QUALITY ASSURANCE PRACTICES AND PROCEDURES
        Billy Fairless, Author and
      Quality Assurance Coordinator
                 U.S. EPA
                 Region V
    Surveillance and Analysis Division
           Chris Timm, Director
        Central Regional Laboratory
           Curtis Ross, Director
           1819 W. Pershing Road
          Chicago, Illinois 60609
               312-353-8370

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                             TABLE OF CONTENTS
                                                                  Page
Introduction	    1
Management of the Quality Assurance Program	    3
General Operating Procedures of Quality Assurance	   10
Quality Assurance of Instrument Operation	   13
Definition of Terms and Mathematical Concepts	   24
Appendix I - A list of Methods in current use	
Appendix II - A list of Quality Assurance Audits and control
              limits for those Methods used most frequently.

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                              -Introduc t ion

     The central idea of a quality assurance program for an environmental
laboratory is to measure the accuracy and precision of all reported data
and to be able to communicate to data users and other offices the quality
of any given set of data values.  In an effort to meet this ambitious and
necessary objective, the Central Regional Laboratory tCRL) has defined
administrative responsibilities, methods of analyses, critical measurement
audits for each method, and control limits for each of the audits used
routinely at the CRL.  This document describes these Quality Assurance
practices and should provide sufficient information for the user to
estimate the data quality for any set of data reported by the CRL.  Only
those results in which all quality assurance audits were passed satisfac-
torily will be reported without qualification.
     The underlying principle of our program is that a sufficient number
of quality assurance audits be conducted to insure that the accuracy and
precision of» a measurement are within the limits defined in this document.
Since some error is associated with all measurements, our goal is to
define for the data user the precision and accuracy of data values we report
on a routine basis, and to be in a position to estimate the costs of im-
proving the accuracy, sensitivity or precision if requested to do so.
     It has been the CRL's experience that some elements of a quality
assurance program are general in nature and frequently taken for granted.
One example would be sample collection.  If a representative sample is not
taken, no amount of laboratory effort will result in a useful result.  A
second example of this type of element is community instrument calibration
and maintenance.  Frequently "everyone" is responsible for an instrument
such as the balance but no one performs calibration and maintenance
functions on a regular basis to insure the balance is operating properly
each time it is used.
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     Other elements of quality 'assurance are quite specific and must be
performed on a parameter by parameter basis.  We do not believe quality
assurance for such diverse items as insuring qualitative methylation of
an acid pesticide, calibrating an ozone monitor and setting up a bio-
chemical oxygen demand analysis can be adequately treated in general dis-
cussion.  The production of analytical data of known quality requires
that both types of elements be addressed in the quality assurance program.

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       II.  Management of the Quality Assurance Program

            The relationships between selected Region V offices is described

            in the organizational chart shown below.
                                Regional Administrator
       Air & HM
       Division
  Enforcement
   Division
S&A Division
Air Surveillance
    Branch
Quality Assurance
    Office
Water
Division
Management
Divisions
       Laboratory
       Support
        -Administration
        -Engineering
   Central     Field    Great        Technical
   Regional    Support  Lakes        Support
   Laboratory  Branch   Surveillance Branch
                        Branch
                                      Director
                                  Deputy Director
         Biology
         Section
         — Macrobiology
         — Microbiology
                            —Radioecology
            Inorganic
            Chemistry
            Section
            —Nutrients
            r-Metals
                             -Air
                  Organic
                  Chemistry
                  section

                  —Pesticides
                  —Toxic Substances
                                  '—Petroleum Products

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     The Quality Assurance Office (QAO)  is responsible for and has been
given the responsibility to establish quality- assurance policy for the
Surveillance S Analysis Division.  Approved policies carry the signature
of the Director of the S&A Division and apply to those phases of a program
that affect data quality.  The Quality Assurance Office is responsible for
requesting support from the CRL for all quality assurance activities which
it cannot complete with QAO personnel. The CRL will respond to those
requests approved in the annual work plans and any other requests for which
resources are available.
     The Central Regional Laboratory is responsible for the operation of
all laboratory programs in the Region.  This responsibility includes the
definition, implementation and maintenance of programs to conduct measure-
ments in all areas of environmental interest such as the chemistry, micro-
biology and biology of samples taken from air, surface water, drinking
water, sediment, soil and biological medias.
     The program offices are responsible for defining project objectives,
the numbers and types of measurements to be made and the desired data
quality.  Once these items are known, the Central Regional Laboratory, using
general policy established by the Quality Assurance Office, selects appro-
priate analytical methods, conducts the measurements and reports the results.
     Within the Central Regional Laboratory, the Quality Assurance Coordinator
is responsible for all aspects of data quality including those within the
traditional disciplines of microbiology, biology, inorganic and organic
chemistry.
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Each administrative unit adheres to the same quality assurance program
as described in this document.  Other offices and laboratories who per-
form measurement functions for the Central Regional Laboratory are also
required to conduct the quality assurance audits as described in this
document and to maintain the data for inspection and evaluation.
     It is the responsibility of the CRL line supervisors to interpret,
implement and-maintain approved policy decisions.  The procedures the CRL
will follow in implementing new and current QA programs are described below.
a)   All personnel will follow the directions of their immediate super-
     visor on all quality assurance matters.  All requests for quality
     assurance support from other offices should be referred to the
     Director, CRL.
b)   Bench scientists are responsible for following all quality assurance
     procedures as described in this manuscript as they apply to their
     assigned parameters.  Questions will be explained by their immediate
     supervisor or the CRL quality assurance coordinator.  The scientists
     should always be in a position to provide QA audit results to
     support reported data.  This includes both specific (duplicate
     analysis)  and general (balance calibration) audit measurements.
     If any instance occurs where an approved audit has not been made,
     the bench scientist is responsible for reporting the incident to
     his Section Chief.
     Any instrument used in the course of the analysis should be checked
as outlined in Appendix II of this document.  Furthermore,  any quanti-
zation should be done by standardizing the instrument such that the
unknown concentration is between two of the standard concentrations.
Standards are to be made daily as needed, unless stability is known and
documented.  Unstable solutions should be refrigerated in an explosion
proof refrigerator when necessary.  Any qualitative analysis made by gas
chromatography is to be confirmed by using a column of different polarity,
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by using GS/MS, IR, or NMR for identification purposes.

c)   The Quality Assurance Coordinator will initiate all changes in
     quality assurance procedures through normal administrative channels.
     Implementation of quality assurance decisions will  occur as soon
     as possible after a recommended policy is approved  by the S&A
     Division Director.

     The Quality Assurance Coordinator will review and update the CRL
     QA program including parameter audit procedures, control limits,
     etc., and prepare a program document prior to March of each year.
     The program document will define the level of quality assurance for
     each measurement to be made during the next fiscal  year.

     New analytical procedures should receive approval before they are
     used to analyze samples.   Approval procedures for methods to be used
     to analyze samples for the NPDES are described in the December 1,
     1976 Federal Register.  Approval for the NPDES is made in writing'
     by the Regional Administrator.  Approval to use new methods for
     other programs will be made by the CRL Quality Assurance Coordinator,
     after he has received sufficient documentation to support use of
     the new procedure.  Generally, the supporting documentation will
     consist of a comparison between new and referee procedures as required
     to obtain alternate test procedure status for the NPDES program.  For
     example, although the fluoride probe cannot be used to analyze certain
     industrial wastes directly, it works perfectly well for most drinking
     waters.  Any change in an existing analytical procedure that changes
     the chemistry, equipment, precision, accuracy or detection limit
     will result in a new analytical procedure.  Approved procedures
     are those described in this document plus those procedures approved
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 by the Quality Assurance Coordinator.

 It is realized that certain analysis are requested on a one time
 basis, especially in the Organic Section,  and which do not justify
 complete method validation.  In such cases the proposed analytical
 procedures should be approved in writing by the Section Chief before
 the analysis begins, and a complete description of quality assurance
 criteria should be submitted with the  results.  This will provide
 the users with information from which  data quality may be estimated.

 Each time a scientist is asked to perform a measurement which is
 new to him, the Section Chief will either assume full responsibility
 for data quality or provide an appropriate training program.   After
 the training program is completed, the scientist will analyze at
 least 10 quality assurance samples and the results will be reported
 to the Quality Assurance Coordinator to document that the scientist
 can perform the assigned task in a satisfactory manner.  The  qulaity
 assurance coordinator will maintain a  file listing those measure-
 ments each scientist is qualified to make  independently.

 The CRL Quality Assurance Coordinator  or personnel from the Quality
 Assurance office will request to review all quality assurance data
 for a given method from time to time.   These requests will usually
 be to collect information to support reported data or to estimate
 confidence levels for a given data set.  The responsibile analyst
 should therefore be sure that he is familiar with the location of
 all such quality assurance data files  for  each of his assigned
-parameters and that all files are up to  date and complete.

 Section Chiefs are responsible for interpreting and administering
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approved quality assurance policies as they apply to those para-
meters and instruments assigned to the Section.  They have authority
to invalidate analytical results.  They are responsible for re-
viewing and approving all parameter QA practices and reporting summaries
to the Quality Assurance Coordinator.  They are also responsible for
submitting updated sections of this document prior to January of each year.

The Section Chiefs will assign samples for both routine and non-
routine parameters to the appropriate laboratory personnel.  For
non-routine tests, the person responsible for the analysis will
make a detailed flow chart indicating all steps to be taken to
complete the analysis.  The Section Chief will approve it or make
changes as necessary.  Once the flow chart is finalized, it should.
not be changed without the approval of the Chief.  A minimum of one
CRL distilled water blank and one laboratory control standard is
to be analyzed with each set of samples making up a laboratory run.
If the CRL blank contains material in excess of 5% of any measured
concentration value or above the method audit control limit as
defined in Appendix II, the Section Chief is to be consulted for
his action.
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III.        GENERAL OPERATING PROCEDURES OF QUALITY ASSURANCE
a)   Sample Collection
     In order to determine the variability in data which may be attri-
     buted to sample collection, the CRL is requesting that each sampling
     crew collect, in duplicate, one of each twenty or fewer samples
     collected during a days work.  It is assumed that all samples are
     labeled properly and are as representative of the sampled media as
     is feasible.  All samples should be preserved immediately as de-
     scribed by the Quality Assurance Office.  For all preserved samples,
     at least one reagent blank containing the preservative diluted with
     distilled water should be submitted with each 20 or fewer samples
     collected during a given work period.  These requests will impose
     a minimum 10% quality assurance overhead on all projects.

     The samples are shipped by United Parcel Service to the CRL as soon
     as possible after sample collection.

     When the samples are received at the CRL shipping and receiving
room, all bottles constituting each sample are arranged according to the
preservative used.  For example, ten samples may be received and each
sample might consist of a bottle preserved with nitric acid (metals),
another bottle preserved with sulfuric acid (nutrients)  and up to 22 other
bottles each containing a sample aliquot preserved for a specific group
of analyses.  Each bottle label is checked against the appropriate analysis
request form and if correct, the sample is logged in.  If errors are de-
tected, the originating office is contacted and a decision made prior to
sample log in about proper disposition of the sample.
     Once the samples are logged in, appropriate pages of the analysis
request form are provided to each Section Chief and all bottles are
transferred from shipping and receiving to their laboratory area.  The
Section Chiefs are then responsible for completing all requested analyses
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prior to the project due date.  The Section Chiefs discard all non-
custody samples and custody samples completely consumed during analyses
immediately after the requested analyses are completed.  Custody samples
which are not completely consumed are transferred to custody storage
pending release.
     If samples are received and their identity cannot be clearly estab-
lished by consultation with the submitting office, the samples are dis-
carded.  If the Section Chiefs discover bottles that have not been pre-
served properly, the submitting office is advised that the samples cannot
be analyzed.  If it is impossible to analyze a sample within the specified
holding time, the submitting office is advised of the situation and re-
quested to provide advice as to sample disposition.  For all other similar
problems the Quality Assurance Coordinator will decide whether or not the
samples should be analyzed after consulting with the originating office.
b)   All samples are analyzed using one of the approximately 500 different
     numbered methods listed in Appendix I or by a procedure approved by
     the Section Chief as described previously.  It should be noted that
     each of these methods have been documented or referenced and that
     selected quality assurance audits with associated control limits
     have been defined for each method (Appendix II).  The audits listed
     in Appendix II are "over-all" audits for monitoring the entire
     measurement procedure.
c)   In general, the CRL will not correct any analytical data for high
     reagent blanks.  Instead, the submitting office will be advised of
     the problem and requested to take corrective action.
     The QA data are to be summarized and given to the Section Chief
with the data set when completed.  Each fall, the Section Chief will
assign personnel to compile and summarize QA data for the year.  These
summaries, and all supporting documentation, will be made available to
the Quality Assurance Office for revision of this document and calculation
of up-dated control limits listed in Appendix II.  These control limits
which are calculated from historical data for each of the defined frequency
of audits are the basis for our best estimates of a minimal quality assurance
program which still insures that reliable results are reported.
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IV.            QUALITY ASSURANCE OF INSTRUMENT OPERATION

General
     Each instrument must have a logbook in which the usage and the
condition of the instrument are entered on a regular basis.  The Chief
of each Section is responsible for each instrument located in his
Section and to insure that all instruments are properly used and that
each instrument logbook is filled out in a timely manner.  It is the
responsibility of the user to enter all requested information in the
logbook when the instrument is used.  This logbook will be checked
by the CRL QAC on a case by case basis.

A.   Gas Chromatographs
     The gas Chromatographs are to be checked for the detector linearity
     (useable ranges) every time a new or reconditioned detector and/or
     electrometer is installed.  This information should be summarized
     in the instrument logbook.  The Chief, Organic Section, will assign
                                                                    •
     personnel to perform this as needed.  The standard used should be a
     hydrocarbon for the flame ionization detector,  a chlorinated hydro-
     carbon for the E.G. detector and a phosphorous containing organic
     compound for the flame photometric detector.  The actual compound
     depends on the gas chromatographic column used in the instrument.
     Before the instrument is used to analyze "real" samples, a standard
     (chosen as described above)  and a blank Cair injection) are to be
     analyzed.  The sensitivity setting when analyzing the blank should
     be set at the highest level which will be used to analyze any of the
     "real" samples.  The purpose of analyzing a standard is to check the
     general overall performance of the instrument.  The air blank, which
     is to be analyzed after the standard, is the check for column bleed
     and syringe cleaning technique.  Corrective actions are to be taken
     by the operator if the two analyses indicate unsatisfactory perform-
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     ance (as dictated by the type of "real" samples to be analyzed).
     The Section Chief is to be consulted when any ambiguity arises.

B.   Balances
     The balances are to be checked once each month or prior to preparing
     a new set of primary standards.   The Section Chief will designate a
     person responsible for performing the balance check.   A record of
     this is to be kept in the logbook.   The check consists of weighing
     and recording a set of standard weights.  For the analytical balances
     the following weights are to be used: 10 gm, 1 gm and 10 mg.  For
     open pan balances the following weights are to be used:  1 kg, 10 gm
     and 1 gram.

C.   Infra-red Spectrophotometers
     The gain, balance, 0% and 100% transmission are to be checked daily
     prior to instrument use.  If any of these controls are adjusted,
     mention should be made in the logbook.  Furthermore,  a spectrum of a
                      »
     standard polyethelene film is to be taken daily, "prior to instrument
     use.  If the spectrum is not identical to the published standard
     polyethelene spectrum the Chief of the Section should be promptly
     notified.  These spectra should be kept in a folder in a file cabinet
     designated by the Chief, Organic Section.  The first person using the
     instrument on a given day is responsible for performing the above checks.

D.   Gel Permeation Chromatograph
     Spikes (sample plus added components), blanks Cjust solvent) and
     control samples (blank plus added componentsI are to be analyzed
     with every ten samples.  If the blanks indicate incomplete elution
     or if the control or spike do not indicate greater than 90% re-
     covery the Chief of the Organic Section is to be promptly notified.
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E.   High Pressure Liquid Chromatograph
     The same analytical quality control used for gas chromatographs is
     used for this instrument.  In addition, the same solvents and volumes
     as are injected for laboratory and reference standards are to be
     used for samples.

F.   Computerized Gas Chromatograph/Mass Spectrophotometer
     The mass spectrometer is to be calibrated each day it is used after
     all the electronics Cexcept the filament and computer)  have been
     turned on for at least h hour.  A mass spectra of the standard
     (FC13 or of PFTPP) is to be collected and saved after the instrument
     is calibrated.  The mass range should include from AMU 33 to AMU 650.
     This spectrum should be filed in a mass spectra AQC binder.  The
     collected spectrum should be compared to that of the same standard
     which was collected after the instrument's resolution and sensitivity
     were properly set.  If the intensity of any of the corresponding AMU
     peaks in the two spectra differ by more than 10%, the instrument's
     resolution is to be adjusted.  The calibration, resolution and
     sensitivity adjustments are to be made in accordance with the pro-
     cedures given in the instrument manual accompanying the instrument
     or in accordance with the latest procedures written by the Mass
     Spec Users Group.

     A spectrum of FC43 or PFTPP is also to be taken at the end of the
     day and compared to the spectrum taken right after calibration.
     If the intensity of corresponding AMU peaks in the two spectra differ
     by more than 10%, the Chief of the Organic Section is to be consulted
     as to the disposition of the data collected during the day.

     The gas chromatograph portion of the instrument is checked by
     analyzing a standard (determined by the type of gas chromatographic
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     column used)  and a solvent blank before any real samples are ana-
     lyzed.  The former is to check the performance of the gas chromato-
     graph and-of the separator.  The latter is to check for column bleed.
     If the results don't indicate satisfactory performance, corrective
     actions Cchange to a new column, clean the separator, change the
     septum, etc.)  are to be taken by the operator.

G.   Hewlett-Packard (.HP) Data System
     The HP chromatograph data system should be made operational as
     outlined in the operation manual, with the following additions:

     1)  A linear range plot (using Aldrin) showing the concentration
         range over which the total system (G.C. detector, interface
         electronics and data system) is linear, is to be obtained any
         time a new or reconditioned detector is installed and after any
         electronics involved with the detector signal conditioning are
         changed.   This plot is to be placed in the logbook provided
                             i
         for the instrument.

     2)  The window, i.e., the maximum variation allowed in the RRT of
         a peak, used for peak identification is to be no greater than
         3x the standard deviation in the RTT of the peak obtained by
         analyzing a set of standards a minimum of ten times.

     3)  A chart is to be kept in the logbook (for each E.G. detector)
         on which the response factor for Aldrin is recorded on a daily
         basis.  The Chief of the Organic Section is to be notified and
         consulted when the response factor shows a marked decrease  in
         detector sensitivity.

     4)  Calibration standards are to be made with compounds of known
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         maximum possible purity.   New standards should be made at least
         every 6 months and more often in questionable cases.   The stand-
         ards solutions are to be stored in an explosion-proof refriger-
         ator when not in use and each new batch of standards  should be
         compared to an old batch to insure they are correct.

H.   Atomic Absorption Spectrometers
     The atomic absorption instruments (PE-303, PE-306, PE-503, IL-453
     and Varian-600) are to be set up according to the manufacturer's
     specifications.  If changes are necessary, they should be documented
     in the instrument logbook and initialed by the first line supervisor.

     A blank, two calibration standards and a laboratory quality control
     sample are run daily  prior to the analysis of actual samples.   The
     calibration standard concentrations are to be in the linear range of
     the absorbance verses concentration curve.  If the sensitivity
     (concentration required to give an absorbance of 0.0044 absorbance
     units) differs from the previously established value for  the metal
     being run by more the 2% or if the standard is outside the control
     limits the fact should be recorded in the logbook, the problem
     corrected and the above steps repeated.  If the problem cannot be
     corrected, consult the first line supervisor.

I.   Emission Spectrometer System
     Quantitative instrument control checks listed in Section  7.0 of the
     document titled "Simultaneous Analysis of Liquid Samples  for Metals
     by Inductively Coupled Argon Plasma - Atomic Emission Spectroscopy
     (ICAP-AES)" will be obtained once data manipulation by the NOVA-840
     computer is finalized.  In the interim, the following quality control
     checks will be used to assess instrument performance.
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     1)  The concentration readout of the 1000 yg/1 calibration standard
         should be within ± 50 yg/1 during a sample analysis run.  Restand-
         ardization becomes mandatory if this limit is exceeded.

     2)  A laboratory quality control standard will be analyzed each
         day samples are run and these results will be kept in a logbook.
         If the difference between the running average and the daily
         analysis exceed 5%, the source of this disagreement should be
         identified and corrected, prior to the analyses of "real" samples.

J.   Technicon Auto Analyzers
     The electronic zero and full scale are set and the colorimeters,
     recorders, and printer are synchronized.  The baseline is set with
     wash solution and reagents running.  The instrument is standardized
     with a mid-scale standard, followed by a high and a low standard.
     These are followed by two blanks and two control standards.   The  control
     standards are prepared by an idependent analyst.  The remainder of
     the 40 sample wheel is loaded with samples.  One duplicate is run
     with each wheel.  The duplicates are spaced at least 10 samples apart.
     Each wheel after the first follows the same pattern, but only the
     first is used for standardization.  The second of each pair of blanks,
     the control standards, the duplicate samples, and the instrument  cal
     are recorded in the logbook.  If the control standards or blanks  are
     out of control limits, or if the cal is unusually high or low, the
     data associated with these values are not accepted.  The problem  is
     identified and corrected, the instrument is recalibrated, and the
     samples are rerun.

     If a sample of high concentration is followed by a sample of low
     concentrations so that the second sample is on the shoulder of the first,
     the second sample is repeated.  The data of preparation of all reagents
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 and standards,  columns,  etc.,  are  recorded  in  the  lobgook.  Reference
 standards  and results, and  any other  significant information concern-
 ing the  analyses  are  also recorded in the lobgook.

 Specific procedures for  individual automated methods are as follows:
 NH  -N  and  NO.+NO  -N:  Turbid samples are centrifuged prior to analysis.
  J	^   ~J	
 TP  - Persulfate Method;  Non-uniform  samples are blended prior  to
 digestion.   The calibration standards are made from an inorganic
 phosphorus compound and  the control standards are made from an  organic
"phosphorus compounds.  If a sample exceeds  the full scale concentration
 value, the original sample  is  diluted and redigested.  Turbid samples
 are centrifuged prior to analysis.
 TP  + TKN - Kjeldahl Method;  Same as TP - persulfate method, but loading
 pattern  begins  with set  standard,  followed  by 3 blanks, 3 calibration
 standards, 2 control  standards, then  samples.  The instrument is
 recalibrated for  every 40 sample set.  The  baseline is set with the
 blanks.  If a sample  results in an odd-shaped peak, the original is
 diluted  and redigested.
 COD; Non-uniform  samples are blended  prior  to digestion.  The instru-
 ment is  zeroed  with four blanks which preceded the first loading
 pattern.  Any samples that  appear  to  have leaked during digestion
 are repeated.
 Mercury;  A complete  standard  curve is prepared each day samples are
 analyzed.  The  standards are prepared from methylmercuric chloride .
 Control  standards, made  from QAO reference  standards, are analyzed
 each day.  Criteria used to establish that  the HGZ Spectro Products
 Mercury  analyzer  and automated sample handling system are performing
properly are:   The amount of current  applied to the mercury and
 reference lamps to balance the detector, the signal-to noise ratio
at  a constant damping and the rate of baseline drift.
Sulfate; To eliminate interference from cations,  the samples are
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     passed through an ion-exchange column.   Calcium is added to a stand-
     ard which is exceeded.

K.   Total Organic Carbon Analyzers
     The instrument is set up according to the manufacturer's specifica-
     tions.  Whenever a column is repacked or any other changes are made,
     a five standard calibration curve is run.  The high level standard
     is set at full scale.  This standard curve is used for subsequent
     analysis.  Each day that the instrument is used, the high level
     standards is set at full scale.  Two control standards and a blank
     are then injected.

     All standards, blanks and controls are run in duplicate, and the
     duplicates must agree to within one chart unit.  The control standards
     and blank are repeated approximately once each hour of analysis.  All
     samples are acidified and blended before injection.  They are then
     re-blended and reinjected until the peak height no longer decreases.
     The values are accepted when two or three replicate analyses agree to
     within one chart unit.  Duplicate samples are run approximately once
     each hour.  They are spaced at least 10 samples apart.  The blank, the
     control standards, the spaced duplicates, and the instrument gain are
     recorded in the logbook.  If the control standards or blank are out
     of control limits, the data associated with these values are not
     accepted.  The problem is identified and corrected, the instrument is
     recalibrated, and the samples are rerun.

L.   Sample Drying Oven
     The oven temperature is checked with a thermometer each time it
     is used.

M.   Diluters
     The diluter is checked by diluting a standard each day that the diluter
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     is used.  The results are recorded in the lobgook under the
     parameter for which the diluter is used.

N.   Dispensers
     Before the dispenser is used, the solution is visually inspected to
     be sure that the reagent is in solution.

O.   Titralyzers
     The titralyzer is calibrated with a pH 4 buffer, and two controlled
     standards are run and recorded in a logbook.

P.   Specific Electrode lonanalyzers
     The meter is calibrated with three standards of different concentra-
     tions and a record is kept of the control standards.

Q.   pH Meters
     A daily calibration is run using a pH 4 and pH 7 buffer.  Also two
     control standards are run and recorded in a logbook.

R.   Turbidimeters
     The instrument is calibrated on three different ranges with Formazin
     or Jackson turbidity standards.

S.   Conductivity Meters
     Samples and standards are incubated at 25°C in a 2095 Forma
     Scientific Bath.  The two control standards are recorded in a
     logbook.

T.   Dissolved Oxygen Meters
     The meter is checked for zero and temperature before each use.
     The DO is determined by the Winkler Method.  Two bottles are
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     checked on the meter, and the meter is calibrated to read this
     concentration.

U.   Controlled Environmental Rooms
     The environmental room is thermostatically controlled at 20°C.
     A Hg thermometer is kept inside the incubator to check on the
     accuracy of the temperature controller and recorder.

V.   Ultra Micro Balances
     Before using the balance,the zero is checked and set.  It is then
     calibrated at lOmg.  During each set of weighings, the zero and the
     calibration is rechecked several times.

W.   Colorimeters
     All Spectronic 70 and 88 spectrophotometers are calibrated using
     a Chemetrics "Spectro-Standard" kit.  The instruments are checked
     for:  stray light rejection at 340 nm; wavelength accuracy at
     360.9 nm, 418.4 nm, 453.2 nm, 536.2 nm and 637.5 nm using a holmium
     oxide filter; linearity between 400-900 nm at 13, 25, 40, 50 and 70%
     transmittance using neutral density filters; bandpass at 360 nm.
     If the instrument meets all of the specifications it is so labeled.-
     If not, the instrument is serviced.

V.   A Definition of Terms and Mathematical Concepts
     During the past is has proven to be necessary to define several
     terms used in the following tables in order to avoid confusion.
     In addition, the CRL has found it to be convenient to represent
     the magnitude of scatter or error associated with data from
     selected performance audits by a single number.  These terms are
     defined and used in this document as follows:
     1)  Reagent Blank - A sample prepared by adding distilled water
                                     -20-

-------
    and preservative to a sample bottle and then analyzing as a
    routine sample.

2)  Duplicate Analyses - The collection of two samples from the
    same field site which are analyzed at different times but
    usually on the same day.

3)  Relative percent error for duplicate analyses - 100 times the
    difference in the measured concentration for the duplicate
    pair divided by the average of the concentration.

4)  Laboratory Control Standard - A standard of known concentration
    prepared by the analyst.

5)  Relative percent error for laboratory control standards -
    The difference between the measured value and the theoretically
    correct value times 100 and divided by the correct value.

6)  Calibration standard - A standard prepared by the analyst for
    the purpose of calibrating an instrument.  Laboratory control
    standards are prepared independently from calibration
    standards for most methods.

7)  Spiked sample - A solution prepared by adding a measured
    volume of a laboratory control standard to a known volume
    of a sample.

8)  Percent recovery of a sample spike - The measured concen-
    tration of the spiked solution minus the measured sample
    concentration times 100 and divided by the concentration
    resulting from the spike.
                             -21-

-------
 9)   Reference Standard - A solution obtained from an outside
     source having a known value and analyzed as a blind sample.

10)   Relative percent error of a Reference Sample Analysis -
     The difference between the correct and measured values times
     100 and divided by the correct concentration.

11)   Detection limit - That number obtained by adding two standard
     deviations to the average value obtained for a series of reagent
     blanks that are analyzed over a long time (several weeks or
     months) period.
                               -22-

-------
Appendix I

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