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氧化锌中铅、镉、汞的icp-oes法测定(Determination of lead, cadmium and mercury in Zinc Oxide by ICP-OES)

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氧化锌中铅、镉、汞的icp-oes法测定(Determination of lead, cadmium and mercury in Zinc Oxide by ICP-OES)氧化锌中铅、镉、汞的icp-oes法测定(Determination of lead, cadmium and mercury in Zinc Oxide by ICP-OES) 氧化锌中铅、镉、汞的icp-oes法测定(Determination of lead, cadmium and mercury in Zinc Oxide by ICP-OES) Determination of lead, cadmium and mercury in Zinc Oxide by ICP-OES Yang Liu...

氧化锌中铅、镉、汞的icp-oes法测定(Determination of lead, cadmium and mercury in Zinc Oxide by ICP-OES)
氧化锌中铅、镉、汞的icp-oes法测定(Determination of lead, cadmium and mercury in Zinc Oxide by ICP-OES) 氧化锌中铅、镉、汞的icp-oes法测定(Determination of lead, cadmium and mercury in Zinc Oxide by ICP-OES) Determination of lead, cadmium and mercury in Zinc Oxide by ICP-OES Yang Liu, Liu Xinqun, Wang Jin (Zhuzhou times new material Polytron Technologies Inc technology center, Hunan, Zhuzhou 412007) Abstract: a method for determination of lead, cadmium and mercury in Zinc Oxide by inductively coupled plasma atomic emission spectrometry (ICP-OES) has been developed. The interference of matrix zinc was eliminated by matrix matching, and the working parameters and conditions were optimized. The detection limits of Pb, Cd and Hg were 0.0474 g/mL, 0.0043 g/mL, 0.0574 g/mL, respectively. The relative standard deviation was between 1.5% and 3.7% (n=5), and the recovery was 94% ~ 106.4%. The method is rapid, accurate and sensitive. It is suitable for the determination of lead, cadmium and mercury in Zinc Oxide. Keywords: ICP-OES; ROHS directive; rubber industry; Zinc Oxide; lead; cadmium; mercury In recent years, due to the introduction of the ROHS directive, environmental protection laws and regulations and regulations and a series of REACH, forming a "green barrier" of rubber products in China's exports, China's rubber production industry is facing tremendous pressure on environmental protection [1]. Zinc Oxide is an essential raw material for rubber and tire industry. It is often used as a vulcanizing agent and a reinforcing agent for natural rubber, synthetic rubber and latex. Zinc Oxide often contains heavy metal impurities. The content of lead, cadmium and mercury is directly related to whether rubber products can be detected by ROHS. Therefore, it is of great significance to study the method of rapid determination of heavy metals in Zinc Oxide. The determination of heavy metals in Zinc Oxide mainly consists of chemical and atomic absorption spectrophotometry, [2][3]. The time of chemical method is long and the operation is complicated. Atomic absorption spectrometry can only be measured by a single element, so it can not meet the requirement of rapid detection. Inductively coupled plasma atomic emission spectrometry (ICP-OES) was used for the determination of lead, cadmium and mercury in Zinc Oxide. The results were satisfactory by scale recovery experiments. 1 Experiment 1.1 main instruments and reagents GENESIS type inductively coupled plasma emission spectrometer (German SPECTRO company); glass instrument in (1 + 1) used after 24h immersion in HNO3 solution; preparation of standard solution used by all agents GR, and other reagents were of pure water for two times, the laboratory distilled water. 1.2 instrument operating parameters ICP-OES working conditions: frequency 27.12MHz, power 1300W, plasma cooling gas flow 12L/min, auxiliary gas flow 1L/min, atomizing gas flow 1L/min, flushing time: 45s, reading times: 3 Author: Yang Liu (1981), female, master of analytical chemistry, Zhuzhou times new material technology center of Polytron Technologies Inc, the instrument is now engaged in polymer materials analysis. Time. Preparation of 1.3 standard solution Lead standard reserve liquid (1.000g/L): weigh 1.0000g high purity metal lead in beaker, add a small amount (1 + 1) HNO3 dissolved, use 5%HNO3 into 1000mL polyethylene volumetric bottle, and dilute to calibration, shake. Cadmium standard stock solution (1.000g/L): 1.1423g GR cadmium oxide in the beaker, add 20mL (1+1) HNO3 with 5%HNO3 in 1000mL solution, polyethylene volumetric flask and diluted to the scale, shake. Standard storage solution for mercury (1, g/L): Tianjin Research Institute of fine chemical industry. Zinc matrix solution (20 g/L): weigh 6.2235g high purity Zinc Oxide in beaker, dissolve with 40 mL (1+1) HNO3, then transfer into the 250mL volumetric flask with 5% HNO3 and dilute to calibration, shake well. The working solution is gradually diluted by standard stock solution. 1.4 sample preparation Take Zinc Oxide sample accurately, 0.2000g in small beaker, add 5mL (1+1) HNO3, dissolve, transfer to 25mL capacity bottle, and use water for constant volume to be measured. 2. results and discussion 2.1 instrument condition optimization Selection of spectral lines for 2.1.1 analysis For the choice of analytical spectral lines, usually according to the content of the element to be measured, and the interference elements present in the sample, select the net line emission intensity, signal to noise ratio, the coexistence of spectral lines of elements less interference for the analysis of the measured elements of the spectral line. In this experiment, we investigated several sensitive lines of Pb, Cd and Hg. After comprehensive comparison, we selected the best analysis lines as follows: Pb 220.353, Cd 228.802, Hg194.227. The influence of 2.1.2 matrix interference The content of the elements to be measured and other impurities in the Zinc Oxide is very low, and the interference between them is also very low. The interference mainly comes from the element zinc in the matrix. In order to eliminate the interference of matrix zinc, the zinc equivalent to the sample was added to the standard solution. Selection of transmit power for 2.1.3 RF In this paper, the effect of RF on the emission intensity of Pb, Cd and Hg was investigated by using 1 g/mL Pb, Cd and Hg standard solutions, respectively. The effects of 90010001100120013001400W were studied. Experimental results show that the increase of three elements with the power spectral intensity increased to 1300W, the strength tends to be stable, considering the limit of detection and the effect of tube power increases the service life of the moment, the choice of power generator for 1300W RF. The influence of 2.1.4 atomization gas flow Gas flow is one of the important factors affecting the signal intensity, as the atomization gas flow increases, increase the amount of samples increase, the spectral line intensity also increases, but the mist flow usually lower the plasma is more stable. In this paper, 1 g/mL Pb, Cd and Hg standard solutions were used to investigate the influence of atomization gas flow on the spectral intensity of 0.60, 0.70, 0.80, 0.90, 1, 1.10 and 1.20L/min respectively. Considering the selection, the atomizing gas flow rate is 1.00L/min. Detection performance of 2.2 methods 2.2.1 operating curve and detection limit of each element Pb, Cd and Hg were divided into series of standard solutions containing zinc matrix, and the standard curves were measured under working conditions. The linear regression equation and correlation coefficients were shown in table 1. Table 1 working curves and correlation coefficients of elements Element linear regression equation of linear range correlation coefficient (g/mL) detection limit (g/mL) Pb I=17932C+13867 0~10.0 0.9999 Cd I=290679C+4820.5 0.0474 0~2.0 0.9999 Hg 0.0043 I=46369C+7813.5 0.9985 0~2.0 0.0574 Table 2 sample determination and recovery rate Sample element determination (g/g) plus scalar (g/g) determination value (mu g/g) RSD/% (n = 5) with Zinc Oxide No. 1 Pb 650.2500 1158 1.5 101.6 100.050 147.6 2.3 95.2 Cd /% recycled rubber Zinc Oxide 2 for rubber Zinc Oxide 3 for rubber Hg 22.350 71.2 2.8 97.8 359.1500 884.1 2.9 105 48.650 Pb 101.8 Cd 3.1 Hg 106.4 N.D 5047 2.1 94 136.3500 630.6 3.7 98.9 Pb Cd 15.950 67.3 2.5 102.8 5047.7 3.3 95.4 Hg N.D note: N.D = precision and recovery rate of 2.2.2 method was not detected By this method, three kinds of Zinc Oxide samples were spiked recovery experiments, the recovery of various samples in Pb, Cd, Hg at the rate of 94% ~ 106.4%, the relative standard deviation of 1.5% to 3.7%, to meet the requirements of the determination and analysis. The results are shown in table 2. Reference [1], Wang Qiaofu, Tang Wenzao, Xie Zhonglin, etc.. Environmental protection rubber products Monitoring and control, [J]., rubber industry, 2008,55 (3): 166-172. [2] Long Jing. Determination of iron [J] in Zinc Oxide by atomic absorption spectrometry. Physical and chemical tests: chemical fascicle, 1997,33 (4):175. [3] Dong Wenwu, Le Susu, Tu Yongjie. Atomic absorption spectrometry for the determination of metal impurities in Zinc Oxide [J]. tire industry, 2006, 26 (6): 372-373.Determination of Lead, Cadmium and Mercury in Zinc oxide by ICP-OES YANG, Liu, LIU, Xin-qun, WANG, Jin (Zhuzhou, Times, New, Material, Technology, Co., Ltd., Zhuzhou, 412007, China) Abstract:, A, method, for, of, lead, cadmium, and, mercury, in, zinc, determination, oxide, by, ICP-OES,, has, been, developed. 采用基体匹配消除氧化锌的干扰,ICP-OES和条件操作参数进行了优 化,检测限分别为铅:0.0474μμg,ml,光盘:0.0043μμg,ml, 汞:0.0574μμg,mL,相对标准偏差为1.5% ~范围3.7%,回收率在 94% ~ 106.4%范围。该法快速、准确、灵敏度高,可用于氧化锌中铅、 镉、汞的测定。 关键词:ICP-OES,ROHS,橡胶工业,氧化锌,铅,镉,汞 * [ jimisoft:未注册的软件只转换部分文件~阅读帮助以了解如何 注册。
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