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ASTM D1399-95(2000)

(Test Method)

Standard Test Method for Unsaponifiable Contents of Tricresyl Phosphate (Withdrawn 2005)

Standard Test Method for Unsaponifiable Contents of Tricresyl Phosphate (Withdrawn 2005)

SCOPE
1.1 This test method covers the determination of the amount of unsaponifiable impurities in tricresyl phosphate.  
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 hazard statements, see Section 7.
1.3 For hazard information and guidance, see the supplier's Material Safety Data Sheet.
WITHDRAWN RATIONALE
This test method covers the determination of the amount of unsaponifiable impurities in tricresyl phosphate.
Formerly under the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this test method was withdrawn in May 2005. This standard is being withdrawn without replacement because of its limited use by industry.

General Information

Status
Withdrawn
Publication Date
09-May-2000
Withdrawal Date
20-Jun-2005
ICS
87.060.30 - Solvents
Technical Committee
D01 - Paint and Related Coatings, Materials, and Applications
Drafting Committee
D01.35 - Solvents, Plasticizers, and Chemical Intermediates
Current Stage
Ref Project

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ASTM D1399-95(2000) - Standard Test Method for Unsaponifiable Contents of Tricresyl Phosphate (Withdrawn 2005)ASTM D1399-95(2000) - Standard Test Method for Unsaponifiable Contents of Tricresyl Phosphate (Withdrawn 2005)
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ASTM D1399-95(2000) - Standard Test Method for Unsaponifiable Contents of Tricresyl Phosphate (Withdrawn 2005)
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation: D 1399 – 95 (Reapproved 2000)
Standard Test Method for
Unsaponifiable Contents of Tricresyl Phosphate
This standard is issued under the fixed designation D 1399; 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 5.2 Separatory Funnel, having a capacity of 250 mL.
5.3 Evaporating Dish, porcelain or glass, having a capacity
1.1 This test method covers the determination of the amount
of 120 mL.
of unsaponifiable impurities in tricresyl phosphate.
5.4 Steam Bath.
1.2 This standard does not purport to address all of the
5.5 Drying Oven, thermostatically controlled, at a tempera-
safety concerns, if any, associated with its use. It is the
ture of 75 6 5°C.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
6. Reagents
bility of regulatory limitations prior to use. For specific hazard
6.1 Purity of Reagents—Unless otherwise indicated, it is
statements, see Section 7.
intended that all reagents shall conform to the specifications of
1.3 For hazard information and guidance, see the supplier’s
theCommitteeonAnalyticalReagentsoftheAmericanChemi-
Material Safety Data Sheet.
cal Society, where such specifications are available. Other-
2. Referenced Documents wise, the best available grade shall be used.
6.2 Purity of Water—References to water shall be under-
2.1 ASTM Standards:
stood to mean reagent water conforming to Type IV of
D 1193 Specification for Reagent Water
Specification D 1193.
3. Summary of Test Method 6.3 Petroleum Ether, having a boiling range from 30 to
65°C.
3.1 The specimen is refluxed in the presence of an aqueous
6.4 Sodium Hydroxide (NaOH) Pellets.
solution of sodium hydroxide which converts the phosphate
estertowater-solublesalts.Thesaponifiedmaterialisextracted
7. Hazards
with petroleum ether which dissolves any unsaponifiable or
7.1 Tricresyl phosphate is hazardous through inhalation or
water-insoluble material. The combined extracts are evapo-
skin absorption. Care should be taken in handling the material.
rated in a tared evaporating dish, and the residual nonvolatile
7.2 Ortho-isomer of tricresyl phosphate is considered toxic.
material is determined.
Trace amounts may be present in tricresyl phosphate speci-
4. Significance and Use
mens.
4.1 This test method determines the amount of unsaponifi-
8. Procedure
able impurities in tricresyl phosphate remaining after manu-
8.1 Place approximately 30 mL of water in the 250-mL
facture or that may be introduced during handling and storage.
Erlenmeyer flask and to this carefully add approximately 10 g
4.2 Water-insoluble materials, which do not evaporate on a
of NaOH pellets. Carefully swirl the flask to dissolve the
steam bath or in a drying oven operated at 75 6 5°C for 1 h,
NaOH, and cool the solution to room temperature.
will be included as unsaponifiable material.
8.2 By means of a weighing pipet, transfer a 10-g specimen,
5. Apparatus weighed to 1 mg, to the flask. Add several boiling-stones,
connect the flask to the reflux condenser, and reflux for 1 h.
5.1 Reflux Apparatus, consisting of a 250-mL Erlenmeyer
(Warning—See 7.1 and 7.2.)
flask equipped with a 24/40 standard-taper joint attached to an
8.3 At the end of the refluxing period remove the flask from
Allihn-type reflux condenser similarly eq
...

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5.1 In order to calculate the volatile organic content (VOC) of paints containing EPA exempt solvents, it is necessary to know the acetone, methyl acetate, or parachlorobenzotrifluoride content. This gas chromatographic test method provides a simple and direct way for measuring these solvents. Each analyte is measured with respect to a unique internal standard. For acetone, the internal standard used is acetone-d6, for methyl acetate it is methyl acetate-d3, and for PCBTF it is metachlorobenzotrifluoride (MCBTF). These unique analyte/internal standard pairs behave very nearly as single solvents with respect to evaporation rate and adsorption rate onto a coated silica fiber (SPME) but are separable on a gas chromatograph (GC) capillary column. The only critical analytical technique required for successfully performing this test method is the ability of an analyst to weigh a paint sample and internal standard, corresponding to the analyte of interest, into a septum capped vial. After weighing, solvent evaporation has no effect on the final value of the determination. Since whole paint is not injected into the gas chromatograph, the analytical system is never compromised.
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1.1 This test method is for the determination of acetone, methyl acetate, or parachlorobenzotrifluoride (PCBTF), or combination of any of the three, in paints and coatings, by solid phase microextraction (SPME) headspace sampling, and subsequent injection into a gas chromatograph. It has been evaluated for cellulose nitrate, acrylic, and urethane solvent-borne systems. The established working range of this test method is: acetone, 28 to 90 %; methyl acetate, 12 to 22 %; parachlorobenzotrifluoride, 10 to 17 %. There is no reason to believe that it will not work outside these ranges. A minor modification of this test method would make it suitable for the analysis of the same analytes in water-borne coatings (see Note 1).
Note 1: Water-borne paints are internally standardized and diluted with water followed by addition of solid sodium chloride.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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