Determination of copper,lead,zinc,chromium and nickel in drilling sludge by X-ray fluorescence spectrometry with microcrystalline cellulose pressed powder pellet
LI Pengfei, QIAO Hao, DENG Changsheng, WANG Bintang, LIANG Wenzhan
Detection and Research Institute,No.216 Geologic Party, CNNC, Urumqi 830000,China
Abstract：Understanding the content of related metals in drilling sludge could provide the basis for the treatment and utilization of drilling sludge. X-ray fluorescence spectrometer (XRF) was often used for the determination of heavy metals in sludge. When boric acid was used as edging substrate material to prepare the sample pellet, it was found that boric acid was easily volatilized by heating, which increased the risk of instrument corrosion. The microcrystalline cellulose was employed to replace boric acid powder for sample preparation. The certified reference materials of soil, stream sediment and rock series were selected to establish the calibration curves. The matrix effect and spectral interference were corrected by empirical coefficient method and Compton scattering RhKα internal standard method. Thus, a method for determination of copper, lead, zinc, chromium and nickel in drilling sludge samples was realized by wavelength dispersive X-ray fluorescence spectrometry (WDXRF). The mechanical strength, high temperature stability and structure stability of sample pellet prepared by two edging substrate materials, i.e., boric acid and microcrystalline cellulose, were investigated. The results showed that the sample pellet prepared by microcrystalline cellulose as the edging substrate material had better mechanical strength, better high temperature stability and better structure stability compared to that prepared by boric acid as the edging substrate material. Therefore, the possibility of cracking, chip falling or fracture was lower in the testing process. Moreover, the risk of deterioration of physical properties for edging substrate material due to temperature variation was lower, which had smaller influence of dust accumulation on the instrument. The certified reference materials of rock and soil with similar composition to the drilling sludge matrix were selected. The drilling sludge sample was also collected. After the sample pellets were prepared with microcrystalline cellulose powder as the edging substrate material, the contents of copper, lead, zinc, chromium and nickel were determined according to the proposed method. Meanwhile, inductively coupled plasma mass spectrometry (ICP-MS) was used for method comparison. For the certified reference materials of rock and soil, the results were basically consistent with the certified values and those obtained by ICP-MS. The relative standard deviations (RSD, n=11) were between 0.9% and 4.7%. For the actual sample, the results were basically consistent with those obtained by ICP-MS. The relative standard deviations (n=11) were between 1.1% and 3.9%.
[1] 中华人民共和国国土资源部.DZ/T 0279.1—2016 区域地球化学样品分析方法 第1部分:三氧化二铝等24个成分量测定 粉末压片-X射线荧光光谱法[S].北京:中国标准出版社,2016. [2] 刘燕德,万常斓.X射线荧光光谱技术在重金属检测中的应用[J].激光与红外,2011,41(6):605-611. LIU Yande,WAN Changlan.Application of X-ray fluorescence spectrometer technique in detection of heavy metal[J].Laser ＆ Infrared,2011,41(6):605-611. [3] 彭梦微,黄彦明,李业燕.波长色散型X射线荧光光谱法测定固体废物中的重金属含量[J].环境与发展,2020,32(6):30-34. PENG Mengwei,HUANG Yanming,LI Yeyan.Determination of heavy metals in solid waste by wavelength dispersive X-ray fluorescence spectrometry[J].Environment and Development,2020,32(6):30-34. [4] 贺忠翔.能量色散X射线荧光光谱法测定污染企业周边土壤重金属[J].环境与发展,2019,31(2):163-164. HE Zhongxiang.Determination of heavy metal elements in soil peripheral of contaminated enterprises by energy dispersion X-ray fluorescence spectrometry[J].Environment and Development,2019,31(2):163-164. [5] 田瑜.粉末压片制样X射线荧光光谱法测定土壤中的几种重金属[J].安阳工学院学报,2018,17(6):24-27. TIAN Yu.Determination of several heavy metals in soil by X-ray fluorescence spectrometry through pressed powder pellet sample[J].Journal of Anyang Institute of Technology,2018,17(6):24-27. [6] 刘江斌,党亮,殷桃刚,等.粉末压片-X射线荧光光谱法测定土壤中的铜铅锌砷锑钴铬镍等重金属元素[J].分析测试技术与仪器,2015,21(1):42-46. LIU Jiangbin,DANG Liang,YIN Taogang,et al.Determination of heavy metals elements copper,lead, zinc,arsenic,antimony,cobalt,chromium,and nickel in soil by X-ray fluorescence spectrometry with powder pelleting[J].Analysis and Testing Technology and Instruments,2015,21(1):42-46. [7] 赵文志,张填昊,卢兵.粉末压片制样-波长色散X射线荧光光谱法测定土壤和水系沉积物中溴氯氟磷硫[J].冶金分析,2021,41(4):27-33. ZHAO Wenzhi,ZHANG Tianhao,LU Bing,et al.Determination of bromine,chlorine,fluorine,phosphorus and sulfur in soil stream by wavelength dispersive X-ray fluorescence spectrometry with pressed powder pellet[J].Metallurgical Analysis,2021,41(4):27-33. [8] 张蕾,陈宁娜,许超.粉末压片-X射线荧光光谱法测定含碳化硅铝质耐火材料中8种组分[J].冶金分析,2022,42(6):51-56. ZHANG Lei,CHEN Ningna,XU Chao.Determination of components in aluminum refractory containing silicon carbide by X-ray fluorescence spectrometry with pressed powder pellet[J].Metallurgical Analysis,2022,42(6):51-56. [9] 王世芳,韩平,王纪华,等.X射线荧光光谱分析法在土壤重金属检测中的应用研究进展[J].食品安全质量检测学报,2016,7(11):4394-4400. WANG Shifang,HAN Ping,WANG Jihua,et al.Application of X-ray fluorescence spectrometry on the detection of heavy metals in soil[J].Journal of Food Safety and Quality,2016,7(11):4394-4400. [10] 陈宣,王丽香,承书振,等.高精度便携式X射线荧光光谱仪对污水厂剩余污泥重金属的快速测定[J].净水技术,2019,38(12):17-21,35. CHEN Xuan,WANG Lixiang,CHENG Shuzhen,et al.Rapid determination of heavy metals in excess sludge of WWTP with high-precision portable X-ray fluorescence spectrometer[J].Water Purification Technology,2019,38(12):17-21,35. [11] 张勤,李国会,樊守忠,等.X射线荧光光谱法测定土壤和水系沉积物等样品中碳、氮、氟、氯、硫、溴等42种主次和痕量元素[J].分析试验室,2008,27(11):51-57. ZHANG Qin,LI Guohui,FAN Shouzhong,et al.Study on determination of 42 major,minor and trace elements in soil and stream sediment samples[J].Chinese Journal of Analysis Laboratory,2008,27(11):51-57. [12] 殷惠民,杜祯宇,任立军,等.波长色散X射线荧光光谱谱线重叠和基体效应校正系数有效性判断及在土壤、沉积物重金属测定中的应用[J].冶金分析,2018,38(7):1-11. YIN Huimin,DU Zhenyu,REN Lijun,et al.Coefficient effectiveness judgment of overlapping line and matrix effect correction in wavelength dispersive X-ray fluorescence spectrometry and its application in determination of heavy metal elements in soil and sediment samples[J].Metallurgical Analysis,2018,38(7):1-11. [13] 赵慧,王银海.X射线衍射测量晶体材料的热膨胀[J].广东钻探大学学报,2011,28(1):38-40. ZHAO Hui,WANG Yinhai.Measuring thermal expansion of materials by X-ray diffraction[J].Journal of Guangdong University of Technology,2011,28(1):38-40. [14] 朱丽,杨永琼,顾汉念,等.电感耦合等离子体质谱-X射线衍射法研究云南玉溪和美国内华达地区黏土型锂资源矿物学特征[J].岩矿测试,2021,40(4):532-541. ZHU Li,YANG Yongqiong,GU Hannian,et al.Mineralogical characteristics of two clay-type lithium resources in Yuxi,China,and Nevada,the United States of America[J].Rock and Mineral Analysis,2021,40(4):532-541.
