ASTM D1631-10(2018)e1

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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Designation: D1631 − 10 (Reapproved 2018)
Standard Test Method for
Water in Phenol and Related Materials by the Iodine
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.
ε NOTE—Section 14 was editorially corrected in February 2018.
1. Scope* 2. Referenced Documents
2.1 ASTM Standards:
1.1 This test method covers the determination of water in
D1364 Test Method for Water in Volatile Solvents (Karl
phenol and related materials such as cresols, xylenols,
Fischer Reagent Titration Method)
naphthalene, pyridine, and quinoline.
D3437 Practice for Sampling and Handling Liquid Cyclic
1.2 This test method has been found applicable to a variety
Products
of materials varying in water content from 100 mg/kg to
D3852 Practice for Sampling and Handling Phenol, Cresols,
solutions containing a relatively high percent of water.
and Cresylic Acid
D4790 Terminology ofAromatic Hydrocarbons and Related
1.3 In determining the conformance of the test results using
Chemicals
this method to applicable specifications, results shall be
D6809 Guide for Quality Control and Quality Assurance
rounded off in accordance with the rounding-off method of
Procedures for Aromatic Hydrocarbons and Related Ma-
Practice E29.
terials
E29 Practice for Using Significant Digits in Test Data to
1.4 The values stated in SI units are to be regarded as
Determine Conformance with Specifications
standard. No other units of measurement are included in this
E691 Practice for Conducting an Interlaboratory Study to
standard.
Determine the Precision of a Test Method
1.5 This standard does not purport to address all of the 3
2.2 Other Document:
safety concerns, if any, associated with its use. It is the
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
responsibility of the user of this standard to establish appro-
1910.1200
priate safety, health, and environmental practices and deter-
3. Terminology
mine the applicability of regulatory limitations prior to use.
For specific hazard statements, see Section 9.
3.1 See Terminology D4790 for definition of terms used in
this test method.
1.6 This international standard was developed in accor-
dance with internationally recognized principles on standard-
4. Summary of Test Method
ization established in the Decision on Principles for the
4.1 When solutions of iodine in methanol and of sulfur
Development of International Standards, Guides and Recom-
dioxide in pyridine are mixed in the presence of water, the
mendations issued by the World Trade Organization Technical
following reaction occurs:
Barriers to Trade (TBT) Committee.
→
I 1SO 1H O 2HI1SO (1)
2 2 2 ← 3
4.1.1 Sufficientpyridineispresentinthereagenttoconsume
the hydriodic acid and sulfur trioxide:
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This test method is under the jurisdiction of ASTM Committee D16 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi- Standards volume information, refer to the standard’s Document Summary page on
bility of Subcommittee D16.02 on Oxygenated Aromatics. the ASTM website.
Current edition approved Feb. 15, 2018. Published February 2018. Originally Available from U.S. Government Printing Office, Superintendent of
approved in 1959. Last previous edition approved in 2010 as D1631 – 10. DOI: Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://
10.1520/D1631-10R18E01. www.access.gpo.gov.
*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
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D1631 − 10 (2018)
6.2 If ketones are present in the sample, interference from
them can be avoided by employing the glycol-pyridine sample
solvent specified in Test Method D1364.
7. Apparatus
7.1 The apparatus shall be assembled as shown in Fig. 1.
Any suitable modification permitting equal facility and accu-
4.1.2 The pyridine sulfur trioxide salt reacts with the
racy may be used. Automatic titration equipment is commer-
methanol, this preventing a second mole of water from being
cially available and may be used.
consumed:
8. Reagents
8.1 Reagent grade chemicals shall be used in all tests.
Unless otherwise indicated, it is intended that all reagents shall
conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society, where such
4.2 Whenthepyridinesolutioncontainswaterandthesulfur
specifications are available. Other grades may be used, pro-
dioxide is titrated with iodine in methanol solution, the
vided it is first ascertained that the reagent is of sufficiently
platinum electrodes remain polarized until all the water reacts.
high purity to permit its use without lessening the accuracy of
A slight excess of iodine depolarizes the electrodes, allowing
the determination.
current to flow through the microammeter which indicates the
8.2 Iodine Solution—Dissolve 150 g of iodine (I ) crystals
end point.
in 3 Lof anhydrous methanol. Place the solution in the reagent
bottle connected to the buret as shown in Fig. 1.
5. Significance and Use
8.3 Methanol, anhydrous, containing less than 0.05 % wa-
5.1 This test method is particularly useful for determining
small amounts of water in hygroscopic materials. This test ter.
method is suitable for setting specifications on materials
8.4 Pyridine Solution—Place 4000 mL of refined grade
referenced in the scope. It may also be used as an internal
pyridine in a 5000-mL distilling flask. Distill over and discard
quality control tool and in development or research work.
400 mLof forecut at atmospheric pressure. Distill off 3400 mL
of center cut and transfer to a suitable glass bottle fitted with a
6. Interferences
two-hole stopper. Through one hole of the stopper insert a
6.1 This test method is not applicable in the presence of
piece of glass tubing that extends almost to the bottom of the
mercaptans, peroxides, or appreciable quantities of aldehydes
bottle; through the other hole insert a short piece of glass
or amines.
tubing to serve as a vent. Through the long tube add 400 g of
refrigerant-grade sulfur dioxide (SO ) dried through concen-
trated sulfuric acid (H SO sp gr 1.84), and allow the solution
2 4
to cool. Fit the vent tube with a drying tube and an aspirator
bulb; connect the long tube with an adapter suitable for
introducing the reagent into the titration flask. For convenience
in measuring, a suitable reservoir may be placed in the system.
NOTE 1—In place of the divided reagents described in 8.2, 8.3, and 8.4
it is permissible to employ the single solution reagent specified in Test
Method D1364 or commercial Karl Fischer reagents. Pyridine-free re-
agents are available from various laboratory suppliers and may be used if
suitable for the material being tested.
8.5 When handling Karl Fischer reagent refer to Practice
D3437.
9. Hazards
9.1 Consult current OSHA regulations supplier’s Safety
Data Sheets and local regulations for all materials used in this
test method.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Ch
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