ANALYTICAL CHEMISTRY
?62
contains a N-N linkage. Hydriodic acid was also found to be unsatisfactory on certain compounds of this type. CONCLUSIONS
The adaptations of the Kjeldahl method of nitrogen determination herein described make it possible to determine nitrogen in such compounds as azines, hydraaones, oximes, and semicarhasones. The method is also satisfactory for use with other types of compounds containing nitrogen to oxygen linkages and for refractory nitrogen compounds such as pyridine and quinoline derivatives. ACKNOWLEDGMENT
It is a pleasure to acknowledge the help and encouragement received from E. D. Amstute and N. R. Easton during the progress of this work. The author is also grateful to the members of the organic research staff who have tested these methods.
Contrihuted b y MAX R. WILLIAMS
AND
LITERATURE CITED
Bradatreot. R. B..ANAL C a z ~ .21, . 1012 (1949). (2) Clark, E. P., J . Assoc. Osc. Agr. Chernista, 24, 641 (1941). (3) Cole, J. O., and Parks, C. R., IND.ENG.CKEM.,ANAL.ED.. 18, (1)
G1-2 (1946).
Friedrich. A.. Kuhaas.. E... and Schnuvoh. R.. Z. ohu~iol.Ciiern.. 216, 60 (1933). ( 5 ) Grillemord. H.. BuU. doc. chim.. 1, 1 9 6 2 0 0 (1907) ( 6 ) Kirk, P. L.. ANAL,Cmnr.. 22, 354-8 (1915n) ..,. (7) Ogg, C . L., and Willits. C. 0.. Ihid., 23, 47-51 (19511. (8) Patel. S. M.. and Sreenivasan.A.. 16id..20. 63 (i948): KAI.. NO. (9) Pepkbwitu, L. P.,and Shive. J. W., IND.'E Eo., 14, 914 (1942). 110) Rose, E. D.. and Ziliotto. H., Ibid.. 17, 211 (1945). Shaefer. W. E., and Beoker. W. W.. Ibqid, 19, 307 (1947). Shirley, R. L.. and Beeker, W. W., 1bir1., 17, 437 (1945). Shuey. P.MoG.. Ibid.. 19.882 (1947). WillitB, C. 0.. and Ogg, C. L.. J . Assoc. OBc. A0 ', 33, (4) . .
.-n 0 0 ,.nzn> 1,v-00 ,'VU",.
RzcErvEDforreview June20, 1951. Accepted Ortnber 31, 1911.
W. P. VAN M ETER, D e p a r t m e n t of Chemistry, Oregon S t a t e College, Colvallif i, Ore.
7.r
11:-C-N-N-0 11 11 H I1 0 Structural Formula for 8-Acetylphenylhydrazine XCELLENT crystals of p-acetylphenylhydraaine I can be obtained from acetone, ethyl alcohol, and thymol. Acetone and thymol solutions give tablets or plates, while alcohol solutions tend t o give a needle habit. Figure 1shows crystals from thymol. Figure 2 is an orthographic projection of a typical tablet from solution.
E
Formula Weights per Cell. 8 (8.06 calculated fmm x-ray data). Formula Weight. 150.18. Density. 1.280 (Rotation and specific gravity balance); 1.286 (x-ray). Prinoipsl Lines d 10.88 5.18 4.74 4.64 4.35 4.01 3.96 3.73 3.45 .%,,lllrjr .L---
---
I/Iz 1.00
0.61 0.39 0.30 0.09 0.30 0.14
0.28 0.30
io.77(ozo) 5.22(121) 4.78(200) 4.e5(210) 4,371220) 4.oo(141) 3.98(211) 3.7~(012) 3 . 5 0 112)
3.49h51) -.LA-
yl/ln
d
I/J
Indexn
3.34
0.20
3.37(032)
0.08
a.05(320) 2.92(311) Z.S~(ZZZ) 2.64(212)
Index-
L:.L ,"yLIy
3.06 2.93 2.88 2.66 2.57 2.51 2.43 1:ifi
-:^l.
llllbjll
0.58 0.18 0.14 0.10 0.08 0.05
2.65(003) 2.53 (013) ~.44(302)
2.44(113) i.xe(511)
_^_._ .^ "" alii
:L...^ u"IIIII"""~
,:..""
"1151s L.llrv
"-2
the indicated indexes are only suggested as wssible contributing renections.
Figure 1. B-Aoetylphenylhydrazine I Crom Solution
CRYSTAL MORPHOLOGY Crystal System. Orthorhombic. Form and Habit. Plates and tablets !ying on mnrropinncoid, 100, and needles elongated along e showing prierns, { I I O I , pyramids, 11111, and brachydomes, I O l l l . Axid Ratio. a:b:e: = 0.444:1:0.3_5. Int_erfacial Angles (Polar). 12OA120 = 57" (83.2", x-ray); 101A101 = 76" (77.2', x-ray). X-RAYDIFFRACTION DATA Cell Dimensions. a = 9.55 A,; h = 21.54 A,; e = 7.04 A
V O L U M E 2 4 . N O . 4. A P R I L 1 9 5 2
Figure 3.
7633
8-Aeetylphenylhydra.ine from Fusion
Form I1 Frystallired fmm melt
PROPERTIES Refractive Indexes (5803 11.; 25" C,). a = 1.586 =t0.002 D = 1.609 + 0.002; y = 1.75 f 0.01. Optical Axial Angles (5893 A,; 25' C.). 2V = 48"; 2 8 = 81". Dispersion. \Veak, little or none. Optic Axial Plane. 100. Sign of Double Refraction. Positive. Acute Bisoctrix. y = b.
Or.rrcAr,
This book, as its title indicates, is concerned with the theory of automatic control. While addressed to those who ''are interested in any of the applications of automatic control," the book is written from the somewhat narrower viewpoint of plant control. The author discussed the types of oontrol that can be used, the typea of systems that can be controlled, and how the systems act while being controlled. The discussion is largely of idealiGed systems, visualized as clectried analogs, and is carried out in mathemstical terms. Thc mathem&cal discussion, while a t times lengthy, ia adequate and presupposes little mathematical knowledge other than ordinary C~ICUIUB. A great number of diagrams accompany the text, and a helpful table is included which lists the equivalent electrical pneumatic, mechanical, and tpermal analogies. It seems to the reviewer that more discussion of actual systems could profitably have been included. The reader is warned t h a t most actual systems ar,e much more complicated than the idealized systems discussed in the hook hut is given little advice as to how to acbieve optimum control over them or how to modify a system 80 as to improve its controllability. However, a6 an introduction to the theory of ltutomxtic control, the hook is to be recommended. F. W. MITCHELL
NEW BOOKS
land.
WUU.
The Barker Index of Crystals. M . W . Porter and R. C. Spiller. \ ~ o l . l , P a r t s I s n d 2 . P i r t l,ix+25Opages. PastZ,x+1027 pages. W. Heffer & Sons, Ltd., Cambridge, E n & ~ l . Two ])art,s $6 (Pert 1 separately, 30s; part^ 2 scpwatdy, $4 10s.)
Society of Public Analysts
Figure 4.
8-Aoetylphenylhydra.ine Fusion
Form I11 arystalliring fmm s number of
from poi&
nuoleation d t h i n melt form I1 cvatalliring hottom of fieure
of at
Extinction. Parallel and symmetrical. Molecular Refraction ( R )(5893 A,; 25" C.). . \ l / z y = 1.647. R(ca1cd.) = 42.7. R(obsd.) = 42.6. FUSIONDATA. &Acetylphenylhydrazine melts at 128-129' C. with neither decomposition nor sublimation. Crystals from solu tion, form I (Figure I), show a solid-solid transformation to form I1 which melts a t 128-129" C. Either form I1 (Figure 3) or form 111 (Figure 4 ) crystallizes from the melt, depending upon the degree of wpercoaling. Form 111forms easily an supercooling to 30' to 50" C. {or seveval m i n u t s but also trandomis io form 11 on beating. CONTR~UTION ofB oryatsllogiapl~iodata for t,bia ~eetionrliorild be sent to Walter C. MoCione, s i i ~ e ~ v i s o rAnalytiod , Section, Arrnour Research Foundation of the Illinois Institute of Technology,Chicago 16, Ill.
The 78th annual geneTal meeting of the Society of Public Analysts and Other Analytical Chemists was held March 7 in London. Membership was reported as 1578, an increase of 16 over last year. In addition to nix ordinary meetings of the society, sixteen meetings were held by seotions and groups during the year. The following officers and members of the council were elected for the coming year: President. J. R. Nicholls
Honorar? secretary. K. A. Williams Counoil.. C. A. Adams, D. C. M. Adsmson, N. L. Allport, A. J. Amos, B. S. Cooper, N. Heron, T. McLaohlan, H. E. Monk, G. E. Osborn. A. A. Smales. H. C. S. de Whnllev. E. C . Wood. Ex-offici< Haslam, H. 0. J. Collier A t the 35th meeting of the Physical Methods Group of the sooiety, held in London, Fehrunry 19, the fallon~ingpapers were presented and discussed: Electrographic Analysis. A Brief Survey of Its Development with Special Referenoe to Recent British Appmatus. P. R. MONK. Identifieahion of Certain Alloys and Stainless Steels by Elcctrogrzphic Methods. G. C. CLARKAND E. E. HALE.
