To determine the gaseous impurities in the choice of two options for applying the method of vacuum melting: with and without platinum bath tub. More attention should be given a second way, because it is much easier. Preliminary samples of boron powder are pressed into briquettes and then otlomlennye pieces weighing 3-20 mg placed in a graphite crucible.
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The sample was melted in a vacuum furnace with induction heating under continuous pumping of gases evolved. For the determination of hydrogen sufficient heating to 500 ° C, while the determination of hydrogen, oxygen and nitrogen, the temperature was raised to 1900 ° C.
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The extraction time of the gas sample is 15 min. The amount of hydrogen is determined by the pressure difference before and after pumping the gas mixture through a palladium filter is heated to 600-700 ° C, oxygen - to change the pressure after the oxidation of carbon to C02 in the copper oxide and freezing in a trap with liquid nitrogen, a residual pressure of nitrogen is determined . The accuracy of the analysis of ~ 10%. Sensitivity of hydrogen 5 10-3% of the oxygen-10 and 2% for nitrogen 1-10 ~ 2%. The scheme of the instrument and the details of the method are given in the work.
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Chemical and Spectral Determination of beryllium, magnesium, calcium, barium, aluminum, titanium, vanadium, tungsten, chromium, manganese, iron, cobalt, nickel, copper, silver, gold, zinc, cadmium, indium, tin, lead, bismuth, gallium and ANTIMONY IN BORON, boric anhydride and boric acid. The method consists in pre-concentration of chemical impurities, followed by spectral analysis of the concentrate obtained in a dc arc between carbon electrodes.
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The concentrate of impurities from a mixture of carbon powder with 5% NaN03 obtained by distillation of the framework boron mixture of HNO3 and HF, ratio of enrichment of impurities in the concentrate is 25, the standards are also prepared from a mixture of coal powder and NaNCl.
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3. At the same time on one spectrogram determined 24 trace elements: Be, Mg, Ca, Ba, Al, Ti, V, W, Cr, Mn, Fe, Co, Ni, Cu, Ag, Au, Zn, Cd, In, Sn, Pb, Bi, Ga and Sb with an accuracy of 15-20%.