Melting point sample preparation

Adding 2,4-dinitrophenylhydrazine to a sample of the unknown have similar melting points, but preparing the semicarbazone ... 

The student should read Sections 1,10 to 1,16 carefully before commencing any experimental work. A supply of melting point capillaries is prepared as described in Section 11,10 (compare Fig. 77, R , I). The apparatus illustrated in Fig. 77. 10, 2, a is assembled with concentrated sulphuric acid as the bath liquid the thermometer selected should have a small bulb. The melting points of pure samples of the following compounds are determined in the manner detailed in Section 11,10 —... 

P,17P-Dihydroxyestr-4-en-3-one 1-acetate. The 6-hydroxy compound is removed from the column with 15-17% acetone. Recrystallization of the crude product (1.92 g) from acetone-hexane gives 1.25 g of crystals melting at 165-166° and 0.13 g melting at 162-164° (12.1% yield). When the analytical sample was prepared from the same solvent mixture, the melting point rose to 192-193° (Lit 166° 189-190°) [a] -59.5° (CHCI3) 2, 236 m/i (fi 14,500). 

Sodium-zinc alloys for phase diagram determination are prepared by melting the elements in glass tubes under H2- Samples of NaZujj are prepared by heating zinc for several hours above the melting point of NaZn,3 (557°C) with xs Na in alundum extraction thimbles with N2 or Ar in a steel bomb scaled with copper gaskets. Excess Na was removed by extraction with liq NHj. Both KZn,3 and KCd,2 were prepared in this manner. ... 

Purification of the radioactive tracer was modified to include a fractional sublimation before a single extraction—recrystallization cycle to conserve the tracer material. Microgram samples were prepared in melting point capillaries for assay by mass spectroscopic analysis (Table III), made by direct probe injection of the sample into the ion source (18). The probe was heated rapidly to 200°C, and mass spectra were obtained during vaporization of the sample. Tri-, tetra-, and pentachlorodibenzo-p-dioxins vaporized simultaneously with no observed fractionation. 

The eutectics examined and their melting points are given in Table 3.1. The compounds were melted in 10 mm inner diameter pyrex tubes, and polished sections were prepared from the solidified eutectic samples. 

Like other 2,2-diaryltrichloroethanes, DFDT undergoes dehydrohalogenation in the presence of a base to yield l,l-dichloro-2,2-bis(p-fluorophenyl)-ethylene. The rate of this reaction has been found to be directly proportional to the temperature, and the rate constant for DFDT is approximately one seventh that for DDT at ordinary temperatures (18, 110). This ethylene derivative has been oxidized by the use of chromic anhydride to p,p -difluorobenzophenone, a sample of which did not depress the melting point of an authentic sample prepared by a different route (10). 

The best fail-safe way of telling whether a freshly prepared compound is identical to a sample prepared previously is to perform a mixed-melting-point experiment. 

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