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ASTM D4471-00(2004)

(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

SIGNIFICANCE AND USE
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%.
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
31-May-2004
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

Replaces
ASTM D4471-00 - Standard Test Method for Pyridine Bases in Cresylic Acid by Direct Titration
Effective Date
01-Jun-2004
Replaced By
ASTM D4471-10 - Standard Test Method for Pyridine Bases in Cresylic Acid by Direct Titration
Effective Date
01-Jan-2010

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ASTM D4471-00(2004) - Standard Test Method for Pyridine Bases in Cresylic Acid by Direct TitrationASTM D4471-00(2004) - Standard Test Method for Pyridine Bases in Cresylic Acid by Direct Titration
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ASTM D4471-00(2004) - 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D4471–00(Reapproved2004)
Standard Test Method for
Pyridine Bases in Cresylic Acid by Direct Titration
This standard is issued under the fixed designation D4471; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope OSHA Regulations,29 CFR, paragraphs 1910.1000 and
1910.1200
1.1 This test method covers the determination of pyridine
and other basic nitrogen impurities in crude and refined
3. Terminology
cresylic acids streams, including mixtures.
3.1 For definitions of terms used in this test method see
1.2 Thistestmethodisapplicableforpyridinebaselevelsof
Terminology D4790.
0.001 % to 0.5 %.
1.3 The following applies to all specified limits in this
4. Summary of Test Method
standard: For purposes of determining conformance with this
4.1 This test method is a direct, nonaqueous titration tech-
standard, an observed value or a calculated value shall be
nique utilizing perchloric acid in acetic acid as titrant and the
rounded off “to the nearest unit” in the last right-hand digit
cresylic acid itself as titration solvent. Endpoints may be
used in expressing the specification limit, in accordance with
established potentiometrically as well as by indicator so that
the rounding-off method of Practice E29.
the method is applicable to highly colored as well as lighter
1.4 This standard does not purport to address all of the
colored materials. This test method will detect basic compo-
safety concerns, if any, associated with its use. It is the
nents other than pyridine bases should they be present. All
responsibility of the user of this standard to establish appro-
basic compounds detected by this procedure are calculated and
priate safety and health practices and determine the applica-
expressed as percent pyridine.
bility of regulatory limitations prior to use. For specific hazard
statements, see Section 8.
5. Significance and Use
5.1 The pyridine base content of cresylic acids is important
2. Referenced Documents
2 in certain applications. This test method may be used as a tool
2.1 ASTM Standards:
for quality control and specification purposes by producers and
D3852 Practice for Sampling and Handling Phenol,
users.
Cresols, and Cresylic Acid
D4790 TerminologyofAromaticHydrocarbonsandRelated
6. Apparatus
Chemicals
6.1 Titrimeter or pH meter,equippedwithglassandcalomel
E29 Practice for Using Significant Digits in Test Data to
electrodes. The pair of electrodes shall be mounted to extend
Determine Conformance with Specifications
well below the liquid level. Storage in water between titrations
2.2 Other Document:
is essential because prolonged immersion in nonaqueous me-
dium significantly deadens response.
This test method is under the jurisdiction of ASTM Committee D16 on
6.2 Buret, 50-mL capacity.
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
6.3 Magnetic Stirrer, with TFE-fluorocarbon or glass cov-
Subcommittee D16.02 on Oxygenated Aromatics.
ered stirring bar.
Current edition approved June 1, 2004. Published June 2004. Originally
approved in 1985. Last previous edition approved in 2000 as D4471 – 00. DOI: 6.4 Autotitration Equipment may be used if available.
10.1520/D4471-00R04.
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 AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
the ASTM website. 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4471–00 (2004)
7. Reagents 10.2.1 Indicator—Afewdropsofquinaldineredindicatoris
added to the solution. The titration is terminated when the red
7.1 Purity of Reagents—Reagent grade chemicals shall be
color disappears and the color of the sample returns to its
used in all tests. Unless otherwise indicated, it is intended that
original hue.
all reagents shall conform to the specifications of the Commit-
10.2.2 Potentiometric—The electrodes are inserted into the
tee onAnalytical Reagents of theAmerican Chemical Society,
specimen and the observed potentials are plotted as a function
where such specifications are available. Other grades may be
of the titrant volume consumed. The point where DE/DV is the
used, provided it is first ascertained that the reagent is of
greatest is taken as the endpoint.
sufficiently high purity to permit its use without lessening the
10.3 Repeat 10.1 through 10.2, but with no specimen to
accuracy of the determination.
obtain a reagent blank when titration solvent i
...

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

SIGNIFICANCE AND USE
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
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