ASTM D4471-10

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 In determining the conformance of the test results using this method to applicable specifications, results shall be rounded off in accordance with the rounding-off method of Practice E29.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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. For specific hazard statements, see Section 8.

General Information

• Status: Historical
• Publication Date: 31-Dec-2009
• ICS: 71.080.30 - Organic nitrogen compounds
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.02 - Oxygenated Aromatics

Relations

• Replaces: ASTM D4471-00(2004) - Standard Test Method for Pyridine Bases in Cresylic Acid by Direct Titration
• Effective Date: 01-Jan-2010

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4471 − 10
Standard Test Method for
1
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* 2.2 Other Document:
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
1.1 This test method covers the determination of pyridine
3
1910.1200
and other basic nitrogen impurities in crude and refined
cresylic acids streams, including mixtures.
3. Terminology
1.2 Thistestmethodisapplicableforpyridinebaselevelsof
3.1 For definitions of terms used in this test method see
0.001 % to 0.5 %.
Terminology D4790.
1.3 In determining the conformance of the test results using
4. Summary of Test Method
this method to applicable specifications, results shall be
rounded off in accordance with the rounding-off method of
4.1 This test method is a direct, nonaqueous titration tech-
Practice E29.
nique utilizing perchloric acid in acetic acid as titrant and the
cresylic acid itself as titration solvent. Endpoints may be
1.4 The values stated in SI units are to be regarded as
established potentiometrically as well as by indicator so that
standard. No other units of measurement are included in this
the method is applicable to highly colored as well as lighter
standard.
colored materials. This test method will detect basic compo-
1.5 This standard does not purport to address all of the
nents other than pyridine bases should they be present. All
safety concerns, if any, associated with its use. It is the
basic compounds detected by this procedure are calculated and
responsibility of the user of this standard to establish appro-
expressed as percent pyridine.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific hazard
5. Significance and Use
statements, see Section 8.
5.1 The pyridine base content of cresylic acids is important
in certain applications. This test method may be used as a tool
2. Referenced Documents
for quality control and specification purposes by producers and
2
2.1 ASTM Standards:
users.
D3852 Practice for Sampling and Handling Phenol, Cresols,
and Cresylic Acid
6. Apparatus
D4790 Terminology ofAromatic Hydrocarbons and Related
6.1 Titrimeter or pH meter, equipped with half cell or
Chemicals
combination glass pH and Ag/AgCl reference electrodes. The
D6809 Guide for Quality Control and Quality Assurance
pair of electrodes shall be mounted to extend well below the
Procedures for Aromatic Hydrocarbons and Related Ma-
liquid level. Storage in water between titrations is essential
terials
because prolonged immersion in nonaqueous medium signifi-
E29 Practice for Using Significant Digits in Test Data to
cantly deadens response.
Determine Conformance with Specifications
6.2 Buret, 50-mL capacity.
6.3 Magnetic Stirrer, with TFE-fluorocarbon or glass cov-
ered stirring bar.
1
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
6.4 Autotitration Equipment may be used if available.
Subcommittee D16.02 on Oxygenated Aromatics.
Current edition approved Jan. 1, 2010. Published January 2010. Originally
7. Reagents
approved in 1985. Last previous edition approved in 2004 as D4471 – 00 (2004).
DOI: 10.1520/D4471-10.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
3
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.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D4471 − 10
7.1 Purity of Reagents—Reagent grade chemicals shall be 10.2.2 Potentiometric—The electrodes are inserted into the
used in all tests. Unless otherwise indicated, it is intended that specimen and the observed potentials are plotted as a function
all reagents shall conform to the specifications of the Commit- of the titrant volume consumed. The point where∆E/∆V is the
tee onAnalytical Reagents of theAmerican Chemical Society, greatest is taken as the endpoint.
4
where such specifications are available. Other grades may be
10.3 Repeat 10.1 through 10.2, but with no specimen to
used, provided it is first ascertained that the reagent
...

This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D4471–00(Reapproved2004) Designation: D4471 – 10
Standard Test Method for
1
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*
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 %.
1.3The 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
1.3 In determining the conformance of the test results using this method to applicable specifications, results shall be rounded
off in accordance with the rounding-off method of Practice E29.
1.4
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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. For specific hazard statements, see Section 8.
2. Referenced Documents
2
2.1 ASTM Standards:
D3852 Practice for Sampling and Handling Phenol, Cresols, and Cresylic Acid
D4790 Terminology of Aromatic Hydrocarbons and Related Chemicals
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
2.2 Other Document:
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.1200
3
OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.1200
3. Terminology
3.1 For definitions of terms used in this test method see Terminology D4790.
4. Summary of Test Method
4.1 This test method is a direct, nonaqueous titration technique utilizing perchloric acid in acetic acid as titrant and the cresylic
acid itself as titration solvent. Endpoints may be established potentiometrically as well as by indicator so that the method is
applicable to highly colored as well as lighter colored materials.This test method will detect basic components other than pyridine
bases should they be present. All basic compounds detected by this procedure are calculated and expressed as percent pyridine.
5. 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.
1
This test method is under the jurisdiction ofASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee
D16.02 on Oxygenated Aromatics.
Current edition approved JuneJan. 1, 2004.2010. Published June 2004.January 2010. Originally approved in 1985. Last previous edition approved in 20002004 as
D4471 – 00 (2004). DOI: 10.1520/D4471-00R04.10.1520/D4471-10.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from U.S. Government Printing Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D4471 – 10
6. Apparatus
6.1 Titrimeter or pH meter,equippedwithhalfcellorcombinationglasspHandcalomelAg/AgClreferenceelectrodes.Thepair
of electrodes shall be mounted to extend well below the liquid level. Storage in water between titrations is essential because
prolonged immersion in nonaqueous medium significantly deadens response.
6.2 Buret, 50-mL capacity.
6.3 Magnetic Stirrer,
...