本文關(guān)鍵詞： 輝光放電 離子色譜 陰離子 吸附 鉛離子　出處：《東華大學(xué)》2016年碩士論文　論文類型：學(xué)位論文

【摘要】：隨著現(xiàn)代工業(yè)的發(fā)展,環(huán)境污染問題日益嚴(yán)重,大量的重金屬及有毒陰離子被排入土壤、河流及海洋等水體中,嚴(yán)重危害土壤及水體生態(tài)環(huán)境。因此,實(shí)現(xiàn)便捷、高效、快速的金屬離子及陰離子檢測(cè)技術(shù)對(duì)于環(huán)境監(jiān)測(cè)具有重要意義。目前,液體陰極輝光放電原子發(fā)射光譜法(Solution Cathode Glow Discharge Atomic Emission Spectroscopy,SCGD-AES)是其中發(fā)展最快,最有應(yīng)用潛力的金屬離子檢測(cè)方法之一,在原子光譜分析中作為一種新興的元素檢測(cè)技術(shù)而備受關(guān)注。與傳統(tǒng)原子光譜儀器(原子吸收光譜、等離子體光譜/質(zhì)譜等)相比,液體陰極輝光放電具有可在大氣壓下操作,不需乙炔或高純氬氣等工作氣體,儀器功率要求低(放電功率小于100 W),樣品進(jìn)樣時(shí)無需使用霧化器等優(yōu)點(diǎn)。然而低溫等離子體由于其激發(fā)溫度的限制,對(duì)某些重金屬離子的檢測(cè)靈敏度還無法滿足應(yīng)用需求。本文的研究內(nèi)容主要圍繞實(shí)驗(yàn)室已構(gòu)建的液體陰極輝光放電光譜裝置而展開。首先,對(duì)儀器的原子化器進(jìn)行了改進(jìn),使得等離子體放電的穩(wěn)定性提高,為以后儀器的小型化及便攜式提供了可能。實(shí)驗(yàn)考察了電壓大小、進(jìn)樣流速、電解液種類、電解液pH值對(duì)儀器性能的影響。結(jié)果表明,儀器操作的最佳條件為:放電電壓為1060 V,進(jìn)樣流速為2 mL/min,p H=1的硝酸作為電解液溶液。為了提高儀器對(duì)重金屬鉛的靈敏度,采用固相萃取技術(shù)將液體陰極輝光放原子發(fā)射光譜儀與流動(dòng)注射儀聯(lián)用,并根據(jù)文獻(xiàn)制備了一種氧化石墨烯/介孔SBA-15復(fù)合材料作為鉛的吸附劑,建立了在線分析檢測(cè)溶液中鉛的分析方法。實(shí)驗(yàn)確定了聯(lián)用裝置的最佳條件,固相萃取盤填料量為30 mg,富集流速為1 mL/min,洗脫劑為0.1 M硝酸,對(duì)鉛的富集倍數(shù)為15。為了驗(yàn)證方法的可靠性,對(duì)標(biāo)準(zhǔn)物質(zhì)GBW09101b(人發(fā))及GBW07310(水系沉積物)進(jìn)行分析,實(shí)驗(yàn)結(jié)果與電感耦合等離子體質(zhì)譜(Inductively Coupled Plasma-Mass Spectrometry,ICP-MS)測(cè)定值比較相一致,并與參考值吻合。在Schwartz等人的基礎(chǔ)上,采用鋰離子交換柱作為交換器,將不同陰離子所配位的H+等摩爾比地置換成鋰離子,并利用液體陰極輝光光譜儀作為離子色譜的檢測(cè)器,通過檢測(cè)鋰離子的變化值實(shí)現(xiàn)對(duì)陰離子的檢測(cè),建立了一種可用于陰離子分析的高靈敏檢測(cè)方法。聯(lián)用裝置檢測(cè)陰離子的最佳條件為:最佳電壓為1060V,最佳補(bǔ)充液流速為0.9 mL/min,最佳淋洗液濃度為15 mM的KOH。在該優(yōu)化條件下,對(duì)F~-、Cl~-、Br~-、NO_2~-、NO_3~-、CH_3COO~-和SO_4~(2-)等陰離子的檢出限在4~17μg/L之間。將此方法用于自來水及河水中陰離子的檢測(cè)并與離子色譜儀的檢測(cè)值比較,結(jié)果令人滿意。
[Abstract]:With the development of modern industry, the problem of environmental pollution is becoming more and more serious. A large number of heavy metals and toxic anions are discharged into soil, rivers and oceans, which seriously endanger the ecological environment of soil and water bodies. Rapid detection of metal ions and anions is of great significance for environmental monitoring. At present, the solution Cathode Glow Discharge Atomic Emission spectroscopySCGD-AESs are the fastest growing. One of the most promising methods for the detection of metal ions has attracted much attention as a new technique for the detection of elements in atomic spectrum analysis, compared with conventional atomic spectrometer (atomic absorption spectrum, plasma / mass spectrometry, etc.). Liquid cathode glow discharge can be operated at atmospheric pressure, without the need of acetylene or high purity argon and other working gases, The instrument requires low power (discharge power less than 100WN, sample injection without atomizer, etc.). However, the low temperature plasma is limited by its excitation temperature. The detection sensitivity of some heavy metal ions can not meet the requirement of application. This paper mainly focuses on the liquid cathode glow discharge spectrometer which has been constructed in the laboratory. Firstly, the atomizer of the instrument is improved. The stability of plasma discharge is improved, which provides the possibility for the miniaturization and portable of the instrument in the future. The effects of voltage, injection velocity, electrolyte type, pH value of electrolyte on the performance of the instrument are investigated experimentally. The optimum operating conditions are as follows: the discharge voltage is 1060V, and the injection rate is 2 mL / min / min / h ~ (-1) nitric acid as electrolyte solution. In order to improve the sensitivity of the instrument to heavy metal lead, Solid phase extraction (SPE) technique was used to combine liquid cathodic glow discharge atomic emission spectrometer with flow injector, and a graphene oxide / mesoporous SBA-15 composite was prepared as the adsorbent of lead according to the literature. An on-line analytical method for the determination of lead in solution was established. The optimum conditions of the combined device were determined. The solid phase extraction disk packing amount was 30 mg, the enrichment flow rate was 1 mL / min, and the eluent was 0.1 M nitric acid. The enrichment ratio of lead is 15. In order to verify the reliability of the method, the standard materials GBW09101b (human hair) and GBW07310( sediment of water system) are analyzed. The experimental results are in good agreement with the results of inductively Coupled Plasma-Mass spectrometric ICP-MSs determined by inductively coupled plasma mass spectrometry (ICP-MS). On the basis of Schwartz et al, the lithium ion exchange column was used as the exchanger, the H coordinated by different anions was replaced to lithium ion at the same molar ratio, and the liquid cathodic glow spectrometer was used as the detector of ion chromatography. The detection of anions can be achieved by detecting the variation of lithium ions. A highly sensitive detection method for anion analysis was established. The optimum conditions for the detection of anions by the combined device were as follows: the optimum voltage was 1060V, the optimal flow rate of the supplementary solution was 0.9 mL / min, and the optimum concentration of eluant was 15 mm. The detection limits of the anions such as FCU ClCl-CU Br-nO _ 2C _ 2C _ 2C _ 2C _ (C) -C _ 3COOO ~ (-) and so _ (4) C _ (2)) are in the range of 4 ~ 17 渭 g / L. The method has been applied to the determination of anions in tap water and river water with satisfactory results compared with the determination values of ion chromatograph. The results are as follows: (1) the detection of anions in tap water and river water is satisfactory.
【學(xué)位授予單位】：東華大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2016
【分類號(hào)】：O657.3

【參考文獻(xiàn)】

相關(guān)期刊論文 前2條

1 鄭培超;王鴻梅;李建權(quán);韓海燕;席曉琴;儲(chǔ)焰南;;大氣壓電解液陰極輝光放電發(fā)射光譜檢測(cè)水體中的金屬殘留[J];光譜學(xué)與光譜分析;2010年07期

2 席曉琴;鄭培超;王鴻梅;李建權(quán);韓海燕;儲(chǔ)焰南;;電解液陰極大氣輝光放電原子發(fā)射光譜檢測(cè)水硬度[J];分析化學(xué);2010年03期

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本文編號(hào)：1503852