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72. dlBinic Acid I Contributed by JOHN KRC, JR., Armour Research Foundation of Illinois Institute of Technology, Chicago 16,111. Prinoipal Lines d In, 6.53 6.22 5.85 5.59 5.06 4.51 4.22 3.87 3.74 3.01 3.43 3.24 3.11 2.87 2.84 2.70 2.72 2.62 2 55 2.39 2.29 2.25 2.20 2.18 2.08 2.00
H,C-C-CH, ,CH2C02H
.&, I
Structural Formula for F'inic Acid ECENT
research conducted by the Bureau of Agricultural and
fi Industrial Chemistry, U. S. Department of Agriculture,has
shown that excellent synthetic lubricants for turbojet engines can be made from pinic acid. The Department of Agriculture has contracted with Armour Research Foundation to study methods for producing pinic acid from or-pinene, one of the components of turpentine. The crystals of pinic rtcid used for this orystallagraphic description were furnished through the cooperation of Frank Hollowav. Jovce Anderson and Walter Rodin forindntion rnemnnn~l
a
6 5
1
10 7 9 9 1
4 3 1 1 5 3 3 3 5 2 3 3
'C
1
2
1 1 1
1
Formula Weights per Cell. 4. Formula Weight. 186. Density. 1.23 (flotation and density balance); 1.21 (x-ray), CRYSTAL MORPHOLOGY C r y s t a l System. Monoclinic. Orthographic ProForm a Typical dl-Pinie Acid Rods and 1 I Crystal gated parall el to b lying on orthopiiiacoid llOO} or basal pi,iacoid [ 001 I showing paNsitive bemipyramid [ 1IT). Axial Ral,lo. a:b:c = 1.983:1:1,52_9, Interfacia., 1 Anrrla. f P A a m ~ 1 1 1 ~ 1 1 1 - , n o . , rnnanni 114"; lOOAOOl = 66". Beta Angle. 114'. Clesvaee. Poor. OPTICALPROPERTIES Refractive (5893 A.; 25' C.). a = 1.452 =t0.002. c.* , Indices nnnn
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II
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Excellent crystals of dkpinic acid I can he obtained by recrystallization on a macro scale from water, ethyl alcohol, acetone, ether, and chloroform. Recrystallization upon a microscope slide is usually difficultbecause of the tendency of this compound to supercool and because crystal growth proceeds very slowly. Figure 1 shows crystals of d2-piuic acid I from water; Figure 2 is an orthographio projeotion of a typical dl-pinic acid I crystal.
Figure 3. dt-Pinio Acid 111 Crystallizing fmm Supercooled Melt
DIFFRACTION DATA Cell Dimensions. a = 14.22 A.; b = 7.17 A.; c = 10.96 A.
X-RAY
Crossed Niools
1420
V O L U M E 2s. NO. 9, S E P T E M B E R 1 9 5 3 Optic Axial Angles (5893 A.; 25‘ C.). 2E = 84.5’. 2V = 84.5”(calculated from 8 and 2x1; 2V = 85“ (calculated from a, 8, and 7 ) . Dispersion. o r , weak. Optic Axial Plane. 010. Sign of Double Refraction. Negative. Acute Bisectrix. a. Extinction, a A a = approximately 12” in acute 8. Molecular Refraction ( E ) (5893 A: 25” C.). = 1.509. R(ea1cd.) = 45.1; D‘-h-A ’ - ’ ” c “
1421
determined the x-ray powder data, and of Ralph Hinch, Jr., who the projection, LITERATURE CITED
(1) Bseyer, A,, Be?., 29. 3 (1896). Co~~marnon ofs orystallogralio data for this eection should be sent to Walter C. McCrane. Analvtical Seation. Armour Research Foundation of Iilinois I
n
Textbook of Quantitative Analysis. 1. .!I. K d ~ h u ~~ Jr r dE . / I . Sandell. xv 759 pages. The Macmillan Go., 60 Fifth Ave., New York, N. Y., 1952. Price, $6.50.
+
d
c
Figure 4.
Polymorphic Transformations for dZ-Pinio Acid in Fusion Analysis
O o s a e d Niools Modifi~ation111 es observed completely orystallimd from melt Modificafisn I1 with mwing spherulite. of modific~tionI after trsneformation of511 to I1 and nucleation of I et 55’42. o. Modification I growing after melting of modification I1 at 68’C. d . Modification I sod crystals of modification I1 after cooling from
0.
b.
70’ to 60-
C.
This reviewer began teaching quantitative analysis almost ~iinultaaeouslywith the first appearance of this text, and 60 bas watched and participated in some of the recent developments which have brought along this third edition. The first edition was orthodox classiml quantitative analysis, but unmistakably colored by the progressive research interests and activities of the writers; the present revision has brought into the book new matter and a retouching of the old, in line with changing requirements for methods and their users, but with broad appreciation of the fundamentals of good sndyticsl &dueation. The chapter on “Analysis by Physical Methods” has been changed extensively; lesser alterations have been made in the chapters on “Quantits, tive Separation’’and “The Mass Action Law.” The authors divide the whole subject into the two large areas of “Gravimetric Andysk” (4W pp.), and “Volumetric Analysis” (200 pp.), with shorter sections on “Physical and Physimchemiml Methods of Analysis” (50 pp.) and “Analysis of Complex Materials” (60 pp.). Inside these major divisions the authors solve one old pedagogic problem by divorcing theory and practice, and another by using three sizes of type for matter of varying level of importance or applicability, Both devices seem to have been used thoughtfully and conaistently. These devices, however, contribute to a probably unavoidable student complaint that althouglt the book is full of useful fact and theory, it.is unattractive and bard to read. Part of this fault might he avoided by change in a number of small style details of typogmphy and format: in symbolism, capitalbation, arrangement and punctuation of side heads, setoff rules above footnotes, smaller type for and more care in planning of formulas, and better styling of some of the tabular matter. Proofreading and presswork are excellent. ALLEND. BLISS
X-Ray Analysis
ACKNOWLEDGMENT
The author acknowledges the assistance of Joan French, who
Two books on “Data for X-Ray Analysis” have recently been published. Vol. I, by W. Parrish and B. W. Irwin, contains charts for solution of Bragg’s equation. They cover radiation for molybdenum, copper, cobalt, iron, and chromium. Vol. 11, by W. Parrish, M. G. Eksteio, and B. W. Irwin, contains tables for computing the lattice constant of cubic crystals, a table giving lattice constants of cubic substances, and a chart showing 33 representative cubic diffraction patterns. The books are available for $2.00 each from the Research & Control Instruments Division, North American Philips Co., 750 South Fultan Ave., Mount Vernon, N. Y.
