ASTM D1631-99
(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
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 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.
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.
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Designation: D 1631 – 99
Standard Test Method for
Water in Phenol and Related Materials by the Iodine
Reagent Method
This standard is issued under the fixed designation D 1631; 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 OSHA Regulations, 29 CFR, Paragraphs 1910.1000 and
1910.1200
1.1 This test method covers the determination of water in
phenol and related materials such as cresols, xylenols, naph-
3. Terminology
thalene, pyridine, and quinoline.
3.1 See Terminology D 4790 for definition of terms used in
1.2 This test method has been found applicable to a variety
this test method.
of materials varying in water content from 100 mg/kg to
solutions containing a relatively high percent of water.
4. Summary of Test Method
1.3 The following applies to all specified limits in this
4.1 When solutions of iodine in methanol and of sulfur
standard: for purposes of determining conformance with this
dioxide in pyridine are mixed in the presence of water, the
standard, an observed value or a calculated value shall be
following reaction occurs:
rounded off “to the nearest unit” in the last right-hand digit
→
used in expressing the specification limit in accordance with
I 1 SO 1 H O 2HI 1 SO (1)
2 2 2 ← 3
the rounding-off method of Practice E 29.
4.1.1 Sufficient pyridine is present in the reagent to consume
1.4 This standard does not purport to address all of the
the hydriodic acid and sulfur trioxide:
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific hazard
statements, see Section 9.
2. Referenced Documents
2.1 ASTM Standards: 4.1.2 The pyridine sulfur trioxide salt reacts with the metha-
D 1364 Test Method for Water in Volatile Solvents (Karl nol, this preventing a second mole of water from being
Fischer Reagent Titration Method) consumed:
D 3437 Practice for Sampling and Handling Liquid Cyclic
Products
D 3852 Practice for Sampling and Handling Phenol and
Cresylic Acid
D 4790 Terminology of Aromatic Hydrocarbons and Re-
lated Chemicals
4.2 When the pyridine solution contains water and the sulfur
E 29 Practice for Using Significant Digits in Test Data to
dioxide is titrated with iodine in methanol solution, the
Determine Conformance with Specifications
platinum electrodes remain polarized until all the water reacts.
2.2 Other Document:
A slight excess of iodine depolarizes the electrodes, allowing
current to flow through the microammeter which indicates the
end point.
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
5. Significance and Use
Subcommittee D16.02 on Oxygenated Aromatics.
Current edition approved June 10, 1999. Published August 1999. Originally
5.1 This test method is particularly useful for determining
published as D 1631 – 59 T. Last previous edition D 1631 – 94.
small amounts of water in hygroscopic materials. This test
Annual Book of ASTM Standards, Vol 06.04.
method is suitable for setting specifications on materials
Annual Book of ASTM Standards, Vol 14.02.
Available from Superintendent of Documents, U.S. Government Printing
Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1631–99
referenced in the scope. It may also be used as an internal vided it is first ascertained that the reagent is of sufficiently
quality control tool and in development or research work. high purity to permit its use without lessening the accuracy of
the determination.
6. Interferences
8.2 Iodine Solution—Dissolve 150 g of iodine (I ) crystals
in 3 L of anhydrous methanol. Place the solution in the reagent
6.1 This test method is not applicable in the presence of
bottle connected to the buret as shown in Fig. 1.
mercaptans, peroxides, or appreciable quantities of aldehydes
8.3 Methanol, anhydrous, containing less than 0.05 % wa-
or amines.
ter.
6.2 If ketones are present in the sample, interference from
8.4 Pyridine Solution—Place 4000 mL of refined grade
them can be avoided by employing the glycol-pyridine sample
pyridine in a 5000-mL distilling flask. Distill over and discard
solvent specified in Test Method D 1364.
400 mL of forecut at atmospheric pressure. Distill off 3400 mL
of center cut and transfer to a suitable glass bottle fitted with a
7. Apparatus
two-hole stopper. Through one hole of the stopper insert a
7.1 The apparatus shall be assembled as shown in Fig. 1.
piece of glass tubing that extends almost to the bottom of the
bottle; through the other hole insert a short piece of glass
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 D 1364 or commercial Karl Fischer reagents. Pyridine-free
reagents 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
D 3437.
9. Hazards
9.1 Consult current OSHA regulations supplier’s Material
Safety Data Sheets and local regulations for all materials used
in this test method.
9.2 Phenol, pyridine, and related materials are extremely
toxic when ingested and corrosive to the skin. Appropriate
precaution must be exercised when handling them.
10. Sampling
FIG. 1 Titration Assembly
10.1 Sample in accordance with Practice D 3852 for proper
sampling and handling of phenol and related materials ana-
Any suitable modification permitting equal facility and accu-
lyzed by this test method (see 9.1 and 9.2.).
racy may be used. Automatic titration equipment is commer-
10.2 Precautions must be taken in sampling to preclude any
cially available and may be used.
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