ASTM D2522-03(2008)e2
(Test Method)Standard Test Method for Chlorine Content of Polybutenes Used for Electrical Insulation (Withdrawn 2017)
Standard Test Method for Chlorine Content of Polybutenes Used for Electrical Insulation (Withdrawn 2017)
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.
WITHDRAWN RATIONALE
This test method describes the determination of the total chloride content of polybutenes used for electrical insulation.
Formerly under the jurisdiction of Committee D27 on Electrical Insulating Liquids and Gases, this test method was withdrawn in July 2017 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
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Designation: D2522 − 03 (Reapproved 2008)
Standard Test Method for
Chlorine Content of Polybutenes Used for Electrical
Insulation
This standard is issued under the fixed designation D2522; 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.
´ NOTE—In 7.7, 20 L was changed to 2 L editorially in August 2009.
1. Scope sodium chloride formed is extracted with dilute nitric acid, and
the chlorine content of the aqueous phase is determined by
1.1 This test method describes the determination of the total
potentiometric titration.
chloride content of polybutenes used for electrical insulation.
1.2 Warning—Mercury has been designated by EPA and
4. Significance and Use
many state agencies as a hazardous material that can cause
4.1 Chlorine is normally present in polybutenes in small
central nervous system, kidney, and liver damage. Mercury, or
amounts,usuallybelow50ppm,asorganicallyboundchlorine.
its vapor, may be hazardous to health and corrosive to
Inorganic chloride is normally not present.
materials.Cautionshouldbetakenwhenhandlingmercuryand
NOTE1—Thequalitativepresenceorabsenceofinorganicchloridemay
mercury-containing products. See the applicable product Ma-
be tested by Test Method D878.
terial Safety Data Sheet (MSDS) for details and EPA’s website
(http://www.epa.gov/mercury/faq.htm) for additional informa-
5. Interferences
tion. Users should be aware that selling mercury or mercury-
5.1 The presence of substances which form insoluble silver
containingproducts,orboth,inyourstatemaybeprohibitedby
compounds, such as sulfides, will give high results. Such
state law.
substances are not normally present in polybutenes.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
6. Apparatus
responsibility of the user of this standard to establish appro-
6.1 Separatory Funnel, 250-mL.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.Forspecifichazards
6.2 Potentiometeric Titrimeter, automatic recording, or
information, see Section 8. manual.
6.3 Electrodes:
2. Referenced Documents
6.3.1 Silver and glass electrode combination is preferred.
2.1 ASTM Standards:
6.3.2 A silver electrode with a mercurous sulfate reference
D878 Test Method for Inorganic Chlorides and Sulfates in
electrode is an acceptable alternative.
Insulating Oils
6.4 Microburet, 5-mL, with 0.01-mL divisions.
D1193 Specification for Reagent Water
7. Reagents
3. Summary of Test Method
7.1 Purity of Reagents—Use reagent grade chemicals in all
3.1 Organically bound chlorine is converted into sodium
tests.Unlessotherwiseindicated,itisintendedthatallreagents
chloride by reaction with sodium biphenyl solution. The
shall conform to the specifications of the Committee on
Analytical Reagents of theAmerican Chemical Society, where
This test method is under the jurisdiction of ASTM Committee D27 on
such specifications are available. Other grades may be used,
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
approved in 1969. Last previous edition approved in 2003 as D2522 – 03. DOI: Reagent Chemicals, American Chemical Society Specifications , American
10.1520/D2522-03R08E02. 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
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D2522 − 03 (2008)
provided it is first ascertained that the reagent is of sufficiently the solution to a separatory funnel. Rinse the beaker several
high purity to permit its use without lessening the accuracy of times with a total of 25 mL toluene and add the rinses to the
the determination. funnel.
7.2 Purity of Water—Unlessotherwiseindicated,references 9.2 Add an excess of sodium biphenyl solution into the
to water shall be understood to mean reagent grade water as separatory funnel. Excess reagent is evidenced by a blue or
defined by Type I conforming to Specifications D1193. green color. (See Note 2.) Stopper and mix thoroughly by
gentle shaking. Vent occasionally to release slight pressure.
7.3 Dilute Nitric Acid (2.1 M)—Dilute 134 mL of concen-
trated nitric acid to 1.0 L with water. 9.3 Allow the blue-green mixture to stand 5 min to ensure
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
NOTE 2—Dry the silver nitrate overnight in a desiccator before making
chlorine results significantly, the following procedure is rec-
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 funne
...
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