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A simple and rapid semi-micro gravimetric procedure for the determination of carbon dioxide (0.005-60%) in coal, rocks and minerals is described. Particular advantages include small sample weights (0.25-1.0 g), high precision (relative standard deviation 0.01%) and improved speed of analyses (20 min). The apparatus is designed as a simple vertical layout to minimize bench space requirements and utilizes commercially available components to reduce the number of joints and rubber tubing connections. The low swept volume (165ml) gives good sensitivity and reduced analysis time, and the scavenging train ensures removal of water, halogens and gaseous sulphur compounds.

A method is described for the spectrophotometric determination of 0-4% silicon in ferrophosphorus, following fusion with sodium peroxide in a zirconium crucible. Silicomolybdic acid is formed with sodium molybdate. The acidity is increased to 2N and the solution stood for 10 min to destroy phosphomolybdic and arsenomolybdic acids. The silicomolybdic acid is reduced with ascorbic acid and the absorbance measured at 810 nm. The colour is stable, and a standard deviation of 0.006% was achieved for 0.7% silicon. Results obtained for three samples with alternative procedures are compared.

Five sample presentation techniques were examined for the X-ray fluorescence spectrometric analysis of tungsten carbide alloys in powder and cemented forms. Powder samples may be oxidized by air at 600 degrees before fusion (I), or preferably by lithium nitrate during fusion (II); the fusion is effected with lithium-lanthanum tetraborate followed by briquetting with graphite. Powder samples may also be blended with wax and briquetted (III). Cemented carbides are surface-prepared with silicon carbide before analysis (V). Briquettes prepared by blending carbide powder, lithium-lanthanum tetraborate and graphite (IV), give poor reproducibility, however, owing to micro-absorption effects the technique is not recommended. The determination of eight common elements in tungsten carbide is discussed and the relative standard deviations are 0.002-0.004 for major and 0.008-0.01 for minor elements.

The selective-electrode procedure described for determining 0.2-2.5% of nitrogen in coal and coke offers significant advantages over Kjeldahl distillation and titration. The Kjeldahl digest is diluted, neutralized, cooled, diluted to volume, adjusted to a standard temperature and rendered alkaline prior to measurement with an ammonia-selective electrode. Accuracy and precision of 1% relative are demonstrated by comparative analyses of a range of samples. Important experimental aspects discussed include the role as neutralization indicator played by vanadium derived from the catalyst, precision of the mV-meter, the influence of solution temperature and concentration, the repeatability of the readings, and interferences.