V O L U M E 25, NO. 6, J U N E 1 9 5 3 The results obtained by the two methods of analysis agree quite well. DISCUSSION
This method of analysis has the same advantages of simplicity and rapidity as the method far the analysis of monazite sands of Banks and Byrd ( 8 ) . The separation of such small amounts of thorium from nsturally occurring mixtures of minerals and the precision attained confirms the analytical value oi this method. This method has not been extended to include analysis of noumonaeites. It has been established that the method will require some modification before it is applicable to these thaiiumcontaining 01e8.
993 ACKNOWLEDGMENT
The authors wish to express their appreciation to Reuben Kronstadt of the United States Bureau of Mines for providing the black sands samples used in this work. LITERATURE CITED
,
(1) Ayres, G. H., ANAL.CHEM., 21, 652-7 (1949).
(2) Banks, C. Y.. and Byrd. C . H., Ibid.,25,416-19 (1953). (3) Kronstadt, R., and Eberle, A. R.. Atomic Energy Commission. Re@. RMO-838 (1952). R ~ c s r v i nfor review January 19. 1953. looepted April 6 , 1953. Contribution No. 231. Institute for Atomic Research and Department of Chemistry. Iowa State College, Ames, Iowa. Work W&Q performed in the Ames Laboratory of the Atomic Energy Commission.
69. trans-Diethylstilbestrol Iontributed by AARRY A. ROSE, Eli Lilly & Co., Indianapolis, lnd., AND RALPH J. HINCH AND WALTER C. MCCRONE, Arm our Research Foundation of Illinois Institute of Technology, Chicago, Ill.
CR,
I
-.. 6H
H O - a - C =
I
.C
I
1 S t r u c t u r a l Formula of trans-Diethylstilbestml trans-Diethylstilbestrol forms solvates when recrystallized from chloroiorm, benzene, ether, 2-propanol, methanol, and acetic acid. These solvated crystals decompose readily under vacuum or on heating to give an anhydrous powder. Crystals formed by slow addition of hydrogen chloride to a basic aqueous solution are also hydrated. Anhydrous crystals suitable for opticd studies may he prepared by sublimation (Figuro 1). .The
powder x-ray pattern may he obtained on the sublimate or on the solvates after proper steps are taken to remove the solvent. CRYSTAL Mon~ao~dc~ Crystal System. Orthorhombio. Form and Habit. On sublimation long rods elongated parallel to e are formed (Fieure 2). Forms shown include the orisms I l l O l and 112Oi. ?he braohvdome 10111. the rnacrddames llOl!and {lhZ},andthebipyr;Lmid{lllj. .' Axial Ratio. 0.783: 1:0.277. Interfacial AnglesiPolar). 110 A ilO_= 103"51'. 120 A-iZO = 64'36'. 011 A011 = 149". 101 A101 = 141". 102A102 = 10920'. Cleavage. 001. OPTICALPROPERTIES Refractive Indices (5893 b.; 25" C.). LI = 1.594 f 0.002. P = 1.611 i0.002. Y = 1.73 f 0.01 (calculated from a,0, and ZV).
-4
,Figure 1.
Crystals Formed b y Sublimation in a Kofler Block
Figure 2.
994
ANALYTICAL CHEMISTRY Optio Axial Plane. 100. Golecular Refraction ( R ) (5893 A.:25' C.). = 1.645. R(calod.) = 80.7; R(absd.) = 82.7. X-RAYDIFFRACTION DATA Cell Dimensions. a = 15.01 A,; b = 19.18 A,; e = 5.32 A. Formula Weights per Cell. 4 (3.97 calculated from x-ray data). Fdrmula Weight. 268.34. Denrity. 1.1615 (Rotation and density halsnce); 1.1636 I~ .
a
~
FUSION DATA. trans-Diethylstilbestrol melts in the range Figure3.
Crystals fraJrn "lvlelt - ' Dietb-lstilbestml
Of"
trans-
i 6 9 " to 172' C. (Kofler hot stage) with considerable sublimation.
UnI cooling, large blades having negative elongation and parallel exitinction and showing an inclined Bx, figure are formed. The blaidesdevelop transversecracks on coolina (Figure3). ~~
Optic Axial Angles (58Q3 A,; 25' C.), 2H = (+)45'. 2V = (+)42' (calculated from B and2H). 2E = ( + ) i l ' . Dispersion. Strong v > r.
vations in Electroanalytical Chemistry. James J Linrane. th Bnnual Priestley Lectures. 61 pages. The Pennsylvania State College, S h t e College, Pa., 1953. Price, $2.00. The Priestley Lectures were inaugurated in 1927 a t the Pennsylvania State College primarily to establish a living memorial for Joseph Priestley, who spent his last years in Northumberland, Pa., and whose home and relics ase the property of the college. I n addition, the sponsors wished to honor a succession of American scientists and to demonstrate that theoretieal chemistry is a vital functional part of modern applied chemistry. This 27th lecture has admirahly fulfilled all these objectives. Before embarking on innovations in the field, Lingane gives a brief, lucid introduction to electroanalytical chemistry. This is followed by a detailed consideration of new eleetroanalytical techniques including polarographic, caulometrio, and eleotrographic analyses, and electro spot testing. Various modifioations of these methods, such as amperometric titration, controlled potential analyses, and the very recently reported coulogravimetric analysis, are also discussed. The theoretical basis upon which each of these techniques is founded is presented systematically and clearly. The practical application of electroanrtlytichl metbods is illustrated throughout with experimental d a h .
Progrls RBcents de la Chromatographie. Deuxisme Partie. Chimie Mindrale. Michael Lederer. 131 pp. Hermann & Cie, Paris, France, 1952. Price, 1200 francs. Applied belatedly to the examination of inorganic substances, Tswett's chromatographic analysis has now been widely applied to the resolution of mixtures of various inorganic materials. These applications me summarized clearly and concisely by Lederer, who has already mademany contributions in this field. His monograph follows the style of the earlier volume (Premihre Partie, 1949, by Edgar Lederer) which was devoted to chro,
Co KTRIBUTIDNB of orystdlogrsphio data for this
be sent to Research Foundation of
seotion should
W S,Iter C. MoCrone, lnalytioal Sectmn, Armour TI,. iz~rnoieInstitute oi Technology, Chicago 16, Ill.
matography in organic and biological chemistry. It includes separations n-ith inorganic and organic sorbents, with 1,artition sorbents, withpaper, and with ion exchange resins. It tirests the paper chromatography of the various analytical groups and the currently popular field of eleetrochromatography. The bibliogrrt-ohv " of 361 entries indicates the extensiveness of the subjeet. In spite of extensive investigation, chromatography has not provided a systematic analytical procedure for mixtures 01 many diffeIent inorganic substances. Multicomponent mixtures are commonly resolved into groups by conventional chemical methods, and these groups are then resolved by chromatography based upon sdsorption, partition, or ion exchange. Lederer's book surveys the chromatographic applications. I n this respect i t differs greatly from the recent monograph by 0. C. Smith, "Inorganic Chromatography," and from the brochure by Harriet Fillinger, "Chromatographic Analysis for the Metal Ions of a First Course in Qualitative Analysis," which stress particnlw N
The reviewer, along with man y others, recalls with gratitud e the apwarance of the first editioi1 of this book in 1931. Tippet,t .. J-A-:,-J -..---:A:-" ^ P d."L:-&:-~ was among the first to attempt a u~uaut.u r n p ~ u u VI ~ uD U ~ ~ L D U techniques that had been concisely set forth in R. A. Fisher's "Statistical Methods for Research Workers" (1925). Tippett's book has continued to he a favorite, even though now a. fairly long list of introductory books is available to the person starting from scratch in statistics. This new edition retains the merits of its predecessors. It is ahout a third longer through the inclusion of new material. The
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