Standard Test Method for Free Formaldehyde Content of Amino Resins (Withdrawn 2006)

SCOPE
1.1 This test method covers the determination of free formaldehyde in amino resins and their aqueous and nonaqueous solutions. Amino resin-free formaldehyde levels from about 0.02 to 5.0% can be determined by this test method. The applicability of this test method to other matrices is unknown.
1.2 This standard does not purport to address the safety problems associated with its use. It is the responsibility of the user of 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WITHDRAWN RATIONALE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 free formaldehyde in amino resins and their aqueous and non-aqueous solutions. Amino resin-free formaldehyde levels from about 0.02 to 5.0 % can be determined by this test method. The applicability of this test method to other matrices is unknown.
Formerly under the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this test method was withdrawn in February 2006 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by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Withdrawn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
09-Nov-1997
Withdrawal Date
26-Feb-2006
Current Stage
Ref Project

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ASTM D1979-97 - Standard Test Method for Free Formaldehyde Content of Amino Resins (Withdrawn 2006)
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D1979–97
Standard Test Method for
Free Formaldehyde Content of Amino Resins
This standard is issued under the fixed designation D 1979; 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 4. Significance and Use
1.1 This test method covers the determination of free 4.1 The amount of free formaldehyde in amino resins may
formaldehyde in amino resins and their aqueous and non- be of concern to both producer and user, as its presence in air
aqueous solutions.Amino resin-free formaldehyde levels from above threshold amounts may produce objectionable odors and
about 0.02 to 5.0 % can be determined by this test method.The irritant effects. This test method can be useful for evaluating
applicability of this test method to other matrices is unknown. suppliers’ products and for quality control.
1.2 This standard does not purport to address all of the
5. Apparatus
safety concerns, if any, associated with its use. It is the
5.1 Analytical Balance, 60.1 mg.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 5.2 Magnetic Stirrer and Stir Bar—A “heavy duty” mag-
netic stirrer is necessary.
bility of regulatory limitations prior to use.
5.3 Buret, 50 mL manual or electronic. Manual burets
2. Referenced Documents
should be of the type designed to minimize the exposure of
2.1 ASTM Standards: reagent to air. Electronic burets are preferred.
D 1193 Specification for Reagent Water 5.4 Beakers, glass, 100 mL, 600 mL, and 1500 mL.
D 1959 Test Method for Iodine Value of Drying Oils and 5.5 Stopwatch or Timer.
Fatty Acids 5.6 Graduated Cylinders, glass, 50 mL and 250 mL.
5.7 Glass Pipet, 2 mL.
3. Summary of Test Method
5.8 Thermometer, subdivision 1°C.
3.1 Specimens are mixed with borate buffer solution and ice
6. Reagents
water, then kept cool in an ice bath. Excess sodium sulfite is
added to consume free formaldehyde as follows: 6.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated it is intended that
CH O 1 Na SO 1 H O→ HOCH SO Na 1 NaOH (1)
2 2 3 2 2 3
all reagents conform to the specifications of the Committee on
3.2 The excess sodium sulfite is removed by titration with
Analytical Reagents of the American Chemical Society where
iodine using starch as the indicator as follows:
such specifications are available. Other grades may be used,
Na SO 1 I 1 H O→ Na SO 1 2 HI (2)
2 3 2 2 2 4 provided it is first ascertained that the reagent is of sufficient
high purity to permit its use without lessening the accuracy of
3.3 The sodium sulfite-formaldehyde complex is then de-
the determination.
composed with sodium carbonate to quantitatively regenerate
6.2 Purity of Water—Unless otherwise indicated, references
sodium sulfite and formaldehyde as follows:
to water shall be understood to mean reagent water as defined
HOCH SO Na 1 Na CO → CH O 1 Na SO 1 NaHCO (3)
2 3 2 3 2 2 3 3
by Type II of Specification D 1193.
3.4 Theliberatedsodiumsulfiteistitratedwithiodine(Eq2)
6.3 Acetic Acid Solution (1.0 M)—Dissolve 60 mL of
and free formaldehyde is calculated from this second iodine
glacial acetic acid (CH CO H) in water and dilute to 1 L.
3 2
titration.
6.4 Boric Acid Buffer Solution—Prepare a sodium hydrox-
ide solution (1.0 M) by dissolving 40 g of sodium hydroxide
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of Reagent Chemicals, American Chemical Society Specifications, American
Subcommittee D01.33 on Polymers and Resins. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Current edition approved Nov. 10, 1997. Published June 1998.Originally listed by the American Chemical Society, see Analar Standards for Laboratory
published as D 1979 - 91. Last previous edition D 1979 - 91(l997). Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 11.01.
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 06.03. MD.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
D1979
(NaOH) in water and diluting to 1 L. Dissolve 12.39 g of boric boric acid buffer. Continue extraction for 5 min. Uninterrupted
acid (H BO ) in 100 mL of 1.0 M NaOH, then dilute to 1 L. stirring must be maintained through 7.5-7.10.
3 3
Maintain temperature at 0°C in an ice bath. The pH at 0°C 7.5 While constantly stirring the specimen solution, pipet 2
should be 9.4 (glass electrode). mL of 1.0 M sodium sulfite solution into the beaker.
6.5 Ice, finely crushed. 7.6 Continue stirring for 15 min.
6.6 Iodine Solution (0.1
...

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