ASTM D1631-10
(Test Method)Standard Test Method for Water in Phenol and Related Materials by the Iodine Reagent Method
Standard Test Method for Water in Phenol and Related Materials by the Iodine Reagent Method
SIGNIFICANCE AND USE
This test method is particularly useful for determining small amounts of water in hygroscopic materials. This test method is suitable for setting specifications on materials referenced in the scope. It may also be used as an internal quality control tool and in development or research work.
SCOPE
1.1 This test method covers the determination of water in phenol and related materials such as cresols, xylenols, naphthalene, pyridine, and quinoline.
1.2 This test method has been found applicable to a variety of materials varying in water content from 100 mg/kg to solutions containing a relatively high percent of water.
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 9.
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Designation: D1631 − 10
Standard Test Method for
Water in Phenol and Related Materials by the Iodine
1
Reagent Method
This standard is issued under the fixed designation D1631; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope* D6809 Guide for Quality Control and Quality Assurance
Procedures for Aromatic Hydrocarbons and Related Ma-
1.1 This test method covers the determination of water in
terials
phenol and related materials such as cresols, xylenols,
E29 Practice for Using Significant Digits in Test Data to
naphthalene, pyridine, and quinoline.
Determine Conformance with Specifications
3
1.2 This test method has been found applicable to a variety
2.2 Other Document:
of materials varying in water content from 100 mg/kg to
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
solutions containing a relatively high percent of water.
1910.1200
1.3 In determining the conformance of the test results using
3. Terminology
this method to applicable specifications, results shall be
rounded off in accordance with the rounding-off method of
3.1 See Terminology D4790 for definition of terms used in
Practice E29. this test method.
1.4 The values stated in SI units are to be regarded as
4. Summary of Test Method
standard. No other units of measurement are included in this
4.1 When solutions of iodine in methanol and of sulfur
standard.
dioxide in pyridine are mixed in the presence of water, the
1.5 This standard does not purport to address all of the
following reaction occurs:
safety concerns, if any, associated with its use. It is the
→
I 1SO 1H O 2HI1SO (1)
responsibility of the user of this standard to establish appro- 2 2 2 ← 3
priate safety and health practices and determine the applica-
4.1.1 Sufficientpyridineispresentinthereagenttoconsume
bility of regulatory limitations prior to use. For specific hazard
the hydriodic acid and sulfur trioxide:
statements, see Section 9.
2. Referenced Documents
2
2.1 ASTM Standards:
D1364 Test Method for Water in Volatile Solvents (Karl
Fischer Reagent Titration Method)
D3437 Practice for Sampling and Handling Liquid Cyclic
Products
4.1.2 The pyridine sulfur trioxide salt reacts with the
D3852 Practice for Sampling and Handling Phenol, Cresols,
methanol, this preventing a second mole of water from being
and Cresylic Acid
consumed:
D4790 Terminology ofAromatic Hydrocarbons and Related
Chemicals
1
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
Subcommittee D16.02 on Oxygenated Aromatics.
Current edition approved Jan. 1, 2010. Published January 2010. Originally
4.2 Whenthepyridinesolutioncontainswaterandthesulfur
approved in 1959. Last previous edition approved in 2004 as D1631 – 99 (2004).
dioxide is titrated with iodine in methanol solution, the
DOI: 10.1520/D1631-10.
2
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
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 ----------------------
D1631 − 10
4
platinum electrodes remain polarized until all the water reacts. specifications are available. Other grades may be used, pro-
A slight excess of iodine depolarizes the electrodes, allowing vided it is first ascertained that the reagent is of sufficiently
current to flow through the microammeter which indicates the high purity to permit its use without lessening the accuracy of
end point. the determination.
8.2 Iodine Solution—Dissolve 150 g of iodine (I ) crystals
2
5. Significance and Use
in 3 Lof anhydrous methanol. Place the solution in the reagent
5.1 This test method is particularly useful for determining
bottle connected to the buret as shown in Fig. 1.
small amounts of water in hygroscopic materials. This test
8.3 Methanol, anhydrous, containing less than 0.05 % wa-
method is suitable for setting specifications on materials
ter.
referenced in the scope. It may also be used as an internal
8.4 Pyridine Solution—Place 4000 mL of refined grade
quality control tool and in development or research work.
pyridin
...
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:D1631–99(Reapproved2004) Designation:D1631–10
Standard Test Method for
Water in Phenol and Related Materials by the Iodine
1
Reagent Method
This standard is issued under the fixed designation D1631; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope*
1.1 This test method covers the determination of water in phenol and related materials such as cresols, xylenols, naphthalene,
pyridine, and quinoline.
1.2 This test method has been found applicable to a variety of materials varying in water content from 100 mg/kg to solutions
containing a relatively high percent of water.
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 9.
2. Referenced Documents
2
2.1 ASTM Standards:
D1364 Test Method for Water in Volatile Solvents (Karl Fischer Reagent Titration Method)
D3437 Practice for Sampling and Handling Liquid Cyclic Products
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
3
2.2 Other Document:OSHA Regulations, 29CFR, Paragraphs 1910.1000 and 1910.1200
OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.1200
3. Terminology
3.1 See Terminology D4790 for definition of terms used in this test method.
4. Summary of Test Method
4.1 When solutions of iodine in methanol and of sulfur dioxide in pyridine are mixed in the presence of water, the following
reaction occurs:
(1) I 2 1 SO2 1 H2O←→ 2HI 1 SO3
4.1.1 Sufficient pyridine is present in the reagent to consume the hydriodic acid and sulfur trioxide:
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 Aug.Jan. 1, 2004.2010. Published August 2004.January 2010. Originally approved in 1959. Last previous edition approved in 19992004 as
D1631 – 99 (2004). DOI: 10.1520/D1631-99R04.10.1520/D1631-10.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. 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 ----------------------
D1631–10
4.1.2 The pyridine sulfur trioxide salt reacts with the methanol, this preventing a second mole of water from being consumed:
4.2 When the pyridine solution contains water and the sulfur dioxide is titrated with iodine in methanol solution, the platinum
electrodes remain polarized until all the water reacts.Aslight excess of iodine depolarizes the electrodes, allowing current to flow
through the microammeter which indicates the end point.
5. Significance and Use
5.1 This test method is particularly usef
...
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