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
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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.
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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.
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Appendix I
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