ASTM E191-64(2005)
(Specification)Standard Specification for Apparatus For Microdetermination of Carbon and Hydrogen in Organic and Organo-Metallic Compounds
Standard Specification for Apparatus For Microdetermination of Carbon and Hydrogen in Organic and Organo-Metallic Compounds
ABSTRACT
This specification covers the design requirements of each component and basic equipment comprising the apparatus used for the microdetermination of carbon and hydrogen in organic and organometallic compounds along the lines of the conventional method of Pregl, but with modifications more in line with modern practice. Due to the diversity of this apparatus by which correct results can be obtained, this specification is intended to indicate what is acceptable rather than what is mandatory. The components covered here are the oxygen supply, pressure, regulator, drying and purifying tube, flowmeter, combustion unit, absorption tubes, guard tube, Mariotte bottle, and weighing accessories.
SCOPE
1.1 This specification covers apparatus and basic equipment for the determination of carbon and hydrogen in organic and organometallic compounds along the lines of the conventional method of Pregl, but with modifications more in line with modern practice. Owing to the diversity of apparatus by which correct results can be obtained, this specification is intended to indicate what is acceptable rather than what is mandatory. Note 1Specifications for several items subsequently listed were developed by the Committee for the Standardization of Microchemical Apparatus, Division of Analytical Chemistry, American Chemical Society.
1.2 The values stated in inch-pound units are to be regarded as the standard. The metric equivalents of inch-pound units may be approximate.
General Information
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E191 – 64 (Reapproved 2005)
Standard Specification for
Apparatus For Microdetermination of Carbon and
Hydrogen in Organic and Organo-Metallic Compounds
This standard is issued under the fixed designation E191; 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 (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope 4. Pressure Regulator
1.1 This specification covers apparatus and basic equipment 4.1 The pressure regulator, shown in Fig. 1 and Fig. 2,
for the determination of carbon and hydrogen in organic and consisting of a bell and inlet tube submerged in a suitable
organometallic compounds along the lines of the conventional confining liquid, shall be used to supply air or oxygen, or both,
method of Pregl, but with modifications more in line with at constant pressure to the combustion system. Substitution of
modern practice. Owing to the diversity of apparatus by which a fine gas-control valve and flowmeter for the pressure regu-
correct results can be obtained, this specification is intended to lator is optional.
indicate what is acceptable rather than what is mandatory.
5. Drying and Purifying Tube
NOTE 1—Specifications for several items subsequently listed were
5.1 The conventional bubble-container U-tube shown in
developed by the Committee for the Standardization of Microchemical
Fig. 3 shall be used for drying and purifying the entering air or
Apparatus, Division of Analytical Chemistry, American Chemical Soci-
oxygen, or both.
ety.
1.2 The values stated in inch-pound units are to be regarded
6. Flowmeter
as the standard. The metric equivalents of inch-pound units
6.1 The rate of gas flow shall be determined by the bubble
may be approximate.
counter of the bubble-counter U-tube, or by a more accurate
flow-meter, such as the floating ball-in-column.
2. Referenced Documents
2.1 ASTM Standards:
7. Combustion Unit
E124 Specification for Weighing and Drying Apparatus for
7.1 The combustion unit shall consist of a long furnace, a
Microchemical Analysis
sample furnace, a constant-temperature heating mortar, a
E148 SpecificationforApparatusforMicrodeterminationof
combustion tube, and a combustion-tube closure.
Nitrogen by the Dumas Method
7.1.1 Long Furnace:
7.1.1.1 The long furnace shall have a maximum over-all
3. Oxygen Supply
length of 8 in. (203 mm) with the wall thickness at the ends not
3.1 Any cylinder or other suitable source of oxygen free of
to exceed ⁄4 in. (6 mm). The furnace shall accommodate
hydrogen and organic impurities may be used. Oxygen pre-
combustion tubes up to 13 mm in outside diameter. Electric
pared from liquid air is satisfactory.
heating elements shall be easily replaceable. The furnace shall
be mounted firmly on a substantial support.
This specification is under the jurisdiction of ASTM Committee E41 on
7.1.1.2 Thefurnaceshallbecapableofcontinuousoperation
Laboratory Apparatus and is the direct responsibility of Subcommittee E41.01 on
attemperaturesupto900°Casmeasuredinsidethecombustion
Apparatus.
tube at the middle of the furnace. The temperature drop from
Current edition approved May 1, 2005. Published October 2005. Originally
approved in 1962. Discontinued in 1988 and reinstated in 1989. Last previous the center to points 1 in. (25 mm) and 1 ⁄4 in. (45 mm) from
e1
edition approved in 1999 as E191 – 64 (1999) . DOI: 10.1520/E0191-64R05.
either end shall not exceed 15 and 7 %, respectively, based
Committee for the Standardization of Microchemical Apparatus. Division of
Analytical Chemistry,American Chemistry Society, 1949 Report on Recommended
Specifications for Microchemical Apparatus, Carbon-Hydrogen, Dumas Nitrogen,
Sulfur, and Halogen, Analytical Chemistry Vol 21, p. 1555 (1949).
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Furter, M. F., and Steyermark, A., “Pressure Regulator for Use in Microdeter-
Standards volume information, refer to the standard’s Document Summary page on mination of Carbon and Hydrogen,” Analytical Chemistry, Vol 20, 1948, p. 257.
the ASTM website. Kuck, J. A., and Altieri, P. L., “Spherical Ground-Glass Joints vs. Rubber
Withdrawn. The last approved version of this historical standard is referenced Tubing Connectors on the C and H Absorption Train,” Mikrochimica Acta, 1956 ,
on www.astm.org. p. 1556.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E191 – 64 (2005)
FIG. 1 Pressure Regulator, Glass Parts
upon the temperature in the middle of the furnace. Means manual setting at any point. Whether the furnace has only one
shall be provided for varying the temperature. or more than one speed of movement over this distance, the
1 5
7.1.1.3 The furnace shall be equipped with some device for rates of travel shall be within the limits of ⁄8 to ⁄8 in. (3 to 16
indicating the temperature at the middle of the furnace. mm)/min. An automatic control shall be provided to stop the
7.
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.