V O L U M E 20. NO. 7. J U L Y 1 9 4 8
6S7
dioxide in the samples by gravimetric assay (empirical faotor 1.1500) were (1) 99.06. (2) 98.57, (3) 97.77. and (4) 96.68: by volumetric assay (Diehl-Topf, uncorrected) '(1) 96.46, (2) 95.19, (3) 94.65, and (4) 90.33. Obviously, the Diehl-Topi assays were low. The corrected percentages of active oxygen in the samples (empirical oxygen equivalent, 0.78 gram per liter) were (1) 6.30, (2) 6.25, (3) 6.27, and (4) 5.92. Free lead monoxide was assayed by an improved extraction method. The results were negative, except sample 4 which contsined 1.82%. Total water was assayed by an improvised absorption method and canfirmed,by the Penfield method. The averaged percentages obtained were (1) 0.38, (2) 0.76, (3) 0.86, and (4) 0.67. Residual water in lead dioxide at 225" C . was found t o be approximately 0.22% (average of samples 1 , 2 , and 3). The percentages of gravimetric nonlead substance and silica. in the samples were (1) 0.73, (2) 0.83, (3) 1.26, and (4) 0.57. Oxygen deficiencies occurred in. all the samples and are best ahown approximately by the empirical formulas (1) PbOi.,r, (2) PbOl.az, (3) P b O m , and (4) Pb0l.m From the averaged formula PbOt.lb the tentativegrwimimetricfmtor (lead dioxide), 1.1500, and and the active oxygen decinormal equivalent 0.78 gram per Mer were calculated. The grayimetric and Kinch summations of analysis w-ere within the limits, 99.75 and 100.60'%, assigned for satisfactory mineral analyses. LITERATURE CITF"
L., "Applied X-Rays," 3rd ed.. p. 362. New York, McGrzw-Hill Book Co., 1940. Cumming and Xaye, "Quantitative Chemical Andysis," p. 241. 7th ed. rev.. New York, D. Van Nostrand Co., 1939. Day, T. J., and Sohrenk, W. T., School Mines Met. Univ. M i s souri, Bull. Teeh.Ser. 2, No. 10, 31-6 (1935). Dennstedt, M., and Hassler, F., Ber., 45. 1197 (1910). Diehl-Topf, U. S. Bur. Standards. Ci7.c.90 (May 25,1922). Hawkins and Hawkins, Am. I.Science, 38,165 (1889). Hillebrernd, W. F., "Analysis of Silicate and Carbonate Rocks," U. S. Geol. Survey, Bull. 305 (1907). Hillebrand, W. F., and Lundell, G. E. F., "Applied Inorganic Analysis." p. 181,Xth print.. New York, John Wiley & Sons: London, Chapman & Hall, 1944. Ibbotson and Aitohison. "Analysis of Non-Ferrous Ailoya," New York, Longmans, Green and Go., 1915. Kinch,E., M i n e d o ~ . M a g . 7.63 , (1886). LeBlano, M., erndEbereus, E., Z.ana2. Chem., 89.81 (1932). L6we, J.,DiwlersPolylech. I.. 271.472 (1889). Lunge and Bed, "Tech. Chem. Research Methods," Vol. 8, 797 (1924). rewritten and revised by Ernst Bed, Berlin, J. Springer, 1921. Lux, A,, 2. anal. Chem., 19, 153 (1880). Mellor J. W.. "Higher Mathematictics for Students of Chemistry and Physios," pp. 548-9, New York, Longmans, Green and Co., 1922. Mrgudioh, J. N., and Clark, G. L., Im. END.C ~ E MANAL. ., Eo., 9, 256 (1937). Nissensen and Dennell, 2.elekt. chen., 9,760 (1903). Noyes and Bray, Tech. &uar.terly, 19,235 (1906). Pamfilov, A. V., and IvanEove, E. G., Z . anal. Chen., 88, 23 (1932). Reinders, R., andHamberger, L.. Z.anorg. Chem.. 89, 71 (1914). Sand, Chem. News, 100.264 (1909). "T ' l " l ~ ~ ~ l ~ ~>~~~,", l ' " Vol. 1. p. Clerk. G.
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