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ASTM D3272-76(2003)

(Practice)

Standard Practice for Vacuum Distillation of Solvents From Solvent-Reducible Paints For Analysis (Withdrawn 2008)

Standard Practice for Vacuum Distillation of Solvents From Solvent-Reducible Paints For Analysis (Withdrawn 2008)

ABSTRACT
This practice covers the vacuum distillation process used to separate solvents from the nonvolatile portions of paints for analysis. The procedure entails adding tricresyl phosphate to a sample of the whole paint and heating the mixture using a silicon oil bath. The distillation is then allowed to proceed for a time before vacuum is applied and then dry air is made to pass through the system to facilitate the removal of any high-boiling solvents present. The apparatus needed for this practice include a custom made apparatus, a vacuum punp, a septum sample vial, and a safety shield. Methylene chloride or acetone, silicone oil, and tricresyl phosphate are used as reagents.
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 D 3271.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 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.
WITHDRAWN RATIONALE
This practice covers a vacuum distillation procedure that separates the solvents from the nonvolatile portion of paints so they may be analyzed.
Formerly under the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this practice was withdrawn in November 2008. This standard is being withdrawn without replacement because there are now several methods in use.

General Information

Status
Withdrawn
Publication Date
30-Nov-2003
Withdrawal Date
18-Nov-2008
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

Replaces
ASTM D3272-76(1998) - Standard Practice for Vacuum Distillation of Solvents From Solvent-Reducible Paints For Analysis
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
01-Dec-2003

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ASTM D3272-76(2003) - Standard Practice for Vacuum Distillation of Solvents From Solvent-Reducible Paints For Analysis (Withdrawn 2008)ASTM D3272-76(2003) - Standard Practice for Vacuum Distillation of Solvents From Solvent-Reducible Paints For Analysis (Withdrawn 2008)
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ASTM D3272-76(2003) - Standard Practice for Vacuum Distillation of Solvents From Solvent-Reducible Paints For Analysis (Withdrawn 2008)
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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:D3272–76(Reapproved2003)
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 connections and distances as small as possible. Include a gage
in the assembly for measuring pressure.
1.1 Thispracticecoversavacuumdistillationprocedurethat
4.2 Vacuum Pump, capable of pulling 2 mm Hg or less of
separates the solvents from the nonvolatile portion of paints so
vacuum pressure.
they may be analyzed.
4.3 Septum Sample Vial, PTFE-fluorocarbon-faced.
1.2 An alternative procedure for the analysis of solvents in
4.4 Safety Shield.
paints is described in Practice D 3271.
1.3 The values stated in SI units are to be regarded as the
5. Reagents
standard. The values given in parentheses are for information
5.1 Methylene Chloride or Acetone.
only.
5.2 Silicone Oil.
1.4 This standard does not purport to address all of the
5.3 Tricresyl Phosphate.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
6. Procedure
priate safety and health practices and determine the applica-
6.1 Immerse the receiver in a bath containing dry ice with
bility of regulatory limitations prior to use.
methylene chloride or acetone of sufficient depth that the liquid
reaches to the bottom level of the rubber stopper.
2. Referenced Documents
6.2 Pour approximately 15 g of the whole paint sample into
2.1 ASTM Standards:
the 50-mLdistillation flask. Immediately follow with 10 mLof
D 3271 Practice for Direct Injection of Solvent-Reducible
tricresyl phosphate and without delay mix the contents of the
Paints into a Gas Chromatograph for Solvent Analysis
flask.
3. Summary of Practice 6.3 Assemble the apparatus and close the needle valve and
stopcock attached to the capillary tubing. Immerse the distil-
3.1 The sample of whole paint with added tricresyl phos-
lation flask by raising a silicone oil bath preheated to 155 to
phate is heated by means of a silicone oil bath. The distillation
160°C (Warning—Care should be taken to prevent the tem-
is allowed to proceed for a period of time and then vacuum is
perature of the silicone oil exceeding 160°C because of
applied. Finally dry air is passed through the system to
possible formation of explosive mixtures of air and solvents
facilitate the removal of any high-boiling solvents present.
from the sample being analyzed.) until it reaches the side arm
4. Apparatus
(Note 1). Allow the distillation to proceed for 15 min without
vacuum.
4.1 Apparatus is shown in Fig. 1. It is essential in assem-
bling this apparatus, that the volume of the portion preceding
NOTE 1—The liquid level in the oil bath should be as high as is
the flask be kept to a minimum by using diameters of
practical.
6.4 After 15 min apply vacuum slowly and carefully to
avoid bumping or rapid distillation until 2 mm Hg is reached.
This pract
...

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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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