ASTM E191-1964(2005) Standard Specification for Apparatus For Microdetermination of Carbon and Hydrogen in Organic and Organo-Metallic Compounds《微量测量有机及有机金属化合物中碳和氢含量用仪器的标准规范》.pdf

《ASTM E191-1964(2005) Standard Specification for Apparatus For Microdetermination of Carbon and Hydrogen in Organic and Organo-Metallic Compounds《微量测量有机及有机金属化合物中碳和氢含量用仪器的标准规范》.pdf》由会员分享，可在线阅读，更多相关《ASTM E191-1964(2005) Standard Specification for Apparatus For Microdetermination of Carbon and Hydrogen in Organic and Organo-Metallic Compounds《微量测量有机及有机金属化合物中碳和氢含量用仪器的标准规范》.pdf（6页珍藏版）》请在麦多课文档分享上搜索。

1、Designation: E 191 64 (Reapproved 2005)Standard Specification forApparatus For Microdetermination of Carbon andHydrogen in Organic and Organo-Metallic Compounds1This standard is issued under the fixed designation E 191; the number immediately following the designation indicates the year oforiginal a

2、doption 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.This standard has been approved for use by agencies of the Department of Defense

3、.1. Scope1.1 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

4、whichcorrect results can be obtained, this specification is intended toindicate what is acceptable rather than what is mandatory.NOTE 1Specifications for several items subsequently listed weredeveloped by the Committee for the Standardization of MicrochemicalApparatus, Division of Analytical Chemist

5、ry, American Chemical 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:3E 124 Specification for Weighing and Drying Apparatus forMicrochemical AnalysisE 148 Sp

6、ecification for Apparatus for Microdeterminationof Nitrogen by Dumas Method3. 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 i

7、n Fig. 1 and Fig. 2,4conisting 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 P

8、urifying 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

9、 floating ball-in-column.57. 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 m

10、m) with the wall thickness at the ends notto exceed14 in. (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 c

11、ontinuous operationat temperatures 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 134 in. (45 mm) fromeither end shall not exceed 15 and 7 %, respectively, based1This specification is under the jurisdicti

12、on of ASTM Committee E41 onLaboratory Apparatus and is the direct responsibility of Subcommittee E41.01 onApparatus.Current edition approved May 1, 2005. Published October 2005. Originallyapproved in 1962. . Discontinued in 1988 and reinstated in 1989.Last previousedition approved in 1999 as E 191 6

13、4 (Reapproved 1999)e12Committee 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.

14、1555 (1949).3For referenced 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.4Furter, M. F., and Steyermark, A., “Pressure Reg

15、ulator for Use in Microdeter-mination of Carbon and Hydrogen,” Analytical Chemistry, Vol 20, 1948, p. 257.5Kuck, J. A., and Altieri, P. L., “Spherical Ground-Glass Joints vs. RubberTubing Connectors on the C and H Absorption Train,” Mikrochimica Acta, 1956, p.1556.1Copyright ASTM International, 100

16、Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.upon the temperature in the middle of the furnace.6Meansshall be provided for varying the temperature.7.1.1.3 The furnace shall be equipped with some device forindicating the temperature at the middle of the furnace.7.1.

17、2 Sample Furnace, Traveling Type (Note 2) :7.1.2.1 The sample furnace shall have an over-all length notless than 212 in. (64 mm) nor more than 4 in. (102 mm) withwall thickness at the ends not to exceed14 in. (6 mm). Thefurnace shall accommodate combustion tubes up to 13 mm inoutside diameter. Elect

18、ric heating elements shall be easilyreplaceable. The furnace shall be mounted firmly on a substan-tial support.7.1.2.2 The sample furnace shall be capable of continuousoperation up to 900C as measured inside the combustion tubeat the middle of the furnace. The temperature drop from thecenter to poin

19、ts34 in. (19 mm) from either end shall not exceed17 % of the temperature at the middle of the furnace.5Meansshall be provided for varying the temperature.7.1.2.3 The sample furnace shall be designed so that it maybe either moved away from the combustion tube or turned offand cooled rapidly. In the l

20、atter case, the time for cooling toroom temperature and reheating to operating temperature shallnot exceed 30 min.7.1.2.4 The sample furnace shall be equipped with somedevice for indicating the temperature at the middle of thefurnace.7.1.2.5 If the furnace is moved mechanically, it shall travela min

21、imum distance of 614 in. (159 mm) with provision formanual setting at any point. Whether the furnace has only oneor more than one speed of movement over this distance, therates of travel shall be within the limits of18 to58 in. (3 to 16mm)/min. An automatic control shall be provided to stop thetrave

22、l of the sample furnace when it reaches the long furnace.NOTE 2The stationary multiple-section type of sample furnace maybe used instead of the traveling type, which differs from the traveling typeas follows: It consists of not less than three sections with a maximumlength of 7 in. (178 mm) and a ma

23、ximum wall thickness of14 in. (6 mm)at the ends of any section. Each section shall be provided with itsindividual adjustable time switch, which can be set to go on or offautomatically for any time from 0 to 30 min. Provision shall be made forat least two sequences of heating of the various sections.

24、 Each section,when operated alone, shall be capable of continuous operation at tem-peratures up to 900C as measured inside the combustion tube at themiddle of the section.7.1.3 Heating MortarAny type of heating mortar2may beused provided it is capable of maintaining constant temperatureto within 61C

25、 in the range from 175 to 190C. If electric, theelements shall be easily replaceable. It shall accommodatecombustion tubes of 13 mm in outside diameter. Means shallbe provided for heat transfer to the inlet capillaries of the waterabsorption tube to prevent condensation of water.7.1.4 Combustion Tub

26、e The combustion tube shall have atip and side arm. Depending upon the length of furnaceassembly used, the tube shall be either as specified in Fig. 4 ofSpecification E 148 with a body length of 520 to 530 min,2orof similar construction with a body length of 620 to 630 mm.7.1.5 Combustion Tube Closu

27、reA solid stopper of rubberor suitable substitute, such as cork, neoprene, etc., withdimensions as specified in Fig. 5 of Specification E 148, shallbe used.6Several types of commercially available electric furnaces meet these require-ments.FIG. 1 Pressure Regulator, Glass PartsE 191 64 (2005)28. Abs

28、orption Tubes28.1 Absorption tubes, preferably of soda-lime glass, shall beused. Two suitable sizes are shown in Fig. 4.9. Guard Tube29.1 The guard tube shall be as shown in Fig. 5.10. Mariotte Bottle210.1 A Mariotte bottle, as shown in Fig. 6, shall be usedwith the pressure regulator described in S

29、ection 4.11. Weighing Accessories11.1 Weighing accessories needed in the microdetermina-tion of carbon and hydrogen are described in SpecificationE 124.12. Keywords12.1 carbon; compounds; hydrogen; microdeterminationFIG. 2 Pressure Regulator, Details of ConstructionE 191 64 (2005)3FIG. 3 Drying and

30、Purifying TubeFIG. 4 Absorption TubeE 191 64 (2005)4ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rig

31、hts, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for

32、 revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing

33、 you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.FIG. 5 Guard TubeFIG. 6 Mariotte BottleE 191 64 (2005)5This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).E 191 64 (2005)6