Shiji ~ DOI /j. cnki. hxsj ARL Perform'X. Pb60Sn40 GBW GBW GBW % ~ 4.

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1 X- 43 DOI /j. cnki. hxsj ~ X- * X % ~ 4. 2% X- O A Determination of As Cu Sb Sn Bi and Pb in Lead Alloy by X-Ray Fluorescence Spectroscopy LU Xiao-bin LI Ying FENG Xiu-mei * LU Wei CHEN Jun Jiangyin Product Quality Supervision and Testing Institute Jiangyin China Huaxue Shiji ~ Abstract A rapid detection method of As Cu Sb Sn Bi and Pb in lead alloy by X-ray fluorescence spectroscopy was established. The optimum parameters of the detection was established by optimizing the test condition which can effectively avoid the interference of other elements. Calibration curve of the elements was draw using the experience influence coefficient correction method based on the strength and concentration of the interference elements. The experimental results show that As Cu Sb Sn Bi and Pb have a good linear relationship in a certain concentration range and the correlation coefficients of Bi Sb and Sn was above The test results of precision show that the relative standard deviation was between 0. 02% and 4. 2%. The test results of accuracy show that the measured value is consistent with reference value. Key words X-ray fluorescence lead alloy As Cu Sb Sn Bi Pb GB /T ARL Perform'X 4-8 GB /T GPY-Ⅱ 9 X- Pb60Sn40 GBW GBW GBW X fengxiumei@ jqt-cn. com

2 GBW YT8801 Bi Lα 2θ ~ Pb Kα As Kα ZChSnSbD4-4 ZChSnSbD % 2θ Bi Lα % Pb50Sn50 P10 90% % 10% % 99. 8% Bi Lα 2θ ~ Fig. 1 Bi Lα line for 2θ angle in the range of X ~ MPa 22 s 5 s 5 s 9 s Sb Kα 2θ 18 ~ 20 2 Sn Kα Sb Kα X- Sn Kα 1 1 Tab. 1 Analysis conditions of lead alloy 40 kv 60 ma Kα Lα Bi Lα 2 Sb Kα 2θ 18 ~ 20 Fig. 2 Sb Kα line for 2θ angle in the range of 18 ~ 20 2θ / /s As Kβ Bi Lα K L Cu Kα Kα Pb Lβ Kα As Kα Pb Lα 2θ Sb Kα Sn Kα Cu Cu LiF200 SC PHD 40 ~ 105 As Kβ Pb Lβ2θ Bi Lα Bi Lα 2θ As Kα X- 2

3 X Tab. 2 Reference value of the standard samples % c i = a 0 + a 1 I i + n a j I j a 0 + a 1 I i a j I j / / n n a. b. 3 As 15 α 16 Fig. 3 Calibration curve of As element Tab. 3 Linear range and correlation coefficient of each element w /% As ~ Pb Sb AI Bi ~ Pb AI Cu ~ Pb ~ Sn MC Sb ~ Pb Sn MC Sn ~ Pb MC As y = x Bi y = x Cu y = x Pb y = x Sb y = x Sn y = 0. 51x a j AI Addtive intensity 2 3 3a b As 3a 3b a. b. 4 Sb Fig. 4 Calibration curve of Sb element MC Multiplicative concentration c i = a 0 + a 1 I i 1 + n a j c j

4 i j a j a 0 + a 1 I i 1 + n a j c j 2 X- 3 Sb 4a 4b Sb 4a 4b X % ~ 5. 8% 1. - J J Tab. 4 Test results for precision 3. ICP-AES w /% J GB /T S GB /T S % 3. 4% 0. 25% 0. 30% 1. 2% 0. 04% 3 S GB /T S /% X-. GB /T GB /T S. Tab. 5 Test results for accuracy GB /T S

5 QuEChERS - 51 GC-ECD produce J. J. AOAC Int QuEChERS / - J LEHOTAY S J KOK A D HIEMSTRA M et al. Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables 1 GUILLARME D CASETTA C BICCHI C et al. High throughput qualitative analysis of polyphenols in tea samples by ultra-high pressure liquid chromatography coupled to UV and mass spectrometry detectors J. J. Chromatogr. A XU Xiao-min YU Cun HAN Jian-long et al. Multi-residue analysis of pesticides in tea by online SEC-GC /MS J. J. Sep. Sci PANG Guo-fang FAN Chun-lin ZHANG Feng et al. High-throughput GC /MS and HPLC /MS /MS techniques for the multiclass multiresidue determination of 653 pesticides and chemical pollutants in tea J. J. AOAC Int HUANG Zhi-qiang LI Yong-jun CHEN Bo et al. Simultaneous determination of 102 pesticide residues in Chinese teas by gas chromatography-mass spectrometry J. J. Chromatogr. B YANG Xin XU De QIU Jian et al. Simultaneous determination of 118 pesticide residues in Chinese teas by gas chromatography-mass spectrometry J. Chem. Pap HU Yan-yun ZHENG Ping HE You-zhao et al. Response surface optimization for determination of pesticide multiresidues by matrix solid-phase dispersion and gas chromgatography J. J. Chromatogr. A / ANASTASSIADES M LEHOTAY S J STAJNBAHER D et al. Fast and easy multiresidue method employing acetonitrile extraction / partitioning and dispersive solid-phase extraction for the determination of pesticide residues in using gas and liquid chromatography and mass spectrometric detection J. J. AOAC Int DPX-Q / 102 J GONZ LEZ-CURBELO M HERN NDEZ-BORGES J. Determination of pesticides and their metabolites in processed cereal samples J. Food Addit. Contam. Part A Chem. Anal. Control. Expo. Risk Assess KANRAR B MANDAL S BHATTACHARYYA A. Validation and uncertainty analysis of a multi-residue method for 42 pesticides in made tea infusion and spent leaves using ethyl acetate extraction and liquid chromatography-tandem mass spectrometry J. J. Chromatogr. A J GUAN Ya-qin TANG Hua CHEN Da-zhou et al. Modified QuEChERS method for the analysis of 11 pesticide residues in tea by liquid chromatography-tandem mass spectrometry J. Anal. Methods CHEN Hong-ping YIN Peng WANG Qing-hua et al. A modified QuEChERS sample preparation method for the analysis of 70 pesticide residues in tea using gas chromatography-tandem mass spectrometry J. Food Anal. Methods FPD J YS /T X- S X- J D J X- 16. X-. X J X- 9 J X- D.

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