ASTM E147-61(2006)

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.

General Information

• Status: Historical
• Publication Date: 31-Oct-2006
• ICS: 71.040.20 - Laboratory ware and related apparatus
• Technical Committee: E41 - Laboratory Apparatus
• Drafting Committee: E41.01 - Laboratory Ware and Supplies

Relations

• Replaces: ASTM E147-61(2001) - Standard Specification for Apparatus For Microdetermination Of Nitrogen By Kjeldahl Method
• Effective Date: 01-Nov-2006
• Replaced By: ASTM E147-61(2011) - Standard Specification for Apparatus for Microdetermination of Nitrogen by Kjeldahl Method
• Effective Date: 01-Dec-2011
• Referred By: ASTM E1377-99(2022) - Standard Specification for Laboratory Glass Kjeldahl Flasks
• Effective Date: 01-Nov-2006

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E147 – 61 (Reapproved 2006)
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.
TABLE 1 Digestion Flasks
1. Scope
Capacity, mL Figure Use
1.1 This specification covers digestion and distillation ap-
10 1 with digests of 1 mL or less
paratus used for the microdetermination of nitrogen by the
30 2 with digests of 1 to 4 mL
Kjeldahl method, and modifications thereof at atmospheric
30 (Soltys) 3 with digests of 1 to 4 mL when
pressure.
danger of spattering is
great.
NOTE 1—This specification is based on those originally developed by
the Committee on Microchemical Apparatus, Division of Analytical
2
Chemistry, American Chemical Society.
Specification E124, are recommended for use with waxy and nonvolatile
liquid samples.
2. Referenced Documents
3
2.1 ASTM Standards:
5. Digestion Rack
E124 Specification for Weighing and Drying Apparatus for
5.1 The micro Kjeldahl digestion rack shall be portable and
Microchemical Analysis
shall consist of flask heaters (either gas or electric), a flask
support,andafumeduct.Therackshallbesuppliedwithaheat
3. Tolerances
deflector mounted under the burners to prevent overheating of
3.1 The following commercial length tolerance shall be
the bench top.
adhered to, unless otherwise specified:
Up to 10 mm 61mm
10 to 100 mm 62mm
100 to 200 mm 63mm
200 mm 64mm
4. Digestion Flasks
4.1 Digestion flasks of three types shall conform to the
requirements prescribed in Table 1 and Fig. 1, Fig. 2, and Fig.
3. The flasks shall be made of shock-resistant glass with linear
−7
coefficient of expansion not greater than 33.5 310 cm/cm
·°C.
NOTE 2—The weighing tubes described in Specification E124 Figs.
12–14 are recommended for introducing solid samples into the micro
Kjeldahl digestion flasks. Combustion boats, Fig. 1 and Fig. 2 of
1
This specification is under the jurisdiction of ASTM Committee E41 on
Laboratory Apparatus and is the direct responsibility of Subcommittee E41.01
Apparatus.
Current edition approved Nov. 1, 2006. Published December 2006. Originally
approved in 1959. Last previous edition approved in 2001 as E147–61 (2001).
DOI: 10.1520/E0147-61R06.
2
Committee on Microchemical Apparatus, “Recommended Specification for
MicrochemicalApparatus, Micro Kjeldahl Nitrogen,” Analytical Chemistry,Vol 23,
1951, p. 523.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. FIG. 1 10-mL Kjeldahl Flask
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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E147 – 61 (2006)
5.1.1 Heaters—The source of heat may be either electric or
gas. In operation, each heater shall supply sufficient heat to a
30-mL flask to cause 15 mL of water at 25°C to come to a
rollingboilinnotlessthan2ormorethan3min.Adeviceshall
be provided for regulating the amount of heat supplied to the
flask so that these conditions can be met. The amount of heat
supplied to the flasks also shall be so adjustable that low-
temperature digestions are possible. Switches and controls
shall be conveniently located and shall remain cool enough to
handle even after long periods of operation.
NOTE 3—Boiling chips shall be added when testing the heaters to
minimize superheating, and the burners and rack shall be at equilibrium
temperature.
5.1.2 FlaskSupport—Thesupportonwhichthebulbsofthe
flasks rest shall shield the necks of the flasks from excessive
heating during digestion and shall be provided with circular
openingsnotexceeding26mmindiameter,centeredovereach
heater.
5.1.3 Fume Duct—The fume duct shall provide means for
adequately removing the fumes evolved during the digestion
andshallsupportthenecksoftheflasksatananglegreaterthan
35° to the horizontal. Fume ducts meeting these specifications
FIG. 2 30-mL Kjeldahl Flask areshowninFig.4andFig.5.ThefumeductillustratedinFig.
4 is supported and held in place by suitable clamps mounted at
either end of the digestion rack. The fume duct in Fig. 5 rests
upon a circular support plate and is held in place by springs
from the plate to the four glass hooks. The concave center
permits clearance for the nut which fastens the support plate to
the center support post.
6. One-Piece Distillation Apparatus
6.1 The one-piece model distillation apparatus shall con-
...