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 troubleshooting various test methods.
1.2 This guide establishes the x-chart control limits to be used when continuously monitoring those tests listed in Section . Alternatively, these control limits may be used as a basis for comparison to testing precision computed within a laboratory.
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.
1.4 This guide provides a statistical procedure for improving test reproducibility when a laboratory cannot physically calibrate its apparatus to obtain the standard values of the ASTM SRBs, within the ranges given in the precision statement of the test method.
1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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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Historical
Publication Date
14-Dec-2005
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ASTM D4821-05 - Standard Guide for Carbon Black—Validation of Test Method Precision and Bias
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D4821–05
Standard Guide for
Carbon Black—Validation of Test Method Precision and
1
Bias
This standard is issued under the fixed designation D4821; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope D1510 Test Method for Carbon Black—IodineAdsorption
Number
1.1 ThisguidecoversaprocedureforusingASTMStandard
2
D1513 Test Method for Carbon Black, Pelleted—Pour
Reference Blacks (SRBs) to continuously monitor the preci-
Density
sion of those carbon black test methods for which standard
D1765 Classification System for Carbon Blacks Used in
values have been established. It also offers guidelines for
Rubber Products
troubleshooting various test methods.
D2414 Test Method for Carbon Black—Oil Absorption
1.2 This guide establishes the x-chart control limits to be
Number (OAN)
usedwhencontinuouslymonitoringthosetestslistedinSection
D3037 Test Methods for Carbon Black-Surface Area by
2.Alternatively, these control limits may be used as a basis for
5
Nitrogen Adsorption
comparison to testing precision computed within a laboratory.
D3191 Test Methods for Carbon Black in SBR (Styrene-
1.3 This guide uses statistical control chart methodology as
3
Butadiene Rubber)—Recipe and Evaluation Procedures
discussed in STP-15-D to determine if a laboratory’s test
D3192 Test Methods for Carbon Black Evaluation in NR
results differ significantly from the accepted values of the
(Natural Rubber)
SRBs.
D3265 Test Method for Carbon Black—Tint Strength
1.4 This guide provides a statistical procedure for improv-
D3493 Test Method for Carbon Black—Oil Absorption
ing test reproducibility when a laboratory cannot physically
Number of Compressed Sample (COAN)
calibrate its apparatus to obtain the standard values of the
D3765 Test Method for Carbon Black—CTAB (Cetyltrim-
ASTM SRBs, within the ranges given in the precision state-
ethylammonium Bromide) Surface Area
ment of the test method.
D4820 Test Methods for Carbon Black—Surface Area by
1.5 The values stated in SI units are to be regarded as the
Multipoint B.E.T. Nitrogen Adsorption (Discontinued
standard. The values given in parentheses are for information
5
2000) Replaced by D 6556
only.
D5816 Test Methods for Carbon Black—External Surface
1.6 This standard does not purport to address all of the
Area by Multipoint Nitrogen Adsorption (Discontinued
safety concerns, if any, associated with its use. It is the
5
2000) Replaced by D 6556
responsibility of the user of this standard to establish appro-
D6556 Test Method for Carbon Black—Total and External
priate safety and health practices and determine the applica-
Surface Area by Nitrogen Adsorption
bility of regulatory limitations prior to use.
3. Significance and Use
2. Referenced Documents
4 3.1 Oneofthemajorcausesofpoortestprecisionisthelack
2.1 ASTM Standards:
of calibration or standardization of instruments, apparatus,
reagents, and technique among laboratories. The sum of all
1
ThisguideisunderthejurisdictionofASTMCommitteeD24onCarbonBlack
sources of testing error is unique for an individual laboratory.
andisthedirectresponsibilityofSubcommitteeD24.61onCarbonBlackSampling
A least-squares regression of a laboratory’s actual test values
and Statistical Analysis.
for reference materials to the established mean values will
Current edition approved Dec. 15, 2005. Published January 2006. Originally
result in a unique least-squares regression line (and equation)
approved in 1988. Last previous edition approved in 2004 as D4821–04.
2
Standard Reference Blacks are available from Laboratory Standards & Tech-
for that laboratory. Generally, there are two reasons for using
nologies, Inc., 227 Somerset St., Borger, TX 79007.
the SRBs in testing: (1) to monitor testing performance (see
3
Symposium on Manual on Presentation of Data and Control Chart Analysis,
Section4)toensurethatnosystematicerrororbiasisaffecting
ASTM STP 15D, ASTM International, 1976.
4
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
Standards volume information, refer to the standard’s Document Summary page on
5
the ASTM website. Withdrawn.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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D4821–05
TABLE 1 SRB 6 Control Chart Limits
NOTE—See Test Method D3765 for an algorithm to calculate CTAB values from the STSA values for the SRB 6 set.
Test Property ASTM Standard SRB Target Value 3 s Value Lower Control Limit Upper Control Limit
Iodine D
...

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