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Determination of carbon by the oxidation reduction reaction with chromium

Free carbon was determined in silicon and boron carbides in ash, oxides, and other materials by oxidation to carbon dioxide with a mixture of K2Cr2O7 + H2SO4. The determination was made from the amount of CR(6) consumed, by adding excess Mohr's salt and titrating with a standard solution of KMnO4. The amount of Cr(6) self reduced was determined in a blank test. Optimum oxidation and conditions were achieved when the volumes of 5% k2Cr2Oz and H2SO4 were equal. The mixture was boiled for 1-2 hours using a reflex condenser. The volume should not be reduced, in order to avoid an increase in the sulfuric acid concentration. The relative error was 4-7% for 0.005-0.04 g C and less than or equal to 3.5% for 0.1 g C.

Mashkovich, L.↗

Interatomic Auger transitions in maximal valent V and Cr compounds

The sensitivity of the intensities of the L(3)M(23)M(45) and L(3)M(45)M(45) Auger transitions toward the 3d character in the valence band has been demonstrated by using argon ion bombardment as a means of in situ reduction for the valence state of V and Cr in their maximal valent compounds. The selected V(5+) and Cr(6+) compounds were V2O5, NH4VO3, K2Cr2O7, K2CrO4, and CrO3. Auger and X-ray photoelectron spectra of fresh samples were obtained, and the samples were then subjected to ion bombardment of various durations. The subsequent spectra were recorded to monitor possible alterations due to the reduction of the cation valence state. The interatomic to intraatomic transitions of the Auger spectra transitions of the Auger spectra were observed dynamically and in situ. In particular, the intensity of the cation L(3)M(23)N(45) transitions was observed to increase dramatically with ion bombardment. The correlation between the interatomic Auger transition and covalency as well as the movements of the 3d electrons are discussed.

Yin, L. I.↗