ASTM D3733-93(1998)

Standard Test Method for Silicon Content of Silicone Polymers and Silicone-Modified Alkyds by Atomic Absorption (Withdrawn 2007)

SCOPE
1.1 This test method covers the determination of the silicon content of silicone polymers and silicone modified alkyds when present in the nonvolatile portion of polymers, resins, or liquid coatings to the extent of 1% or more.  
1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
WITHDRAWN RATIONALE
This test method covers the determination of the silicon content of silicone polymers and silicone modified alkyds when present in the nonvolatile portion of polymers, resins, or liquid coatings to the extent of 1 % or more.
Formerly under the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this test method was withdrawn in March 2007 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the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

• Status: Withdrawn
• Publication Date: 31-Dec-1992
• Withdrawal Date: 19-Mar-2007
• ICS: 71.100.55 - Silicones
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.33 - Polymers and Resins

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation: D 3733 – 93 (Reapproved 1998)
Standard Test Method for
Silicon Content of Silicone Polymers and Silicone-Modified
Alkyds by Atomic Absorption
This standard is issued under the fixed designation D 3733; 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. Apparatus
1.1 This test method covers the determination of the silicon 5.1 Atomic Absorption Spectrophotometer, consisting of an
content of silicone polymers and silicone modified alkyds atomizer and a single-slot burner; gas pressure-regulating and
when present in the nonvolatile portion of polymers, resins, or -metering devices for nitrous oxide (N O) and acetylene; a
liquid coatings to the extent of 1 % or more. silicon hollow-cathode lamp with a regulated constant current
1.2 This standard does not purport to address all of the supply; a monochromator and associated optics; a photosensi-
safety concerns, if any, associated with its use. It is the tive detector connected to an electronic amplifier; and a
responsibility of whoever uses this standard to consult and read-out device.
establish appropriate safety and health practices and deter- 5.2 Centrifuge.
mine the applicability of regulatory limitations prior to use. 5.3 Pipets, 5, 10, 15, and 20-mL capacity.
5.4 Volumetric Flasks, 25, 50, 100, and 1000-mL.
2. Referenced Documents
6. Reagents
2.1 ASTM Standards:
D 1153 Specification for Methyl Isobutyl Ketone 6.1 Purity of Reagents—Reagent grade chemicals shall be
D 1193 Specification for Reagent Water used in all tests. Unless otherwise indicated, it is intended that
D 2372 Practice for Separation of Vehicle from Solvent- all reagents shall conform to the specifications of the Commit-
Reducible Paints tee onAnalytical Reagents of theAmerican Chemical Society,
D 2698 Test Method for Determination of the Pigment where such specifications are available. Other grades may be
Content of Solvent-Reducible Paints by High-Speed Cen- used, provided it is first ascertained that the reagent is of
trifuging sufficiently high purity to permit its use without lessening the
D 2832 Guide for Determining Volatile and Nonvolatile accuracy of the determination.
Content of Paint and Related Coatings 6.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent water conforming
3. Significance and Use
to Type II of Specification D 1193.
3.1 The silicon content of silicone modified alkyds has a
6.3 Octaphenylcyclotetrasiloxane.
direct relationship to the cost and performance characteristics, 6.4 Methyl Isobutyl Ketone (MIBK), complying with
especially heat resistance of coatings prepared from them.
Specification D 1153.
6.5 Silicon, Standard Stock Solution (100µ g/mL)—Weigh
4. Summary of Test Method
exactly 0.709 g of octaphenylcyclotetrasiloxane and quantita-
4.1 The polymer solution or separated coating vehicle is
tively transfer to a 1-L flask. Dilute to volume with MIBK.
diluted with methyl isobutyl ketone, and the silicon content is
determined by atomic absorption spectroscopy.
Reagent Chemicals, American Chemical Society Specifications, American
This test method is under the jurisdiction of ASTM Committee D-1 on Paint Chemical Society, Washington, DC. For suggestions on the testing of reagents not
and Related Coatings, Material, and Applications and is the direct responsibility of listed by the American Chemical Society, see Analar Standards for Laboratory
Subcommittee D 01.33 on Polymers and Resins. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Current edition approved April 15, 1993. Published June 1993. Originally and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
e1
published as D 3733 – 78. Last previous edition D 3733 – 78 (1984) . MD.
2 6
Annual Book of ASTM Standards, Vol 06.04. Available as Standard Reference Material No. 1066a from Office of Standard
Annual Book of ASTM Standards, Vol 11.01. Reference Materials, Room B-314, Chemistry Building, National Institute of
Annual Book of ASTM Standards, Vol 06.01. Standards and Technology, Washington, DC 20234.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 3733 – 93 (1998)
NOTE 3—Iftheapproximatesiliconcontentisknown,usethefollowing
7. Calibration and Standardization
specimen weights to optimize analytical results:
7.1 Prepare the following standard solutions from the 100
Expected Silicon Optimum Weight of Solids,
µg/mLsilicon standard stock solution, diluting to the indicated
Content, % mg
volumes with MIBK:
4 150
Concentration,
2 300
Stock Solution, mL Dilute to, mL µg/mL
1 600
20 25 80
15 25 60 8.3 Aspirate each specimen solution and determine the
10 25 40
absorbance in the same manner in which the instrument was
525 20
calibrated. Determine the concentration of silicon in micro-
550 10
5 100 5 grams per millilitre from the calibration curve. If the absor-
bance is above the range covered by the calibration curve,
7.2 Operational instructions for atomic absorption spectro-
dilute an aliquot of the sample solution to a suitable volume
photometers vary with different models. Consult the manufac-
with MIBK. If the absorbance is below the range covered by
turer’s literature for establishing optimum conditions for the
the calibration curve, repeat the analysis using a larger speci-
specific instrument used.
men size.
7.3 Turn t
...