發(fā)布時間：2018-04-23 12:10

  本文選題：X射線熒光光譜儀 + 雪松松針　； 參考：《煙臺大學》2016年碩士論文

【摘要】：X射線熒光光譜法適用于對物質成分分析,可直接對固體(塊狀或粉末狀)和液體樣品中主量元素、微量元素進行多元素同時分析。當結合薄樣技術時,具有高靈敏度,用樣量少等優(yōu)點。隨著分析技術的發(fā)展和科研水平的提高,分析領域愈發(fā)關注待測成分復雜和含量低等特點課題,對儀器本身提出更高要求。本課題組由田宇~淌詿煜略諶瓷鋁射線熒光分析儀研究基礎上對儀器進行了改進,研制出一臺高靈敏度的新型X射線熒光光譜儀。論文對儀器結構進行介紹,并將儀器主要應用到微量元素的分析。本論文主要包括四個部分:第一部分:介紹了X射線熒光產生原理、X射線熒光光譜儀發(fā)展史及應用、常見樣品前處理方法及聯(lián)用方法的原理和應用。同時,闡明了本論文的立題思想及主要研究內容。第二部分:介紹了本課題組研制的新型X射線熒光光譜儀結構裝置、儀器定量分析方法,并對儀器進行了性能實驗工作。新型X射線熒光光譜儀主要包括激發(fā)系統(tǒng)、探測器系統(tǒng)、記錄單元、高壓電源和真空泵等部分。采用鉬靶和鈦靶雙靶X光管激發(fā)系統(tǒng),由X-123型硅漂移探測器和DPP數字脈沖處理器組裝而成;其定量分析是通過薄樣技術和內標法結合實現的;通過靈敏度校準曲線可以看出,K線系各元素的偏差均小于±1%,L線系所得各元素的偏差均小于±2%;精密度(RSD)(n=6)在2.2%~5.8%之間;各元素方法檢出限及定量下限相對較好。第三部分:將新型X射線熒光光譜儀應用于雪松松針及其花粉中無機元素的分析。結合薄樣技術及內標法建立了對雪松松針及其花粉中多種無機元素同時分析的方法,并系統(tǒng)的研究了雪松松針在全年生長周期內多種無機元素含量變化情況。數據表明:雪松松針及其花粉在生長過程均含有植物體所需要的K、Ca、Ti、Cr、Mn、Fe、Ni、Cu、Zn、Rb、Sr等多種無機元素,其中,K、Ca含量居高,Mn、Fe次之;同一元素在低、中、高三種不同加標水平下的平均加標回收率在94%~104%之間,能滿足微量測定要求;XRF法與ICP-AES法對實際樣品測定結果基本吻合;三地點雪松松針在一年生長周期內各無機元素含量雖然存在不同,但整體呈現一定規(guī)律性;雪松老針樣品中各元素含量并未因月份不同有較大變動,含量較為穩(wěn)定。第四部分:將電沉積技術與新型X射線熒光光譜儀聯(lián)用應用于沉積單個銅離子的基礎研究。對沉積最佳pH、沉積最佳電位、沉積時間、不同鹽度對沉積銅離子的影響、不同玻碳電極工作面積對沉積銅離子的影響、多離子共存時對沉積銅離子的影響及不同濃度的銅標準溶液沉積率進行實驗研究,同時進行實際樣品的回收率實驗。結果表明:銅離子的最佳沉積pH為pH=5的醋酸-醋酸鈉緩沖體系;銅離子的最佳沉積電位為-0.6V;鹽度的提高會增強溶液離子強度,使銅離子沉積率有所提高,但不是影響銅離子沉積的主要因素;銅離子的沉積率與沉積時間和玻碳電極工作面積呈正相關關系;多離子共存時并未影響銅離子的沉積;將XRF檢測結果與ICP-AES檢測結果進行對比,結果較為一致;不同濃度下標準銅離子的沉積率較為接近,均在1.26%~2.06%之間;電沉積技術與新型X射線熒光光譜聯(lián)用技術應用到實際樣品檢測時,其加標回收實驗與標準銅離子檢測時數據相吻合。
[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.

【學位授予單位】：煙臺大學
【學位級別】：碩士
【學位授予年份】：2016
【分類號】：O657.34

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