ASTM D4821-01

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.

General Information

• Status: Historical
• Publication Date: 09-Dec-2001
• 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 D4821-99 - Standard Guide for Carbon Black—Validation of Test Method Precision and Bias
• Effective Date: 10-Dec-2001
• Replaced By: ASTM D4821-01a - Standard Guide for Carbon Black—Validation of Test Method Precision and Bias
• Effective Date: 10-Dec-2001
• Referred By: ASTM D8466-22 - Standard Guide for Recovered Carbon Black—Carbon Black Test Methods for Testing rCB
• Effective Date: 10-Dec-2001
• Referred By: ASTM D1510-23 - Standard Test Method for Carbon Black—Iodine Adsorption Number
• Effective Date: 10-Dec-2001
• Referred By: ASTM D3265-23 - Standard Test Method for Carbon Black—Tint Strength
• Effective Date: 10-Dec-2001
• Referred By: ASTM D6915-23 - Standard Practice for Carbon Black—Evaluation of Standard Reference Blacks
• Effective Date: 10-Dec-2001
• Referred By: ASTM D2414-23 - Standard Test Method for Carbon Black—Oil Absorption Number (OAN)
• Effective Date: 10-Dec-2001
• Referred By: ASTM D8043-20 - Standard Guide for Carbon Black—Shelf Life
• Effective Date: 10-Dec-2001
• Referred By: ASTM D3493-21 - Standard Test Method for Carbon Black—Oil Absorption Number of Compressed Sample (COAN)
• Effective Date: 10-Dec-2001

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 4821 – 01
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.
4
1. Scope ducibility Using ASTM Reference Blacks
D 3493 Test Method for Carbon Black—Oil Absorption
1.1 This guide covers a procedure for using ASTM Standard
4
2
Number of Compressed Sample
Reference Blacks (SRBs) to continuously monitor the preci-
D 3765 Test Method for Carbon Black—CTAB (Cetyltrim-
sion of those carbon black test methods for which standard
4
ethylammonium Bromide) Surface Area
values have been established. It also offers guidelines for
D 4820 Test Methods for Carbon Black—Surface Area by
trouble-shooting various test methods.
5
Multipoint B. E. T. Nitrogen Adsorption
1.2 This guide establishes the limits within which the
D 5816 Test Methods for Carbon Black—External Surface
statistical calibration procedure of Practice D 3324 shall be
5
Area by Multipoint Nitrogen Adsorption
applied and establishes the limits for an out-of-calibration
condition beyond which the statistical calibration procedure of
3. Significance and Use
Practice D 3324 shall not be applied.
3.1 One of the major causes of poor test precision is the lack
1.3 This guide uses statistical control chart methodology as
3 of calibration or standardization of instruments, apparatus,
discussed in STP-15-D to determine if a laboratory’s test
reagents, and technique among laboratories.
results differ significantly from the accepted values of the
3.2 In addition to the calibration of a test method by
SRBs and provides a format for reporting test data for specified
physicochemical means, Practice D 3324 describes a statistical
tests on the SRB blacks.
method for achieving calibration of a test method.
1.4 The values stated in SI units are to be regarded as the
3.3 This guide outlines the use of control charts to graphi-
standard. The values given in parentheses are for information
cally present calibration test data determined for the ASTM
only.
SRBs for those test methods given in Section 2. These control
1.5 This standard does not purport to address all of the
charts shall be used to validate the testing precision and bias of
safety concerns, if any, associated with its use. It is the
an individual laboratory.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Procedure
bility of regulatory limitations prior to use.
4.1 Select six SRBs from the SRB 4 and SRB 5 series to
2. Referenced Documents cover the range of interest, being sure to include one each of
the A, B, C, D, E, and F (see Note 1) SRBs.
2.1 ASTM Standards:
D 1510 Test Method for Carbon Black—Iodine Adsorption
NOTE 1—F-5 will not be available for purchase until F-4 is depleted.
4
Number
4.2 Prepare a control chart for each of the selected SRBs for
D 2414 Test Method for Carbon Black—Oil Absorption
each test method as presented by Part 3 of ASTM STP 15D.
4
Number
4.3 The target values given in Table 1 and Table 2 are the
D 3037 Test Methods for Carbon Black—Surface Area by
nominal SRB values reported in Practice D 3324. Values are
4
Nitrogen Adsorption
used as control chart limits plus or minus three single test
4
D 3265 Test Method for Carbon Black—Tint Strength
repeatability standard deviations as given in the precision
D 3324 Practice for Carbon Black—Improving Test Repro-
section of each applicable test method for the SRB 4s or as
determined during the validation of the SRB 5s.
1
This guide is under the jurisdiction of ASTM Committee D24 on Carbon Black
4.4 Plot the uncorrected values for the selected six SRBs
and is the direct responsibility of Subcommittee D24.61 on Carbon Black Sampling
until a repeatability control limit is exceeded (see Note 2).
and Statistical Analysis.
Perform a retest immediately. If the retest falls outside the
Current edition approved May 10, 2001. Published July 2001. Originally
published as D4821 – 88. Last previous edition D4821 – 99. repeatability control limits, then begin a search for an assign-
2
Standard Reference Blacks are available from Titan Specialties, P. O. Box
able cause. (See Section 5 for a list of assignable causes.) If the
2316, Pampa, TX 79066–2316.
3
Symposium on Manual on Presentation of Data and Control Chart Analysis,
5
ASTM STP 15D, ASTM, 1976. Discontinued 2000; replaced by Test Method D 6556; see 1999 Annual Book of
4
Annual Book of ASTM Standards, Vol 09.01. ASTM Standards, Vol 09.01.
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