ever, in the author's opinion, the use of calomel (yielding mercurous oxide) described in this chapter, provides the simplest and most efficient means
TOST? GLAZED
^ - 8 1 0 . 5 MM O.D.
I.5-2MM I.D.
FIG. 102. Mercury valve for carbon dioxide generator (pressure regulator) for use with dry ice—details of construction.
FIG. 103. Diagram of Gustin automatic modification. Combustion and absorption system. ( A ) Flow meter, 5 - 3 0 0 ml./min. flow range. ( B - l , B-2, and B - 3 ) Capillary stopcock, 2 mm. straight bore plug. ( C - l and C-2) Capillary stopcock, three way, 1 2 0 ° , 2 mm. bore plug. ( C - 3 ) Capillary stopcock, 2 mm. straight bore plug. ( D ) Synthetic rubber pressure tubing (neoprene), y± inch i.d., % inch o.d. ( E ) Combustion tube, 9 6 % silica, 7 mm. i.d., 9 mm. o.d. ( F - l and F-2) Sample furnace, movable split type, 2^ 2 3 inches long 1 2 1 3 mm. i.d. opening, at 850° C. ( F 3 ) Heater, 4 inches long at 4 0 0 -500° C. (micro C & H preheater type, A. H. Thomas Co., Philadelphia, Pennsylvania).
( G ) CuO wire, 2 0 - 6 0 mesh, ignited. ( H ) Pyrex glass-wool retainer. ( I ) Constant temperature tube, Pyrex, 8 mm. i.d., 10 mm. o.d., ca. 6 inches long. ( J ) Copper wire, 2 0 - 6 0 mesh. ( M ) Bar magnet, plastic covered, l/2 m cn long. ( N ) Absorption chamber, 36 mm. o.d., 6 inches high, 31/? inches to capillary column, side opening ca. 15 mm.
from base suitable for No. 2 rubber stopper. ( N A ) Capillary column, 2 mm. i.d., ca. 2 l /2
inches long, having a 1 mm. constriction in the column ca. 10 mm. long, reference line etched around mid-point of the constriction. § 1 2 / 2 socket joint top. ( N B ) Rigid side arm, 18 mm. o.d., top level with socket joint, 2 mm. i.d. capillary connection to absorp
tion chamber. ( R ) Natural rubber policeman, % inch i.d., τβ inch o.d., ca. 1 inch long, with 4 - 6 mm. slit cut in side, connected to capillary inlet, 2 mm. i.d. with J 1 2 / 2 socket joint. ( S ) Syringe, precision ground, 5 ml. capacity. ( V ) Direct reading counter, four digits, attached to syringe to show syringe displacement precisely to 0.001 ml.
177 Additional Information for Chapter 7
frothing is very bad—see Reagents. Niederl and N i e d e r l1 3 9-1 4 0 recommended heavy petroleum jelly and lanolin as a stopcock grease.
Instead of placing the sample in a porcelain b o a t ,2 5-4 8 weighed amounts of finely powdered substances have been placed in mixing tubes, fine copper oxide powder added, and the mixture transferred to the combustion tube using a dry w a s h .1 1'1 2'5 8'5 9'1 3 9-1 4 0-1 5 8-1 6 3-1 6 6 The author feels that this procedure is a
FIG. 104. Coleman nitrogen analyzer.
dangerous one, since materials that are slightly sticky or carry electrostatic charges cannot be always completely transferred.
A completely automatic combustion apparatus has been developed by G u s t i n6 1 - 6 3 (and now has become commercially available*3 0). Figures 103 and 104 show the diagram of Gustin's setup and a photograph of the commercial
* As this book goes to press the author has seen only a demonstration of the com
mercial u n i t3 0 and as yet one has not been delivered to his laboratory. Consequently, he can make no positive statement regarding these units.
model, respectively. Instead of the usual micronitrometer, a precision ground, 5 ml. capacity syringe is used in combination with a direct reading counter which makes it possible to read precisely to 0.001 ml. After the sample-packed combustion tube is attached, the automatic control is started. At the end of the cycle, the increased volume resulting from the combustion is read. W i t h this apparatus, Gustin completed six analyses per hour.
T A B L E 18
ADDITIONAL INFORMATION ON R E F E R E N C E S * RELATED TO C H A P T E R 7
Following the plan of previous chapters, additional information in the form of the listing of certain references is given in Table 18. (See statement at top of Table 4 of Chapter 1, regarding completeness of this material. ) f
General, miscellaneous
* The numbers which appear after each entry in this table refer to the literature citations in the reference list at the end of the chapter.
f T h e large number of articles on the Dumas determination indicate that the deter
mination is by no means "perfect." T h e author also again wishes to emphasize that both the Dumas and Kjeldahl (Chapter 8 ) methods should be constantly used, the one as a check on the other.
179 Table of References
Ohashi, Takayami, Taki, and Toya, 147 Polley, 154
T A B L E 18 (Continued)
Parks, Bastin, Agazzi, and Brooks, 152 Schôniger, 176
Parkin, Fernandez, Braun, and Rietz, 151 Poth, 156 Di Pietro, Sassaman, and Merritt, 36
Marble used as source of C 02
Salts other than marble used as source of C 02
181 References
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