ASTM D4821-03

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.
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: 09-Jan-2003
• 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 D4821-01a - Standard Guide for Carbon Black—Validation of Test Method Precision and Bias
• Effective Date: 10-Jan-2003
• Replaced By: ASTM D4821-03a - Standard Guide for Carbon Black—Validation of Test Method Precision and Bias
• Effective Date: 01-Dec-2003
• Referred By: ASTM D1510-23 - Standard Test Method for Carbon Black—Iodine Adsorption Number
• Effective Date: 10-Jan-2003
• Referred By: ASTM D8043-20 - Standard Guide for Carbon Black—Shelf Life
• Effective Date: 10-Jan-2003
• Referred By: ASTM D6915-23 - Standard Practice for Carbon Black—Evaluation of Standard Reference Blacks
• Effective Date: 10-Jan-2003
• Referred By: ASTM D3493-21 - Standard Test Method for Carbon Black—Oil Absorption Number of Compressed Sample (COAN)
• Effective Date: 10-Jan-2003
• Referred By: ASTM D3265-23 - Standard Test Method for Carbon Black—Tint Strength
• Effective Date: 10-Jan-2003
• Referred By: ASTM D8466-22 - Standard Guide for Recovered Carbon Black—Carbon Black Test Methods for Testing rCB
• Effective Date: 10-Jan-2003
• Referred By: ASTM D2414-23 - Standard Test Method for Carbon Black—Oil Absorption Number (OAN)
• Effective Date: 10-Jan-2003

Standards Content (Sample)

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: D 4821 – 03
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.
1. Scope D 1765 Classification System for Carbon Blacks Used in
4
Rubber Products
1.1 This guide covers a procedure for using ASTM Standard
2
D 2414 Test Method for Carbon Black—Oil Absorption
Reference Blacks (SRBs) to continuously monitor the preci-
4
Number
sion of those carbon black test methods for which standard
4
D 3265 Test Method for Carbon Black—Tint Strength
values have been established. It also offers guidelines for
D 3493 Test Method for Carbon Black—Oil Absorption
troubleshooting various test methods.
4
Number of Compressed Sample
1.2 This guide establishes the x-chart control limits to be
D 6556 Test Methods for Carbon Black—Total and Exter-
used when continuously monitoring those tests listed in Section
4
nal Surface Area by Nitrogen Adsorption
2. Alternatively, these control limits may be used as a basis for
comparison to testing precision computed within a laboratory.
3. Significance and Use
1.3 This guide uses statistical control chart methodology as
3 3.1 One of the major causes of poor test precision is the lack
discussed in STP-15-D to determine if a laboratory’s test
of calibration or standardization of instruments, apparatus,
results differ significantly from the accepted values of the
reagents, and technique among laboratories. The sum of all
SRBs.
sources of testing error is unique for an individual laboratory.
1.4 This guide provides a statistical procedure for improv-
A least-squares regression of a laboratory’s actual test values
ing test reproducibility when a laboratory cannot physically
for reference materials to the established mean values will
calibrate its apparatus to obtain the standard values of the
result in a unique least-squares regression line (and equation)
ASTM SRBs, within the ranges given in the precision state-
for that laboratory. Generally, there are two reasons for using
ment of the test method.
the SRBs in testing: (1) to monitor testing performance (see
1.5 The values stated in SI units are to be regarded as the
Section 4) to ensure that no systematic error or bias is affecting
standard. The values given in parentheses are for information
the test results, or (2) to establish a statistical calibration (see
only.
Section 5) when the correction of assignable causes (see
1.6 This standard does not purport to address all of the
Section 6) does not yield in-control test results.
safety concerns, if any, associated with its use. It is the
3.2 In addition to the calibration of a test method by
responsibility of the user of this standard to establish appro-
physicochemical means, a statistical method for achieving
priate safety and health practices and determine the applica-
calibration of a test method is presented.
bility of regulatory limitations prior to use.
3.3 This guide outlines the use of control charts to graphi-
2. Referenced Documents cally present calibration test data determined for the ASTM
SRBs for those test methods given in Section 2. All laborato-
2.1 ASTM Standards:
ries are encouraged to utilize statistical control charts and the
D 1510 Test Method for Carbon Black—Iodine Adsorption
4
SRBs because this allows a comparison of testing precision
Number
within a laboratory to the “industry average” values found in
Table 1.
1
This guide is under the jurisdiction of ASTM Committee D24 on Carbon Black 3.4 The techniques of this guide can be used to continuously
and is the direct responsibility of Subcommittee D24.61 on Carbon Black Sampling
monitor testing execution and precision for other tests that are
and Statistical Analysis.
not listed in Section 2 or for materials that fall outside the range
Current edition approved Jan. 10, 2003. Published February 2003. Originally
of the SRBs for those tests listed in Section 2. In these cases,
approved in 1988. Last previous edition approved in 2001 D 4821 – 01a.
2
Standard Reference Blacks are available from Laboratory Standards & Tech-
each laboratory will have to establish the applicable mean and
nologies, Inc., 227 Somerset St., Borger, TX 79007. Phone/fax: [phone].
control limit values for the “local reference.” The monitoring
E-mail: jwbal@infinitytx.net.
3 will then consist of a comparison of present test results for the
Symposium on Manual on Presentation of Data and Control Chart Analysis,
ASTM STP 15D, ASTM, 1976.
4
Annual Book of ASTM Standards, Vol 09.01.
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