Gutzeit 法を利用した微量ヒ素のけい光X線分析法による定量

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  • Determination of microgram levels of arsenic by a combination of the Gutzeit method with X-ray fluorescence spectrometry
  • Gutzeitホウ オ リヨウ シタ ビリョウ ヒソ ノ ケイコウ Xセン ブンセキホウ ニ ヨル テイリョウ

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For the purpose of investigating simple and rapid determination of microgram levels of arsenic, arsenic was collected on silver nitrate test paper by the Gutzeit method and was determined by X-ray fluorescence spectrometry.<BR>The apparatus to evolve and capture arsine was composed of a 200 ml Erlenmeyer flask and a trap bottle made of plastics. The surface of the test paper with a diameter of 22 mm was used to capture arsine.<BR>The basic procedure to determine arsenic was as follows : To a 100 ml sample solution containing less than 50 μg of arsenic, 5 ml of concentrated sulfuric acid and 10 g of granular zinc was added in the flask. The flask was allowed to stand for an hour to evolve the arsine in room temperature. Then the test paper was removed from the bottle and was pasted with a filter paper. The paper was set on an accessory sample holder of the equipment and was used as a sample for X-ray analysis. The intensity of AsKα line (2θ= 33.98) was measured in a vacuum by using a tungsten target X-ray tube (50 kV-20 mA) and LiF crystal.<BR>The calibration curve with a slope of about 45 cps/μg was linear in the arsenic range 0 to 50 μg passing through a zero point. The slope had to be inspected by a known amount of arsenic treated in parallel with samples whenever the test was done. The standard deviation of this method was within 4% at 10 μg of arsenic in a five times repeat of experiment.<BR>The X-ray fluorescence spectrometry facilitated the quantity indication and the preservation, whereas they are difficult in the ordinary Gutzeit method. Arsenic collected on the test paper was stable even for a month, so it showed no variation in the counts.<BR>In the case of practical analysis, stannous chloride, potassium iodide and ferric salt were added to the sample solution if necessary for eliminating interferences and obtaining an optimum evolution of arsine. Good results were obtained on the practical analysis of soft solders, steels and waters.

収録刊行物

  • 分析化学

    分析化学 22 (10), 1312-1316, 1973

    公益社団法人 日本分析化学会

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