Standard Practice for Reporting Results from Methods of Chemical Analysis

SCOPE
1.1 This practice covers the approximate number of digits required to express the expected precision of results reported from standard methods of chemical analysis. This practice provides selection criteria and proper form and symbols for coding results when necessary to indicate the relative reliability of results having small values.

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09-May-1998
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ASTM E1950-98 - Standard Practice for Reporting Results from Methods of Chemical Analysis
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: E 1950 – 98
Standard Practice for
Reporting Results from Methods of Chemical Analysis
This standard is issued under the fixed designation E 1950; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3.2.3 null limit, NL, n—the analyte content below which
results are so near zero that averaging is unlikely to yield a
1.1 This practice covers the approximate number of digits
value significantly different from zero.
required to express the expected precision of results reported
3.2.4 quantitative, adj— relating to results, having a nu-
from standard methods of chemical analysis. This practice
merical value that includes at least one significant digit (see
provides selection criteria and proper form and symbols for
Practice E 29).
coding results when necessary to indicate the relative reliability
of results having small values.
4. Significance and Use
1.2 Specifically excluded is consideration of report forms
4.1 A result should be stated to a sufficient number of digits
and the associated informational content of reports in which
so that a user receives both quantitative information and a
results are tabulated or transmitted. It is assumed that the
measure of the variability of the value reported.
reporting laboratory has established a report format to ensure
4.2 The range of application of most methods of chemical
proper identification of the materials tested, the nature and
analysis is based upon the presumption that the quantitative
conditions of the test, the responsible personnel, and other
results produced are to be used to compare the analyte content
related information in accordance with existing regulations and
of the test material with specified limiting values. However,
good laboratory practices.
analytical results may be used legitimately for other purposes.
2. Referenced Documents If the same material is analyzed a number of times or a product
is analyzed periodically during an interval of production, each
2.1 ASTM Standards:
set of results may be averaged to yield an average result having
E 29 Practice for Using Significant Digits in Test Data to
improved reliability. Results that fall below the lower limit,
Determine Conformance with Specifications
although not quantitative individually, contain compositional
E 135 Terminology Relating to Analytical Chemistry for
information and shall be reported. The reporting system in this
Metals, Ores, and Related Materials
practice permits the analyst to indicate which values are likely
E 1601 Practice for Conducting an Interlaboratory Study to
to be rendered quantitative by averaging and which are not.
Evaluate the Performance of an Analytical Method
4.3 The system is simple enough to be used routinely in
E 1763 Guide for Interpretation and Use of Results from the
reporting results from standard methods and assists those
Interlaboratory Testing of Chemical Analysis Methods
untrained in statistics to apply results appropriately.
3. Terminology
5. Rounding Calculated Values
3.1 Definitions:
5.1 Use information from the precision section of the
3.1.1 For definitions of terms, refer to Terminology E 135.
method to determine the appropriate number of digits to report
3.2 Definitions of Terms Specific to This Standard:
as follows:
3.2.1 lower limit, L, n—the lower limit of the quantitative
5.1.1 Estimate the reproducibility index, R, at the analyte
analyte concentration range.
level of the result, C, from an equation of R as a function of
3.2.2 low-level reproducibility index, K , n—the reproduc-
R
concentration or from the table of statistical information.
ibility index constant (for low analyte levels) determined in
5.1.2 Calculate the percent relative reproducibility index:
accordance with Guide E 1763.
R 5 100 3 R / C (1)
rel%
5.1.3 For results within the range of application specified in
This practice is under the jurisdiction of ASTM Committee E-1 on Analytical
the method, round the values to the number of digits specified
Chemistry for Metals, Ores and Related Materials and is the direct responsibility of
Subcommittee E01.22 on Statistics and Quality Control.
in Table 1 (see A1.1.1 through A1.1.2).
Current edition approved May 10, 1998. Published August 1998.
5.1.4 For results less than the lower limit, proceed in
Annual Book of ASTM Standards, Vol 14.02.
3 accordance with Section 6 to establish the number of digits and
Annual Book of ASTM Standards, Vol 03.05.
appropriate coding for rounding and reporting the values.
Annual Book of ASTM Standards, Vol 03.06.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E1950–98
TABLE 1 Rounding Guide
6.3.2 Results Less Than L—Round values to the second
R Number decimal place of L, and enclose in parentheses before report-
rel%
of Digits
ing. Examples: For L equal to 1.5, round to x.x and report (x.x);
5-50% 2
for L equal to 0.22, round to 0.xx and report (0.xx); for L equal
0.5-5% 3
to 0.00050, round to 0.000xx and report (0.000xx).
0.05 - 0.5 % 4
6.3.3 Results Less Than NL—If the method is a “biased-
< 0.05 % 5
zero” procedure, treat in accordance with 6.4; otherwise, round
in accordance with 6.3.2, and enclose in parentheses followed
by an asterisk before reporting. Examples: (-0.2)*, (0.04)*, and
5.2 Calculated values shall be rounded to the required (-0.00003)*.
number of digits in accordance with the rounding-off method 6.4 Special Rule for “Biased-Zero” Methods:
of Practice E 29. 6.4.1 For results from “biased-zero” methods only, do not
5.2.1 The procedure is summarized as follows: report numerical values for results less than NL. Replace them
5.2.1.1 When rounding off a number to a specified number with the symbol (– –)*.
of digits, choose that digit that is nearest. If two choices are 6.5 Reference to the Method:
possible, as when the digits dropped are exactly a five or a five 6.5.1 Cite the designation of the standard method used to
followed only by zeros, choose that ending in an even digit. determine each analyte reported.
6.6 Explanations of Coding Symbols:
6. Procedure 6.6.1 If results less than L are reported for any analyte,
append the following explanation:
6.1 Preliminary Precaution—For a method to be used to
analyze materials with analyte content very near zero, the NOTE 1—Results in parentheses are not reliable for individual compari-
sons.
analyst shall determine that it is capable of producing “unbi-
ased” estimates of zero. If the method occasionally yields
6.6.2 If results less than NL are reported for any analyte,
negative results for low analyte levels, that capability is
append the following explanation: * These values cannot be
demonstrated. Proceed in accordance with 6.2.
distinguished from zero.
6.1.1 Test for “Biased-Zero” Methods—Prepare the method
6.6.3 If the symbol (– –)* is reported for any analyte,
to perform determinations. Include all aspects of instrument
append the following explanation: (– –)* The method cannot
preparation and calibration. Apply the method to a “blank”
report an unbiased estimate at this low analyte level.
sample or one known to have a negligible analyte content but
7. Use of Uncoded and Coded Values
that meets the method’s scope requirements in all other
7.1 Uncoded Data:
respects. If the method yields a negative result, it is not a
7.1.1 Numerical values reported without enclosing paren-
“biased-zero” method; proceed in accordance with 6.2. If,
theses are quantitative results and may be used for comparisons
during the course of at least ten replicate determinations,
with specified limiting values.
several zeros but no negative values are observed, it is a
7.2 Coded Data:
“biased-zero” method. Apply the biased-zero rule of 6.4 in
7.2.1 Values enclosed in parentheses are not quantitative,
reporting results lower than NL (see 6.2.2).
that is, individual values are not suitable for comparisons.
6.2 Critical Concentrations:
However, data in parentheses not followed by an asterisk, may
6.2.1 From the method, obtain the value of the lower limit,
yield values that are quantitative if a sufficient number are
L, to two digits (add a final zero, if necessary). Determine the
averaged (see A2.2.3).
decimal place of the second digit.
7.2.2 Values coded with an asterisk are from materials that
6.2.2 Calculate the null limit as follows:
are likely to produce randomly occurring negative values for
NL 5 L / 4 (2)
repeated determinations. They may be averaged, but unless the
6.3 Basic Rules:
average includes a large number of individual results (more
6.3.1 Numerical values shall be reported for every result
than 25), even the first digit is not likely to be significant.
(including negative values) obtained from a properly con-
8. Keywords
ducted method except as provided for certain results from
“biased-zero” methods in accordance with 6.1.1 and 6.4.
8.1 quantitative results; reporting results
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E1950–98
ANNEXES
(Mandatory Information)
A1. STATISTICAL BASIS FOR QUANTITATION CRITERIA
A1.1 Quantitation is the ability to determine a result whose report four digits (the first three are significant.) If R is 0.05
rel%
% or less, report five digits (the first four are significant.)
value may be compared with specified limiting values. Practice
E 29 adds the concept of significant digits. This term is used in
A1.2 Results from materials with analyte content less than
this practice to identify the digits in a value that are not
L are not quantitative as defined in this practice, but their
expected to change appreciably if the result is redetermined.
values contain information concerning the analyte content.
The statistical basis for quantitation is found in Practice E 1601
These results are reported, but their use for individual com-
and Guide E 1763. The lower limit (L) of a method’s
parisons is discouraged.
quantitative range is calculated from its reproducibility index,
A1.2.1 Guide E 1763 provides calculations for K , the
R
R, which is determined in the interlaboratory study (ILS). The
constant value R achieves at analyte contents near L and lower.
analyte content of a material must be greater than that limit if
This value of R divided by 2.8 yields the reproducibility
results are to exhibit at least one significant digit.
standard deviation, s , which, added to and subtracted from a
R
result, signifies a confidence interval. While indicating uncer-
A1.1.1 R represents the largest difference between results
tainty, this approach does not lend itself to easy recognition of
obtained in two laboratories on the same material that is not
a value’s reliability because the user must apply a rather
expected to be exceeded in more than 1 in 20 comparisons (95
complex interpretive process to decide how the data may be
% confidence level). L is arbitrarily defined as the analyte
used.
content at which R represents a 50 % relative error. At this
A1.2.2 The ultimate user, if willing to expend time and
analyte content, the average difference (50 % confidence level)
resources, can reduce variability by averaging a number of
between results in two laboratories is about 18 % of their mean.
results from the same material obtained in different laborato-
Results at this analyte level are quantitative with approximately
ries. For example, if a material having an analyte content of R
one significant digit, and, in accordance with Practice E 29 and
is analyzed once in four laboratories, the relative variability of
common statistical practice, are reported with two digits to
such an average (four values) is 50 %, the same as the
preserve the statistical information it contains. Only the first
variability of single results from a material with twice the
digit is considered significant.
analyte content (that is, at L).
A1.1.2 Users of standard methods (or data obtained from
A1.2.3 The limit to the enhancement in precision by repli-
them) can use R values reported at the analyte levels of the test
cation is established only by the resources the user is willing to
materials (Practice E 1601) or the equation relating R to analyte
expend. A reasonable (though arbitrary) limit is the null limit,
concentration (for ILS evaluated in accordance with Guide E
NL = R/2 (which is equivalent to L/4). The null limit is the
1763) to estimate the reliability of data at any concentration
lowest analyte level at which the average of 16 or more results
within the quantitative range of the method. If R is5%or
yields an average value having at least one significant digit.
rel%
less relative to the determined value, report results with three Results below NL are, for practical purposes, indistinguishable
digits (the first two are significant.) If R is 0.5 % or less, from zero.
rel%
A2. PRACTICAL BASIS FOR QUANTITATION CRITERIA
A2.1 The practical basis for quantitation must provide quantitative, but averages are also unlikely to be quantitative.
guidance to analysts and users of results who have little Individual and average values that are less than NL are
statistical training. The criteria should be consistent with the
expected to be estimates of zero.
ILS statistics and criteria discussed in Annex A1, simple to
A2.2.3 Class 2 consists of results with values falling within
understand, and convenient to use. The coding applied to each
the range NL to L. Individual results are not quantitative, but
value should give an unmistakable visual indication of its
averages of values obtained in different laboratories may be
reliability.
quantitative. The number of values needed to obtain a quanti-
tative average ranges from 2 (at analyte levels just less than L)
A2.2 A system to meet these requirements classifies results
into three concentration ranges: to 16 (at analyte levels just greater than NL).
A2.2.1 Class 1 consists of results with values falling be-
A2.3 The classifications in A2.2 meet the requirements in
tween the upper and lower application limits stated in the
A2.1. The analyst classifies each result by comparing its value
method. These results are expected to be quantitative as
with L (from the method’s scope) and the calculated value of
discussed in Annex A1.
A2.2.2 Class 3 consists of results with values les
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