1、Designation:D 6069 01Standard Test Method forTrace Nitrogen in Aromatic Hydrocarbons by OxidativeCombustion and Reduced Pressure ChemiluminescenceDetection1This standard is issued under the fixed designation D 6069;the number immediately following the designation indicates the year oforiginal adopti
2、on 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.Scope*1.1 This test method covers the determination of totalnitrogen(organic and inorgani
3、c)in aromatic hydrocarbons,their derivatives and related chemicals.1.2 This test method is applicable for samples containingnitrogen from 0.2 to 2 mgN/kg.For higher nitrogen concen-trations refer to Test Method D 4629.1.2.1 The detector response of this technique within thespecified scope of this te
4、st method is linear with nitrogenconcentration.1.3 The following applies to all specified limits in this testmethod:for purposes of determining conformance with thistest method,an observed value or a calculated value shall berounded off“to the nearest unit”in the last right-hand digitused in express
5、ing the specification limit,in accordance withthe rounding-off method of Practice E 29.1.4 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
6、 determine the applica-bility of regulatory limitations prior to use.For specific hazardstatements,see Section 9.2.Referenced Documents2.1 ASTM Standards:D 1555 Test Method for Calculation of Volume and Weightof Industrial Aromatic Hydrocarbons2D 3437 Practice for Sampling and Handling Liquid Cyclic
7、Products2D 4629 Test Method for Organically Bound Trace Nitrogenin Liquid Petroleum Hydrocarbons By Syringe/Inlet Oxi-dative Combustion and Chemiluminescence Detection3E 29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications4E 691 Practice for Conducting an
8、 Interlaboratory Study toDetermine the Precision of a Test Method42.2Other Documents:OSHA Regulations,29CFR,paragraphs 1910.1000 and1910.120053.Terminology3.1 Definitions:3.1.1 reduced pressure chemiluminescencea chemical re-action at pressure less than 760 mm mercury(Hg)in whichlight is emitted.3.1
9、.2 oxidative pyrolysisa process in which a sampleunder goes combustion in an oxygen rich environment attemperatures greater than of 650C.3.1.2.1 DiscussionOrganic compounds pyrolytically de-compose to carbon dioxide,water and elemental oxides.4.Summary of Test Method4.1 A specimen is introduced into
10、 a gas stream,at acontrolled rate,and carried into a high temperature furnace(900C)where an excess of oxygen is added.Pyrolysisconverts organic material in the specimen to carbon dioxideand water.Organic nitrogen and inorganic nitrogen com-pounds,present in the specimen,are converted to nitric oxide
11、(NO).Nitric oxide reacts with ozone in the detector producingnitrogen dioxide molecules in an excited state.As the excitednitrogen dioxide molecules relax to ground state,light isemitted.This light is detected by a photomultiplier tube withthe resulting signal proportional to the concentration of ni
12、tro-gen in the sample.Operating the detector at a reduced pressure,lowers the probability of the excited nitrogen dioxide mol-ecules colliding with other molecules before they undergochemiluminescence.Thus,reduced pressure provides im-proved sensitivity and lower noise.5.Significance and Use5.1 This
13、 method has been prepared to detect and quantitate1This test method is under the jurisdiction of ASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility ofSubcommittee D16.04 on Instrumental Analysis.Current edition approved June 10,2001.Published August 200
14、1.Originallypublished as D 6069 96.Last previous edition D 6069 96.2Annual Book of ASTM Standards,Vol 06.04.3Annual Book of ASTM Standards,Vol 05.02.4Annual Book of ASTM Standards,Vol 14.02.5Available from the Superintendent of Documents,U.S.Government PrintingOffice,Washington,DC 20402.1*A Summary
15、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.nitrogen-containing compounds such as N-formylmorpholine(4-formylmorpholine,Chemical Abstract Service numbers(CAS)No.250-37-6)or 1-methy
16、l-2-pyrrolidinone(NMP)(CAS)No.872-50-42 at a concentration of 1.0 mgN/kg or lessin aromatic hydrocarbons used or produced in manufacturingprocesses.These nitrogen-containing compounds are undesir-able in the finished aromatic products and may be the result ofthe aromatic extraction process.This test method may be usedin setting specifications for determining the total nitrogencontent in aromatic hydrocarbons.NOTE1Virtually all organic and inorganic nitrogen compounds willbe detected by this tech