ASTM E147-61(2011)
(Specification)Standard Specification for Apparatus for Microdetermination of Nitrogen by Kjeldahl Method
Standard Specification for Apparatus for Microdetermination of Nitrogen by Kjeldahl Method
ABSTRACT
This specification covers the design and dimensional requirements for the digestion and distillation apparatus used for the microdetermination of nitrogen by the Kjeldahl method, and modifications thereof at atmospheric pressure. This apparatus is comprised primarily of digestion flasks, micro Kjeldahl digestion rack, one-piece model distillation apparatus, and Pregl (Parnas-Wagner) type distillation apparatus.
SCOPE
1.1 This specification covers digestion and distillation apparatus used for the microdetermination of nitrogen by the Kjeldahl method, and modifications thereof at atmospheric pressure.
Note 1—This specification is based on those originally developed by the Committee on Microchemical Apparatus, Division of Analytical Chemistry, American Chemical Society.
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Designation:E147 −61 (Reapproved 2011)
Standard Specification for
Apparatus for Microdetermination of Nitrogen by Kjeldahl
1
Method
This standard is issued under the fixed designation E147; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
Specification E124, are recommended for use with waxy and nonvolatile
1. Scope
liquid samples.
1.1 This specification covers digestion and distillation ap-
5. Digestion Rack
paratus used for the microdetermination of nitrogen by the
Kjeldahl method, and modifications thereof at atmospheric
5.1 The micro Kjeldahl digestion rack shall be portable and
pressure.
shall consist of flask heaters (either gas or electric), a flask
support,andafumeduct.Therackshallbesuppliedwithaheat
NOTE 1—This specification is based on those originally developed by
the Committee on Microchemical Apparatus, Division of Analytical deflector mounted under the burners to prevent overheating of
2
Chemistry, American Chemical Society.
the bench top.
5.1.1 Heaters—The source of heat may be either electric or
2. Referenced Documents
gas. In operation, each heater shall supply sufficient heat to a
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2.1 ASTM Standards:
30-mL flask to cause 15 mL of water at 25°C to come to a
E124Specification for Weighing and Drying Apparatus for
rollingboilinnotlessthan2ormorethan3min.Adeviceshall
Microchemical Analysis
be provided for regulating the amount of heat supplied to the
flask so that these conditions can be met. The amount of heat
3. Tolerances
supplied to the flasks also shall be so adjustable that low-
3.1 The following commercial length tolerance shall be temperature digestions are possible. Switches and controls
adhered to, unless otherwise specified:
shall be conveniently located and shall remain cool enough to
handle even after long periods of operation.
Up to 10 mm ±1 mm
10 to 100 mm ±2 mm
NOTE 3—Boiling chips shall be added when testing the heaters to
100 to 200 mm ±3 mm
minimize superheating, and the burners and rack shall be at equilibrium
200 mm ±4 mm
temperature.
4. Digestion Flasks
5.1.2 FlaskSupport—The support on which the bulbs of the
4.1 Digestion flasks of three types shall conform to the
flasks rest shall shield the necks of the flasks from excessive
requirements prescribed in Table 1 and Fig. 1, Fig. 2, and Fig.
heating during digestion and shall be provided with circular
3. The flasks shall be made of shock-resistant glass with linear
openingsnotexceeding26mmindiameter,centeredovereach
−7
coefficient of expansion not greater than 33.5×10 cm/cm
heater.
·°C.
5.1.3 Fume Duct—The fume duct shall provide means for
adequately removing the fumes evolved during the digestion
NOTE 2—The weighing tubes described in Specification E124 Figs.
andshallsupportthenecksoftheflasksatananglegreaterthan
12–14 are recommended for introducing solid samples into the micro
Kjeldahl digestion flasks. Combustion boats, Fig. 1 and Fig. 2 of 35° to the horizontal. Fume ducts meeting these specifications
areshowninFig.4andFig.5.ThefumeductillustratedinFig.
4 is supported and held in place by suitable clamps mounted at
1
This specification is under the jurisdiction of ASTM Committee E41 on
either end of the digestion rack. The fume duct in Fig. 5 rests
Laboratory Apparatus and is the direct responsibility of Subcommittee
upon a circular support plate and is held in place by springs
E41.01Apparatus.
Current edition approved Dec. 1, 2011. Published December 2011. Originally
from the plate to the four glass hooks. The concave center
approved in 1959. Last previous edition approved in 2006 as E147–61 (2006).
permits clearance for the nut which fastens the support plate to
DOI: 10.1520/E0147-61R11.
the center support post.
2
Committee on Microchemical Apparatus, “Recommended Specification for
MicrochemicalApparatus, Micro Kjeldahl Nitrogen,”AnalyticalChemistry,Vol 23,
6. One-Piece Distillation Apparatus
1951, p. 523.
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.1 The one-piece model distillation apparatus shall con-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
form to the requirements of Fig. 6. The steam-generator vessel
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. illustrated in Fig. 7 and the immersion heater in Fig. 8 are
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E147−61 (2011)
TABLE 1 Digestion Flasks
Capacity, mL Figure Use
10 1 with digests of 1 mL or less
30 2 with digests of 1 to 4 mL
30 (So
...
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