ANALYTICAL CHEMISTRY
198
Optic Axial Angles (5893 A,; 25" C.). 2V = 52". 2E = 96"; 91" 33' (3). Dispemion. Axial dispersion with change of sign. Optic Axial Plane. 1010 with y A C = 6 " in acute 4. Sign of Double Refmct,ion. > 4070 A,, positive; < 4070, negative. Acute Bisectrix. BX. A c = 6" in acute p (X < 4070 A,); B X . I1 b (X A 4070 A,). Eutinction. y A c = 6" in acute p. Molecular Refraction (R) (5893 A,; 2.5" C.). g z = 1.758. R (ealcd.) = 59.2. R (obsd.1 = 65.5. F u x o s DATA tmns-Stilbene melts at 124125°C. with some tendency to sublime. The crystals of sublimate are usually rounded, hut show the characteristic rhomb shape with a 49-30, profile angle. The melt supercools somewhat, hut always solidifies spontaneously to give broad rods growing rapidly parallel to c with a sharp pointed crystal front (profile angle, 49"30'). The optical properties are consistent with the fact that only the view lying on 100 is shown.
F i g u r e 1. trans-Stilbene L d t . Large crystals from ethyl aloohol on dow ooolinp Right. Thvrnol mired fusion, crossed Niools
Axial Ratio. a:b:c = 2.77:1:2.17; 2.1702:1:1.4003 (8); 1.077:1:1.415 ( 1 ) . A o i l = 126" 30'. 113" 48'(6); 114" (4,6).
It is a pleasure to acknowledge the help of Miss Anne Humphreys in determining the powder x-ray diffraction spacings and intensities. LITERATURE CITED
b = 5.73 A,; e = 12.4:Z A. : 15.92 A. (6). a = 12.20 A.; a = 12.42 A,; b = 5.73 A,; e=16,0A.(4). a = 9 . 6 A . ; ' h ' = 8 . 9 A . ; c = 1 2 . 6 A . ( Z ) . Formula Weights per Cell. 4. Formula Weight. 180.24. Density. 1.131 (flotation); 1.166 (x-ray); 1.159 (4). i.;
Prinoipal Lines I/II
d
(1) Beeker, K.. and Rose, H.,Z. Physik, 14,369 (1923). (2) Bryant, W. M. D.,1.Am. Chem. Soc.. 65. 96 (1943). (3) Groth, "Chemisehe Kristsllographie," Vol. 5. p. 192, Leipuig. Engelmann, 1919. (4) Hengatenberg. J., and Mark. H., Z. Krist., 70, 283 (1929). (5) Prssad, M., Phil. Mag.,16, 639 (1933). (6) Robertson, J. M., and Woodward, J., Pioc. Roy. SOC.London, (A) 162. 568 (1937).
I/Ii
d
Textile Testing, Physical, Chemical and Microscopic. John H. Slcinkle. 2nd edition. xii 353 pages, Chemical Publishing Co., Inc., 26 Court St., Brooklyn, N. Y., 1949. Price, $7.75.
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Figure 2. Orthographic Projection of Typical Crystal of trans-Stilbene
OPTICALPROPERTIES Refractive Indexes (5893 A,; 25" C.). 4 = 1.728 * 0.002; y = 1.844 * 0.005.
a =
1.704
+
0,002;
Dispersion D a t a by B r y a n t ( 2 ) Wave Length
a
3650
(1.797) 1,769 1.751 1.726 1.712 1.706
4047 4358
4916
5461
5780 6234 6908
P (1.975) (1.864) (1.823)
1.772 1.743 I.732
1.699
1.721
1.691
1.708
7
2V.'
(2.03)
53
(1.873)
90 80.5 67 57.5
(1.940) 1.893
1.860 1.848 1.835 1.818
53.5
50 45
The second edition of this little hook has gained through the addition of new material, the revision of old, and a distinct improvement in format. No change has been made in the outline of the hook, hut the section a n statistical methods has been revised and the sections on water resistance and identification of organic finishing agents have been rewritten. The methods for analysis of fiber mixtures and microscopic identification of fibers include the newer commercial fibers. Curiously, the second edition like the first contains no information on the widely used and extremely important tests for color fastness t o light, laundering, perspiration, etc., and no explanation is given for the omission of these tests. The revision of the references t o literature, listed a t the end of each chapter, t o include more recent publications is commendable, but the gap between the date of the latest reference, 1945, and the date of publication of the book, 1949, presumably attrihutahle to conditions in the printing industry, is to be deplored. The book is in general clearly and oaneisoly written. It contains a surprising amount of useful information and should be of increased value, especially to students, WM. D. AWEL
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Practical Spectroscopy. C . Candler. viii 190 pages. Hilger and Watts, Ltd., 98 St. Pancras Way, Camden Road, London, N.W. 1, England, 1949. Price, $6.10, This book was written partly t o provide instruction for purchasers of the Hilger wave-length spectrometer and partly as an introduction to general spectroscopy. The first purpose is ful-
V O L U M E 2 2 , N O . 1, J A N U A R Y 1 9 5 0 filled amply; the second purpose leaves much to be desired. The topics treated are qualitative and quantitative spectrochemical analysis, absorption spectra, infrared and Raman spectra, interferometers, and the structure of line spectra. Candler presents the basic principles of each topic in a brief and elementary form, listing some fundamental experiments and a bibliography. The treatments of the topics and subtopics show considerable variation-for example, Candler describes the measurement of wave lengths rather fully, including even the use of Edser-Butler plates, R hile his discussions of light Sources and sensitometry are much too limited to be of practical or educational value. Much of the theory and application is oversimplified and the bibliographies a t the end of each section are incomplete, particularly in so far as developments since 1941 are concerned. The contributions of Sawyer, Duffendack, OMens, Enns, Dieke, Kaiser, and Barnes, to name only a few, are conspicuous by their absence from the text as well as the literature references. These defects limit the usefulness of the book to the first intended purpose of the publishers as mentioned above. Laboratory analysts and practical spectroscopists will find little new information of practical value in thiq hook JICOB CHOLAK Physical Methods of Organic Chemistry. -1. W’eissberger, editor. Part I. 2nd ed. ix 1072 pages. Interscience Publishers, Inc., 215 Fourth dve., Selv Tork 3, ?;. T . , 1949. Price, 512.50.
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This volume is nearly half again as large as the first edition. Three chapters (X-Ray Diffraction, Electron Diffraction, and Refractometry) have been moved forward into a forthcoming Part I1 and four chapters have been added: Temperature Measurement; Temperature Control (both by J. Ll. Sturtevant); Determination of Vapor Pressure iG. W.Thomson); and Determinations with the Ultracentrifuge (J. B. Sichols and E. D. Bailey). Ten of the original chapters have been more or less revised: Melting and Freezing Temperatures (E. L. Skau, H. Rakeham) ; Boiling and Condensation Temperatures (W. Swietoslawski and J. R. Anderson); Density (S. Bauer); Solubility (R. D. Vold and M. J. Vold); Surface and Interfacial Tension (IT. D. Harkins) including a section on the Parachor by G. W. Thomson; Properties of Monolayers and Duplex Films (W. D. Harkins); Calorimetry (J. 11.Sturtevant) : Microscopy ( E . E. Jelley) ; Crystal Form (hl. A. Peacock) ; and Crystallochemical Analysis (J. D. H. Donnay). Three chapters have been rewritten: Viscosity (T. E. hlcGoury and H. Mark); Osmotic Pressure iR. H. Wagner); and Diffusivity (-i. L. Geddes). The treatment of each chapter varies with the scope of the topic covered; some chapters are more theoretical than others;
199
thus density requires only t\!o OI tliier pages of theory, whereaa vapor pressure requires nearly forty for adequate treatment. The authors of the various chapters and the editor must be commended both for achieving their stated purpose and for maintaining throughout what is probably an optimum balance between theorl and description. Any chemist, organic or otherwise, who aants to learn a lot about an instrumental technique 01 the theory behind it, or who wants to build good equipment, will find this authoritative invaluable. It is well illustrated and documented, and save t o r one or two minor duplications--e.g., pages 581 and 648-4 is vw 1 uell edited The reviewei’h copy spends little time on the lihrari shelf.
THOMAS R. P. GIBB, JR Manual of Spectroscopy. Theodore A . Cutting. 220 pager. Chemical Publishing Co., Inc., 26 Court St., Brooklyn, 1.Y., 1949. Price, $6.50. This manual, the author says, “has been written to assist tliusr who v h h to analyze ores, minerals, alloys and inorganic chemicals. or wish to teach others to do so.” The contents suggest that aiiy amateur mineralogist, can find $10,000 \vorth of uranium wit11 a $2.50 spectroscope! The history and theory of spectroscopy are presented in 6 scant pages, light sources in 11, spectroscopes in 38, and spectroscopic analysis in 30. The next 85 pages deal with elementary mineralogy and visible spectral lines of 70 elements including such nonspectroscopic material as the discovery, sources, uses, properties. and prices of elements. (The paragraphs on illinium and masurium are obsolete, and the price of xenon is grossly inflated a t 5600 per liter.) The last 38 pages give approximate wave lengths arid intensities of strong linea selected from “M.I.T. Wavelength Tahles.” 1 bibliography of 16 items contains 8 works on mineralogy (from 1907), a manual of clinical therapeutics, and the Smyth Report, hut ignores all spectroscopic publications since 1939. Obviously, this book will not be of use to anyone escept possibly thr tyros for whom it was written.
WILLIAMF. MEGGERC
laboratory and Workshop Notes In the review of “Laboratory and Workshop Notes,” by liutli Lang [ANAL.CHEM.,21, 1431 (1949)], i t was stated that the Institute of Physics is to receive the royalties on the hook In the case of this and other books, the royalties go to the Renewlent Fund of the Institute of Physics, set up to help physiri\t. and their dependents who find themselves in strained cBir ( n n i stances because of some miqfortune.
Fifth Southwest Regional Meeting HE Fifth Southwest Regional Meeting, sponsored by the
Tthree was Oklahoma Sections of the AMERICANCHEMICAL SOCIETY, held December 8 to 10 in Oklahoma City. Abstracts of the papers presented before the Section on Analytical Chemistry are given below. Colorimetric Determinations of Oxidizing -igents Using the Cadmium Iodide-Linear Starch Reagent. PAULARTHUR, THosr.is E. MOORE,A N D JACK LAVBERT,Oklahoma 4 . and X4. College, Stillwater, Okla. A stable starch-iodide reagent, using cadmium iodide and the linear A (butanol-precipitated) starch fraction isolated by Schoch, has been developed for the quantitative determination of osidizing agents. This reagent is stable indefinitely toward atmospheric ouygen, diffused sunlight, and the growth of microorganisms. The reagent responds to oxidizing agents according to the pH of t h e solution. Weak oxidizing agmts, such as selenious acid, are
reduced only in highly acid solutions, whereas stronger oxidiziiig agents, such as hypochlorite, react even in neutral solution. The blue starch-iodine color produced shows maximum absorption at about 615 mp and obeys Beer’s law closely when absorption i* plotted against concentration of the oxidizing agent. Permanent outside standards for the linear starch-iodine blur color can be prepared by adding a small amount of potassiuni chromate to a solution of nickel hexammine sulfate and making the proper dilutions, always keeping the solutions concentratell with ammonium hydroxide. A colorimetric method of analysis for trace amounts of seleriiurii (as HPSe03)in water has been developed using the cadmium iodide-linear starch reagent. The reagent is also used in a nirthod being developed for the determination of minute concentration. of chlorine in water in the presence of chloramines. Biochemical Oxygen Demand of Some Common Organic Coinpounds Present in Chemiral Wastes. E. R. STROSG,JR.,C. I.
