Selenium in determination of nitrogen by Kjeldahl method - Analytical

Selenium in determination of nitrogen by Kjeldahl method. J. Tennant, H. L. Harrell, A. Stull. Ind. Eng. Chem. Anal. Ed. , 1932, 4 (4), pp 410–410. ...
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Vol. 4, No. 4

ANALYTICAL EDITION

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FIGURE 4. TOP VIEW OF UNIT OF RACK

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A , glass T; B , rubber tubing. C, clamp; D ,stopoook; E , suotiod flask

FIGURE 5. SIDEVIEW OF UNITOF RACK top view of one of the units, and Figure 5 is a side view of A , glass T; B , rubber tubing; C, clamp; D,stopoook: E , suction flask the same unit. As now constructed, the rack is composed of eight such units (Figure 6). The frame is constructed tubing, glass T connections, and flasks. The individual of ordinary 8/4-inch lumber finished with a heavy coat of stopcocks afford several conveniences: The rack may be shellac as protection against used for less than the usual moisture. I n Figure 5 n u m b e r of s a m p l e s b y the i n c l i n e d shelf may be simply t u r n i n g off the unseen. Upon this shelf the used units, or, if a few sammanifold a n d s t o p c o c k s ples filter before the others are mounted by means of the group, they may be of brass clips. T h e shelf c u t o u t a n d a l l of t h e serves a double purpose in vacuum utilized in speeding that it affords a m e a n s of up the remaining ones. securing the parts and I n addition to its present helps to p r e v e n t p o s s i b l e use, it is quite possible that c o n t a m i n a t i o n of the filt h e rack^ m a y b e used i n FIGURE 6. FILTER RACKOF EIGHTUNITS trates should they spray or connection with other filterfoam up into the connecting ing devices such as Biichner tubes. Flasks of 250 ml. capacity are used, and since 200 funnels, conventionally mounted in the mouths of the filter to 700 ml. of filtrate are required, the flasks have to be emptied flasks. Uneven distribution of vacuum may easily be cleared several times. This is accomplished easily, as the filters are up by inserting additional T’s a t convenient places in the disconnected from the flasks and removed in a group, leaving manifold; one connection a t each end is used a t present. the flasks completely accessible from the front and in posi- The number of units in the rack may be varied to suit the intion to be disconnected with an ease comparable to that dividual need of the user. of breaking an electrical connection by means of the conLITERATURE CIT~D ventional attachment plug. After emptying, the flasks are (1) Olmstead, L. B., Alexander, L. T., and Middleton, H. E., U. S . replaced in the same manner. Since the rubber connections Dept. Agr., Tech. Bull. 170 (1930). are securely fastened and in individual units, the analyst is spared the confusion attached to the usual tangle of loose RECEIVED June 27, 1932.

Selenium in Determination of Nitrogen by Kjeldahl Method J. TENNANT, H. L. HARRELL, AND A. STULL, New York Hospital, New York, N. Y. AURO (a), from results on cereal extracts, has suggested the use of selenium in place of copper sulfate as a catalyst to reduce the time of digestion in Kjeldahl nitrogen determinations. I n the aqueous extracts used in the Allergy Clinic of the New York Hospital, standardization is based on the nitrogen content as determined by the conventional Kjeldahl method ( I ) . As the digestion of these extracts required several hours, Lauro’s modification was applied to their standardization. It will be evident from Table I khat these extracts are of wide variety. Analyses of extracts, on which parallel nitrogen determinations were run using copper sulfate and amorphous precipitated selenium, showed checking results with a decrease of one-half to two-thirds the time necessary for digestion where selenium was used. Owing to the variation in burners and the fact that heating in some cases was carried on longer than necessary in order to assure complete digestion, the time factor is not absolute. The results were considered sufficiently conclusive to adopt the modification in these analyses.

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T A B LI.~ ANALYSESOF EXTRACTS EXTRACT

COPPERSWLFATE M g . N/cc.

Date

0.53

Pumpkin Potato flour

0.17

Horse epithelium

Green pepper Guinea p1.g epithelium Pumpernickel Birch pollen Ash pollen Oak pollen Poplar pollen Plantain pollen Ragweed pollen 1 Ragweed pollen 2 Ragweed pollen 32 Timothy pollen 31 Timothv Dollen 32 Cashew-nit Urjne 1 Urine 2

0.07 0.04 0.26 0.88 1.26 0.58 0.43 0.58 0.92 1.00 0.43 0.39 0.98 0.62 0.31 0.40 3.73 7.29 9.85

Min.

IS0 150 300 165 140 140 175 170 215 180 170 166 170 135 180 75

SELENIWM Mg. N / c c . Min. 0.56 0.53 0.18 0.06 120 0.27 0.86 1.26 0.56 0.42 0.60 0.94 1.00 0.46 0.37 0.99 0.63 0.32 0.40 3.72 7.26 9.90

(1) Assoc. Official Agr. Chem., Methods, 2nd ed., 1925. (2) Lauro, M. F., IND.ENO.CHBM.,Anal. Ed., 3,401 (1931). REC~IVED May 3, 1932.

75 150 90 50 75 136 85 135 90 95 90 90 60 150 35