ASTM D4821-04

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 2. 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.
1.6 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.

General Information

• Status: Historical
• Publication Date: 31-May-2004
• ICS: 83.040.20 - Rubber compounding ingredients
• Technical Committee: D24 - Carbon Black
• Drafting Committee: D24.61 - Carbon Black Sampling and Statistical Analysis

Relations

• Replaces: ASTM D4821-03a - Standard Guide for Carbon Black—Validation of Test Method Precision and Bias
• Effective Date: 01-Jun-2004
• Replaced By: ASTM D4821-05 - Standard Guide for Carbon Black—Validation of Test Method Precision and Bias
• Effective Date: 15-Dec-2005
• Referred By: ASTM D8043-20 - Standard Guide for Carbon Black—Shelf Life
• Effective Date: 01-Jun-2004
• Referred By: ASTM D3265-23 - Standard Test Method for Carbon Black—Tint Strength
• Effective Date: 01-Jun-2004
• Referred By: ASTM D8466-22 - Standard Guide for Recovered Carbon Black—Carbon Black Test Methods for Testing rCB
• Effective Date: 01-Jun-2004
• Referred By: ASTM D2414-23 - Standard Test Method for Carbon Black—Oil Absorption Number (OAN)
• Effective Date: 01-Jun-2004
• Referred By: ASTM D3493-21 - Standard Test Method for Carbon Black—Oil Absorption Number of Compressed Sample (COAN)
• Effective Date: 01-Jun-2004
• Referred By: ASTM D6915-23 - Standard Practice for Carbon Black—Evaluation of Standard Reference Blacks
• Effective Date: 01-Jun-2004
• Referred By: ASTM D1510-23 - Standard Test Method for Carbon Black—Iodine Adsorption Number
• Effective Date: 01-Jun-2004

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:D4821–04
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 Den-
Reference Blacks (SRBs) to continuously monitor the preci-
sity
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
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
5
Multipoint B.E.T. Nitrogen Adsorption
standard. The values given in parentheses are for information
D5816 Test Methods for Carbon Black-External Surface
only.
5
Area by Multipoint Nitrogen Adsorption
1.6 This standard does not purport to address all of the
D6556 Test Method for Carbon Black—Total and External
safety concerns, if any, associated with its use. It is the
Surface Area by Nitrogen Adsorption
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
3. Significance and Use
bility of regulatory limitations prior to use.
3.1 Oneofthemajorcausesofpoortestprecisionisthelack
2. Referenced Documents of calibration or standardization of instruments, apparatus,
4 reagents, and technique among laboratories. The sum of all
2.1 ASTM Standards:
sources of testing error is unique for an individual laboratory.
A least-squares regression of a laboratory’s actual test values
1
for reference materials to the established mean values will
ThisguideisunderthejurisdictionofASTMCommitteeD24onCarbonBlack
andisthedirectresponsibilityofSubcommitteeD24.61onCarbonBlackSampling
result in a unique least-squares regression line (and equation)
and Statistical Analysis.
for that laboratory. Generally, there are two reasons for using
Current edition approved June 1, 2004. Published June 2004. Originally
the SRBs in testing: (1) to monitor testing performance (see
approved in 1988. Last previous edition approved in 2003 as D4821–03a.
2
Standard Reference Blacks are available from Laboratory Standards & Tech- Section4)toensurethatnosystematicerrororbiasisaffecting
nologies, Inc., 227 Somerset St., Borger, TX 79007.
the test results, or (2) to establish a statistical calibration (see
3
Symposium on Manual on Presentation of Data and Control Chart Analysis,
Section 5) when the correction of assignable causes (see
ASTM STP 15D, ASTM International, 1976.
4
Section 6) does not yield in-control test results.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. 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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D4821–04
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 Propert
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