ASTM D2522-03(2008)
(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
SIGNIFICANCE AND USE
Chlorine is normally present in polybutenes in small amounts, usually below 50 ppm, as organically bound chlorine. Inorganic chloride is normally not present.
Note 1—The qualitative presence or absence of inorganic chloride may be tested by Test Method D 878.
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.
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Designation:D 2522–03 (Reapproved 2008)
Standard Test Method for
Chlorine Content of Polybutenes Used for Electrical
1
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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 6. Apparatus
6.1 Separatory Funnel, 250-mL.
1.1 This test method describes the determination of the total
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.Forspecifichazards electrode is an acceptable alternative.
information, see Section 8. 6.4 Microburet, 5-mL, with 0.01-mL divisions.
2. Referenced Documents 7. Reagents
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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.Unlessotherwiseindicated,itisintendedthatallreagents
Insulating Oils shall conform to the specifications of the Committee on
D 1193 Specification for Reagent Water Analytical Reagents of theAmerican Chemical Society, where
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such specifications are available. Other grades may be used,
3. Summary of Test Method
provided it is first ascertained that the reagent is of sufficiently
3.1 Organically bound chlorine is converted into sodium
high purity to permit its use without lessening the accuracy of
chloride by reaction with sodium biphenyl solution. The the determination.
sodium chloride formed is extracted with dilute nitric acid, and
7.2 Purity of Water— Unless otherwise indicated, refer-
the chlorine content of the aqueous phase is determined by encestowatershallbeunderstoodtomeanreagentgradewater
potentiometric titration. as defined by Type I conforming to Specifications D 1193.
7.3 Dilute Nitric Acid (2.1 M)—Dilute 134 mL of concen-
4. Significance and Use
trated nitric acid to 1.0 L with water.
4.1 Chlorine is normally present in polybutenes in small
7.4 Isopropyl Alcohol.
amounts,usuallybelow50ppm,asorganicallyboundchlorine.
7.5 Silver Nitrate, Standard Solution (0.025 N)—Weigh
Inorganic chloride is normally not present.
accurately 0.4247 g of silver nitrate (AgNO ). Transfer it to a
3
1-L volumetric flask and add water to dissolve.Add 3.0 mL of
NOTE 1—Thequalitativepresenceorabsenceofinorganicchloridemay
concentrated nitric acid (HNO , relative density (specific
be tested by Test Method D 878. 3
gravity) 1.42) and then add water to the 1-L mark of the
5. Interferences
volumetric flask. Standardize this solution against a pure
chloridestandard.Checkthesolutionatleastmonthlytoassure
5.1 The presence of substances which form insoluble silver
a constant reagent.
compounds, such as sulfides, will give high results. Such
7.6 Sodium Chloride, NIST Standard Reference Material
substances are not normally present in polybutenes.
919A.
NOTE 2—Dry the silver nitrate overnight in a desiccator before making
1
This test method is under the jurisdiction of ASTM Committee D27 on
Electrical Insulating Liquids and Gases and is the direct responsibility of Subcom-
mittee D27.06 on Chemical Test.
3
Current edition approved May 1, 2008. Published June 2008. Originally Reagent Chemicals, American Chemical Society Specifications , American
approved in 1969. Last previous edition approved in 2003 as D 2522 – 03. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D 2522–03 (2008)
up the solution. Both the solid material and the solution must be protected
ommended for removal of the sulfur compounds: Charge the
from light by storage in brown glassware in the dar
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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:D 2522–95 Designation: D 2522 – 03 (Reapproved 2008)
Standard Test Method for
Chlorine Content of Polybutenes Used for Electrical
1
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 (´) indicates an editorial change since the last revision or reapproval.
1. 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D 878 Test Method for Inorganic Chlorides and Sulfates in Insulating Oils Oils
D 1193Specification for Reagent Water
2
D2296Specification for Continuity of Quality of Electrical Insulating Polybutene Oil for Capacitors Specification for Reagent
Water
3. Summary of Test Method
3.1 Organically bound chlorine is converted into sodium chloride by reaction with sodium biphenyl solution. The sodium
chloride formed is extracted with dilute nitric acid, and the chlorine content of the aqueous phase is determined by potentiometric
titration.
4. Significance and Use
4.1 Chlorine is normally present in polybutenes in small amounts, usually below 50 ppm, as organically bound chlorine.
Inorganic chloride is normally not present.
NOTE 1—The qualitative presence or absence of inorganic chloride may be tested by Test Method D 878.
5. Interferences
5.1 Thepresenceofsubstanceswhichforminsolublesilvercompounds,suchassulfides,willgivehighresults.Suchsubstances
are not normally present in polybutenes.
6. Apparatus
6.1 Separatory Funnel, 250-mL.
6.2 Potentiometeric Titrimeter , automatic recording, or manual.
6.3 Electrodes:
6.3.1 Silver and glass electrode combination is preferred.
6.3.2 A silver electrode with a mercurous sulfate reference electrode is an acceptable alternative.
6.4 Microburet, 5-mL, with 0.01-mL divisions.
7. Reagents
7.1 PurityofReagents—Usereagentgradechemicalsinalltests.Unlessotherwiseindicated,itisintendedthatallreagentsshall
conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such
1
This test method is under the jurisdiction of ASTM Committee D-27D27 on Electrical Insulating Liquids and Gases and is the direct responsibility of Subcommittee
D27.06 on Chemical Test.
Current edition approved March 15, 1995.May 1, 2008. Published May 1995.June 2008. Originally published as D2522–69.approved in 1969. Last previous edition
D2522–89.approved in 2003 as D 2522 – 03.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. ForAnnualBookofASTMStandards
, Vol 10.03.volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D 2522 – 03 (2008)
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specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the determination.
7.2 Purity of Water— Unless otherwise indicated, references to water shall be understood to mean reagent grade water as
defined by Type I conforming to Specifications D 1193.
7.3 Dilute Nitric Acid (2.1 M)—Dilute 134 mL of concentrated nitric acid to 1.0 L with water.
7.4 Isopropyl Alcohol.
7.5 Silver Nitrate, Standard Solution (0.025 N)—Weigh accurately 0.4247 g of silver nitrate (AgNO ). Transfer it to a 1-L
3
volumetric flask and add water to dissolve.Add 3.0 mLof concentrated nitric acid (HNO , relative density (specific gravity) 1.42)
3
and then add water to the 1-L mark of the volumetric flask. Standardize this solution against a pure chloride standard. Check the
solution at least monthly to assure a constant reagent.
7.6 Sodium Chloride, NIST Standard Reference Material 919A.
NOTE 2—Dry the silver nitrate overnight in a desiccator before making up the solution. Both the solid material and the solution must be pr
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