A course in inorganic preparations - ACS Publications

42, 527 (1948). “Hybridization,” W. C. Price, Ann, Reports, 1939, pp. 47-61. .... 9. 10. 11. 12. Sodium chloride purification. Rock salt is the st...
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A COURSE IN INORGANIC PREPARATIONS KARL H. GAYER and MICHAEL J. ELKIND Wayne University, Detroit, Michigan

T m s suggested senior-year course in preparative inorganic chemistry is the outgrowth of a series of lectures and laboratory experiments conducted during the past several years at Wayne University by the authors. The sixteen-week course consists of one or two fifty-minute lectures and eight laboratory hours per week, which present to senior college and firstyear graduate students a brief but comprehensive introduction to the aspects of preparative and theoretical inorganic chemistry. The work is designed to meet the requirements of not only inorganic students, but also those interested in organic chemistry and other fields. The students entering this course are assumed to have had freshman chemistry and qualitative and quantitative analysis. We also assume that they have had or are taking an intermediate inorganic course and thereby having a thorough review of principles. The lectures of the preparative course then are slanted to supplement the intermediate course. We find that this review course is necessary since seniors seem to retain very little inorganic descriptive knowledge from their general or qualitative chemistry. The lectures are arranged chronologically and are intended to round out the student's understanding of the laboratory work. An outline of weekly lecture topics follows. Certain necessary laboratory techniques are discussed in the first two weeks, enabling the student to begin laboratory work. Among the topics discussed are safety, handling of dangerous chemicals, techniques in crystallization, sublimation, distillation, filtration, drying, and solubility. The lectures on purification procedures are exemplified in the laboratory by such msignments as rock salt, mercury purification, etc. Outside reading for these lectures is suggested in the following texts:

such as ovens, furnaces, vacuum pumps, pH meters. microscopes, refractometers, etc. There is need for the student to be able to use the more common laboratory instruments correctly. We have found our students' previous experience, in the use of the above apparatus, inadequate or even nonexistent. Some of the laboratory preparations are chosen for their value in demonstrating the need for a chemist to construct his own tools and apparatus. Simple techniques in glassblowing manipulations are taken up and demonstrated. A student, we feel, should be able to construct simple pieces of glass apparatus and make a small vacuum line for handling certain gases. Suggested reading is in the following texts:

Maomillan, 1949. HOBART HURDWILLARD, LYNNEL. MERRITT,AND JOHN A. DEAN, "Instrumentd Methods of Analvsis." . . D. Van ~ o s t r a n d 1948. , DAVIDF. BOLTZ."Modern Instrumental Analvsis." Edwards

The fifth-week lecture is devoted to the newer ideas of nomenclature, the student having by this time run up against the problem of correctly naming his preparations. The student's elementary concept of the subject, is reviewed and expanded to include recent ideas on the naming of complexes. The following articles are recommended: W. P. JORISSEN,H. BASSETI; A. DAMIENS,F. FIGHTER, A ~ H. REMY."I.U.C. reoort-1940," J . Am. Chem. Sac... 63.889 . (1941).

W. CONARD FERNELIUS, EDWINM. LARSEN, LOUISE. MARCHI, AND CARLL. ROLLINSON, Chem. & Eng. News, 26, 520 (1948).

W. CONARD FERNELIUS, ibid., 26, 161-163 (1946). JANET D. Scom~ Reviews, 32*73-96 JANET D. SCOW,C h m . Abstnzets, 39,5869 (1945). ATHERTON SEIDELL., "Limit&ms ~ ~ ~ ~upon the~ unification ~ of chemical nomenclature," J. CREM.EDUC.,6, 720 (1929). GERALDR. BEEZER,"Latin and Greek roots in chemical terminology," ibid., 17, 63 (1940). MARYALICEEWING,'What's in a name,'' ibid., 15,123 (1938). W. P. JOEISSEN,H. BASSETT,A. DAMIENS,F. FICHTER,AND H. REMY,"Rules for naming inorganic compounds," J. Am. Chem. Soc., 63, 889 (1941). GEoRaE W. WAIT, "The designation of special isotopes in the names and formulas of inorganic compounds," Science, 108, 2818 (December 31, 1948).

HAROLD F.WALTON,"Inorganic Preparations," Prentice-Hall, 1948.

Wan. E, H~~~~~~~~AND W. cONARD F~~~~~ IUB, U I Preparations," McGraw-Hill, 1938. H~~~~~~~ AND wjLHEm BILTZ,wX,T.H ~ AND~ ~ ,A, BLANCEARD, "Laboratory Methode of Inorganic Chemistry," John Wiley, 1928. EEENE~ER H. BLANCEARD AND JOBEPA W. PmLAN, "Synthetic Inorganic Chemistry,,' John Wiley, 1922. ALEXANDER KING, "Inorganic Preparations," D. Van Nostrand, 1936. pure ~~~~~~~i~ E~~~ H~~~~ A~~.~~~~, IIpreparation Substances," John Wiley, 1932. JOEL HENRYHILDEBRAND, "Solubility," A. C. S. Monograph, 2nd ed., Reinhold, 1936.

The lectures during the third and fourth week are devoted to the use and handling of laboratory apparatus

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The sixth and seventh lectures are devoted to phase rule theory and its application in the separation of salts and the stabilization of salt hydrates. Use and interpretation of diagrams is illustrated on the blackboard.

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Outside reading is suggested in the usual physical chemistry texts, also: ALEXllNnER FINDLAY, "The Phase Rule," Longmans, 1938.

By the middle of the semester some assignments are made from original sources; one object of the course being to parallel research procedures as much as possible; hence, the eighth lecture is devoted to library methods. Students are asked to use library references to obtain preparation procedures from the original workers. In some cases the formula is assigned, in others the name is given. A working knowledge of library methods and systems is needed by the student; therefore, a briefing lecture on literature surveys is important. Not only does this type of assignment afford the students the opportunity to obtain practice in the uses of the library, but it also permits them to utilize their knowledge of foreign languages. Students, we find, develop respect for their work if the "cookbook" procedure is minimized. '

References: BYRON A. SOULE,"Library Guide for the Chemist," McGrawHill, 1938. C R ~ AND E AUSTINM. PATTERSON, "A Guide to the EVANJOY Literature of Chemistry," John Wiley, 1927. MELVINBUY MELLON,"Chemical Publications," McGrawHill, 1940.

The latter part of the series of lectures is devoted to the theoretical concepts of inorganic chemistry, enabling the student to understand the chemistry of the compounds prepared in the laboratory. The niuthweek lectures, occurring after a midsemester test, are a review of the periodic system. Use of the periodic system in predicting chemical reactions is emphasized. The tenth-week lectures are devoted to oxidationreduction potentials and a review of what prediction can be made therefrom. The eleventh-week lecture material reviews valence and the relation of bond orbitals to valence. The twelfth- and thirteenth-week lectures are used to discuss complex compounds. The following subjects are taken up: role of central atom, coordinating groups, stability, general properties, types of isomerism. .The last two lectures are devoted to discussion of the structure and means of evaluating the structure of compounds. The following hooks and articles are suggested outside reading during the second part of the course. Harold F. Walton.. . . . . . . . . . ."Inorganic Preparations'' Wm. E. Henderson and W. Conard Fernelius. . . . . . . . . .."Inorganic Preparations" Harold Simmons Booth. . . .."Inorganic Synthesis," Vol. I W. Conard Fernelius . . . . . . . . ."Inorganic Synthesis," Vol. I1 Ludwig Frederick Audrieth.. . ."Inorganic Synthesis," Vol. I11 James Riddick Partington of Inorganic (Macmillan, 1950). . . . . . . . . ."TextBook Chemistry" Wendell M. Latimer and Joel H. Hildebrand (Macmillan, 1947). . . . . . . . . . . . . . . . . . . . ."Principles of Chemistry" N. V. Sidgwiok (Oxford Press, 1951). . . . . . . . . . . . . . . . . . . .. T h e Electronic Theory of Valence"

G. N. Lewis (Chem. Cntalog

Co.. 1923). . . . . . . . . . . . . . . . ."Valence m d Structure of the

N. V. Sidgwick (Cornell Press, 1933). . . . . . . . . . . . . . . . . . . . ."The Covalent Link in Chemiat,rv" ....

Edward Brtadford Mexted (Oxford Press, 1947). ...... ."Modem Advances in Inorganic Chemistry" Wm. George Palmer (Cambridge Prem, 1948). . . . . . . . ."Vdency" Alexmder Frank We118 (Oxford Press, 1947). . . . . . . . . . ."Structural Inorganic Cbemistrv" Wm. Thomas (Blackie & Son, 1924). . . . . . . . . . . . . . . . . . . .."Complex Salts" Robert Sohwan (Wiley, 1023). ."The Chemistry of Inorganic Complex Compounds-An Introduction to Werner's Coordination Theory" H. J. Emeleus and J. S. -4nderson (Van Nostrand, 1947). . . . . . . . . . . . . . . . . . . . . "Modern Aspects of Inorganic. Chemistry" Wendell M. Latimer (Prentice-Hall, 1938). . . . . . . . . . . . "Oxidation Potentialsu N. V. Sidgwick (Oxford and Ciarendon Press, 1950). . . . . "Elements and Their Camnoands" ">lolreulnr Orl,ituls," RAI.VHI,EI.IER I