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ASTM_E_191_-_64_2017.pdf

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1、Designation:E19164(Reapproved 2017)Standard Specification forApparatus For Microdetermination of Carbon andHydrogen in Organic and Organo-Metallic Compounds1This standard is issued under the fixed designation E191;the number immediately following the designation indicates the year oforiginal adoptio

2、n or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S.Department of Defense.1.Scope1

3、.1 This specification covers apparatus and basic equipmentfor the determination of carbon and hydrogen in organic andorganometallic compounds along the lines of the conventionalmethod of Pregl,but with modifications more in line withmodern practice.Owing to the diversity of apparatus by whichcorrect

4、 results can be obtained,this specification is intended toindicate what is acceptable rather than what is mandatory.NOTE1Specifications for several items subsequently listed weredeveloped by the Committee for the Standardization of MicrochemicalApparatus,Division of Analytical Chemistry,American Che

5、mical Soci-ety.21.2 The values stated in inch-pound units are to be regardedas the standard.The metric equivalents of inch-pound unitsmay be approximate.2.Referenced Documents2.1 ASTM Standards:3E124 Specification for Weighing and Drying Apparatus forMicrochemical AnalysisE148 Specification for Appa

6、ratus for Microdetermination ofNitrogen by the Dumas Method(Withdrawn 1987)43.Oxygen Supply3.1 Any cylinder or other suitable source of oxygen free ofhydrogen and organic impurities may be used.Oxygen pre-pared from liquid air is satisfactory.4.Pressure Regulator4.1 The pressure regulator,shown in F

7、ig.1 and Fig.2,5consisting of a bell and inlet tube submerged in a suitableconfining liquid,shall be used to supply air or oxygen,or both,at constant pressure to the combustion system.Substitution ofa fine gas-control valve and flowmeter for the pressure regu-lator is optional.5.Drying and Purifying

8、 Tube25.1 The conventional bubble-container U-tube shown inFig.3 shall be used for drying and purifying the entering air oroxygen,or both.6.Flowmeter6.1 The rate of gas flow shall be determined by the bubblecounter of the bubble-counter U-tube,or by a more accurateflow-meter,such as the floating bal

9、l-in-column.67.Combustion Unit7.1 The combustion unit shall consist of a long furnace,asample furnace,a constant-temperature heating mortar,acombustion tube,and a combustion-tube closure.7.1.1 Long Furnace:7.1.1.1 The long furnace shall have a maximum over-alllength of 8 in.(203 mm)with the wall thi

10、ckness at the ends notto exceed14in.(6 mm).The furnace shall accommodatecombustion tubes up to 13 mm in outside diameter.Electricheating elements shall be easily replaceable.The furnace shallbe mounted firmly on a substantial support.7.1.1.2 The furnace shall be capable of continuous operationat tem

11、peratures up to 900C as measured inside the combustiontube at the middle of the furnace.The temperature drop fromthe center to points 1 in.(25 mm)and 134in.(45 mm)fromeither end shall not exceed 15 and 7%,respectively,based1This specification is under the jurisdiction of ASTM Committee E41 onLaborat

12、ory Apparatus and is the direct responsibility of Subcommittee E41.01 onLaboratory Ware and Supplies.Current edition approved Jan.1,2017.Published February 2017.Originallyapproved in 1962.Discontinued in 1988 and reinstated in 1989.Last previousedition approved in 2011 as E191 64(2011).DOI:10.1520/E

13、0191-64R17.2Committee for the Standardization of Microchemical Apparatus.Division ofAnalytical Chemistry,American Chemistry Society,1949 Report on RecommendedSpecifications for Microchemical Apparatus,Carbon-Hydrogen,Dumas Nitrogen,Sulfur,and Halogen,Analytical Chemistry Vol 21,p.1555(1949).3For ref

14、erenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.4The last approved version of this historical standard is referenced onwww

15、.astm.org.5Furter,M.F.,and Steyermark,A.,“Pressure Regulator for Use in Microdeter-mination of Carbon and Hydrogen,”Analytical Chemistry,Vol 20,1948,p.257.6Kuck,J.A.,and Altieri,P.L.,“Spherical Ground-Glass Joints vs.RubberTubing Connectors on the C and HAbsorption Train,”Mikrochimica Acta,1956,p.15

16、56.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.1 upon the temperature in the middle of the furnace.7Meansshall be provided

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