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ASTM D3272-76(1998)

(Practice)

Standard Practice for Vacuum Distillation of Solvents From Solvent-Reducible Paints For Analysis

Standard Practice for Vacuum Distillation of Solvents From Solvent-Reducible Paints For Analysis

SCOPE
1.1 This practice covers a vacuum distillation procedure that separates the solvents from the nonvolatile portion of paints so they may be analyzed.  
1.2 An alternative procedure for the analysis of solvents in paints is described in Practice D3271.
1.3 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address all of the safety problems 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.

General Information

Status
Historical
Publication Date
09-May-1998
ICS
87.060.30 - Solvents
Technical Committee
D01 - Paint and Related Coatings, Materials, and Applications
Drafting Committee
D01.21 - Chemical Analysis of Paints and Paint Materials
Current Stage
Ref Project

Relations

Replaced By
ASTM D3272-76(2003) - Standard Practice for Vacuum Distillation of Solvents From Solvent-Reducible Paints For Analysis (Withdrawn 2008)
Effective Date
01-Dec-2003
Referred By
ASTM D6133-02(2021) - Standard Test Method for Acetone, <emph type="ital">p</emph>-Chlorobenzotrifluoride, Methyl Acetate or <emph type="ital">t</emph>-Butyl Acetate Content of Solventborne and Waterborne Paints, Coatings, Resins, and Raw Materials by Direct Injection Into a Gas Chromatograph
Effective Date
10-May-1998

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ASTM D3272-76(1998) - Standard Practice for Vacuum Distillation of Solvents From Solvent-Reducible Paints For AnalysisASTM D3272-76(1998) - Standard Practice for Vacuum Distillation of Solvents From Solvent-Reducible Paints For Analysis
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ASTM D3272-76(1998) - Standard Practice for Vacuum Distillation of Solvents From Solvent-Reducible Paints For Analysis
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 3272 – 76 (Reapproved 1998)
Standard Practice for
Vacuum Distillation of Solvents From Solvent-Reducible
Paints For Analysis
This standard is issued under the fixed designation D 3272; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope 4.4 Safety Shield.
1.1 Thispracticecoversavacuumdistillationprocedurethat
5. Reagents
separates the solvents from the nonvolatile portion of paints so
5.1 Methylene Chloride or Acetone.
they may be analyzed.
5.2 Silicone Oil.
1.2 An alternative procedure for the analysis of solvents in
5.3 Tricresyl Phosphate.
paints is described in Practice D 3271.
1.3 This standard does not purport to address all of the
6. Procedure
safety concerns, if any, associated with its use. It is the
6.1 Immerse the receiver in a bath containing dry ice with
responsibility of the user of this standard to establish appro-
methylene chloride or acetone of sufficient depth that the liquid
priate safety and health practices and determine the applica-
reaches to the bottom level of the rubber stopper.
bility of regulatory limitations prior to use.
6.2 Pour approximately 15 g of the whole paint sample into
2. Referenced Documents the 50-mLdistillation flask. Immediately follow with 10 mLof
tricresyl phosphate and without delay mix the contents of the
2.1 ASTM Standards:
flask.
D 3271 Practice for Direct Injection of Solvent-Reducible
2 6.3 Assemble the apparatus and close the needle valve and
Paints into a Gas Chromatograph for Solvent Analysis
stopcock attached to the capillary tubing. Immerse the distil-
3. Summary of Practice lation flask by raising a silicone oil bath preheated to 155 to
160°C (Warning—see Note 1) until it reaches the side arm
3.1 The sample of whole paint with added tricresyl phos-
(Note 2). Allow the distillation to proceed for 15 min without
phate is heated by means of a silicone oil bath. The distillation
vacuum.
is allowed to proceed for a period of time and then vacuum is
applied. Finally dry air is passed through the system to
NOTE 1—Warning: Care should be taken to prevent the temperature of
facilitate the removal of any high-boiling solvents present.
the silicone oil exceeding 160°C because of possible formation of
explosive mixtures of air and solvents from the sample being analyzed.
4. Apparatus
NOTE 2—The liquid level in the oil bath should be as high as is
3 practical.
4.1 Apparatus is shown in Fig. 1. It is essential in assem-
bling this apparatus, that the volume of the portion preceding 6.4 After 15 min apply vacuum slowly and carefully to
the flask be kept to a minimum by using diameters of avoid bumping or rapid distillation until 2 mm Hg is reached.
connections and distances as small as possible. Include a gage This step s
...

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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.  
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