ASTM D4983-89(1996)

Standard Test Method for Cyclohexylamine, Morpholine, and Diethylaminoethanol in Water and Condensed Steam by Direct Aqueous Injection Gas Chromatography (Withdrawn 2002)

SCOPE
1.1 This test method covers the general considerations for the qualitative and quantitative determination of volatile amines such as cyclohexylamine, morpholine, and diethylaminoethanol in steam condensates and surface water by gas-liquid chromatography.    
1.2 This test method may be applied to water samples containing the amines in concentrations from 2 to 15 mg/L by direct injection of alkaline aqueous samples. Higher concentrations may be determined by appropriate dilution.
1.3 Although this test method is written for flame ionization detector, the basic technology is applicable to any highly sensitive nitrogen-specific detector provided water does not interfere with the measurement.
1.4 The test method may be extended to steam condensates containing low levels of these amines by adopting suitable concentration techniques such as steam distillation to bring the analyte concentration to an accurately quantifiable range.
1.5 The test method is applicable to other chromatographable amines by appropriately varying the chromatographic parameters. This must be validated by the individual analysts.
1.6 This test method has been used successfully with reagent-grade and boiler steam condensate waters. It is the user's responsibility to assure the validity of this test method for any untested matrices.
1.7 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• Status: Withdrawn
• Publication Date: 31-Dec-1995
• Withdrawal Date: 09-Jun-2002
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: D19 - Water
• Drafting Committee: D19.06 - Methods for Analysis for Organic Substances in Water

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NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn.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 4983 – 89 (Reapproved 1996)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Cyclohexylamine, Morpholine, and Diethylaminoethanol in
Water and Condensed Steam by Direct Aqueous Injection
1
Gas Chromatography
This standard is issued under the fixed designation D 4983; 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.
4
1. Scope D 1193 Specification for Reagent Water
D 2777 Practice for Determination of Precision and Bias of
1.1 This test method covers the general considerations for
4
Methods of Committee D-19 on Water
the qualitative and quantitative determination of volatile
D 2908 Practice for Measuring Volatile Organic Matter in
amines such as cyclohexylamine, morpholine, and diethylami-
5
Water by Aqueous-Injection Gas Chromatography
noethanol in steam condensates and surface water by gas-liquid
,
2 3
D 3370 Practices for Sampling Water from Closed Con-
chromatography.
4
duits
1.2 This test method may be applied to water samples
E 355 Practice for Gas Chromatography Terms and Rela-
containing the amines in concentrations from 2 to 15 mg/L by
6
tionships
direct injection of alkaline aqueous samples. Higher concen-
trations may be determined by appropriate dilution.
3. Terminology
1.3 Although this test method is written for flame ionization
3.1 Descriptions of Terms Specific to This Test Method:
detector, the basic technology is applicable to any highly
3.1.1 vapor phase inhibitors—a class of paraffinic, alicyclic,
sensitive nitrogen-specific detector provided water does not
or heterocyclic, neutralizing amines that co-distill with steam
interfere with the measurement.
and are carried throughout the distribution system in order to
1.4 The test method may be extended to steam condensates
react with carbonic acid present in the system.
containing low levels of these amines by adopting suitable
3.2 Definitions—For definitions of other terms used in this
concentration techniques such as steam distillation to bring the
test method, refer to Terminology D 1129 and Practice E 355.
analyte concentration to an accurately quantifiable range.
1.5 The test method is applicable to other chromatograph-
4. Summary of Test Method
able amines by appropriately varying the chromatographic
4.1 The sample is preserved by adjusting the pH to 3.0 by
parameters. This must be validated by the individual analysts.
addition of phosphate solutions. Prior to analysis the pH is
1.6 This test method has been used successfully with
raised to >10.0. After centrifugation, the sample is analyzed by
reagent-grade and boiler steam condensate waters. It is the
direct aqueous injection gas chromatography using an alkaline
user’s responsibility to assure the validity of this test method
polyethylene glycol liquid phase and a flame-ionization detec-
for any untested matrices.
tor.
1.7 This standard does not purport to address all of the
4.2 When high levels of these amines (>15 mg/L) are found
safety concerns, if any, associated with its use. It is the
in water samples, positive identification of the component(s) is
responsibility of the user of this standard to establish appro-
required by supplemental testing, such as the use of different
priate safety and health practices and determine the applica-
gas chromatographic column packings; a nitrogen-specific
bility of regulatory limitations prior to use.
detector, derivatization, mass spectrometry, or a combination
2. Referenced Documents of these techniques should also be used.
4.3 In this test method, the elution profile of the subject
2.1 ASTM Standards:
4
amines occurs in the order: morpholine, cyclohexylamine, and
D 1066 Practice for Sampling Steam
4
diethylaminoethanol. (Refer to the chromatogram in Fig. 1.)
D 1129 Terminology Relating to Water
5. Significance and Use
1
This test method is under the jurisdiction of ASTM Committee D-19 on Water 5.1 Vapor phase inhibitors such as morpholine, cyclohexy-
and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
lamine, and diethylaminoethanol are added to water to reduce
Organic Substances in Water.
corrosion in steam-generating and distribution systems by
Current edition approved Nov. 10, 1989. Published March 1990.
2
Di Corcia, A., and Samperi, R., Analytical Chemistry, Vol 46, 1974, p. 977.
3
(a) Supelco Inc. (Bellefonte, PA 16823) Bulletin 737B Copyright 1973. (b)
5
Supelco Inc. (Bellefonte, PA 16823) Bulletin 738B Copyright 1976. Annual Book of ASTM Standards, Vol 11.02.
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