ASTM D2522-03(2008)e1
(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 Warning—Mercury has been designated by EPA and many state agencies as a hazardous material that can cause central nervous system, kidney, and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution should be taken when handling mercury and mercury-containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPA’s website (http://www.epa.gov/mercury/faq.htm) for additional information. Users should be aware that selling mercury or mercury-containing products, or both, in your state may be prohibited by state law.
1.3 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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´1
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.
´ NOTE—The mercury warning was editorially added in April 2009.
1. Scope 4. Significance and Use
1.1 This test method describes the determination of the total 4.1 Chlorine is normally present in polybutenes in small
chloride content of polybutenes used for electrical insulation. amounts,usuallybelow50ppm,asorganicallyboundchlorine.
1.2 Warning—Mercury has been designated by EPA and Inorganic chloride is normally not present.
many state agencies as a hazardous material that can cause
NOTE 1—Thequalitativepresenceorabsenceofinorganicchloridemay
central nervous system, kidney, and liver damage. Mercury, or
be tested by Test Method D 878.
its vapor, may be hazardous to health and corrosive to
materials.Cautionshouldbetakenwhenhandlingmercuryand 5. Interferences
mercury-containing products. See the applicable product Ma-
5.1 The presence of substances which form insoluble silver
terial Safety Data Sheet (MSDS) for details and EPA’s website
compounds, such as sulfides, will give high results. Such
(http://www.epa.gov/mercury/faq.htm) for additional informa-
substances are not normally present in polybutenes.
tion. Users should be aware that selling mercury or mercury-
6. Apparatus
containingproducts,orboth,inyourstatemaybeprohibitedby
state law.
6.1 Separatory Funnel, 250-mL.
1.3 This standard does not purport to address all of the
6.2 Potentiometeric Titrimeter, automatic recording, or
safety concerns, if any, associated with its use. It is the
manual.
responsibility of the user of this standard to establish appro-
6.3 Electrodes:
priate safety and health practices and determine the applica-
6.3.1 Silver and glass electrode combination is preferred.
bility of regulatory limitations prior to use.Forspecifichazards
6.3.2 A silver electrode with a mercurous sulfate reference
information, see Section 8.
electrode is an acceptable alternative.
6.4 Microburet, 5-mL, with 0.01-mL divisions.
2. Referenced Documents
7. Reagents
2.1 ASTM Standards:
D 878 Test Method for Inorganic Chlorides and Sulfates in
7.1 Purity of Reagents—Use reagent grade chemicals in all
Insulating Oils
tests.Unlessotherwiseindicated,itisintendedthatallreagents
D 1193 Specification for Reagent Water
shall conform to the specifications of the Committee on
Analytical Reagents of theAmerican Chemical Society, where
3. Summary of Test Method
such specifications are available. Other grades may be used,
3.1 Organically bound chlorine is converted into sodium
provided it is first ascertained that the reagent is of sufficiently
chloride by reaction with sodium biphenyl solution. The
high purity to permit its use without lessening the accuracy of
sodium chloride formed is extracted with dilute nitric acid, and
the determination.
the chlorine content of the aqueous phase is determined by
7.2 Purity of Water— Unless otherwise indicated, refer-
potentiometric titration.
encestowatershallbeunderstoodtomeanreagentgradewater
as defined by Type I conforming to Specifications D 1193.
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.
´1
D 2522–03 (2008)
7.3 Dilute Nitric Acid (2.1 M)—Dilute 134 mL of concen- 9.3 Allow the blue-green mixture to stand 5 min to ensure
trated nitric acid to 1.0 L with water. complete reaction. Remove stopper, add 2 mL of isopropyl
7.4 Isopropyl Alcohol. alcohol, and swirl with stopper removed until excess reagent is
7.5 Silver Nitrate, Standard Solution (0.025 N)—Weigh destroyed.
accurately 0.4247 g of silver nitrate (AgNO ). Transfer it to a 9.4 Add slowly 50 mL of dilute nitric acid. Contact organic
1-L volumetric flask and add water to dissolve.Add 3.0 mL of and aqueous phases by gentle swirling and rocking for about 5
concentrated nitric acid (HNO , relative density (specific min. Loosen the stopper occasionally to release slight pressure.
gravity) 1.42) and then add water to the 1-L mark of the Drain the aqueous phase into a beaker. Extract the organic
volumetric flask. Standardize this solution against a pure phase twice more with 50-mL portions of dilute nitric acid.
chloridestandard.Checkthesolutionatleastmonthlytoassure Drain the aqueous phases into the beaker containing the first
a constant reagent. extract.
7.6 Sodium Chloride, NIST Standard Reference Material 9.5 Sulfur compounds are not normally present in poly-
919A. butenes. However, if present in amounts which may affect
chlorine results significantly, the following procedure is rec-
NOTE 2—Dry the silver nitrate overnight in a desiccator before making
ommended for removal of the sulfur compounds: Charge the
up the solution. Both the solid material and the solution must be protected
aqueous phase from 9.4 to a separatory funnel and add 15 mL
from light by storage in brown glassware in the dark.
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, nit
...
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.
´1
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.
´ NOTE—The mercury warning was editorially added in April 2009.
1. Scope
1.1 This test method describes the determination of the total chloride content of polybutenes used for electrical insulation.
1.2
1.2 Warning—Mercury has been designated by EPA and many state agencies as a hazardous material that can cause central
nervous system, kidney, and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution
should be taken when handling mercury and mercury-containing products. See the applicable product Material Safety Data Sheet
(MSDS) for details and EPA’s website (http://www.epa.gov/mercury/faq.htm) for additional information. Users should be aware
that selling mercury or mercury-containing products, or both, in your state may be prohibited by state law.
1.3 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 OilsOils
D 1193 Specification 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.
This test method is under the jurisdiction of ASTM Committee D-27 D27 on Electrical Insulating Liquids and Gases and is the direct responsibility of Subcommittee
D27.06 on Chemical Test.
Current edition approved March 15, 1995. Published May 1995. Originally published as D2522–69. Last previous edition D2522–89.
Current edition approved May 1, 2008. Published June 2008. Originally approved in 1969. Last previous edition 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.
´1
D 2522 – 03 (2008)
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
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,
...
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