ASTM D5847-02(2012)
(Practice)Standard Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
Standard Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
SIGNIFICANCE AND USE
In order to be certain that the end user of analytical results obtained from using an ASTM Committee D-19 test method can be confident that the values have been obtained through a competent application of the test method, a demonstration of the proficiency of the analytical system must be performed. Appropriate proficiency is demonstrated by achievement of performance criteria derived from results of the test method collaborative study. The QC measures specified in this practice must be included in each ASTM test method, as applicable, to ensure the quality of measurements.
In order for users of D-19 test methods to achieve consistently valid results, a minimum level of QC must be performed. This minimum level of QC is stipulated in this practice and by the taskgroups developing D-19 test methods. If the specific requirements outlined in this practice are not applicable to the test method, alternative QC must be defined in the test method.
SCOPE
1.1 This practice provides specific, mandatory requirements for incorporating quality control (QC) procedures into all test methods under the jurisdiction of Committee D-19.
1.2 ASTM has adopted the following:
Policy on implementation of requirements for a quality control section in standard test methods generated by Committee D-19 on Water. GENERALBy July 29, 1998, or at the next reapproval or revision, whichever is later, every D-19 Standard Test Method shall contain a QC section that is in full compliance with the requirements of this practice. NEW COLLABORATIVE TESTINGAs of July 29, 1998, each collaborative study design shall include a QC section as part of the method to be tested. Prior to approval of the study design, the Results Advisor shall ascertain the appropriateness of the QC section in meeting the requirements of this Practice and Practice D2777, and shall advise the designer of the study of any changes needed to fulfill the requirements of these practices. Before a collaborative study may be conducted, approval of the study design by the Results Advisor must be obtained. OLDER VALIDATED METHODSStandard test methods that were validated using D-2777-77, D-2777-86, or D-2777-94, when ballotted for reapproval or revision, shall contain a QC section based upon the best information from the historical record. Where appropriate, information derived from the record of the collaborative study shall be utilized for this purpose. The introduction of the QC section into these standard test methods shall not be construed as a requirement for a new collaborative study, though the Subcommittee may opt for such a study. Any information available regarding QC or precision/bias testing shall be included in the appropriate sections of the published method.
1.3 Required QC sections in all applicable test methods are intended to achieve two goals. First, users of Committee D-19 test methods will be able to demonstrate a minimum competency in the performance of these test methods by comparison with collaborative study data. Second, all users of test methods will be required to perform a minimum level of QC as part of proper implementation of these test methods to ensure ongoing competency.
1.4 This practice contains the primary requirements for QC of a specific test method. In many cases, it may be desirable to implement additional QC requirements to assure the desired quality of data.
1.5 The specific requirements in this practice may not be applicable to all test methods. These requirements may vary depending on the type of test method used as well as the analyte being determined and the sample matrix being analyzed. See Explanation 1 in Appendix X1.
1.5.1 If there are compelling reasons why any of the specific QC requirements listed in this practice are not applicable to a specific test method, these reasons must be documented in the QC section of the test method.
1.5.2 With the approval of Committee D-19 on the recommendation o...
General Information
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D5847 −02 (Reapproved 2012)
Standard Practice for
Writing Quality Control Specifications for Standard Test
Methods for Water Analysis
This standard is issued under the fixed designation D5847; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope will be required to perform a minimum level of QC as part of
proper implementation of these test methods to ensure ongoing
1.1 This practice provides specific, mandatory requirements
competency.
for incorporating quality control (QC) procedures into all test
methods under the jurisdiction of Committee D-19. 1.4 This practice contains the primary requirements for QC
of a specific test method. In many cases, it may be desirable to
1.2 ASTM has adopted the following:
implement additional QC requirements to assure the desired
Policy on implementation of requirements for a quality control
quality of data.
section in standard test methods generated by Committee D-19
on Water.
1.5 The specific requirements in this practice may not be
applicable to all test methods. These requirements may vary
GENERAL—By July 29, 1998, or at the next reapproval or revision,
whichever is later, every D-19 Standard Test Method shall contain a depending on the type of test method used as well as the
QC section that is in full compliance with the requirements of this
analyte being determined and the sample matrix being ana-
practice.
lyzed. See Explanation 1 in Appendix X1.
NEW COLLABORATIVE TESTING —As of July 29, 1998, each
collaborative study design shall include a QC section as part of the 1.5.1 Iftherearecompellingreasonswhyanyofthespecific
method to be tested. Prior to approval of the study design, the
QC requirements listed in this practice are not applicable to a
Results Advisor shall ascertain the appropriateness of the QC
specific test method, these reasons must be documented in the
section in meeting the requirements of this Practice and Practice
D2777, and shall advise the designer of the study of any changes QC section of the test method.
needed to fulfill the requirements of these practices. Before a collab-
1.5.2 With the approval of Committee D-19 on the recom-
orative study may be conducted, approval of the study design by the
mendation of the D-19 Results Advisor and the Technical
Results Advisor must be obtained.
OLDER VALIDATED METHODS —Standard test methods that were
OperationssectionoftheExecutiveSubcommittee,astatement
validated using D-2777-77, D-2777-86, or D-2777-94, when ballotted
giving the compelling reasons why compliance with all or
for reapproval or revision, shall contain a QC section based upon the
specificpointsofthispracticecannotbeachievedwillmeetthe
best information from the historical record. Where appropriate, infor-
mation derived from the record of the collaborative study shall be
requirements of both ASTM and this practice.
utilized for this purpose. The introduction of the QC section into
1.5.3 Test Methods developed prior to the approval of this
these standard test methods shall not be construed as a requirement
practice with a QC Section that meet the requirements of
for a new collaborative study, though the Subcommittee may opt for
such a study. Any information available regarding QC or precision/
Specification D5789 are considered in compliance with this
bias testing shall be included in the appropriate sections of the pub-
Practice.
lished method.
1.6 This practice is for use with quantitative methods and
1.3 Required QC sections in all applicable test methods are
may not be applicable to qualitative test methods.
intended to achieve two goals. First, users of Committee D-19
test methods will be able to demonstrate a minimum compe-
1.7 Presently, this practice is applicable primarily to chemi-
tency in the performance of these test methods by comparison
cal test methods. It is intended that, in future revisions, the
with collaborative study data. Second, all users of test methods
practice will be expanded to include other methods such as
microbiological methods.
1.8 This international standard was developed in accor-
dance with internationally recognized principles on standard-
This practice is under the jurisdiction of ASTM Committee D19 on Water and
is the direct responsibility of Subcommittee D19.02 on Quality Systems,
ization established in the Decision on Principles for the
Specification, and Statistics.
Development of International Standards, Guides and Recom-
Current edition approved June 15, 2012. Published June 2012. Originally
mendations issued by the World Trade Organization Technical
approved in 1999. Last previous edition approved in 2007 as D5847 – 02(2007).
DOI: 10.1520/D5847-02R12. Barriers to Trade (TBT) Committee.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5847−02 (2012)
2. Referenced Documents test method to determine whether the analytical system is in
2 control. The LCS must be prepared in the appropriate ASTM-
2.1 ASTM Standards:
gradewaterfromamaterialthatsufficientlychallengesthetest.
D1129 Terminology Relating to Water
See Explanation 3 in Appendix X1. The LCS can be an IRM
D1193 Specification for Reagent Water
obtained from an outside source or prepared in-house from
D2777 Practice for Determination of Precision and Bias of
materials of known purity and concentration.Alternatively, the
Applicable Test Methods of Committee D19 on Water
LCS may be a real sample of the matrix that is typically
D3648 Practices for the Measurement of Radioactivity
analyzed and which has been fully characterized.
D3856 Guide for Management Systems in Laboratories
3.2.5.1 Discussion—The LCS may also be commonly
Engaged in Analysis of Water
known as a “quality control sample” or an “ongoing precision
D4375 Practice for Basic Statistics in Committee D19 on
and recovery sample” (OPR).
Water
D5789 Practice for Writing Quality Control Specifications 3.2.6 matrix spike (MS)—addition of a known concentration
for Standard Test Methods for Organic Constituents ofanalytetoaroutinesamplerepresentingaspecificmatrixfor
the purpose of evaluating interference from matrix compo-
(Withdrawn 2002)
D5810 Guide for Spiking into Aqueous Samples nents. (See Guide D5810.)
3.2.7 method blank (blank)—reagent water (see Specifica-
3. Terminology
tion D1193) either known to be free of the constituent(s) of
3.1 Definitions:
interest or containing only a low, known concentration of the
3.1.1 For definitions of terms used in this practice, refer to
constituent(s) of interest not exceeding five times the estimated
Terminology D1129 and Terminology D4375.
detection limit.
3.2 Definitions of Terms Specific to This Standard:
3.2.7.1 Discussion—The purpose of analysis of the method
3.2.1 batch—a set (group) of samples analyzed such that
blank is to confirm that the reagents or analytical system, or
results of analysis of the QC samples (laboratory control
both, do not contribute a measurable amount of the constitu-
sample, method blank, matrix spike, and duplicate or matrix
ent(s) of interest during analysis of routine samples or, if they
spike duplicate) analyzed with the batch are indicative of the
do, to determine what the contribution is.
quality of the results of analysis of samples in the batch. The
3.2.8 quantitation limit—the minimum concentration or
number of samples in the batch is defined by the task group
amount of a substance that can be measured with a known
responsible for the method. See 6.4 and Explanation 2 in
degree of confidence.
Appendix X1.
3.2.9 sample pretreatment (pretreatment)—any handling,
3.2.1.1 Discussion—When results from tests of any of the
manipulation or treatment of a sample prior to subjecting the
QC samples associated with batch the fail to meet the perfor-
sample to the analysis. Examples are filtration, digestion,
mance criteria, the test method should define the appropriate
dilution, pH adjustment and extraction.
corrective action. To make such a response valid, the batch
mustbeconstructedinsuchawayastoassurethatallvariables
4. Summary of Practice
affecting the batch will affect all samples in the batch in a
statistically equivalent manner.
4.1 This practice provides the writer of a test method in
3.2.2 calibration standard—a solution containing the ana-
Committee D19 specific steps to be included in the QC section
lyte of interest at a known concentration either purchased from of the test method. A QC section is required in all applicable
an external source or prepared in-house from materials of
standard test methods that mandates use of the following QC
known purity or concentration, or both, and used to calibrate measures:
the measurement system.
4.1.1 Periodiccalibrationorverificationofcalibrationofthe
measurement system,
3.2.3 detection limit—the minimum concentration or
4.1.2 Initial demonstration of laboratory capability,
amount of a substance that can be detected with a known
4.1.3 Analysis of at least one blank per batch,
degree of confidence.
4.1.4 Analysis of at least one LCS per batch,
3.2.4 independent reference material (IRM)—a material of
4.1.5 Analysis of at least one MS per batch, where
known purity and concentration obtained either from the
applicable, and
NationalInstituteofStandardsandTechnology(NIST)orother
4.1.6 Periodic analysis of an IRM.
reputable supplier. The IRM shall be obtained from a different
lot of material than is used for calibration.
4.2 Duplicate analysis of at least one sample per batch is
3.2.5 laboratory control sample (LCS)—a sample of known suggested. The duplicate analysis may be of a sample or of a
concentration and composition that is taken through the entire matrix spike (matrix spike duplicate; MSD). See Explanation 4
in Appendix X1.
4.3 If there are valid reasons why any of the above QC
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
requirements are inapplicable to a specific test method (see
Standards volume information, refer to the standard’s Document Summary page on
Section 1), these reasons must be documented in the QC
the ASTM website.
section of the test method. See 1.5 and Explanation 1 in
The last approved version of this historical standard is referenced on
www.astm.org. Appendix X1.
D5847−02 (2012)
5. Significance and Use chemical and physical properties. Therefore, authors ofASTM
test methods for radioactivity measurements should provide
5.1 In order to be certain that the end user of analytical
specific guidance within each test method, practice or guide
results obtained from using an ASTM Committee D-19 test
relative to applicable QC program requirements. Guidance on
method can be confident that the values have been obtained
the preparation and use of instrument tolerance and control
through a competent application of the test method, a demon-
charts can be found in Practices D3648 and D3856, and in
stration of the proficiency of the analytical system must be
ASTM MNL 7.
performed. Appropriate proficiency is demonstrated by
achievementofperformancecriteriaderivedfromresultsofthe 6.2 Calibration and Calibration Verification—For test
test method collaborative study. The QC measures specified in methods requiring calibration of instrumentation, an appropri-
this practice must be included in each ASTM test method, as ate number of calibration standards must be analyzed during
applicable, to ensure the quality of measurements. daythatananalysisisperformedtoconfirmthattheinstrument
is properly set up and required sensitivity is being obtained.
5.2 In order for users of D-19 test methods to achieve
The actual number of standards required will depend on the
consistently valid results, a minimum level of QC must be
requirements of the test method. For tests run infrequently,
performed. This minimum level of QC is stipulated in this
analysis of a single calibration standard to verify an existing
practice and by the taskgroups developing D-19 test methods.
calibration curve may suffice. For tests run frequently, it may
If the specific requirements outlined in this practice are not
be necessary to intersperse verification standards with test
applicabletothetestmethod,alternativeQCmustbedefinedin
samples. Under these circumstances, it is recommended that a
the test method.
different standard concentration be used each time calibration
is verified. Raw data (absorbance, intensity, etc.) should be
6. Requirements for QC Specifications in Test Methods
compared to data generated in the past under the same
6.1 Every test method must have a quality control (QC)
conditions and should fall within three standard deviations of
section. Listed below are requirements applicable to nearly all
the mean value found in the past based on the pooled single
chemical test methods and that must be followed to ensure that
operator precision. Alternatively, data should be compared to
thetestmethodisincontrolandtovalidatetheaccuracyofdata
the calibration limits stated in the test method or should be
generated for a specific matrix.
developed from collaborative study data. Refer to Guide
6.1.1 The measures that must be specified in the QC section
D3856 and Practice D3648 for further information on calibra-
of test methods and the reasons for these measures are as
tion checks.
follows:
6.2.1 For titrimetric test methods, titrants must be standard-
6.1.1.1 Calibrationandcalibrationverificationarenecessary
ized on a scheduled basis against a standard solution of known
to ensure that the analytical system is properly calibrated
concentration in duplicate or triplicate. The average normality/
during the period that the analysis is performed.
molarity is then used for calculation. The frequency of stan-
6.1.1.2 An initial demonstration of laboratory capability is
dardization is left to the judgment of the writer of the test
necessary to prevent errors as a result of unfamiliarity with the
method and should be based on the stability of the titrant.
test.
6.2.2 An alternate calibration procedure, such as an internal
6.1.1.3 Analysis of a blank with each batch may indicate
standard, external standard, or single-point calibration
that analytes in a test sample are the result of contamination.
procedure, must be specified in the test method.
6.1.1.4 An LCS is run with each batch to determine that the
6.2.3 The test method must establish the frequency of
measurement system is in control at the time samples are being
calibration and calibration verifica
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