X線分析の進歩38別刷

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1 X Ashing Conditions of Lead-Accumulating Blechnum niponicum for X-Ray Fluorescence Spectrometry Hirofumi KODERA, Tomoko UEYAMA, Hiroshi NISHIOKA and Yasuji MURAMATSU Copyright The Discussion Group of X-Ray Analysis, The Japan Society for Analytical Chemistry

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3 X Ashing Conditions of Lead-Accumulating Blechnum niponicum for X-Ray Fluorescence Spectrometry Hirofumi KODERA, Tomoko UEYAMA, Hiroshi NISHIOKA, and Yasuji MURAMATSU, Graduate School of Engineering, University of Hyogo 2167 Shosha, Himeji, Hyogo , Japan Faculty of Engineering, Himeji Institute of Technology 2167 Shosha, Himeji, Hyogo , Japan corresponding author: present address: Hitachi ULSI Systems Co., Ltd Josuihon-cho, Kodaira-shi, Tokyo , Japan (Received 18 December 26, Accepted 2 December 26) To develop a quantitative analysis of heavy metals (Pb and Zn) in Blechnum niponicum using fluorescent X-ray spectrometry (XRF), ashing conditions of the plant samples are evaluated with an electric furnace and a microwave furnace. In the electric furnace method, the ashing conditions are optimized as 7 o C for 5 hr. Although the further optimization of the ashing conditions with the microwave furnace should be necessary, ashing with the microwave furnace can be utilized for the sample ashing. It can be confirmed that ashing is a useful sample treatment for XRF measurements of Pb and Zn in Blechnum niponicum. [Key words] XRF, Ashing, Blechnum niponicum, Lead, Zinc, Phytoremediation Pb Zn X corresponding author: : LSI Adv. X-Ray. Chem. Anal., Japan 38, pp (27)

4 X X X 1. phytoremediation 1 hyperaccumulator 1 mg kg -1 1 mg kg -1 1 mg kg Blechnum niponicum mg kg

5 AAS / ICP-AES/MS 1. g 3 4 X XRF XRF µm XRF 5 6 XRF, g 7 5 SiC g 7 = g.55 g 7 kgf cm mm φ 2 mm T X g RSD =.157 % g

6 Table 1 Quantity of lead and zinc which are added to the 1. g dried samples and the concentrations in the samples. Standard sample # Pb /µg (concentration / mg kg -1 ) (2) (5) (1) (2) (3) Zn /µg (concentration / mg kg -1 ) (1) (2) (5) (1) (15) absorbance y = x R 2 = y = x +.2 R 2 = Pb concentration / mg kg --1 Zn concentration / mg kg --1 Fig.1 Calibration curve for determination of Pb (left panel) and Zn (right) concentrations in ashed plant samples using the atomic absorption spectrometry (AAS). RSD=4.22 % Pb Zn 1. g Table 1 Pb Zn 1 mg L g g X Pb Zn Fig X Zn Kα Pb Lβ X X

7 Table 2 Measurement conditions of X-ray fluorescence spectrometry in the regions of Zn Kα and Pb Lβ using RIX2. X-ray tube Tube voltage Tube current Analyzing crystal Atmosphere Collimator Sample spin Rh target 5 kv 5 ma LiF(2) vacuum (.1 Torr) 1 mm diameter on Element Pb Zn Spectrum Lβ Kα Peak position deg (4 sec) deg (4 sec) Background point deg (1 sec) deg (1 sec) Background point deg (1 sec) deg (1 sec) Rigaku RIX2 LiF(2) Pb Pb Lα Pb Lβ Pteris vittata 7 As Kα Pb Lα X Pb Zn X.6 INT X Table , 5, 6, 65, 7, 75, 8, 9 1 Pb Lβ Zn Kα Fig.2 Pb 7 Zn 75 X X

8 25 X-ray intensity / cps ZnKα PbLβ Ashing temperature / Fig.2 Ashing-temperature-dependence on the fluorescent X-ray intensity (Zn Kα, Pb Lβ ) of the ashed plant samples. Ashing time is fixed at 1 hr. X-ray intensity / cps ZnKα PbLβ Ashing time / hour Fig.3 Ashing-time-dependence on the fluorescent X-ray intensity (Zn Kα, Pb Lβ ) of the ashed plant samples. Ashing temperature was fixed at 7. Pb Zn X Fig.3 Pb Zn 5 X X Pb Zn Fig

9 3 2 X-ray intensity / cps y =.81x R 2 =.9983 y =.72x R 2 =.9966 E.F. M.W y =.92x R 2 =.9457 y =.81x R 2 =.952 E.F. M.W Pb concentration / mg kg Zn concentration / mg kg -1 Fig.4 Calibration curve for determination of Pb (left panel) and Zn (right) concentrations in ashed plant samples using the X-ray fluorescence spectrometry. The samples were ashed by an electric furnace (EF) and a microwave (MW) methods. 5 Pb 3 Zn 2 X Pb Zn mg kg -1 Pb Zn X Table 3 4 sample 1-5 Pb Zn Table 3 Table 4 (Fig. 1) XRF AAS R. E. (XRF) (AAS) /(XRF) 1 % mg kg -1 1 % mg kg -1 1% XRF AAS Pb Zn X Pb Zn

10 Table 3 Quantitative results of lead and zinc in Blechnum niponicum samples ashed with an electric furnace method. Sample # Pb concentration / mg kg -1 Zn concentration / mg kg -1 R.E. / % XRF AAS XRF AAS R.E./ % * *: sample picked at the non-mining area Table 4 Quantitative results of lead and zinc in Blechnum niponicum samples ashed with a microwave method. Sample # Pb concentration / mg kg -1 Zn concentration / mg kg -1 R.E. / % XRF AAS XRF AAS R.E./ % * *: sample picked at the non-mining area Table 3 4 Sample 6 Pb Zn 1 2 Table 3 XRF Pb Zn Fig.5 mg kg -1 Pb mg kg -1 Zn Pb Zn AAS AAS

11 Pb concentration / mg kg Zn concentration / mg kg -1 Fig.5 Correlation between lead and zinc concentration in Blechnum niponicum samples. XRF 5 XRF 1 15 XRF 4. Pb, Zn X 1. g Pb Zn XRF Pb Zn Pb Zn AAS mg/kg -1 1 % XRF AAS Pb

12 Zn XRF Pb Zn X 1 S.Fiorenza, C.L.Oubre, C.H.Ward,, 21 2 Mitch M. Lasat: J. Environ. Qual., 31, (22) H.Nishioka, H.Kodera: Metal accumulating ability of Blechnum niponicum International Chemical Congress of Pacific Basin Societies, PACIFICHEM 25, Honolulu, Hawaii, Dec.15-2 Program number 433 (25), (Abstract in CD-ROM). 5 X (26). 6 54, (25). 7 L.Q.Ma, K.M.Komar, C.Tu, W.Zhang, Y.Cai: Nature, 49, 579 (21)

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