エネルギー分散型蛍光X線分析法による排水試料中の金属イオンめ多元素同時定量

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  • 山田 悦
    京都工芸繊維大学工芸学部廃液処理施設
  • 佐藤 昌憲
    京都工芸繊維大学繊維学部分析化学無機化学講座

書誌事項

タイトル別名
  • エネルギー分散型けい光Ｘ線分析法による排水試料中の金属イオンの多元素同時定量
  • Multielement determination of metal ions in waste water by energy dispersive X-ray fluorescence spectrometr
  • エネルギー ブンサンガタ ケイコウ Xセン ブンセキホウ ニヨル ハイスイ シ

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抄録

The suitable determination procedure for the routine analysis of Mn, Fe, Ni, Cu, Zn, Pb, and Cr contained in waste water of the university campus was investigated. The essential procedure consists of the condensation of trace elements as diethyldithiocarbamate (DDTC) complexes on a Millipore filter and direct multielement determination by energy dispersive X-ray fluorescence analysis. As for the condensation procedure of the elements, the following process was recommended. For the determination of total metals, waste water samples were digested with nitric acid. Then, 10 ml of 1 % DDTC was added to the solution after neutralization by ammonia or acetic acid. After standing the solution for one hour, the precipitate of DDTC-complexes was collected on a 0.45 μm Millipore filter and dried prior to the X-ray fluorescence determination. To determine Cr, the reduction of Cr (VI) to Cr (III) by using ethanol in hydrochloric acid solution was necessary before the addition of ferric ion as a carrier. Then 1 % DDTC was added to the solution after adjustment of pH to 8.5. For the determination of soluble Fe and Mn, the filtrate of sample solution was acidified with (1+1) nitric acid. Then, nickel ion as a carrier, methanol solution of 0.1 % 1- (2-pyridylazo)-2-naphthol (PAN) and ammonia buffer (pH =10) were successively added to the solution. The formed precipitate of PAN-complexes was collected by a Millipore filter and dried prior to X-ray fluorescence determination. The detection limits for Cu, Fe, Mn, Ni, Pb, and Zn are 1 ppb, 2 ppb, 6 ppb, 4 ppb, 7 ppb, and 2 ppb, respectively. The comparison of the results by X-ray fluorescence analysis with those by atomic absorption (AA) analysis for Mn, Fe, Zn, and Cu showed that the present X-ray fluorescence analysis had the sufficient correlation coefficients and comparable detection limits with AA analysis.

収録刊行物

  • 分析化学

    分析化学 32 (11), 654-658, 1983

    公益社団法人 日本分析化学会

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