ASTM D2522-95
(Test Method)Standard Test Method for Chlorine Content of Polybutenes Used for Electrical Insulation
Standard Test Method for Chlorine Content of Polybutenes Used for Electrical Insulation
SCOPE
1.1 This test method describes the determination of the total chloride content of polybutenes used for electrical insulation.
1.2 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 hazards information, see Section 8.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 2522 – 95
Standard Test Method for
Chlorine Content of Polybutenes Used for Electrical
Insulation
This standard is issued under the fixed designation D 2522; 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 6. Apparatus
1.1 This test method describes the determination of the total 6.1 Separatory Funnel, 250-mL.
chloride content of polybutenes used for electrical insulation. 6.2 Potentiometeric Titrimeter, automatic recording, or
1.2 This standard does not purport to address all of the manual.
safety concerns, if any, associated with its use. It is the 6.3 Electrodes:
responsibility of the user of this standard to establish appro- 6.3.1 Silver and glass electrode combination is preferred.
priate safety and health practices and determine the applica- 6.3.2 A silver electrode with a mercurous sulfate reference
bility of regulatory limitations prior to use. For specific hazards electrode is an acceptable alternative.
information, see Section 8. 6.4 Microburet, 5-mL, with 0.01-mL divisions.
2. Referenced Documents 7. Reagents
2.1 ASTM Standards: 7.1 Purity of Reagents—Use reagent grade chemicals in all
D 878 Test Method for Inorganic Chlorides and Sulfates in tests. Unless otherwise indicated, it is intended that all reagents
Insulating Oils shall conform to the specifications of the Committee on
D 1193 Specification for Reagent Water Analytical Reagents of the American Chemical Society, where
D 2296 Specification for Continuity of Quality of Electrical such specifications are available. Other grades may be used,
Insulating Polybutene Oil for Capacitors provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
3. Summary of Test Method
the determination.
3.1 Organically bound chlorine is converted into sodium
7.2 Purity of Water— Unless otherwise indicated, refer-
chloride by reaction with sodium biphenyl solution. The ences to water shall be understood to mean reagent grade water
sodium chloride formed is extracted with dilute nitric acid, and
as defined by Type I conforming to Specifications D 1193.
the chlorine content of the aqueous phase is determined by 7.3 Dilute Nitric Acid (2.1 M)—Dilute 134 mL of concen-
potentiometric titration.
trated nitric acid to 1.0 L with water.
7.4 Isopropyl Alcohol.
4. Significance and Use
7.5 Silver Nitrate, Standard Solution (0.025 N)—Weigh
4.1 Chlorine is normally present in polybutenes in small
accurately 0.4247 g of silver nitrate (AgNO ). Transfer it to a
amounts, usually below 50 ppm, as organically bound chlorine.
1-L volumetric flask and add water to dissolve. Add 3.0 mL of
Inorganic chloride is normally not present.
concentrated nitric acid (HNO , relative density (specific
gravity) 1.42) and then add water to the 1-L mark of the
NOTE 1—The qualitative presence or absence of inorganic chloride may
volumetric flask. Standardize this solution against a pure
be tested by Test Method D 878.
chloride standard. Check the solution at least monthly to assure
5. Interferences
a constant reagent.
7.6 Sodium Chloride, NIST Standard Reference Material
5.1 The presence of substances which form insoluble silver
919A.
compounds, such as sulfides, will give high results. Such
substances are not normally present in polybutenes.
NOTE 2—Dry the silver nitrate overnight in a desiccator before making
up the solution. Both the solid material and the solution must be protected
from light by storage in brown glassware in the dark.
This test method is under the jurisdiction of ASTM Committee D-27 on
Electrical Insulating Liquids and Gasesand is the direct responsibility of Subcom-
Reagent Chemicals, American Chemical Society Specifications, American
mittee D27.06on Chemical Test. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Current edition approved March 15, 1995. Published May 1995. Originally listed by the American Chemical Society, see Analar Standards for Laboratory
published as D 2522 – 69. Last previous edition D 2522 – 89. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 10.03. and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 11.01. MD.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 2522
7.7 Sodium Biphenyl Solution—Transfer 300 mL of dry ommended for removal of the sulfur compounds: Charge the
toluene and 58 g of metallic sodium to a 20 L, three-necked aqueous phase from 9.4 to a separatory funnel and add 15 mL
flask, equipped with a heating mantle, nitrogen gas inlet, of ethyl ether to the mixture. Shake the contents of the funnel
mercury seal stirrer, and reflux condenser. Heat until the vigorously for 1 min, venting to the air frequently. Allow the
toluene refluxes and the sodium melts completely. Start the contents of the funnel to stand until the two layers separate,
stirrer, and stir until the sodium is finely dispersed. Cool to less then draw off the aqueous layer into a beaker. Extract the
than 10°C in a suitable bath (not water). Remove the con- organic layer with two 15-mL portions of water, add the
denser, and add 1250 mL of dry ethylene glycol dimethyl ether. aqueous extracts to the beaker, and discard the organic layer.
While stirring and passing nitrogen gas over the mixture, add Add a few millilitres of 30 % hydrogen peroxide solution, heat
390 g of biphenyl. The reaction should start immediately, as the contents of the beaker on a steam hot plate until the ether
evidenced by the green color of sodium biphenyl. The tem- has evaporated, then boil
...
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