ASTM_D_4983_-_89_1996.pdf

Designation:D 4983 89(Reapproved 1996)Standard Test Method forCyclohexylamine,Morpholine,and Diethylaminoethanol inWater and Condensed Steam by Direct Aqueous InjectionGas Chromatography1This standard is issued under the fixed designation D 4983;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method covers the general considerations forthe qualitative and quantitative determination of volatileamines such as cyclohexylamine,morpholine,and diethylami-noethanol in steam condensates and surface water by gas-liquidchromatography.2,31.2 This test method may be applied to water samplescontaining the amines in concentrations from 2 to 15 mg/L bydirect injection of alkaline aqueous samples.Higher concen-trations may be determined by appropriate dilution.1.3 Although this test method is written for flame ionizationdetector,the basic technology is applicable to any highlysensitive nitrogen-specific detector provided water does notinterfere with the measurement.1.4 The test method may be extended to steam condensatescontaining low levels of these amines by adopting suitableconcentration techniques such as steam distillation to bring theanalyte concentration to an accurately quantifiable range.1.5 The test method is applicable to other chromatograph-able amines by appropriately varying the chromatographicparameters.This must be validated by the individual analysts.1.6 This test method has been used successfully withreagent-grade and boiler steam condensate waters.It is theusers responsibility to assure the validity of this test methodfor any untested matrices.1.7 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:D 1066 Practice for Sampling Steam4D 1129 Terminology Relating to Water4D 1193 Specification for Reagent Water4D 2777 Practice for Determination of Precision and Bias ofMethods of Committee D-19 on Water4D 2908 Practice for Measuring Volatile Organic Matter inWater by Aqueous-Injection Gas Chromatography5D 3370 Practices for Sampling Water from Closed Con-duits4E 355 Practice for Gas Chromatography Terms and Rela-tionships63.Terminology3.1 Descriptions of Terms Specific to This Test Method:3.1.1 vapor phase inhibitorsa class of paraffinic,alicyclic,or heterocyclic,neutralizing amines that co-distill with steamand are carried throughout the distribution system in order toreact with carbonic acid present in the system.3.2 DefinitionsFor definitions of other terms used in thistest method,refer to Terminology D 1129 and Practice E 355.4.Summary of Test Method4.1 The sample is preserved by adjusting the pH to 3.0 byaddition of phosphate solutions.Prior to analysis the pH israised to 10.0.After centrifugation,the sample is analyzed bydirect aqueous injection gas chromatography using an alkalinepolyethylene glycol liquid phase and a flame-ionization detec-tor.4.2 When high levels of these amines(15 mg/L)are foundin water samples,positive identification of the component(s)isrequired by supplemental testing,such as the use of differentgas chromatographic column packings;a nitrogen-specificdetector,derivatization,mass spectrometry,or a combinationof these techniques should also be used.4.3 In this test method,the elution profile of the subjectamines occurs in the order:morpholine,cyclohexylamine,anddiethylaminoethanol.(Refer to the chromatogram in Fig.1.)5.Significance and Use5.1 Vapor phase inhibitors such as morpholine,cyclohexy-lamine,and diethylaminoethanol are added to water to reducecorrosion in steam-generating and distribution systems by1This test method is under the jurisdiction of ASTM Committee D-19 on Waterand is the direct responsibility of Subcommittee D19.06 on Methods forAnalysis forOrganic Substances in Water.Current edition approved Nov.10,1989.Published March 1990.2Di Corcia,A.,and Samperi,R.,Analytical Chemistry,Vol 46,1974,p.977.3(a)Supelco Inc.(Bellefonte,PA 16823)Bulletin 737B Copyright 1973.(b)Supelco Inc.(Bellefonte,PA 16823)Bulletin 738B Copyright 1976.4Annual Book of ASTM Standards,Vol 11.01.5Annual Book of ASTM Standards,Vol 11.02.6Annual Book of ASTM Standards,Vol 14.02.1AMERICAN SOCIETY FOR TESTING AND MATERIALS100 Barr Harbor Dr.,West Conshohocken,PA 19428Reprinted from the Annual Book of ASTM Standards.Copyright ASTMneutralizing acids like carbonic acid.High concentrations ofthese amines must be avoided because,under these conditions,protective metallic oxide coatings on surfaces may slough offvery rapidly,thereby affecting the corrosion inhibition occur-ring in th