新型X射线荧光光谱仪对微量元素的分析研究

发布时间：2018-04-23 12:10

本文选题：X射线荧光光谱仪 + 雪松松针　；参考：《烟台大学》2016年硕士论文

【摘要】：X射线荧光光谱法适用于对物质成分分析,可直接对固体(块状或粉末状)和液体样品中主量元素、微量元素进行多元素同时分析。当结合薄样技术时,具有高灵敏度,用样量少等优点。随着分析技术的发展和科研水平的提高,分析领域愈发关注待测成分复杂和含量低等特点课题,对仪器本身提出更高要求。本课题组由田宇~淌诖煜略谌瓷鋁射线荧光分析仪研究基础上对仪器进行了改进,研制出一台高灵敏度的新型X射线荧光光谱仪。论文对仪器结构进行介绍,并将仪器主要应用到微量元素的分析。本论文主要包括四个部分:第一部分:介绍了X射线荧光产生原理、X射线荧光光谱仪发展史及应用、常见样品前处理方法及联用方法的原理和应用。同时,阐明了本论文的立题思想及主要研究内容。第二部分:介绍了本课题组研制的新型X射线荧光光谱仪结构装置、仪器定量分析方法,并对仪器进行了性能实验工作。新型X射线荧光光谱仪主要包括激发系统、探测器系统、记录单元、高压电源和真空泵等部分。采用钼靶和钛靶双靶X光管激发系统,由X-123型硅漂移探测器和DPP数字脉冲处理器组装而成;其定量分析是通过薄样技术和内标法结合实现的;通过灵敏度校准曲线可以看出,K线系各元素的偏差均小于±1%,L线系所得各元素的偏差均小于±2%;精密度(RSD)(n=6)在2.2%~5.8%之间;各元素方法检出限及定量下限相对较好。第三部分:将新型X射线荧光光谱仪应用于雪松松针及其花粉中无机元素的分析。结合薄样技术及内标法建立了对雪松松针及其花粉中多种无机元素同时分析的方法,并系统的研究了雪松松针在全年生长周期内多种无机元素含量变化情况。数据表明:雪松松针及其花粉在生长过程均含有植物体所需要的K、Ca、Ti、Cr、Mn、Fe、Ni、Cu、Zn、Rb、Sr等多种无机元素,其中,K、Ca含量居高,Mn、Fe次之;同一元素在低、中、高三种不同加标水平下的平均加标回收率在94%~104%之间,能满足微量测定要求;XRF法与ICP-AES法对实际样品测定结果基本吻合;三地点雪松松针在一年生长周期内各无机元素含量虽然存在不同,但整体呈现一定规律性;雪松老针样品中各元素含量并未因月份不同有较大变动,含量较为稳定。第四部分:将电沉积技术与新型X射线荧光光谱仪联用应用于沉积单个铜离子的基础研究。对沉积最佳pH、沉积最佳电位、沉积时间、不同盐度对沉积铜离子的影响、不同玻碳电极工作面积对沉积铜离子的影响、多离子共存时对沉积铜离子的影响及不同浓度的铜标准溶液沉积率进行实验研究,同时进行实际样品的回收率实验。结果表明:铜离子的最佳沉积pH为pH=5的醋酸-醋酸钠缓冲体系;铜离子的最佳沉积电位为-0.6V;盐度的提高会增强溶液离子强度,使铜离子沉积率有所提高,但不是影响铜离子沉积的主要因素;铜离子的沉积率与沉积时间和玻碳电极工作面积呈正相关关系;多离子共存时并未影响铜离子的沉积;将XRF检测结果与ICP-AES检测结果进行对比,结果较为一致;不同浓度下标准铜离子的沉积率较为接近,均在1.26%~2.06%之间;电沉积技术与新型X射线荧光光谱联用技术应用到实际样品检测时,其加标回收实验与标准铜离子检测时数据相吻合。
[Abstract]:X ray fluorescence spectrometry is suitable for the analysis of material components. It can be used for the simultaneous analysis of the main elements and trace elements in solid (lump or powder) and liquid samples. When combining with thin samples, it has the advantages of high sensitivity and less sample size. With the development of analytical techniques and the improvement of scientific research level, the analysis field is becoming more and more important. A new X ray fluorescence spectrometer with high sensitivity has been developed on the basis of the research on the instrument itself, which is based on the research of the instrument itself. This paper introduces the structure of the instrument and introduces the instrument structure. The instrument is introduced and the instrument is introduced. It is mainly applied to the analysis of trace elements. This paper mainly includes four parts: the first part is the introduction of the principle of X ray fluorescence generation, the history and application of X ray fluorescence spectrometer, the principle and application of common sample pretreatment methods and combined methods. At the same time, the idea and main research content of this article are clarified. The second part: Introduction The new type of X ray fluorescence spectrometer developed by our group, the quantitative analysis method of the instrument, and the performance experiment of the instrument are carried out. The new X ray fluorescence spectrometer mainly consists of the excitation system, the detector system, the recording unit, the high voltage power supply and the vacuum pump. The dual target X light tube excitation system using the molybdenum target and the titanium target is used. The X-123 type silicon drift detector and the DPP digital pulse processor are assembled. The quantitative analysis is realized by the combination of thin sample and internal standard. Through the sensitivity calibration curve, the deviation of each element in the K-line system is less than + 1%, and the deviations of each element in the L line system are less than 2%; the precision (RSD) (n=6) is between 2.2%~5.8% and each element. The third part: a new X ray fluorescence spectrometer was applied to the analysis of the inorganic elements in pine needles and their pollen. A method for the simultaneous analysis of a variety of inorganic elements in Cedar pine needles and their pollen was established by combining the thin sample technique and internal standard method, and the pine needles were systematically studied throughout the year. The data show that the pine pine needles and their pollen in the growth process contain various inorganic elements such as K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Rb, Sr, etc. among them, K, the same element is recovered at the low, middle and high levels of the same element. The rate of 94%~104% can meet the requirements of microdetermination, and the results of XRF and ICP-AES are basically consistent with the results of the actual samples. The contents of inorganic elements in the three cedar pine needles in the one year growth period are different, but the overall contents of the pine needles are regular, and the content of each element in the sample of the old cedar pine needles does not vary greatly because of the months. The fourth part: the fourth part: the basic study on the application of electrodeposition and new X ray fluorescence spectrometer to the deposition of single copper ions. The best potential of deposition of pH, the deposition time, the effect of different salinity on the deposition of copper ions, the effect of the area of different glassy carbon electrode on the deposition of copper ions, and the coexistence of multiple ions The influence of copper ion and the deposition rate of copper standard solution at different concentration were experimentally studied, and the experiment of recovery rate of actual samples was carried out at the same time. The results showed that the best deposition pH of copper ion was pH=5 acetic acid sodium acetate buffer system, the optimum deposition potential of copper ion was -0.6V, and the increase of salinity would enhance the ionic strength of the solution and make copper. The deposition rate of ions is improved, but it is not the main factor affecting the deposition of copper ions; the deposition rate of copper ions is positively related to the deposition time and the working area of the glassy carbon electrode; the coexistence of multi ions does not affect the deposition of copper ions; the results of XRF detection are in agreement with the results of ICP-AES detection, and the standard under different concentrations is the standard. The deposition rate of copper ions is close to that of 1.26%~2.06%, and the application of electrodeposition and new X ray fluorescence spectrometry to the test of actual samples is consistent with the data of standard copper ion detection.

【学位授予单位】：烟台大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O657.34

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