聚合鋁形態(tài)的液相色譜分離及其鋁元素分析測(cè)定方法研究
本文選題:混凝 + 鋁形態(tài); 參考:《河北師范大學(xué)》2015年碩士論文
【摘要】:近年來(lái),伴隨著全球工業(yè)化進(jìn)程的加速和世界人口的飛速增長(zhǎng),環(huán)境問(wèn)題已成為世界各國(guó)人民普遍關(guān)注的一個(gè)熱門話題,尤其面臨著水質(zhì)不斷惡化等污染問(wèn)題。電絮凝已廣泛的應(yīng)用到多種行業(yè)的廢水處理中。聚合氯化鋁(PACl)在水處理中是一種常用到的重要的鋁系高分子絮凝劑,聚合氯化鋁的研究在水處理行業(yè)有重要意義。本碩士學(xué)位論文嘗試用C18反相高效液相色譜法對(duì)PACl混凝劑中鋁的不同形態(tài)進(jìn)行色譜分離,并將Ferron逐時(shí)絡(luò)合比色分析與色譜分離相結(jié)合進(jìn)行鋁形態(tài)的分析測(cè)定。對(duì)鋁的色譜分離條件進(jìn)行了優(yōu)化,并分別用石墨爐原子吸收和等離子體質(zhì)譜法對(duì)不同色譜組分中鋁的分析測(cè)定方法進(jìn)行了實(shí)驗(yàn)研究。主要內(nèi)容如下:1.對(duì)實(shí)驗(yàn)室制備的不同堿化度(B值)聚合氯化鋁樣品,以C18反相高效液相色o}柱進(jìn)行了不同鋁形態(tài)的色譜分離,對(duì)流動(dòng)相體系組成和洗脫條件進(jìn)行了實(shí)驗(yàn)優(yōu)化,并結(jié)合Ferron逐時(shí)絡(luò)合比色法對(duì)各色譜組分進(jìn)行了檢測(cè)分析,得到若干不同鋁形態(tài)的色譜分離譜圖。2.針對(duì)聚合鋁及其色譜分離后含復(fù)雜有機(jī)組分基體條件下難原子化元素鋁的分析檢測(cè)問(wèn)題,以石墨爐原子吸收光譜法進(jìn)行了實(shí)驗(yàn)研究,對(duì)熱解涂層石墨管進(jìn)行了涂鉭覆膜修飾處理,優(yōu)化了石墨爐升溫程序,建立了針對(duì)含有有機(jī)溶劑乙腈的PACl樣品中鋁的分析測(cè)定方法,其相對(duì)標(biāo)準(zhǔn)偏差RSD=1.74%,檢出限為1.54μg/L。3.針對(duì)ICP-MS分析具有快速準(zhǔn)確,靈敏度高、檢測(cè)限低等獨(dú)特優(yōu)點(diǎn),在優(yōu)化HPLC分離條件基礎(chǔ)上,對(duì)含有有機(jī)溶劑乙腈的PACl色譜組分樣品中鋁的ICP-MS測(cè)定方法進(jìn)行了實(shí)驗(yàn)研究,并初步嘗試了鋁形態(tài)的HPLC-ICP-MS聯(lián)用分析。所建方法線性相關(guān)系數(shù)達(dá)0.9979,加標(biāo)回收率在98%-103%之間,RSD5%,適合于含有有機(jī)物聚合氯化鋁溶液中總鋁含量的測(cè)定。采用優(yōu)化后石墨爐原子吸收光譜法和ICP-MS方法均檢測(cè)到色譜傳統(tǒng)紫外檢測(cè)器未檢測(cè)到的色譜組分。
[Abstract]:In recent years, with the acceleration of the global industrialization process and the rapid growth of the world population, environmental problems have become a hot topic that people all over the world pay close attention to, especially facing the pollution problems such as the deterioration of water quality. Electroflocculation has been widely used in wastewater treatment in many industries. Polyaluminium chloride (PACL) is an important aluminum flocculant in water treatment, and the study of polyaluminium chloride is of great significance in water treatment industry. In this thesis, we try to use C18 reversed phase high performance liquid chromatography to separate the different forms of aluminum in PACl coagulant, and combine Ferron timed complexation colorimetry with chromatographic separation to determine the aluminum speciation. The chromatographic separation conditions of aluminum were optimized and the analytical methods of aluminum in different chromatographic components were studied by graphite furnace atomic absorption spectrometry and plasma mass spectrometry respectively. The main content is as follows: 1. The samples of polyaluminium chloride with different alkalinity (B value) prepared in the laboratory were separated by chromatography with C 18 reversed phase high performance liquid color o} column. The composition of mobile phase system and elution conditions were optimized. The chromatographic components were detected and analyzed by Ferron timed complexation colorimetry, and some chromatographic separation spectra of different aluminum forms were obtained. In view of the problem of the analysis and detection of aluminum, which is difficult to be atomized under the condition of polyaluminium and its chromatographic separation, the graphite furnace atomic absorption spectrometry (GFAAS) has been used to study the analysis and detection of aluminum with complex organic components. The pyrolytic coated graphite tube was modified with tantalum coated film, and the temperature program of graphite furnace was optimized. A method for the determination of aluminum in PACl samples containing organic solvent acetonitrile was established. The relative standard deviation (RSD) was 1.74 and the detection limit was 1.54 渭 g / L. 3. Aiming at the unique advantages of rapid and accurate analysis, high sensitivity and low detection limit, the ICP-MS method for the determination of aluminum in PACl chromatographic samples containing organic solvent acetonitrile was studied on the basis of optimizing the separation conditions of HPLC. The HPLC-ICP-MS analysis of aluminum morphology was also preliminarily attempted. The linear correlation coefficient of the method is 0.9979, and the recovery rate is between 98% and 103%. The method is suitable for the determination of total aluminum in polyaluminium chloride solution containing organic matter. The optimized graphite furnace atomic absorption spectrometry (GFAAS) and ICP-MS method were used to detect the undetectable components in the traditional UV detector.
【學(xué)位授予單位】:河北師范大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2015
【分類號(hào)】:O652.63;TQ085.4
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