Klemm method

The internal transport numbers may be measured most accurately and precisely by the Klemm method, which was developed for the purpose of isotope separation. This method has the following merits (1) It is insensitive to a small amount of impurities, such as water. (2) Even in the region of very small concentration of an ion of interest, 12 can be measured accurately. (3) It can be applied to additive ternary systems. An apparatus for the Klemm method of measuring 12 in nitrate mixtures is shown in Fig. I. This cell developed for nitrates by Okada s group has the following advantages compared with other electromigration cells ... 

The first preparation of metallic Ac was on the microgram scale and used the metallothermic reduction (Section II,A) of AcClj with K metal vapor (38), which is the same method used by Klemm and Bommer (67) to prepare La metal. The metal produced by this method is mixed with KCl and K metal. X-Ray diffraction revealed that Ac metal was isostructural with P-La, but that the face-centered cubic cell dimension of Ac (5.311 A) was slightly larger than that of La (5.304 A). 

Abstract This chapter reviews the methods that are useful for understanding the structure and bonding in Zintl ions and related bare post-transition element clusters in approximate historical order. After briefly discussing the Zintl-Klemm model the Wade-Mingos rules and related ideas are discussed. The chapter concludes with a discussion of the jellium model and special methods pertaining to bare metal clusters with interstitial atoms. 

Two methods have been employed for the synthesis of thieno[3,2-fc]pyridine which use gas-phase pyrolysis techniques. Klemm and coworkers starting with 2-vinylpyridine prepared (261) in a manner (Scheme 81) (68JHC883) strictly analogous to the synthesis of thieno[2,3-c]pyridine (Scheme 69). Another convenient route to (261) consists of the... 

Sukul NC, Klemm WR. 1988. Influence of dopamine agonist and an opiate antagonist on Agaricus-induced catalepsy, as tested by a new method. Arch int Pharmacodyn 295 40-51. 

Klemm, P. (1984). Manual Edman degradation of proteins and peptides. In Methods in Molecular Biology, Volume 1 Proteins. J.M.Walker, ed. (Clifton, New Jersey Human Press), pp. 243 254. 

The toluene vapour-flow method has been used for estimating the rate of homol-ytic rupture of the carbon-iodine bond in some organic iodides. Yang and Con-way have reported the following Arrhenius parameters for the case of ethyl iodide A = 4.5 x 10 see , E = 50.0 kcal.mole Shilov and Sabirova have reported the values A = 2.l4x 10 " sec E = 51.6 kcal.mole for the same compound. For allyl iodide, Shilov and Sabirova have reported A = 4.2x 10 sec , E = 66.5 kcal.mole . Errors in the use of this technique for iodides have been pointed out by Klemm and Bernstein and by Boyd et al. 

Klemm KM, Klein MJ. Biochemical markers of bone metabolism. In Henry s Clinical Diagnosis and Management by Laboratory Methods. 21 Edition. McPherson RA, Pincus MR (editors). Saunders Elsevier 2007 p. 170-184. 

Klemm and Merrill88 later devised a method for the preparation of the sulfones of thienof2,3-6]-, -[3,2-6 -, and - 2,3-c]pyridines by reaction of the parent heterocycle with sodium hypochlorite and dilute hydrochloric acid. Thienol2,3-6Ipyridine sulfone (68) behaved as a dienophile toward anthracene, naphthacene, and furan and yielded 8-(3-pyridyl)quinoline on heating Klemm proposes the mechanism of Scheme 19 for this interesting reaction. 

This method has been developed largely by Klemm et al. and is discussed in a recent review,7 which gives details on catalysts, procedure, and possible mechanisms Examples include formation of the peri-condensed compounds 35 (29-39%), from bridging at positions 4 and 5 of the phenanthrene molecule 149 at ca. 630°C in the presence of various sulfided mixed metallic oxide catalysts,6,36 and 80 (18%), from similar bridging in the triphenylene molecule 150 at 500°C.37 Since the sulfur bridge forms by substitution at the sterically most hindered positions of these hydrocarbon substrates, method... 

This method of preparation from the elements (in liquid NHg) given by Feher and Berthold, follows in principle the method worked out by Klemm and co-workers for preparing NagS (method I, p. 358). 

Metallic Ga is heated in a stream of N3 or COg laden with Brg vapor, according to Klemm and Tilk s method. A water-clear melt forms first, becoming yellow to red-brown, due to dissolved Brs, when all the Ga has reacted. When the bromination is complete, the GaBrg is distilled in an inert, Brg-free gas stream into a receiver and thus simultaneously freed of dissolved Brg. 

Gallium iodide is prepared by Klemm and Tilk s method in the apparatus shown in Fig. 249. Metallic Ga is placed in the center section of the tube and the stoichiometric quantity of I2 in the right side flask. After evacuation and sealing at a, 13 is sublimed... 

In Klemm and Vogel s method, GagOg is heated in a stream of HgS (purified by liquefaction with COg) for 14 hours at 600-700°C and finally for four hours at 1200°C. Faintly yellow GagSg Is obtained, the color depending on the particle size. 

Direct synthesis from Ga and S is impossible. Thus, excess fused Ga is triturated with GaS, mixed with GagSg to promote better wetting, according to the method of Klemm andVon Vogel, developed by Brukl and Ortner. The mixture is placed in a corundum boat inserted in a quartz apparatus, equipped with a cold finger, in high vacuum. The boat contents are heated to 700-720°C. If these temperatures are exceeded, the sublimed GagS has too low a sulfur content. 

According to Klemm and Von Vogel, GagSea and GaSe are prepared by the method given for GaS (see p. 851). The reaction proceeds with bright red incandescence (flashes of name). 

In Klemm and Dierks method, weighed amounts of the trihalides and the stoichiometric quantity of metallic In are thoroughly fused in an evacuated glass vessel to ensure complete conversion to the corresponding dihalides. The products are purified by vacuum distillation in the case of Inlg the apparatus is sealed off after evacuation to prevent changes in product composition due to loss of iodine. 

In the method of Klemm and Von Vogel, as developed by Thiel and Luckmann, InaOg is reduced with Hg at a temperature less than 400°C until the reduction product acquires a composition... 

According to Klemm and Sodomann, as well as Helms and Klemm, the best method for preparing KOa, RbOa and CsOa is by oxidation of the elements, dissolved in liquid NH3, with Oa at -30 to -50 t . Intermediate products appear first. Their color is light yellow when fresh, then dark. Finally, yellow dioxides are formed. To prevent an explosion, which is common in this reaction. Lux... 

II. In the method of Klemm and Grimm, a stoichiometric mixture of V turnings and 13 is sealed under vacuum into a short quartz tube, with occasional cooling to reduce the 13 vapor pressure. The entire tube is then uniformly heated at 160-170°C. 

The arrangement of Klemm and Dinkelacker also utilizes a small rotaiy milling tool for cleaning of the surface and comminution of the alloy chunk. In this method, however, the alloy is not removed from the crucible but is powdered while still in the crucible. The apparatus is shown in Fig. 353. 

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