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ASTM D4471-00

(Test Method)

Standard Test Method for Pyridine Bases in Cresylic Acid by Direct Titration

Standard Test Method for Pyridine Bases in Cresylic Acid by Direct Titration

SCOPE
1.1 This test method covers the determination of pyridine and other basic nitrogen impurities in crude and refined cresylic acids streams, including mixtures.  
1.2 This test method is applicable for pyridine base levels of 0.001% to 0.5%.
1.3 The following applies to all specified limits in this standard: For purposes of determining conformance with this standard, an observed value or a calculated value shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E29.  
1.4 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. For specific hazard statements, see Section 7.

General Information

Status
Historical
Publication Date
09-Jan-2000
ICS
71.080.30 - Organic nitrogen compounds
Technical Committee
D16 - Aromatic, Industrial, Specialty and Related Chemicals
Drafting Committee
D16.02 - Oxygenated Aromatics
Current Stage
Ref Project

Relations

Replaced By
ASTM D4471-00(2004) - Standard Test Method for Pyridine Bases in Cresylic Acid by Direct Titration
Effective Date
01-Jun-2004

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ASTM D4471-00 - Standard Test Method for Pyridine Bases in Cresylic Acid by Direct TitrationASTM D4471-00 - Standard Test Method for Pyridine Bases in Cresylic Acid by Direct Titration
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ASTM D4471-00 - Standard Test Method for Pyridine Bases in Cresylic Acid by Direct Titration
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 4471 – 00
Standard Test Method for
Pyridine Bases in Cresylic Acid by Direct Titration
This standard is issued under the fixed designation D 4471; 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 4. Summary of Test Method
1.1 This test method covers the determination of pyridine 4.1 This test method is a direct, nonaqueous titration tech-
and other basic nitrogen impurities in crude and refined nique utilizing perchloric acid in acetic acid as titrant and the
cresylic acids streams, including mixtures. cresylic acid itself as titration solvent. Endpoints may be
1.2 This test method is applicable for pyridine base levels of established potentiometrically as well as by indicator so that
0.001 % to 0.5 %. the method is applicable to highly colored as well as lighter
1.3 The following applies to all specified limits in this colored materials. This test method will detect basic compo-
standard: For purposes of determining conformance with this nents other than pyridine bases should they be present. All
standard, an observed value or a calculated value shall be basic compounds detected by this procedure are calculated and
rounded off “to the nearest unit” in the last right-hand digit expressed as percent pyridine.
used in expressing the specification limit, in accordance with
5. Significance and Use
the rounding-off method of Practice E 29.
5.1 The pyridine base content of cresylic acids is important
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the in certain applications. This test method may be used as a tool
for quality control and specification purposes by producers and
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- users.
bility of regulatory limitations prior to use. For specific hazard
6. Apparatus
statements, see Section 8.
6.1 Titrimeter or pH meter, equipped with glass and calomel
2. Referenced Documents
electrodes. The pair of electrodes shall be mounted to extend
2.1 ASTM Standards: well below the liquid level. Storage in water between titrations
D 3852 Practice for Sampling and Handling Phenol and is essential because prolonged immersion in nonaqueous me-
dium significantly deadens response.
Cresylic Acid
D 4790 Terminology of Aromatic Hydrocarbons and Re- 6.2 Buret, 50-mL capacity.
6.3 Magnetic Stirrer, with TFE-fluorocarbon or glass cov-
lated Chemicals
E 29 Practice for Using Significant Digits in Test Data to ered stirring bar.
6.4 Autotitration Equipment may be used if available.
Determine Conformance with Specifications
2.2 Other Document:
7. Reagents
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
7.1 Purity of Reagents—Reagent grade chemicals shall be
1910.1200
used in all tests. Unless otherwise indicated, it is intended that
3. Terminology
all reagents shall conform to the specifications of the Commit-
3.1 For definitions of terms used in this test method see tee on Analytical Reagents of the American Chemical Society,
where such specifications are available. Other grades may be
Terminology D 4790.
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
This test method is under the jurisdiction of ASTM Committee D16 on accuracy of the determination.
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
Subcommittee D16.02 on Oxygenated Aromatics.
Current edition approved Jan. 10, 2000. Published March 2000. Originally Reagent Chemicals, American Chemical Society Specifications, American
published as D 4471 – 85. Last previous edition D 4471 – 94. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Annual Book of ASTM Standards, Vol 06.04. listed by the American Chemical Society, see Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 14.02. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Available from Superintendent of Documents, U.S. Government Printing and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Office, Washington, DC 20402. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 4471
7.2 Perchloric Acid Titrant (0.02 N in glacial acetic acid)— 10.3 Repeat 10.1 through 10.2, but with no specimen to
Add 1.8 mL of 70 % perchloric acid (HClO ) to 1 L of glacial obtain a reagent blank when titration solvent is used.
...

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Standard Test Method for Pyridine Bases in Cresylic Acid by Direct Titration

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5.1 The pyridine base content of cresylic acids is important in certain applications. This test method may be used as a tool for quality control and specification purposes by producers and users.
SCOPE
1.1 This test method covers the determination of pyridine and other basic nitrogen impurities in crude and refined cresylic acids streams, including mixtures.  
1.2 This test method is applicable for pyridine base levels of 0.001 % to 0.5 %.  
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