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
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
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
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
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
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.
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
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.
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 dark.
aqueous phase from 9.4 to a separatory funnel and add 15 mL
of ethyl ether to the mixture. Shake the contents of the funnel
7.7 Sodium Biphenyl Solution—Transfer 300 mL of dry
vigorously for 1 min, venting to the air frequently. Allow the
toluene and 58 g of metallic sodium to a 20 L, three-necked
contents of the funnel to stand until the two layers separate,
flask, equipped with a heating mantle, nitrogen gas inlet,
then draw off the aqueous layer into a beaker. Extract the
mercury seal stirrer, and reflux condenser. Heat until the
organic layer with two 15-mL portions of water, add the
toluene refluxes and the sodium melts completely. Start the
aqueous extracts to the beaker, and discard the organic layer.
stirrer, and stir until the sodium is finely dispersed. Cool to less
Add a few millilitres of 30 % hydrogen peroxide solution, heat
than 10°C in a suitable bath (not water). Remove the con-
the contents of the beaker on a steam hot plate until the ether
denser,andadd1250mLofdryethyleneglycoldimethylether.
has evaporated, then boil for 5 min, and cool to room
While stirring and passing nitrogen gas over the mixture, add
temperature. Proceed in accordance with 9.6.
390 g of biphenyl. The reaction should start immediately, as
9.6 Place the beaker on the titration stand, and insert the
evidenced by the green color of sodium biphenyl. The tem-
electrode system. Start the stirrer and record initial reading.
perature of the reaction mixture should be kept
...
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
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
2.1 ASTM Standards:
D 878 Test Method for Inorganic Chlorides and Sulfates in Insulating Oils Oils
D 1193Specification for Reagent Water
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
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.
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.
D 2522 – 03 (2008)
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
volumetric flask and add water to dissolve.Add 3.0 mLof concentrated nitric acid (HNO , relative density (specific gravity) 1.42)
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 protected from
light by storage in brown glassware in the dark.
7.7 Sodium Biphenyl Solution—Transfer 300 mL of dry toluene and 58 g of metallic sodium to a 20 L, three-necked flask,
equipped with a heating mantle, nitrogen gas inlet, mercury seal stirrer, and reflux condenser. Heat until the toluene refluxes and
the sodium melts completely. Start the stirrer, and stir until the sodium is finely dispersed. Cool to less than 10°C in a suitable bath
(not water). Remove the condenser, and add 1250 mL of dry ethylene glycol dimethyl ether. While stirring and passing nitrogen
gas over the mixture, add 390 g of biphenyl. The reaction should start immediately, as evidenced by the green color of sodium
biphenyl. The temperature of the reaction mixture should be kept below 30°C. When the reaction is complete (1 ⁄2 to 2 h), pour
the reagent into dry 500-mL brown prescription bottles with screw caps and foil liners. The reagent is stable for several months
if refrigerated. (If any unreacted sodium remains in the reaction flask, add 100 mL of isopropyl alcohol, and place the flask in a
hood until the metal has dissolved.)
NOTE 3—Two vials (30 mL) of this reagent are normally required to give excess reagent.
8. Hazards
8.1 Consult OSHA regulations and suppliers’ Material Safety Data Sheets for all materials used in this test method.
9. Procedure
9.1 Dissolve 35.5 6 0.1 g of polybutene in 25 mL toluene in a 150-mL beaker by stirring with a small glass rod. Transfer the
solution to a separatory funnel. Rinse the beaker several times with a total of 25 mL toluene and add the rinses to the funnel.
9.2 Add an excess of sodium biphenyl solution into the separatory funnel. Excess reagent is evidenced by a blue or green
color. (See Note 2.) Stopper and mix thoroughly by gentle shaking. Vent occasionally to release slight pressure.
9.3 Allow the blue-green mixture to stand 5 min to ensure complete reaction. Remove stopper, add 2 mL of isopropyl alcohol,
and swirl with stopper removed until excess reagent is destroyed.
9.4 Add slowly 50 mLof dilute nitric acid. Contact organic and aqueous phases by gentle swirling and rocking for about 5 min.
Loosen the stopper occasionally to release slight pressure. Drain the aqueous phase into a beaker. Extract the organic phase twice
more with 50-mL portions of dilute nitric acid. D
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