ASTM D596-01(2006)
(Guide)Standard Guide for Reporting Results of Analysis of Water
Standard Guide for Reporting Results of Analysis of Water
SIGNIFICANCE AND USE
The proper use of analytical data requires adequate documentation of all inputs, that is, the source and history of the sample, laboratory performing the analysis, method of analysis, date of analysis, precision and bias of the measurements, and related quality assurance information.
In order to have defensible data, the report must be complete and accurate, providing adequate information to evaluate the quality of the data and contain supporting information that documents sampling and analysis procedures.
This guide contains some of the common data qualifiers or “flags” commonly used by laboratories following the Good Laboratory Practices, the Government Contract program, or found in the commercial laboratories. Examples of these qualifiers are the use of (E) for estimated value, (U) for analyzed for but not detected, and (B) for analyte was found in the blank (see 8.11). The qualifiers included in this guide should help the laboratory and its customers to better understand each other by using standardized qualifiers.
Practice D 933 is a comprehensive practice for reporting water-formed constituents such as metal oxides, acid anhydrides, and others.
SCOPE
1.1 This guide provides guidelines for reporting inorganic and organic results of analyses of drinking water, waste water, process water, ground water, and surface water, and so forth, to laboratory clients in a complete and systematic fashion.
1.2 The reporting of bacterial and radiological data are not addressed in this guide.
1.3 The commonly used data qualifiers for reviewing and reporting information are listed and defined. Client and laboratory specific requirements may make use of other qualifiers. This guide does not preclude the use of other data qualifiers.
1.4 This guide discusses procedures for and specific problems in the reporting of low level data, potential errors (Type I and Type II), and reporting data that are below the calculated method detection limit and above the analyte.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D596 – 01 (Reapproved 2006)
Standard Guide for
Reporting Results of Analysis of Water
This standard is issued under the fixed designation D596; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope D5792 Practice for Generation of Environmental Data Re-
lated to Waste Management Activities: Development of
1.1 This guide provides guidelines for reporting inorganic
Data Quality Objectives
and organic results of analyses of drinking water, waste water,
D6091 Practice for 99 %/95 % Interlaboratory Detection
process water, ground water, and surface water, and so forth, to
Estimate (IDE) for Analytical Methods with Negligible
laboratory clients in a complete and systematic fashion.
Calibration Error
1.2 The reporting of bacterial and radiological data are not
E29 Practice for Using Significant Digits in Test Data to
addressed in this guide.
Determine Conformance with Specifications
1.3 The commonly used data qualifiers for reviewing and
reporting information are listed and defined. Client and labo-
3. Terminology
ratory specific requirements may make use of other qualifiers.
3.1 Definitions—For definitions of terms used in this prac-
This guide does not preclude the use of other data qualifiers.
tice, refer to Terminology D1129.
1.4 This guide discusses procedures for and specific prob-
3.2 Definitions of Terms Specific to This Standard:
lems in the reporting of low level data, potential errors (Type
3.2.1 surrogates—compounds that are similar to analytes of
I and Type II), and reporting data that are below the calculated
interest in chemical composition and behavior, separation, and
method detection limit and above the analyte.
measurements, but that are not normally found in environmen-
2. Referenced Documents tal samples.
2.1 ASTM Standards:
NOTE 1—These compounds are added to blanks, standards, samples, or
D933 Practice for Reporting Results of Examination and
spiked samples prior to analysis to confirm the proper operation of the
Analysis of Water-Formed Deposits analytical system.
D1129 Terminology Relating to Water
3.2.2 Type I error—a statement that a substance is present
D2777 Practice for Determination of Precision and Bias of
when it is not.
Applicable Test Methods of Committee D19 on Water
3.2.3 Type II error—a statement that a substance was not
D3856 Guide for Good Laboratory Practices in Laborato-
present (was not found) when the substance was present.
ries Engaged in Sampling and Analysis of Water
4. Significance and Use
D4210 Practice for Intralaboratory Quality Control Proce-
dures and a Discussion on Reporting Low-Level Data
4.1 The proper use of analytical data requires adequate
D4460 Practice for Calculating Precision Limits Where
documentation of all inputs, that is, the source and history of
Values are Calculated from Other Test Methods
the sample, laboratory performing the analysis, method of
D4840 Guide for Sample Chain-of-Custody Procedures
analysis, date of analysis, precision and bias of the measure-
ments, and related quality assurance information.
4.2 In order to have defensible data, the report must be
This guide is under the jurisdiction ofASTM Committee D19 on Water and is
complete and accurate, providing adequate information to
the direct responsibility of Subcommittee D19.02 on General Specifications,
Technical Resources, and Statistical Methods. evaluate the quality of the data and contain supporting infor-
Current edition approved Aug. 15, 2006. Published August 2006. Originally
mation that documents sampling and analysis procedures.
approved in 1940. Last previous edition approved in 2001 as D596 – 01. DOI:
4.3 This guide contains some of the common data qualifiers
10.1520/D0596-01R06.
or “flags” commonly used by laboratories following the Good
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
Laboratory Practices, the Government Contract program, or
Standards volume information, refer to the standard’s Document Summary page on
found in the commercial laboratories. Examples of these
the ASTM website.
qualifiers are the use of (E) for estimated value, (U) for
Withdrawn. The last approved version of this historical standard is referenced
on www.astm.org. analyzed for but not detected, and (B) for analyte was found in
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D596 – 01 (2006)
the blank (see 8.11). The qualifiers included in this guide bias could be made, or review the procedure for determining
should help the laboratory and its customers to better under- single-operator precision of a test method as provided in
stand each other by using standardized qualifiers. Practice D2777 for guidance. The procedure used to derive the
4.4 Practice D933 is a comprehensive practice for reporting detection limit should be identified along with any specific
water-formed constituents such as metal oxides, acid anhy- definitions associated with the derivation. Practice D4210 is
drides, and others. one of many sources for computing single laboratory method
detection limits. Practice D6091 provides an estimate of the
5. Sample Documentation
detection level achievable by multiple laboratories on single
5.1 Information regarding the source and history of the
sample.
sample to be included in the analytical report should define the
6.5 The date and time on which each determination is
sample and include the following, as appropriate:
performed should be recorded, as should other time-critical
5.1.1 Laboratory performing analysis,
processes such as extractions, storage times, drying times, and
5.1.2 Name and address of organization or person request-
so forth.
ing analysis,
6.6 The analytical reports should clearly specify the form in
5.1.3 Specific location of sampling and complete identifica-
which multi-atomic analytes, such as nitrate and orthophos-
tion of sample,
phate, are reported.
5.1.4 Date and time of sampling,
6.7 If a sample is prepared for analysis in a nonstandard
5.1.5 Sample identification number, and
manner or in a manner different from the routine batch
5.1.6 Sampling method, treatment, and preservation.
procedures (that is, special cleanup procedures or dilution
5.2 In addition to the information in 5.1, the following
requiredpriortoanalysis)thenthereportshouldclearlypresent
information should be included as appropriate:
the deviation and the reason why the deviation was required.
5.2.1 Identification of sampling organization and individual
6.8 If a sample is diluted prior to analysis, the sample
sampler,
dilution values should be reported from which the ratios can be
5.2.2 Pressure and temperature of system sampled,
determined and the reason for the dilution documented.
5.2.3 Flow rate of water in a stream, outfall, pipe, and so
forth.
7. Documentation of Quality
5.2.4 Copies of sampling logs with signatures,
7.1 Each sample analysis may have different quality needs
5.2.5 Chain-of-custody forms with signatures (see Guide
basedontheuseofthedataortheDataQualityObjectives(See
D4840),
Practice D5792). This information should be determined be-
5.2.6 Results of field measurements, and
fore sampling and analysis. Based on the information, an
5.2.7 Description information (color, odor, and so forth)
analytical report may include the following information, as
clearly presented.
appropriate:
5.2.8 The information about the sample documented in the
7.1.1 Amount recovered and percent recovery of any surro-
report should be complete enough to provide direct unabridged
gate compounds with laboratory control limits,
links to underlying documents (such as chain-of-custody
7.1.2 Results of corresponding check samples or blank
records and field logs) and information (such as name of
spikes with laboratory control limits,
sampler, lot numbers of the sample bottles, and preservatives).
7.1.3 Results of analysis of duplicate samples or duplicate
matrixspikesamplesandthepercentdifferencewithlaboratory
6. Analysis Documentation
control limits,
6.1 The laboratory system shall provide enough information
7.1.4 Recoveries of any matrix spikes (and matrix spike
to the user or reviewer so that all of the events that could
duplicates) with laboratory control limits,
influence the quality of the data can be reconstructed. The user
7.1.5 Results of all blanks,
maynotneedtohavetheinformationcommunicateddirectlyto
7.1.6 Results of any reference samples run during sample
them, but it must be available upon request. Such information
analysis with laboratory control limits,
shoulddescribehoweffectivelyallprocedureswerecarriedout
7.1.7 Calibration and tuning data, and
and how processes were controlled so that they meet industry
7.1.8 Chromatogram or charts.
and government standards for performance.
6.2 As described in Guide D3856, the test method of
8. Reporting Data
analysis should be specified in the analytical report for each
8.1 Report data in accordance with the customer and labo-
determination performed on a sample.Areference of sufficient
definition or a copy of the test method should be provided to ratoryagreement.Intheabsenceofaspecificagreement,report
the data in accordance with laboratory policy or government
the requestor of the analytical services.
6.3 The report should note any deviation from the specified mandated requirements, if appropriate.
test method. Whenever a choice is allowed, the rational for 8.2 Compound specific analysis may require tentative iden-
selecting a given method should be documented. tification without verification. The criteria for identification
and a copy of the chromatogram or other instrument output
6.4 The precision, bias, and detection limit of each analyti-
cal test method should be disclosed as part of either the test should be included in the report.
method or the analytical report. Consult Guide D3856 for the 8.3 Upon request, the quality documentation found in Sec-
quality control system from which estimates of precision and tion 7 should be included in the report.
D596 – 01 (2006)
8.4 Any deviation from the established method or standard 8.10.2.2 Criteria—Criteriamustbeestablishedastowhena
operating procedure (SOP), must be reported to the customer. result is part of a replicate set. For example, when a dilution is
Reasons for the deviation and the expected impact on the data performed on a sample prior to analysis, the original result and
should be given. the diluted result may both be within the quantitative range of
the analytical method. Although the dilution step produces a
8.5 The procedures, method, or SOP used to report the
analytical values shall be specified. value that is not a true replicate, the added value of reporting
an average of these values may be warranted.
NOTE 2—If there is no deviation from the contract or agreed upon
8.10.2.3 Selection forAveraging—Analyticalresultsmaybe
procedure, then reference to the document may be sufficient.
produced within four discrete ranges. Each of these ranges is
8.6 In cases where the customer desires a summary of the
affected by sample dilution or concentration. Replicates may
data to be transmitted to them, the laboratory will keep
be generated within different ranges for the sample analysis.
sufficient records on file to reproduce the data.
The four discrete ranges are listed as follows in increasing
8.7 Detection limits should be reported in accordance with order of size:
laboratory policy, established procedures, or regulatory re-
(1) Below a limit of detection, where the analyte cannot be
quirement. These polices and procedures must be clearly said to be present with confidence above a set level.
identified and understood by all personnel reporting the analy- (2) Between a limit of detection and a limit of quantitation
sis. Results reported below laboratory established detection where the analyte can be said to be present with a preset limit
limits may be reported upon customer request as discussed in of confidence but the concentration value does not meet a
Section 10.
preset criteria.
(3) Between a limit of quantitation and the upper limit of the
NOTE 3—Some commercial laboratories establish their detection limits
quantitation range of the analytical method. This is the quan-
based on what their average laboratory can achieve over an extended
titation range of the analytical method. This is typically the
period of time. A given laboratory may achieve lower compound specific
highest calibration standard used.
values than the average.
(4) Above the quantitation range of the analytical method.
8.8 Report blank data results and, where appropriate, actual
8.10.2.4 It is important to first establish which of the ranges
data from the equipment. Blanks should not be subtracted from
found in 8.10.2 is applicable to each replicate. Replicates
the sample results unless required by the test method. The
should not be averaged across ranges. The following selection
customer should determine, with advisement form the labora-
criteria for averaging should be followed:
tory, if blank subtraction is necessary or required. (See Section
(1) Select and average only replicates that fall within the
10).
quantitation range of the analytical method. If none exist, then,
8.9 Recording direct measurement test results should be
(2) Select and average only replicates that fall above the
reported by recording all digits that are known plus one that
quantitation range of the analytical method. If none exist, then
may be subject to change on repeated analysis. When calcu-
(3) Select and average only replicates that fall between a
lating results from test data, rounding should be performed
limit of detection and a limit of quantitation. If none exist, then
only on the final result, not upon the intermediate values
(4) Select and average only replicates that fall above the
employed in the calculation.
established limit of detection.
8.10 Frequently, replicate determinations are made. When
NOTE 4—References to range refer to ranges adjusted for sample
replicate results are obtained, useful information is now avail-
concentration or dilution.
ablethatislostiftheresultsofthesereplicatesarenotreported.
It is important that a reporting laboratory establish a consistent
8.10.2.5 Exclusion of Data—Individual values may be ex-
protocol for reporting replicate data. In order to arrive at a
cluded from
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