本文關(guān)鍵詞：基于離子色譜法測定水環(huán)境中氨氮及含磷化合物的研究　出處：《浙江大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

  更多相關(guān)文章： 離子色譜 水環(huán)境 氨氮 含磷化合物 加速溶劑萃取

【摘要】：水域的富營養(yǎng)化是普遍的水環(huán)境問題之一。氮磷化合物則是富營養(yǎng)化的重要因素。氮磷化合物在水質(zhì)中以各種形態(tài)存在,也蓄積在水域沉積物中,不時釋放,因此監(jiān)測水質(zhì)及沉積物中氮磷化合物,具有一定的環(huán)保監(jiān)測意義。離子色譜(IC)是分析各種離子化合物的有效手段之一,其自動化程度高、操作簡便,被廣泛應(yīng)用于環(huán)境、食品、能源及醫(yī)藥化工等眾多領(lǐng)域。本文利用雙系統(tǒng)離子色譜法同時測定了水中氨氮及過硫酸鹽的含量,并對過硫酸鹽的降解作用做了初步研究。采用加速溶劑萃取技術(shù),提取沉積物中無機正磷酸鹽及多聚磷酸鹽,運用離子色譜法進(jìn)行測定。主要研究由以下三章構(gòu)成。第一章:介紹了氮磷化合物的有關(guān)概況,并對氨氮、過硫酸鹽、無機正磷酸鹽、多聚磷酸鹽的有關(guān)檢測方法進(jìn)行了綜述。第二章:建立了一種測定湖水中氨氮和過硫酸根的雙系統(tǒng)離子色譜法。在加熱條件下過硫酸根分解水體中的氨氮,通過雙系統(tǒng)離子色譜,它們分別以甲烷磺酸和氫氧化鉀為淋洗液,抑制電導(dǎo)檢測。該方法實現(xiàn)了同時檢測湖水中陽離子(氨氮)和陰離子(過硫酸鹽)。第三章:采集富營養(yǎng)化水域環(huán)境中的土壤和沉積物,對快速溶劑萃取條件進(jìn)行優(yōu)化,處理及提取樣品后過微孔濾膜和預(yù)柱直接進(jìn)行離子色譜分析。按照從簡到繁,從等度淋洗到梯度淋洗的順序依次摸索,研究了含磷化合物的離子色譜條件。1:選用IonPac AS23為陰離子分析柱,以Na2CO3-NaHCO3-NaOH溶液體系等度淋洗,測定了磷酸鹽和亞磷酸鹽。2:IonPacAS11為陰離子分析柱,氫氧化鉀溶液梯度淋洗,同時測定焦磷酸鹽及其它常規(guī)陰離子。3:以IonPacAS19高容量陰離子交換分析柱進(jìn)行分離,淋洗液自動發(fā)生裝置在線產(chǎn)生KOH進(jìn)行梯度洗脫,抑制型電導(dǎo)檢測,40min內(nèi)同時測定湖底沉積物中三聚磷酸鹽及常規(guī)陰離子和部分含磷化合物(亞磷酸鹽、磷酸鹽、焦磷酸鹽、三偏磷酸鹽)。通過分離度、精密度、準(zhǔn)確度等指標(biāo)判斷,認(rèn)為IonPacAS19為分析柱,氫氧化鉀梯度淋洗的色譜條件下,能有效的分離測定各種含磷化合物和常規(guī)陰離子,該法為最優(yōu)的離子色譜法,操作簡便,完全適合開展各種含磷化合物(亞磷酸鹽、磷酸鹽、焦磷酸鹽、三聚磷酸鹽)和常規(guī)陰離子的分離測定。
[Abstract]:Eutrophication in water is one of the most common problems in water environment. Nitrogen and phosphorus compounds are important factors of eutrophication. Nitrogen and phosphorus compounds exist in various forms in water quality, and they are also accumulated in water sediments and released from time to time. Therefore, the monitoring of nitrogen and phosphorus compounds in water quality and sediment has a certain environmental monitoring significance. Ion chromatography (IC) is one of the effective means for the analysis of various kinds of ionic compounds, its automation is high, and the operation is simple. It has been widely used in many fields such as environment, food, energy, medicine and chemical industry. In this paper, the content of ammonia nitrogen and persulfate in water was determined by double system ion chromatography. The degradation of persulfate was studied. Inorganic orthophosphate and polyphosphate were extracted from sediments by accelerated solvent extraction. The determination was carried out by ion chromatography. The main research was composed of the following three chapters. Chapter 1: the introduction of nitrogen and phosphorus compounds, and the ammonia nitrogen, persulfate, inorganic orthophosphate. In chapter 2, a dual-system ion chromatography method for the determination of ammonia-nitrogen and persulfate in lake water was established. Under the condition of heating, the ammonia-nitrogen in water was decomposed by persulfate radical. By dual system ion chromatography, methanesulfonic acid and potassium hydroxide were used as eluent respectively. Inhibition conductance detection. This method can simultaneously detect cations (ammonia nitrogen) and anions (persulfate) in lake water. Chapter 3: collecting soil and sediment in eutrophic water environment. The conditions of rapid solvent extraction were optimized, the samples were treated and extracted, the microporous filter membrane and the pre-column were directly analyzed by ion chromatography, and the sequence of isotropic elution to gradient elution was studied from simple to complex. The ion chromatographic conditions of phosphate compounds were studied. 1. IonPac AS23 was selected as anion analysis column and isoprene elution was carried out in Na2CO3-NaHCO3-NaOH solution system. The determination of phosphate and phosphite. 2: Ion PacAS11 was carried out on anion analytical column with gradient elution of potassium hydroxide solution. Simultaneous determination of pyrophosphate and other conventional anions. The separation was carried out on a IonPacAS19 high capacity anion exchange analytical column, and the KOH was generated on line by an automatic eluant generator for gradient elution. The inhibitory conductance test was used to simultaneously determine tripolyphosphate, conventional anions and some phosphate compounds (phosphite, phosphate, pyrophosphate) in lake bottom sediments within 40 minutes. Based on the determination of separation degree, precision and accuracy, it is considered that IonPacAS19 is an analytical column with gradient elution of potassium hydroxide. This method is the best ion chromatography method, which is simple and suitable for the development of various phosphate compounds (phosphite, phosphate, pyrophosphate). Separation and determination of tripolyphosphate and conventional anions.
【學(xué)位授予單位】：浙江大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：X832;O657.7

【參考文獻(xiàn)】

相關(guān)期刊論文 前10條

1 周黔蘭;吳紅;李海英;;氣相分子吸收光譜法測定水中氨氮濃度不確定度評定[J];環(huán)境與發(fā)展;2015年04期

2 歐敏萍;;離子色譜法檢測廢水中氨氮含量的應(yīng)用探討[J];科技與創(chuàng)新;2015年10期

3 何洋;張佩;崔晨;韓楓;;絮凝沉淀法前處理對氨氮測定結(jié)果的影響[J];治淮;2015年01期

4 李麗;劉占孟;聶發(fā)揮;;過硫酸鹽活化高級氧化技術(shù)在污水處理中的應(yīng)用[J];華東交通大學(xué)學(xué)報;2014年06期

5 袁明浩;張喜鳳;張文麗;;離子色譜法測定工業(yè)廢水中氨氮[J];河南科學(xué);2014年10期

6 王中賀;李佳偉;劉伶;高蓉;;新型環(huán)保水質(zhì)氨氮快速檢測試劑盒的研制與應(yīng)用[J];中國衛(wèi)生檢驗雜志;2014年15期

7 王秀麗;陳煒斌;;水楊酸法測定水中氨氮的不確定度評定[J];城鎮(zhèn)供水;2014年04期

8 彭蘭慧;;不同納氏試劑測定氨氮的結(jié)果探討[J];淮北職業(yè)技術(shù)學(xué)院學(xué)報;2014年03期

9 章劍揚;陳利燕;馬桂岑;劉新;;加速溶劑萃取/離子色譜法測定菊花中的SO_2殘留[J];分析測試學(xué)報;2014年05期

10 孫浩波;王小芳;;分光光度法測定重鈾酸鹽中的磷酸根[J];鈾礦冶;2014年02期

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