ASTM D2192-06(2012)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D2192 − 06 (Reapproved 2012)
Standard Test Method for
Purity of Aldehydes and Ketones
This standard is issued under the fixed designation D2192; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope* D1193 Specification for Reagent Water
E29 Practice for Using Significant Digits in Test Data to
1.1 This test method covers the determination of the purity
Determine Conformance with Specifications
of certain commercially available aldehydes and ketones.
E200 Practice for Preparation, Standardization, and Storage
1.2 In addition to all aldehydes and ketones, all compounds
of Standard and Reagent Solutions for ChemicalAnalysis
such as vinyl alkyl ethers, acetals, and ketals, that hydrolyze
E222 Test Methods for Hydroxyl Groups Using Acetic
under the conditions of the reaction to form free carbonyl
Anhydride Acetylation
groups, react with the reagent and consequently interfere.
Water,alcohols,saturatedesters,andhydrocarbonsdonotreact
3. Summary of Test Method
withthereagent,butlargeamountsofinertorganicsolventsare
3.1 Hydroxylamine hydrochloride is converted in part to
undesirable because of the effect on the indicator.
free hydroxylamine by reaction with a known amount of
1.3 For purposes of determining conformance of an ob-
aqueous triethanolamine.
served or a calculated value using this test method to relevant
NH OH·HCl1 HOCH CH N→ (1)
~ !
2 2 2
specifications, test result(s) shall be rounded off “to the nearest
unit” in the last right-hand digit used in expressing the
NH OH1 HOCH CH N·HCl
~ !
2 2 2
specification limit, in accordance with the rounding-off method
of Practice E29. The free hydroxylamine reacts with the aldehyde or ketone
to form the corresponding oxime.
1.4 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this RR C 5 01NH OH→RR C 5 H 5 NOH1H O, (2)
1 2 1 2
standard.
where:
1.5 This standard does not purport to address all of the
R = alkyl group and
safety concerns, if any, associated with its use. It is the
R = alkyl group or hydrogen.
responsibility of the user of this standard to establish appro-
The amount of hydroxylamine consumed, which is deter-
priate safety and health practices and determine the applica-
mined by titration of the excess base with standard sulfuric
bility of regulatory limitations prior to use. For specific hazard
acid, is a measure of the aldehyde or ketone originally present.
statements, see Section 7.
1.6 For hazard information and guidance, see the supplier’s
3.2 Since the determination is based on an acidimetric
Material Safety Data Sheet.
titration, a suitable correction must be applied if the sample is
not neutral to bromophenol blue indicator.
2. Referenced Documents
2.1 ASTM Standards: 4. Significance and Use
D268 Guide for Sampling and Testing Volatile Solvents and
4.1 This test method provides a measurement of purity
Chemical Intermediates for Use in Paint and Related
(assay) of aldehydes and ketones. The results of these mea-
Coatings and Material
surements can be used for specification acceptance.
4.2 The precision of this test method is applicable only to
This test method is under the jurisdiction of ASTM Committee D01 on Paint
material having a purity of 98 to 100 %.
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
CurrenteditionapprovedJune1,2012.PublishedJuly2012.Originallyapproved 5. Apparatus
in 1963. Last previous edition approved in 2006 as D2192 – 06 . DOI: 10.1520/
5.1 Pressure Bottle, 200 to 350-mLcapacity, with lever type
D2192-06R12.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or closure and made of heat-resistant glass.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
5.2 Container for Pressure Bottle—Asuitable safety device
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. to contain the pressure bottle.Ametal container with a hinged
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2192 − 06 (2012)
top and perforated bottom, a strong synthetic fabric or canvas 7.2 Add 15 mLof a 0.04 % alcoholic solution of bromophe-
bag, or a safety shield may be used. nol blue indicator to 500 mL of the hydroxylamine hydrochlo-
ride solution. From a buret add 0.5 N triethanolamine until the
5.3 Ampoule, 1 or 2-mL capacity.
solutionappearsgreenish-bluebytransmittedlight.Preparethe
5.4 Weighing Pipet, Lunge or similar type.
solution fresh before each series of analyses.
5.5 Burets, 50-mL capacity.
7.3 Prepare a sufficient number of heat-resistant pressure
bottles to make all blank and sample determinations in dupli-
5.6 Transfer Pipet, 50-mL capacity.
cate.Replacetherubbergasketsifnecessaryandmakesurethe
5.7 Glass Rod, 8-mm, several pieces approximately 1 in.
caps can be fastened securely.
long.
7.4 Using a graduated cylinder, add 65 mL of the neutral-
5.8 Boiling Water Bath.
ized hydroxylamine hydrochloride to each bottle. Using a
transfer pipet, add 50.0 mL of the 0.5 N triethanolamine
6. Reagents and Materials
solution to each bottle.
6.1 Purity of Reagents—Reagent grade chemicals shall be
7.5 Beforecapping,purgethebottlesfor2minwithagentle
used in all tests. Unless otherwise indicated, it is intended that
stream of cylinder nitrogen. This is best accomplished by
all reagents shall conform to the specifications of the Commit-
means of a glass tube inserted through the neck of the bottle
tee onAnalytical Reagents of theAmerican Chemical Society,
and clamped so that the opening is just above the surface of the
where such specifications are available. Other grades may be
liquid.
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
7.6 Reserve two of the bottles for the blank determination.
accuracy of the determination.
Into each of the other bottles introduce an amount of sample
containing not more than 0.015 mol of aldehyde or ketone. For
6.2 Purity of Water—Unless otherwise indicated, references
substantially pure material, weigh the specimen to the nearest
to water shall be understood to mean reagent water conforming
0.1 mg, using the amount and procedure specified in Table 1.
to Type IV of Specification D1193.
7.6.1 Warning: Acetaldehyde is a highly volatile, flam-
6.3 Bromophenol Blue Indicator (0.04 % Alcoholic
mable material; observe all necessary safety precautions.
Solution)—Dissolve 0.04 g of bromophenol blue (tetrabro-
Handle samples only in a fume hood that is free from open
mophenolsulfonphthalein)in100mLofmethylalcohol.Titrate
flames, electric heaters, and other sources of ignition. Cool all
this solution with 0.1 N sodium hydroxide (NaOH) solution to
samples in an ice bath before the containers are opened. Weigh
a reddish-bronze color. If an off-color is obtained at this point,
the acetaldehyde in a sealed glass ampoule. The actual proce-
it is probably due to the age of the indicator and fresh indicator
dure for filling and sealing the ampoule will vary somewhat
should be used to prepare a new solution.
with the type of ampoule being used. One convenient method
6.4 Cylinder Nitrogen.
is to pack commercially available ampoules in powdered, solid
carbon dioxide, introduce the specimen by means of a chilled
6.5 Hydroxylamine Hydrochloride, Standard (0.5 N Alco-
hypodermic syringe, and seal the ampoule with a gas torch.
holic Solution)—Dissolve 35 g of hydroxylamine hydrochlo-
ride (NH OH · HCl) in 150 mLof water and dilute to 1 Lwith
2 7.7 If a sealed glass ampoule is used to weigh the specimen,
99 % isopropanol.
add several pieces of 8-mm glass rod and shake the bottle
vigorously to break the ampoule.
6.6 Isopropanol (99
...