIBRATION
After every ten samples, and at the
end of a sample sequence.
After every ten samples, and at the
end of a sample sequence.
After every ten samples, and at the
end of a sample sequence.
After every ten samples, and at the
end of a sample sequence.
After every ten samples, and at the
end of a sample sequence.
Every ten samples, and at the end
of a sample sequence.
Every ten samples, and at the
end of a sample sequence.
Every ten samples, and at the
end of a sample sequence.
Daily2
Not Applicable
I)
2)
pH calibration will require the use of three standards.
3)
W83, 1236. 03/9J
Analytical balances are calibrated and serviced annually by a contractor. Calibration is checked daily using Class S weights. Deviations from the true weight are recorded and
applied to weighings when appropriate.
Thermometers are calibrated semiannually against an NIST certified thermometer and any required corrections are applied to measurements.
5 -19
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5.7 Monitoring Laboratory Reagent Water
Multipurpose high purity water is prepared on-site. The laboratory measures the
specific conductance. and pH of this water on a daily basis. The records are kept in
chronological sequence in a bound laboratory notebook with the date of each analysis
and responsible analyst. The filters and ion beds of the system are changed as required
to assure that high quality water is constantly available.
5.8 Analysis of Quality Control Samples
Routine quality control samples are analyzed to assure that the operation is within
control as established for the laboratory on the basis of historical data. The routine
qual_ity control consists of blanks, spiked blanks,' spiked samples, duplicate samples and
external check samples analyses. These are discussed separately in the following
sections .
5.8.1 Blanks
Four types of blanks may be associated with any batch of samples. These are: reagent
blank, method blank, trip blank, and field blank. The latter two types are treated by
the laboratory as ordinary samples and are not part of the internal laboratory QC,
although they are very much part of the program QC. Thus, trip and field blanks will
not be discussed here.
5.8.1.1 Reagent Blank
Reagent blanks are set aside whenever the reagents are used for preparation of samples.
The reagent blank is taken from the reagent or group of reagents that is normally used
for sample preparation and that does not go through any of the preparation steps. This
reagent blank is normally not analyzed unless the method blank, discussed in Section
5.8.1.2, shows the presence of contamination' which may have arisen from the
reagents. The reagent blank will be labelled with the QC batch identification, followed
by the letter R. It will be set aside until all the, samples of the QC batch have been
WBJ.1236 -03193 5 -20
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analyzed. At that point, if the method blank was acceptable, the reagent blank may be
discarded.
5.8.1.2 Method Blank
The method blank is a preparation carried through all preparatory steps, except that the
reagents do not come in contact with a sample. Rather, laboratory reagent water is
used in lieu of a real sample. Ideally, the method blank would be prepared using a
matrix that is similar to the matrix of the samples that are being prepared. Since a
reference matrix is not available for matrices other than water, water is the only matrix
used as a method blank.
In preparing the method blank, water is spiked with surrogates and internal standards,
if appropriate for the method, and the water sample is carried through the entire
analytical procedure. The method blank is prepared with every batch of samples that is
being prepared at the same time, provided the batch is no greater than twenty samples.
For batches of greater than twenty samples, a method blank will be prepared for every
sub-batch of twenty samples or part thereof. The preparation lot will then indicate
which samples are associated with the new lot number of reagents.
The method blank is analyzed before any samples are analyzed, and the data of the
' analysis are reviewed. If no analytes are found above the quantitation limit, analyses of
the prepared samples may be undertaken.
If analyte concentrations are found above the quantitation limit, analyses of the
associated samples will not be undertaken until; the contamination source is identified
and isolated. At this stage the reagent blank wjll be analyzed. If it is found that the
reagent blank shows the contamination, the samples will be reprepared1 using a new lot
of reagents.
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5.0 ANALYTICAL PROCEDURES
In order to produce meaningful results, both sampling and analytical procedures must
be sound and complimentary to each other. While close coordination of activities
between the laboratory and field services is highly advisable in order to produce a high
quality product, laboratory services may involve analyses of samples collected through
organizations other than CHESTER Environmental. Thus, the application of strict
procedures regarding the transfer of samples from the field in some cases may involve
conditions beyond the control of the laboratory.
5.1 Coordination of Activities
Analytical services are requested through several sources. The project manager acts as
liaison between the client and the laboratory on all matters pertaining to the project.
However, requests for analytical services may originate with the. laboratory sales
representatives or other key technical persons in the laboratory. The person receiving
the request will enter a description of the requested work on an Analytical Request
Form, shown in Figure 5-1, and the information will be entered into the Laboratory
Information System as proposed work. When the proposed project becomes a definite
task for the laboratory, the Laboratory Director will assign a Project Manager who will
activate the project and distribute the information together with the anticipated
schedule. In that way, the laboratory sections and groups that will be involved in the
analysis are made aware of the upcoming work.
All further coordination and scheduling of the work will be through the assigned
Project Manager.
5 .2 Preparation of Sample Containers
For clients and projects that require the laboratory to supply containers for samples, the
Manager of Sample Receiving will be responsible for preparing the containers, labeling
them, and shipping them to the client. It is the responsibility of the Project Manager to
inform the Manager of Sample Receiving of the need for containers. Such notification
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FlGURES-1
ANALYTICAL REQUEST FORM
Client Contact: Date: -----------
Client: __________ _ ' Telephone:
Address: __________ _ Project Manager:
------------
------------
-------------
#SAMPLES MATRIX PARAMETERS TURNAROUND
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must be received by the Sample Receiving Section at least three working days prior to
the time for which the sample containers are required.
For aqueous field samples, new pre-cleaned :sample bottles with Teflon lined screw
caps will be used. The containers will be prepared with the appropriate preservatives
and will be labelled ·with information regarding the analytes that are to be determined
on the sample.
For solid samples, a variety of containers may be used. For soils, glass containers with
Teflon liners are employed. When the samples are to be collected in polyethylene,
appropriate new and pre-cleaned containers will be used.
Table 4-1 lists the appropriate containers and preservatives for aqueous samples.
5.3 Instrument Maintenance
Maintenance of the instruments in the laboratory consists of two major aspects. The
first is routine preventative maintenance and the second is repair due to malfunction .
Acceptable procedures and specifications in either case confirm to those recommended
by the manufacturer of the specific equipment' as well as any criteria provided in the
applicable approved methods. Written equipment maintenance documentation is part of
the laboratory records for both types of maintenance as described below.
5.3.1 Preventative Maintenance
The manufacturer's recommended schedule 9f preventative maintenance will be
followed to reduce occurrences of instrument failure and to help maintain the reliability
of analytical results. If more frequent routine maintenance is necessary to assure
proper operation, then these practices will be added to the maintenance scheduled, and
will be performed and documented in laboratory records.
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It is the responsibility of the Group Leader to provide the time required for preventative
maintenance. Preventative maintenance records must be kept and include procedures
performed by laboratory personnel and any preventative maintenance contracted for
using outside repair technicians. The Gro~p Leader will insure that preventative
maintenance records are complete, accurate, and comply with the Standard Operating
Procedures dealing · with these laboratory: records. Verification of instrument
performance and recalibration as necessary must take place inunediately after
maintenance has been completed and before resuming sample analys~s.
5.3.2 Repair After Instrument Failure
Unscheduled repairs which result from instrument malfunction are arranged for
inunediately after the failure is detected. Deteriorating equipment performance is
detected both directly through observations during analyses and indirectly through the
routine use of verification samples throughout the course of an analytical run. If
instrument response and performance on verification samples is not within acceptable
criteria, analyses are halted, preceding analytical results to the last acceptable
verification sample of the run are marked "VOID", and repair is undertaken. The
Group Leader will make the decision as to whether the scope of the repair is within the
capability of laboratory personnel or whether a service call to a repair contractor is
necessary.
Data from voided analyses will not be entered into the LIMS. Notice of invalid data
will be given by the Group Leader to the Quality Assurance Deparnnent if data from
the voided analyses have been released by the analytical section to the Information
Services Group. A Corrective Action Notice 'Form, as shown in Figure 5-2, will be
initiated by the Group Leader to track such data so that the appropriate action can be
taken. Other laboratory documentation which results from instrument repairs are the
equipment maintenance records that are described in the previous section on
preventative maintenance. As indicated in the maintenance recordkeeping Standard
Operating Procedures, repairs are documented in logbooks along with related
information which will include the identification of any sample results which have been
affected by the malfunction, and a subsequent verification of performance within
acceptable criteria prior to resuming sample analyses.
W8J, 12J6-03193 5-3
I FIGURE 5-2
CORRECTIVE ACTION NOTICE I _ Work Order: ______________ _
•• Client:
Dept.:
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ACTION
I. State the analysis and/or reporting problem recognized: (Analyst or Manager)
II. State the action taken:
111. Invalid data in UMS? Y/N
Individual completing the necessary corrective action:
APPROVALS I I. MANAGER OF ORIGINATING DEPARTMENT
The problem appears laboratory (e.g. procedure, instrument) related. ----I ____ sample (e.g. matrix, volume) relaled.
II. PROJECT MANAGER Ill. OC MANAGER
.. The client was contacted. ----Additional follow-up
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Signature:
Date:
was not contacted. ----
Signature:
Date:
COMMENTS
1. HOW TO USE: Use sheet to track and document one workorder.
Date: --------
Signature: --------
Date: --------
1s necessary. ----
____ is not necessary.
2. WHEN TO USE: Any time a problem cannot be immediately isolated and corrected.
3. OISTRIBUTION: Complete and submit to QC.
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5.4 Preparation of Standards
A calibration standard is made by the appropriate dilution of a pure substance, the
purity of which is traceable to an approved (e.g., NIST or equivalent) standard.
Because of the high sensitivity of many analytical instruments, the calibration standard
is an extremely dilute version of the pure compound. Because of the high dilution
required, in order to be within the linear range of the instrument, the preparation of the
calibration standard is frequently made by serial dilution rather than in a single step. In
order to provide standard solutions at sufficiently low concentration, a miniscule
I amount of the pure substance will be required,' the measurement of which is subject to
extreme error. Thus, it is preferable to deal with potential dilution errors, rather than
with the large error associated with the measurement of a very small amount of the
pure substance.
The initial pure standard is obtained either as · a pure material or already in solution
prepared as a certified solution of a given concentration of the pure compound or
compounds. In preparing the stock solution of the calibration standard:, great care must
be exercised in measuring weights and volumes as accurately as possible since all the
analyses following the calibration will be based ·on the accuracy of the calibration, and
the accuracy of the ultimate data cannot be any !Jetter than that of the calibration curve.
Table 5-1 summarizes the valid lifetime of primary and secondary standards used in
many tests. These lifetimes should be taken 'as a guide only. It is the analyst's
responsibility to assure that all standards used by him are within the standard solution
holding time, and to prepare fresh standard solutions whenever necessary. In preparing
working solutions, or using working solutions, the analyst must check for signs of
deterioration, such as the formation of cloudiness, precipitation, or discoloration. The
standard must also be periodically compared with previous runs of standards, and with
independently prepared standards to assure that response factors · fall within an
historically accepted range.
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TABLE 5-1
STANDARDS AND SOLUTIONS HOLDING TIMES
HOLDING TIME
PURE STOCK WORKING
MATERIAL COMPOUND SOLUTION SOLUTION
Volatile organic compounds I Yr@ -IO'C 2 Mo@ -IO'C I Wk@ -I0'C for GC or GC/MS analysis
Semivolatile organic compounds
for GC or GC/MS analysis I Yr@4'C I Yr@4'C 6 Mo@ -IO'C
Semivolatile organic compounds
for HPLC analysis I Yr@4'C I Yr@4'C ' 6 Mo@4'C
Pesticides (Cl, P, N ,) and
herbicides I Yr@4'C I Yr@4'C 6 Mo@ -I0'C
Polychlorinated dioxins and
furans I Yr@4'C I Yr@4'C 6 Mo@4'C
Metals for ICP analysis lndef@ RT
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Metals for GFAA analysis Indef@ RT I Yr@RT 6Mo@RT
Mercury Indef@ RT 6 Mo@RT I D@RT
Hexavalent chromium Indef@ RT I Yr@RT I Yr@RT
For anions and other parameters, the holding times of standard solutions should be
checked in the appropriate method.
All standards and standard solutions of organic compounds will be maintained in glass
containers, protected from light, and stored under the conditions specified in the
particular method. The position of the meniscus in each container will be marked after
each time that the container is opened so that changes due to evaporation can be
detected.
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Metals working solutions and stock solutions will be kept in polyethylene containers at
room temperature. The position of the meniscus will be marked each time a solution is
used to insure that concentration changes due to evaporation are detected. Before using
any standard solution, the analyst will examine· it for signs of precipitation and changes
in color. If precipitation has occurred, the solution will be discarded and a new
standard prepared. Discoloration frequently is only a warning sign, but will not affect I the results. If a solution is discolored, the analyst will compare the results with
historically established response factors, to assure that the solution is still within the
operating range of the method, and within experimental error, of its original
concentration.
The preparation of standards is very exacting. 'To facilitate the operation of preparing
standai:ds, a separate area is set in the laboratory equipped with a small hood and
analytical balance. A freezer in the same room is used to store all primary standards
and no other samples or extracts. In this fashion, the contamination of standards by
samples, and vice versa, is minimized.
For each stock standard solution that is prepared, accurate records will be kept in a
special logbook used only the maintenance. of standards data. The following
information will be entered in the logbook at the time of stock standard preparation:
a.
b.
C.
d.
e.
f.
W83, 1236. 03193
Date of preparation and expiration date
Application for which the standard is being prepared (i.e., identification
of. the method)
For each compound, the supplier of the primary standard, the batch
number, and the amount taken
The solvent identification (compound, supplier, batch nu~ber)
The final volume of the stock standard
The identification number assigned to the stock standard preparation
5-6
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These operations are the responsibility of Sample Receiving. The individual steps
are itemized below:
4.2.1 Sample Receipt in the Laboratory
Samples will be received in the laboratory either by commercial carrier, the postal
service, or hand-carried. Personnel in Sample Receiving sign for the receipt of each
shipment of samples and retain a copy of the shipping documents. The individual
receiving the sample shipment will open a sample shipment checklist (see Figure 4-
2) at the time of receiving the shipment.
If, for any reason, the shipping container is not expected to be opened immediately,
then the seals on the container must remain intact.
4.2.2 Shipment Inspection
It is expected that a shipment received in the laboratory will be opened and
inspected immediately upon receipt. Prior to opening the shipping container, the
custody seals will be inspected to assure that no tampering has been done with the
sample containers. The state of the custody seals will be noted on the sample
shipment checklist by the person inspecting th~ shipment.
After the seals are inspected, the ice chest is opened. The temperature of the
interior of the ice chest is measured and recorded. To measure the temperature,
the lid is quickly opened and a thermometer is inserted into the ice chest, and the lid
is closed again for five minutes. At the end of five minutes, the lid is quickly opened
and the temperature read rapidly. The temperature is recorded on the sample
shipment checklist.
The ice chest is opened, the chain-of-custody document is removed from the inside
of the lid, and the individual sample containers are removed from the ice chest. The
sample or sub-sample containers are counted and reconciled with the number of
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FIGURE4--2
CHESTER LABNET-MONROEVll.LE
SAMPLE SHIPMENT CHECKLIST
( ) MOllJOCVillc
108 NO.: _______ _
( ) Howton
DATE SHIPPED:
CUSTOMER: DATE RECEIVED: --------
CUSTOMER CONT ACT: SH IP PED VIA: --------
TELEPHONE NO.: AIR BILL NO.: --------
CHECKED BY: SM OF ORMS: --------
NUMBER OF SHIPPING CONTAINERS (COOLERS, BOXES, ETC.): ___ _
--------
--------
--------
--------
--------
CUSTODY TAPE #OF CHAIN-OF-CUSTODY
PRESENT? INTACT? TEMPERATURE SAMPLE PRESENT/ RECORD AGREE WITH
CONTAINER I.D. (YIN) (YIN) (C) I CONTAINERS ABSENT NO. SAMPLES
...
IRREGULARITIES __ ~NO ___ YES (IF YES, PLEASE EXPLAIN)
SAMPLE I.D. SUB SAMPLE I.D. IRREGULARITY
CLIENT REPRESENTATIVE: TELEPHONE NO.: --------------
CONT A CT ED BY: --------------DATE: ____ TIME: ____ _
WRITTEN FOLLOWUP (YIN)'-: ____________ _ DATE: ----
DECISION: ---------------------------------
SIGNATURE:
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such containers indicated on the chain-of-custody. If the number of retrieved
sample containers is less than that indicated on the chain-of-custody, the packing
materials inside the. ice chest are further checked to make sure that no sample
container has been accidently left in the ice chest.
Each individual sample or sub-sample container is visually inspected to determine
' that no breakage, cracking, external corrosion, or leakage has occurred. If none
have occurred, the individual sample containers may be removed from the fume
hood and placed on a workbench to complete the inspection. If, on the other hand,
there is indication that breakage, cracking, corrosion, or leakage has occurred, the
inspecfton of the sample containers will be completed while the containers are kept
in the fume hood.
The integrity of the individual sample or sub-sample containers is recorded on the
sample shipment checklist .
4.2.3 Reconciliation with Chain-of-Custody Document
Once the integrity of the sample containers has been determined, the sample
containers are reconciled against the records on the chain-of-custody. This is done
by checking the sample identification on the chain-of-custody and on the sample
container label. In addition, the analyte identifications are checked to ensure that
they are correct.
Any discrepancy is noted on the chain-of-custody, signed, and dated. The
discrepancies are also entered on the sample shipment checklist. At this point, the
sample shipment inspection is complete. The sample shipment checklist is signed
' and dated by the person performing the inspection. If there are no discrepancies,
and the shipment is complete as evidenced by the inspection, the shipment of
samples is ready to be logged in. If there are discrepancies or inconsistencies, the
sample shipment checklist is submitted to the Project Manager and the logging in
process is delayed until the discrepancies are resolved.
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4.2.4 Resolution of Shipment Irregularities
If any irregularities are noted during the ,sample shipment inspection, they are
recorded on the sample shipment checklist, and the checklist is submitted to the
Project Manager. The Project Manager will contact the client's representative to
determine the fate of the sample shipment.' The records of the conversation with
the client's representative are entered on the sample shipment checklist, including
name of contact, time and date of the conversation and the resolution of the
irregularities.
There are several possibilities for the resolution of the irregularities. These are:
a. Return the sample shipment to sender.
b. Destroy the entire shipment of samples .
c. Log in and process those samples that are intact.
The sample shipment checklist containing comments regarding resolution of any
irregularities. is returned to Information Services, the personnel of which will act
according to the annotated agreement with the client.
To maintain the custody of the samples, the entire sample shipment during this
period is either locked up in a secure area or is in view of Sample Receiving
personnel.
4.2.5 Sample Log In
Once the_ sample shipment has been inspected and any irregularities resolved, the
sample shipment is ready to be logged in. For laboratory purposes, a single sample
shipment from a specific client constitutes a single job. The shipment may contain
one or many samples and may have arrived in a single shipping container or in many
shipping containers.
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For the log-in process, Sample Receiving staff performing the logging-in will use the
field chain-of-custody and the sample shipment checklist, both with whatever
corrections were required to be made during the inspection and resolution steps.
The log-in process consists of the four steps described below:
'
' 4.2.5.1 Entry in Master Log
The Master Log is a hardbound book in which all jobs received in the laboratory are
chronologically recorded. The following information is entered in the Master Log:
(a) Job Number
(b) Date of Receipt
(c) Date of Logging-in
(d) Name of Client
(e) Number of Samples (not sub-samples)
(f) Due Date
(g) Sample Matrix
The job number consists of a letter followed by a seven digit number. The initial
letter code identifies the laboratory (H -Houston, P -Portland, NI -Neville Island,
M -Monroeville). The four digits following the letter identify the year and the
month of the sample shipment logging-in, and the last three digits are chronological
within the month. Thus, M9309005 is a job number issued by the Monroeville
Laboratory for the fifth job logged in during September 1993.
WlDJD!i: • 03/9] 4-9
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A sample page of the Master Log is shown in Figure 4-3. At the time of entering the job in the Master Log, the job number is manually written on the Field Chain-of-Custody and on the Sample Shipment Checklist. The job number remains the identification of the job in the laboratory and on the job records.
4.2.5.2 Job Traveller
In addition to opening an entry in the Master If>g, a Job Traveller is issued for every job in the laboratory. The Job Traveller is a computer generated document that gives all the pertinent details regarding the individual samples in the job.
For each sample in the job, a unique number is assigned. The unique number consists of the job number followed by three digits, which are sequehtial within the job. This number is entered on the traveller, as well as the original sample identification from the field chain-of-custody,' the date of sampling, the sample matrix, and the parameters for which the sample or sub-sample is to be analyzed. In addition, the traveller heading contains information such as client· identification, project contacts, date of collection, date of logging in, and due date.
A sample of a Job Traveller is shown in Figure 4-;4.
4.2.5.3 Sample Labeling
When the logging-in process is complete, the operator entering the information proofs the input and verifies that all the inforination is correct. The complete laboratory sample or sub-sample identifications are entered on labels. The operator then places the correct label on each container of each sample, and verifies once more that the information has been correctly recorded.
The labelled sample containers are then placed m a secure storage area for preservation at the appropriate temperatures.
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I --.----·-
Job Date Date
Number Received Logged
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FIGURE4-3
SAMPLE MASTER LOG.
Client
Number of
Samples
-----.--
Sample Matrix
Due
Date Soil Water Sludge Oil Other
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FIGURE4-4
CHESTER LABNET-MONROEVILLE
Date: ___________ _ Received By: ------------
Job Name: Date Received: -----------
Customer: -'------------Time Received: --------'-----P.O. Number: ___________ _ Project Number: ___________ _
Description: ------------Priority:
Matrix: ------------
Sample No
SOURCE/
SM!PLE TAG NO ..• ·
DATE COLLECTED
NO. OF CONTAINERS
PRESERVED CORRECTL •
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ft COMMENTS:
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4.2.5.4 Information Distribution and Job Filing
The Job Traveller is the working document for each job. Sample Receiving personnel make a copy of each traveller for each group in the laboratory as well as for the relevant Project Manager and Information Services. The copies are • I distributed to the Group Leaders and Section Managers as required. The original traveller is used to open a file for the job in which the laboratory copy of the field chain-of-custody and the sample shipment checklist are placed. The file is identified by the job number. As the work on the job is completed, the file. will be used to store all laboratory records regarding the job.
The file for the job is placed in the active laboratory central job filing system.
The sample log-in process is extremely critical for the proper functioning of the laboratory. It must be performed rapidly and accurately, so that holding times will be met, and so that the correct analyses will be performed on the appropriate samples.
4.2.6 Custody Transfer Within the Laboratory
Because the laboratory is considered a secure facility, samples will be considered as being in the custody of the laboratory from the time that sample receipt is recorded.
All samples will be maintained at secure locations under supervision of Sample Receiving staff until the group responsible for the sample preparation for analysis is ready to start work on the samples. The group representative will then obtain the samples from their designated storage area. Tl)e person retrieving the samples will fill in a transfer form, a sample of which is shown in Figure 4-5, and submit the form to the Sample Receiving Section.
4-11
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DATE
FIGURE4-S
Chester LabN et-Monroeville
Internal Transfer Forin
SAMPLE NUMBERS ANALYSES
4-lla
JOB: ______ _
RETURNED BY DATE
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When the sample preparation or analysis is completed and residual samples are returned to the original, secure storage location, the analyst will indicate on the Internal Transfer Form which samples, if any, have been completely used up. The Sample Receiving Section will maintain a record of these forms.
4.2.7 Sample Disposal
Sample Disposal is an issue requiring attention to the specific, and often changing, regulatory requirements. For these reasons, laboratory practices in this area are dealt with separately in an SOP written to address these concerns.
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2.0 OBJECTIVES
The Quality Assurance Program at CHESTER LabNet is principally aimed at
producing results of verifiable high quality. Towards this goal, the Program
addresses several areas:
1.
2.
3.
4 .
5.
WaJ,IZ!:J. '1J/9l
Detection of problems through statistical measures of acceptability
and confidence.
Implementation of corrective action.
Documentation procedures designed to produce legally defensible
results.
Establishment of training programs to assure that each person is
thoroughly familiar with the methods, procedures, and documentation
' ' of his area of activity.
Development of a review and validation process to verify that all data
produced by the Lab are within the guidelines defined in this Manual,
and the associated Standard Operating Procedures.
2-1
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3.0 ORGANIZATION Ai'ffi RESPONSIBILITY
The laboratories have been placed within the CHESTER LabNet framework
according to the organizational structure described in this section.
3.1 CHESTER LahNet
CHESTER LabNet-Monroeville is an integral part of a larger organization,
CHESTER LabNet, whose organizational scheme is illustrated in Figure 3-1. The
LabNet Operations Manager is responsible for assuring that the Laboratory
Direct9rs are thoroughly familiar with the Quality Assurance Manual and good
laboratory practices. The role of the Laboratory Directors will be discussed in the
next section.
3.2 Laboratory
3.2.1 Organization
Figure 3-2 illustrates generically the organization of each Laboratory.
3.2.2 Responsibility
The Laboratorv. Director is responsible for assuring that all Section Managers and
Group Leaders are thoroughly familiar with the Quality Assurance Manual and
good laboratory practices and that all laboratory personnel meet the requisite
qualifications for their positions within the laboratory. The Laboratory Director, or
his designee, must review and approve all outgoing reports. The Laboratory
Director is also responsible for effective daily management of the laboratory and its
staff, and for co=unication and liaison with the client.
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FIGURE3-l
CHESTER LABNET ORGANIZATION CHART
Operations Manager
Marketing/
Programs Sales
Office Information
Support Management
Lab Director Lab Director
Monroeville, PA Houston, TX
3-1a
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' INFORMATION
SERVICES
I I . WET
METALS CHEMISTRY
ANALYSIS ANALYSIS
GROUP GROUP
- --· --
FIGURE 3-2
LABORATORY ORGANIZATION
LABORATORY
DIRECTOR
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SAMPLE PROJECT
RECEIVING MANAGEMENT
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ORGANIC HPLC
EXTRACTIONS ANALYSIS
GROUP GROUP
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QA/QC
SECTION
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GC GC/MS
ANALYSIS ANALYSIS
GROUP GROUP
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The Group Leader is responsible for the production of quality results within the
group. To achieve this, the Group Leader must be thoroughly familiar with the
Quality Assurance Manual and Standard Operating Procedures used by the group.
He is also responsible for familiarizing personnel with the Quality Assurance
Manual and Standard Operating Procedures, seeing that required protocols are
followed, reviewing the results, and approving release of the data to the Information
Services Section. The Group Leader, in coordination with Sample Receiving,
Information Services, and the Project Manager is responsible for scheduling work
and conforming to required holding times. The Group Leader, in conjunction with
the Quality Assurance Manager, is responsible for providing the necessary training
to laboratory personnel.
The Analvsts are responsible for performing all analyses as required and noting the
required QC analyses demanded by the analytical method or technique. In order to
provide proper analysis, they must be familiar with the Quality Assurance Manual
and the associated Standard Operating Procedures. They are also responsible for
initiating system or method corrective action should they become aware of a
malfunction. Initiation of corrective action requires appropriate notification, as
discussed later in this manual.
The Manager of Sample Receiving is responsible for the following functions:
sample receipt,· storage, distribution of the information through the laboratory,
sample custody, and sample disposal. It is his responsibility to notify the Group
Leaders and Project Managers should there be any discrepancies or irregularities in
the shipment of samples.
The Manager of Information Services is responsible for maintaining the status of the
work within the Laboratory, coordinating the compilation of the data, and
preparation of reports for review and approval.
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The Quality Assurance Manager is responsible for assuring that the QA/QC
requirements of the Quality Assurance Manual and its associated Standard
Operating Procedures and addenda are strictly followed. He is responsible for
reviewing data validation procedures, alerting the sections and groups should the
need for corrective action exist, performing internal audits, introduction of
performance evaluation samples on a periodic basis, and maintenance of the QC
records. He is also responsible for preparing project-specific QA/QC plans.
The QA/QC Manger functions independently of the laboratory staff. In order to
achieve independence from the pressures of daily production in the laboratory and
maintain the necessary objectivity, the QA/QC Manager reports both to the
Laboratory Director and the Operations Manager.
The Project Manager is a position assigned by the Laboratory Director for specific
projects. Projects may require a specifically assigned manager because of the
unusual nature of the project, complexity of the analytical techniques or reporting
requirements, or the need for coordination of activities in several laboratories. The
responsibility of the Project Manager to the specific project transcends that of the
Laboratory Director. The Project Manager will alert the . Group Leaders if
problems arise in meeting schedules or sample holding times. It is also the Project
Manager's responsibility to assure that work on the project is performed in
accordance wiih project specified protocols, following project specific QC
requirements. Acceptance of results on analyses for the project is subject to
approval by the Project Manager.
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4.0 SAi"\iPLE CUSTODY
To provide for legal defensibility of all work performed at a given site, it is essential
to be able to provide documentation tracing the samples from collection, to the
laboratory, and through the analytical procedures. CHESTER Environmental
performs both sampling functions and analytical functions: however, the laboratory
can guarantee that this Manual is followed from the point of origin only for samples
that are both collected and analyzed by CHESTER Environmental.
Maintaining sample custody consists of two distinct aspects: maintenance of the
samples in the field, and maintenance of the samples from the time of receipt in the
laboratory. These two aspects are discussed separately in the following sections.
Inasmuch as sampling is not necessarily performed by our personnel, the custody
and documentation in the field are included here as a recommendation .
4.1 Custody and Documentation in the Field
The field sample custodian, which, depending upon the project, may be the sampler
or another person in the same sampling group is considered to have custody of the
samples at all times during the field operations, until the samples are shipped to
storage or to the laboratory. Upon collection of a sample in the field, the sampler
tags the sample with its site and type (water, soil, sludge, etc.) identification. The
sampler also indicates on the tag the date and time of sampling. After cleaning the
exterior of the sample container, the field sampler transfers the container with the
tag to the field sample custodian.
Throughout this document, the term sample is used to indicate a quantity of one
type of material collected at one time, at a single location. Thus, a water sample
may be shipped to the laboratory in several containers, depending upon the required
testing and sample preservation dictated by the project. Each container is identified
as a sub-sample, but it is not classified as a unique sample.
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The field sample custodian compares the identification of the individual sample
with the sampling plan, and enters all pertinent information on the chain-of-custody
document and on the label of the sub-sample container. The information that must
be included consists of the following:
Project identification
Sample identification (such as station number and location)
Date of sampling
Time of sampling
Name of sampler
Parameters for which the sample is to be analyzed
Number of containers
Sample matrix (groundwater, surface water, wastewater, soil, sediment, sludge,
unknown waste, etc.)
Added preservatives in each sample container
Ice chest number
Chain of custody number
A sample field chain-of-custody is shown in Figure 4-1.
WBl,1235 • 03/9'3 4-2
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-.-------I --

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---.--
-·------------------------·---·. ----------
CHAIN OF CUSTODY RECORD
·-=-~C~~PROJECTNAME NUMBER t:
··---; ~
SAMPLERS OF i::
tS,gnalutU} CONTAINERS J REMARKS OR
p OBSEAVA 110115 ·--------C • -8 ~
DATE TIME • • I S IATION LOCATION Q
SIA NO. • • I • • I ,_ --~------·---· ------·--
---·· -----------· -·· -------

-
-
-------------·------·-· --·--·-----·---
--------~ --------------
----------·------·-----------· -
------· ---------· -· -·--
-----------------------. ·------·-
--------· -----------------
-----------------------------
----------·------------------·----·-
·--·· ----------------···----· ----· -·
-------·-----·-----------·--·-
--------------------------------------
------------------------·
-----·----------------------
------· --·--·--
Aolinquishod by: ISignafur•J Dale Time Aoceivod by: tSignalwo} Aeliquishod by: lSignalur•J Da10 Time Aocoivod by: ISignaluro)
-------
Rolinquishod by: (SignafuroJ Dato Time necaivod by: (Sig11alu1t1J Aoliquishod by: {Signalur•J Oalo limo RocoivDd by: tS19na1u10J
Roliquishod by: (Signalutll) Dalo Time Rocaivod lor laboralory by: (Signalure) Dalo limo lcti Chest Temp Ice Olest Chain of Cuuody
oc #
'OISlRIBUTION: O1iginal accompanies shipment. Copy lo Coordina10, fiokt Filos.
Tag #
PAGE __ OF ___
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The field sample custodian is then responsible for packaging the sample(s) for
shipping, adding ice if the samples require chilling, signing and dating the chain of
custody document, placing the chain of custody document in a waterproof envelope
and attaching the envelope to the inside of the ice chest lid.
If the samples are to be shipped by a common carrier, then the field sample
custodian must also place custody seal on the ice chest.
Simultaneously with filling out the chain of custody document, the field sample
custodian also records the information in the field logbook. In filing the chain of
custody document and the field logbook, any corrections that need to be made must
be done so that the original incorrect entry is legible. Hence, the incorrect entry is
lined _out, and the change is initialed and dated by the field sample custodian.
Table 4-1 lists the requir~d types of containers, preservatives, and holding times for
each type of analyte. It is the responsibility of the field sample custodian to assure
that each sample or sub-sample are packaged correctly. The samples are considered
formally to be in the custody of the field sample custodian until they are officially
transferred to the carrier, and the transfer is documented on shipping records, or
until the samples are transferred to the laboratory in person.
4.2 Sample Custody in the Laboratory
The laboratory operation, as it penains to the sample custody, consists of several
functions. Specifically, these are: sample receipt, inspection of the samples,
reconciliation of the information on the sample label and the chain-of-custody,
alening the project manager of any inconsistencies in the shipment, logging in of the
samples, placing the samples in appropriate storage areas, distribution of the
information to the laboratory analytical sections, transferring of the custody of the
samples to the analysts, and recovery of the samples at the completion of the
analysis.
WB3J235 • OJ/93 4-3
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I TABLE 4-1
CONTAINERS, PRESERVATIVES, AND HOLDING TIMES
I ANALYSIS CONTAINER PRESERVATIVE HOLDING TIME
I Volatile organics G HCl, Cool to 4°C 14 d
Semivolatile organics G Cool to 4°C 7 d to extraction,
I 40 d for extract.
Organochlorine pesticides G Cool to 4°c 7 d to extraction,
I 40 d for extract.
Herbicides G Cool to 4°C 7 d to extraction,
40 d for extract.
I Organophosphorus pesticides G Cool to 4°c 7 d to extraction,
40 d for extract . .. Metals ( except mercury) p HNO3 6m
Mercury p HNO3 28 d
I Hexavalent chromium p Cool to 4°C 24 h
I Acidity, Alkalinity P,G Cool to 4°C 14 d
Ammonia, COD, total P,G H2SO4, 28 d
Phosphorus, Nitrate-Nitrite Cool to 4°C
I BOD P,G Cool to 4°c 48 h
I Chloride, Fluoride p None 28 d
Color P,G Cool to 4°C 48 h
I Cyanide P,G NaOH, 14 d
Cool to 4°C
I Hardness p HNO3 6m
pH P,G None Immediately
I Nitrogen, Kjeldahl and G H2SO4, 28 d
Total organic, Phenols Cool to 4°C
118
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~-I TABLE 4-1
I CONTAINERS, PRESERVATIVES, A.t'!D HOLDING TIMES
(continued)
I ANALYSIS CONTAINER PRESERVATIVE HOLDING TIME
I Nitrate & Nitrite P,G Cool to 4oc 48 h
Oil and Grease G H2S04, 28 d
Cool to 4°C
I Ortho-phosphate P,G Cool to 4°C 48 h
I Disso!ved oxygen G None Immediately
Residue, Total, Filterable, P,G Cool to 4°C 7d
N onfilterable, Volatile
I Residue, Settleable P,G Cool to 4°C 48 h .. Silica p Cool to 4°C 28 d
Sulfate, Specific P,G Cool to 4°C 28 d
Conductance
I Sulfide P,G Zinc acetate + 7d
NaOH, Cool to 4°c
I Sulfite P,G None Immediately
Surfactants, Turbidity P,G Cool to 4°c 48h I Temperature P,G None Immediately
I TOC G H2S04 28 d
Cool to 4°C
TOX G H2S04 8d I Cool to 4°c
NOTES:
I P = Polyethylene
G = Glass
I h = hours
d = days
m = months
{i
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ATTACHMENT A
LABORATORY QUALITY ASSURANCE MANUAL
CHESTER LABNET
MONROEVILLE, PA
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QUALI1Y ASSURANCE MANUAL
...
CHESTER LABNET
MONROEVILLE
APPROVALS
Approved by:._-1.:..µ.~!-!..I.Ls:i..l<lc,~~.i......:
Approved by:__.._/_L-./ _ ___;;_f.._:._(L ___ _
Laboratory Director
Date: '3 / q / q 3
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TABLE OF CONTENTS
Page
1.0 INTRODUCTION ............................................................................................................... 1-l
2.0 OBJECTIVES ...................................................................................................................... 2-l
3.0 ORGANIZATION AND RESPONSIBILl1Y .............................................................. .3-l
3.1 CHESTER LabNet. ................................................................................................ 3-l
3.2 Laboratory ................................................................................................................ 3-l
3.2.1 Organization ................................................................................................ 3-l
3.2.2 Responsibility .............................................................................................. 3-l
4.0 SAMPLE CUSTODY ...................... ; .................................................................................. 4-l
4.1 Custody and Documentation in the Field .......................................................... .4-1
4.2 Sample Custody in the Laboratory ...................................................................... .4-3
4.2.1 Sample Receipt in the Laboratory .......................................................... .4-6
4.2.2 Shipment Inspection ................................................................................. .4-6
4.2.3 Reconciliation with Chain-of-Custody Document ............................... .4-7
4.2.4 Resolution of Shipment Irregularities .................................................... .4-8
4.2.5 Sample Log In ............................................................................................ .4-8
4.2.5.1 Entry in Master Log ..................................................................... 4-9
4.2.5.2 Job Traveller ............................................................................... 4-10
4.2.5.3 Sample Labelling ....................................................................... 4-10
4.2.5.4 Information Distribution and Job Filing ................................ 4-11
4.2.6 Custody Transfer Within the Laboratory ............................................ 4-11
4.2.7 Sample Disposal ...................................................................................... 4-12
5.0 ANALYTICAL PROCEDURES ........................................................................................ 5-1
5.1 Coordination of Activities ..................................................................................... 5-1
5.2 Preparation of Sample Containers ....................................................................... 5-1
5.3 Instrument Maintenance ....................................................................................... .5-2
5.3.1 Preventative Maintenance ....................................................................... .5-2
5.3.2 Repair After Instrument Failure ............................................................ .5-3
5.4 Preparation of Standards ....................................................................................... 5-4
5.5 Determination of Detection and Quantitation Limits ..................................... .5-8
5.5.1 Instrument Detection Limit ...................................................................... 5-8
5.5.2 Method Detection Limit ........................................................................ 5-10
5.5.3 Quantitation Limits ................................................................................. 5-12
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6.0
TABLE OF CONTENTS
( continued)
5.5.4 Conversion of Detection Limits to Minimum
Page
Detectable Concentration ...................................................................... 5-12 5.5.5 Documentation of Detection Limits .................................................... 5-13 5.5.6 Application of Limits in Data Reporting ............................................ 5-13
5.6 Instrument and Equipment Calibration ........................................................... 5-14
5.7
5.8
5.6.1 Initial Calibration .................................................................................... 5-14 5.6.2 Continuing Calibration ........................................................................... 5-16 5.6.3 Calibration Frequency ............................................................................ 5-17
Monitoring Laboratory Reagent Water ........................................................... 5-20 Analysis of Quality Control Samples ................................................................ 5-20
5 .8.1 Blanks ........................................................................................................ 5-20
5.8.1.1 Reagent Blank ............................................................................ 5-20 5.8.1.2 Method Blank ............................................................................. 5-21
5.8.2 Spiked Blank ............................................................................................ 5-22 5.8.3 Spiked Sample .......................................................................................... 5-22 5.8.4 Sample Duplicate .................................................................................... 5-23 5.8.5 External Quality Control Audit ............................................................ 5-24 5.8.6 Record Keeping on Analysis of QC Samples ..................................... 5-24
5.9 Use of Surrogates ................................................................................................. 5-25 5.10 Establishment of Acceptance Criteria .............................................................. 5-26 5.11 Development of New or Modified Methods ................................................... 5-30
DATA HANDLING ............................................................................................................ 6-1
6.1 Data Recording ....................................................................................................... 6-1
6.1.1 Notebooks .................................................................................................... 6-1 6.1.2 Record Keeping in Sample Prepartion ................................................... 6-2 6.1.3 Record Keeping for Instrument Analysis ............................................... 6-4 6.1.4 Record Keeping in Noninstrument Analyses ......................................... 6-6
6.2 Data Reduction ....................................................................................................... 6-6 6.3 Data V alidation ....................................................................................................... 6-7 6.4 Data Compilation ................................................................................................ 6-10 6.5 Final Review ......................................................................................................... 6-10
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TABLE OF CONTENTS
(continued)
Page
CORRECTIVE ACTION ................................................................................................... 7-1
7.1 Identification of Potential Problem ..................................................................... 7-1
7.2 Problems and Actions ............................................................................................ 7-2
7.2.1
7.2.2
7.2.3
7.2.4
7.2.5
7.2.6
7.2.7
7.2.8
Continuing Calibration Outside Acceptance Range ............................ 7-2
Calibration Standards Exceeding
the Permitted Holding Time .................................................................... 7-2
Laboratory Method Blanks Exceed Method Detection
Limit but are Below Quantitation Limit. ................................................ 7-3
Laboratory Method Blank Exceeds the Quantitaiton Limit. .............. 7-3
Laboratory Control Standard Exhibits Recoveries
Outside the Acceptance Criteria ............................................................. 7-4
~~Ya!t~/!~c~~~~e st~t~ri~!~'.~.~.~.~~.~~.~~·~········· ...................... 1-4
Control Chart Exhibits and Regular Trend ........................................... 7-5
Internal and External Audits and Corrective Actions .......................... 7-5
7.2.8.1 Evaluation of System Audits ....................................................... 7-5
7.2.8.2 Corrective Action and Feedback. ............................................... 7-6
7.2.8.3 Documentation of Corrective Action ........................................ 7-6
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LIST OF TABLES I
Page
I Table 4-1 Containers, Preservative, and Holding Times ................................................... .4-4
Table 5-1 I Table 5-2
Standards and Solutions Holding Times ............................................................. 5-5
Calibrations Frequencies .................................................................................... 5-18
I Table 5-3 Surrogate Compounds and Typical Recoveries .............................................. 5-26
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LIST OF FIGURES
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·Page
I Figure 3-1 Chester LabNet Organization Chart ................................................................ 3-la
Figure 3-2 Laboratory Organization .................................................................................... 3-lb I Figure 4-1 Chain-of-Custody Record ... , ............................................................................... 4-2a
I Figure 4-2
Figure 4-3
Sample Shipment Checklist ................................................................................ 4-6a
Sample Master Log ............................................................................................ 4-l0a
I Figure 4-4 Job Traveller ....................................................................................................... 4-l0b
Figure 4-5 Internal Transfer Form ..................................................................................... 4-1 la
I Figure 5-1 Analytical Request Form .................................................................................... 5-la .. Figure 5-2
Figure 5-3
Corrective Action Notice .................................................................................... 5-3a
Standard Preparation Log .................................................................................. 5-7a
I Figure 6-1
Figure 6-2
Continuous Extraction Bench Sheet. ................................................................ 6-3a
Aqueous Sample Metals Digestion ................................................................... 6-3b
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1.0 INTRODUCTION
CHESTER LabNet is committed to excellence in analysis. All data generated by
CHESTER LabNet must be technically sound, properly documented, legally
defensible, and supported by defined and verified confidence limits. The program
therefore, whenever possible, employs analytical methods derived from EPA,
ASTM, AOAC, or Standard Methods.
This document is designed to serve as a guideline to CHESTER LabNet as a whole.
Specifically, it defines the laboratory objectives, organization, functional activities,
and QA/QC programs that routinely apply to each laboratory. This document is
also supplemented by sets of Standard Operating Procedures. The standard
practices within CHESTER LabNet are set forth; however, for specific projects,
addenda will be prepared corresponding to project needs .
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