本文關(guān)鍵詞： 鋰 現(xiàn)場分析 便攜式Li-K分析儀 鹽湖鹵水 鋰輝石　出處：《中國地質(zhì)科學(xué)院》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：鋰資源作為一種重要的戰(zhàn)略資源,對國民經(jīng)濟(jì)的發(fā)展意義重大,近年來越來越受到世界各國的重視。我國的鋰資源主要集中在西藏、青海、四川、新疆、江西等偏遠(yuǎn)地區(qū),將樣品運(yùn)送至實(shí)驗(yàn)室檢測會(huì)消耗大量的人力與財(cái)力,因而急需建立針對鋰資源中鋰的快速、準(zhǔn)確的現(xiàn)場分析方法,以節(jié)約分析成本,提高分析效率,實(shí)時(shí)指導(dǎo)鋰資源勘查。目前,鋰的檢測方法主要有電感耦合等離子體發(fā)射光譜法、原子吸收光譜法、原子發(fā)射光譜法等,由于這些大型儀器需載氣、燃?xì)獾葰饬鳁l件,一般只能用于室內(nèi)分析;而傳統(tǒng)分析方法如重量法、容量法,操作復(fù)雜,檢測周期長,難以實(shí)現(xiàn)快速分析的需求。便攜式能量色散X射線熒光光譜法常應(yīng)用于野外現(xiàn)場分析,但靈敏度低,不能分析輕元素Li。大氣壓液體陰極輝光放電發(fā)射光譜儀(SCGD-AES)可在大氣壓下工作,無需載氣、燃?xì)狻⒅細(xì)夂驼婵窄h(huán)境,不需要霧化裝置,因而作為便攜裝置具有極大的優(yōu)越性,已在環(huán)境、生物、食品等多種樣品中金屬離子的檢測得到了廣泛的應(yīng)用。本論文采用大氣壓液體陰極輝光放電發(fā)射光譜技術(shù),開展了鹽湖鹵水及鋰輝石樣品中鋰的現(xiàn)場分析方法研究和應(yīng)用示范。1)利用項(xiàng)目組自行開發(fā)的便攜式Li-K分析儀建立了鹽湖鹵水中鋰的分析方法。探討了酸的種類及pH對Li信號(hào)強(qiáng)度的影響。本方法Li的檢出限為4 ng/mL,精密度為1.7%(n=12),鹽湖鹵水(鋰含量較高)中鋰的Li-K分析儀測定值與ICP-MS測量值相對比,相對誤差均小于2%。將建立的鹵水中鋰的分析方法應(yīng)用于察爾汗鹽湖的現(xiàn)場分析,Li-K分析儀的測定值與ICP-AES測量值相比,相對誤差基本上均小于15%,滿足野外現(xiàn)場分析的需求。2)利用便攜式Li-K分析儀建立了鋰輝石樣品中鋰的分析方法。優(yōu)選酸消耗少、消解效率高、環(huán)境友好、具批量快速樣品處理能力的微波消解技術(shù)對鋰輝石樣品進(jìn)行前處理,在最優(yōu)儀器條件下測量鋰含量。鋰輝石樣品中鋰的Li-K分析儀測定值與ICP-MS測量值相對比,相對誤差均小于10%,滿足鋰輝石樣品現(xiàn)場分析需求。3)初步研究鹽湖鹵水及鋰輝石樣品中存在的基體效應(yīng),研究發(fā)現(xiàn)鹽湖鹵水基體和鋰輝石樣品基體均在一定程度上抑制鋰信號(hào)強(qiáng)度。并采用標(biāo)準(zhǔn)加入法克服了基體效應(yīng)對鋰測定的影響,經(jīng)大量實(shí)驗(yàn)數(shù)據(jù)表明,采用2個(gè)點(diǎn)作標(biāo)準(zhǔn)加入法工作曲線即可獲得較高的準(zhǔn)確度,從而大大減少了工作量,提高野外現(xiàn)場樣品的檢測效率。4)為簡化鋰輝石樣品前處理流程,優(yōu)選耐氫氟酸的剛玉材質(zhì)管,設(shè)計(jì)了內(nèi)嵌式陰極-Li-K分析儀,并利用該裝置分析測定了14種鋰輝石樣品中的鋰含量。為避免高原極端環(huán)境下機(jī)械進(jìn)樣裝置無法正常工作,設(shè)計(jì)了自流式進(jìn)樣-Li-K分析儀。利用改進(jìn)的注射器進(jìn)樣-Li-K分析儀實(shí)現(xiàn)現(xiàn)場測定江西宜豐等地近200件花崗巖和偉晶巖樣品中的鋰含量。
[Abstract]:As an important strategic resource, lithium resources are of great significance to the development of the national economy and have attracted more and more attention in recent years. The lithium resources in China are mainly concentrated in remote areas such as Tibet, Qinghai, Sichuan, Xinjiang, Jiangxi, etc. Transporting samples to the laboratory will consume a lot of manpower and financial resources. Therefore, it is urgent to establish a rapid and accurate on-site analysis method for lithium in lithium resources in order to save the analysis cost and improve the analysis efficiency. At present, the detection methods of lithium mainly include inductively coupled plasma emission spectrometry, atomic absorption spectrometry, atomic emission spectrometry and so on. Traditional analytical methods such as gravimetric method, volumetric method, complex operation and long detection period are difficult to meet the requirement of rapid analysis. Portable energy dispersive X-ray fluorescence spectrometry is often used in field analysis. But because of its low sensitivity, it is not possible to analyze the light element Li.Atmospheric pressure liquid cathodic glow discharge emission spectrometer SCGD-AESs can work at atmospheric pressure without the need for carrier gas, gas, auxiliary gas and vacuum environment, and no atomization device. Therefore, as a portable device, it has been widely used in the detection of metal ions in many kinds of samples, such as environment, biology, food and so on. The field analysis method and application demonstration of lithium in salt lake brine and spodumene samples were carried out. The method of lithium analysis in salt lake brine was established by using portable Li-K analyzer developed by the project team. The effect of pH on the signal intensity of Li. The detection limit of Li is 4 ng / mL, the precision is 1. 7%, and the Li-K analyzer is compared with the ICP-MS measurement value in brine of salt lake (high lithium content). The relative errors are less than 2. The established method for the analysis of lithium in brine is applied to the field analysis of Chalhan Salt Lake. The measured value of Li-K analyzer is compared with that of ICP-AES. The relative errors are basically less than 15. The relative error is less than 15. 2) the method of lithium analysis in spodumene samples is established by using portable Li-K analyzer. The method has the advantages of low acid consumption, high digestion efficiency and environmental friendliness. The pretreatment of spodumene samples with microwave digestion technology with batch and rapid sample processing ability was carried out, and the lithium content was measured under the optimal instrument conditions. The Li-K analyzer measured lithium in spodumene sample was compared with the ICP-MS measurement value. The relative error is less than 10. The matrix effect in salt lake brine and spodumene sample is studied preliminarily. It is found that both the salt lake brine matrix and the spodumene sample matrix inhibit the lithium signal intensity to some extent, and the influence of the matrix effect on the determination of lithium is overcome by the standard addition method. Using two points as the standard adding method can get higher accuracy, thus greatly reducing the workload and improving the detection efficiency of field samples. 4) in order to simplify the pretreatment process of spodumene samples, A corundum tube with hydrofluoric acid resistance was selected, and an embedded cathode Li-K analyzer was designed, and the lithium content in 14 kinds of spodumene samples was determined by the device. A self-flow injection-Li-K analyzer was designed. The improved injector injector sample -Li-K analyzer was used to determine the lithium content in nearly 200 samples of granite and pegmatite in Yifeng and other places in Jiangxi province.
【學(xué)位授予單位】：中國地質(zhì)科學(xué)院
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：O657.3;TS312;P585

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