ASTM E191-64(1999)e1
(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
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 1-Specifications 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.
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Designation: E 191 – 64 (Reapproved 1999)
Standard Specification for
Apparatus For Microdetermination of Carbon and
Hydrogen in Organic and Organo-Metallic Compounds
This standard is issued under the fixed designation E 191; 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 (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.
e NOTE—Keywords were added editorially in March 2000.
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 conisting 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
E 124 Specification for Weighing and DryingApparatus for
7.1 The combustion unit shall consist of a long furnace, a
Microchemical Analysis
sample furnace, a constant-temperature heating mortar, a
E 148 Specification for Apparatus for Microdetermination
combustion tube, and a combustion-tube closure.
of Nitrogen by 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.
7.1.1.2 Thefurnaceshallbecapableofcontinuousoperation
This specification is under the jurisdiction of ASTM Committee E-41 on
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 June 15, 1964. Published August 1965. Originally
the center to points 1 in. (25 mm) and 1 ⁄4 in. (45 mm) from
published as E 191 – 62. Last previous edition E 191 – 62 T. Discontinued in 1988
and reinstated in 1989.
Committee for the Standardization of Microchemical Apparatus. Division of
Analytical Chemistry,American Chemistry Society, 1949 Report on Recommended Furter, M. F., and Steyermark, A., “Pressure Regulator for Use in Microdeter-
Specifications for Microchemical Apparatus, Carbon-Hydrogen, Dumas Nitrogen, mination of Carbon and Hydrogen,” Analytical Chemistry, Vol 20, 1948, p. 257.
Sulfur, and Halogen, Analytical Chemistry Vol 21, p. 1555 (1949). Kuck, J. A., and Altieri, P. L., “Spherical Ground-Glass Joints vs. Rubber
Annual Book of ASTM Standards, Vol 14.04. Tubing Connectors on the C and HAbsorption Train,” Mikrochimica Acta, 1956, p.
Discontinued, see 1987 Annual Book of ASTM Standards, Vol 14.02. 1556.
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E 191 – 64 (1999)
FIG. 1 Pressure Regulator, Glass Parts
either end shall not exceed 15 and 7 %, respectively, based manual setting at any point. Whether the furnace has only one
upon the temperature in the middle of the furnace. Means or more than one speed of movement over this distance, the
1 5
shall be provided for varying the temperature.
rates of travel shall be within the limits of ⁄8 to ⁄8 in. (3 to 16
7.1.1.3 The furnace shall be equipped with some device for
mm)/min. An automatic control shall be provided to stop the
indicating the temperature at the middle of the furnace.
travel of the sample furnace when it reaches the long furnace.
7.1.
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