ANALYTICAL EDITION
212
FILTRATE. Evaporate the filtrate nearly to dryness, add 40 cc. of 6 N hydrochloric acid, and extract twice with 40 cc. of alcohol-free ether to remove the greater part of the iron. Evaporate the aqueous solution to complete dryness, dissolve in 12 cc. of 12 N hydrochloric acid, dilute to 400 cc., heat nearly to boiling, add 15 cc. of 3 per cent hydrogen peroxide to prevent the preci itation of titanium, and 20 cc. of a 10 per cent solution of sefenious acid. Allow to stand until any precipitate has coagulated. Filter, wash with hot water, and unite with the corresponding precipitate obtained from the residue below. RESIDUE. Ignite the siliceous residue in platinum. Treat with sufficient hydrofluoric acid (and two drops of concentrated sulfuric acid) to volatilize the silica. Evaporate to dryness and fuse with sodium carbonate. Extract with hot water, filter, wash tvith dilute sodium carbonate solution and then with hot water. Ignite the residue and fuse with potassium pyrosulfate. Dissolve in 100 cc. of hot water containing a few drops of sulfuric acid, make ammoniacal, filter, wash with hot water, and dissolve the precipitate in 25 cc. of 6 N hydrochloric acid. Dilute to 400 cc., heat nearly to boiling, add 15 cc. of 3 per cent hydrogen peroxide and 20 cc. of 10 per cent selenious acid solution, and allow to stand until the precipitate has coagulated. Filter, wash with hot water, and unite with the corresponding precipitate obtained from the main filtrate. Dissolve the combined precipitates in 50 cc. of 18 N sulfuric acid, dilute to 200 cc., warm to 50' C., add 20 cc. of 3 per cent hydrogen peroxide and 50 cc. of a 20 per cent solution of diammonium phosphate, precipitating zirconium phosphate. Allow t o stand 2 hours, filter, wash thoroughly with a 5 per cent solution of ammonium nitrate and ignite slowly. Gradually raise the temperature to the full heat of the Tirrill burner and weigh as ZrP207. RESULTSBY PROPOSED METHOD
In the analyses made by the proposed method, 3 grams of a plain carbon steel were dissolved and to the solution
Vol. 5, No. 3
were added measured amounts of zirconyI chloride solution corresponding to 0.11, 0.28, and 1.41 per cent of zirconium in the original steel. In addition, 20 mg. each of other metals in the form of solutions of their salts were added. The results obtained are shown in Table I. TABLEI. AXALYSISOF PLAIN CARBONSTEELSAMPLES BY THE SELENITE-PHOSPHATE METHOD (Sample = 3 grams) ZIRCONIUMF O U N D Zr present = Zr present = Zr present = 0.0034 gram, 0 0085 gram, 0 0423 gram, 0 11% 0.28% 1 41% Gram % Gram % Upam % 0 0033 0.11 0 0083 0 28 0 0424 1 4 1 0.0034a 0 . 1 1 0.0083a 0.28 0 0420 1 . 4 0
CONSTITUENTB ADDED Nolle
..
T i + + + +UOn , ++, VOa-
0.0032
.. t .
~7Oi--,Ti++++,UOn++,VOs-
.. ..
0.0086 0.29 0.0423
1.41
0 . 1 1 0.0086 0 . 2 9 0.0423 0.0087 0 . 2 9 0.0430 . . 0.0081 0 . 2 7
1.41 1.43
..
..
..
..
1.40
+ + +, VOa0 0033 0 . 1 1 0 0079 0 26 0.0424 Bureau of Standards cast iron No 74 (0 464 per cent P),
1.41
wo4--, Cr a
..
0.0420
,
LITERATURE CITED (1) Simpson, S. G., a n d S c h u m b , W. C., IND.ENQ.CHEM.,Anal. Ed., 5,40 (1933). (2) Simpson, S. G., and S c h u m b , W. C., J. Am. Chem. SOC.,53, 921 (1931). (3) Smith, M. M., and James, C., Ibid., 42, 1764 (1920). R E C E I V EFebruary D 24, 1933.
Windshield for Saybolt Viscometer FRANKJ. VITOVEC,JR. Research and Development Laboratories, Universal Oil Products Company, Riverside, Ill.
B
ECAUSE of air currents which cannot be readily avoided in a large laboratory, the use of a windshield
has been found desirable in the determination of the viscosity of lubricating or fuel oils. The fine stream of oil is otherwise blown out or around the opening of the cup. Temporary shields of cardboard have been utilized with rather unsatisfactory results.
FIGURE 2 FIGURE1
A neat and efficient shield (Figure may be t o fit beneath the American Instrument Company's Saybolt viscometer (Figure 2). Ordinary window glass, machine screws, piano hinges, and galvanized sheet iron may be
utilized. The shield is built around the cup holder and t h e glass may be easily removed for cleaning or replacement. The hinged doors give free access to the cups and may be closed at the start of the determination. RECEIVED March 20, 1933.
