ASTM D4821-01a
(Guide)Standard Guide for Carbon Black—Validation of Test Method Precision and Bias
Standard Guide for Carbon Black—Validation of Test Method Precision and Bias
SCOPE
1.1 This guide covers a procedure for using ASTM Standard Reference Blacks (SRBs) to continuously monitor the precision of those carbon black test methods for which standard values have been established. It also offers guidelines for trouble-shooting various test methods.
1.2 This guide establishes the limits within which the statistical calibration procedure of Practice D3324 shall be applied and establishes the limits for an out-of-calibration condition beyond which the statistical calibration procedure of Practice D3324 shall not be applied.
1.3 This guide uses statistical control chart methodology as discussed in STP-15-D to determine if a laboratory's test results differ significantly from the accepted values of the SRBs and provides a format for reporting test data for specified tests on the SRB blacks.
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D 4821 – 01a
Standard Guide for
Carbon Black—Validation of Test Method Precision and
1
Bias
This standard is issued under the fixed designation D 4821; 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.
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1. Scope Nitrogen Adsorption
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D 3265 Test Method for Carbon Black—Tint Strength
1.1 This guide covers a procedure for using ASTM Standard
2
D 3324 Practice for Carbon Black—Improving Test Repro-
Reference Blacks (SRBs) to continuously monitor the preci-
4
ducibility Using ASTM Reference Blacks
sion of those carbon black test methods for which standard
D 3493 Test Method for Carbon Black—Oil Absorption
values have been established. It also offers guidelines for
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Number of Compressed Sample
trouble-shooting various test methods.
D 3765 Test Method for Carbon Black—CTAB (Cetyltrim-
1.2 This guide establishes the limits within which the
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ethylammonium Bromide) Surface Area
statistical calibration procedure of Practice D 3324 shall be
D 4820 Test Methods for Carbon Black—Surface Area by
applied and establishes the limits for an out-of-calibration
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Multipoint B. E. T. Nitrogen Adsorption
condition beyond which the statistical calibration procedure of
D 5816 Test Methods for Carbon Black—External Surface
Practice D 3324 shall not be applied.
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Area by Multipoint Nitrogen Adsorption
1.3 This guide uses statistical control chart methodology as
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discussed in STP-15-D to determine if a laboratory’s test
3. Significance and Use
results differ significantly from the accepted values of the
3.1 One of the major causes of poor test precision is the lack
SRBs and provides a format for reporting test data for specified
of calibration or standardization of instruments, apparatus,
tests on the SRB blacks.
reagents, and technique among laboratories.
1.4 The values stated in SI units are to be regarded as the
3.2 In addition to the calibration of a test method by
standard. The values given in parentheses are for information
physicochemical means, Practice D 3324 describes a statistical
only.
method for achieving calibration of a test method.
1.5 This standard does not purport to address all of the
3.3 This guide outlines the use of control charts to graphi-
safety concerns, if any, associated with its use. It is the
cally present calibration test data determined for the ASTM
responsibility of the user of this standard to establish appro-
SRBs for those test methods given in Section 2. These control
priate safety and health practices and determine the applica-
charts shall be used to validate the testing precision and bias of
bility of regulatory limitations prior to use.
an individual laboratory.
2. Referenced Documents
4. Procedure
2.1 ASTM Standards:
4.1 Select six SRBs from the SRB 4, SRB 5, or SRB 6 series
D 1510 Test Method for Carbon Black—Iodine Adsorption
4 to cover the range of interest, being sure to include one each of
Number
the A, B, C, D, E, and F (see Note 1) SRBs. Do not mix
D 2414 Test Method for Carbon Black—Oil Absorption
4 materials from different SRB sets. For example, do not use A,
Number
B, and C from set 4 with D, E, and F from set 5. This is
D 3037 Test Methods for Carbon Black—Surface Area by
especially critical for DBP absorptometer calibration. An
absorptometer calibrated with F5 (or F5A) must be checked
with other members of the 5 set. Likewise, an absorptometer
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This guide is under the jurisdiction of ASTM Committee D24 on Carbon Black
calibrated with F6 must be checked with other members of the
and is the direct responsibility of Subcommittee D24.61 on Carbon Black Sampling
6 set.
and Statistical Analysis.
Current edition approved Dec. 10, 2001. Published February 2002. Originally
NOTE 1—SRB 4 and SRB 5 are depleted and not commercially
published as D4821 – 88. Last previous edition D4821 – 01.
available. However, they are still in use in some laboratories.
2
Standard Reference Blacks are available from Laboratory Standards & Tech-
nologies, Inc., 227 Somerset St., Borger, TX 79007. Phone/fax: (806) 273-3006.
E-mail: jwbal@infinitytx.net.
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Symposium on Manual on Presentation of Data and Control Chart Analysis, Discontinued 1999. See 1998 Annual Book of ASTM Standards, Vol 09.01.
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ASTM STP 15D, ASTM, 1976. Discontinued 2000; replaced by Test Method D 6556; see 1999 Annual Book of
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Annual Book of ASTM Standards, Vol 09.01. ASTM Standards, Vol 09.01.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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