【摘要】：大氣中以及水體中的硫的測(cè)試方法很多,但是對(duì)于厭氧環(huán)境中硫的轉(zhuǎn)化仍然有許多不確定的因素(如硫化物、硫代硫酸鹽、亞硫酸鹽、硫酸鹽及單質(zhì)硫),導(dǎo)致其測(cè)定準(zhǔn)確性、可靠性收到一定的限制。本文圍繞各類硫組分(包括硫化物、硫代硫酸鹽、亞硫酸鹽、硫酸鹽及單質(zhì)硫等)的存在形態(tài)進(jìn)行分析及定量測(cè)試。我們?cè)诮栌们叭藱z測(cè)方法的同時(shí),獨(dú)立設(shè)計(jì)了多種檢測(cè)方法(S~0,SO_3~(2-)和S_2O_3~(2-)),從而總結(jié)出多種不同形態(tài)硫的提取及測(cè)試方法利用萃取單質(zhì)硫的方法,通過高效液相色譜法來檢測(cè)溶解態(tài)單質(zhì)硫。利用DTNB作為衍生劑,對(duì)沉積物中硫代硫酸鹽和亞硫酸鹽進(jìn)行分析測(cè)試。從而在酸鹽還原菌(SRB)生物厭氧反應(yīng)器中結(jié)合其他硫組分測(cè)試,分析了硫酸鹽產(chǎn)物的整體變化趨勢(shì)。得到以下結(jié)論:(1)在比較實(shí)驗(yàn)基礎(chǔ)上選取丙酮作為萃取劑,經(jīng)過10分鐘超聲萃取后,可穩(wěn)定高效的萃取出單質(zhì)硫。(2)新設(shè)計(jì)了一種硫單質(zhì)檢測(cè)方法,并計(jì)算出:單質(zhì)硫的檢出限為1.25×10~(-3)mg/L(2.5×10~(-3)μg/kg),檢測(cè)下限為4.18×10~(-3)mg/L(8.36×10~(-3)μg/kg);利用高效液相色譜法對(duì)單質(zhì)硫進(jìn)行測(cè)試的加標(biāo)回收率在100%-120%之間。厭氧發(fā)酵產(chǎn)物中硫化物濃度均在該檢測(cè)范圍內(nèi),因此可利用這種方法對(duì)發(fā)酵產(chǎn)物中單質(zhì)硫進(jìn)行檢測(cè)。(3)硫代硫酸鹽和亞硫酸鹽測(cè)定方法研究中,選取DTNP作為衍生試劑,采用多步梯度淋洗的方式,選擇合適的液相色譜操作條件可得到較好的測(cè)試效果。其中硫代硫酸鹽的檢出限為1.25×10~(-3)mg/L,亞硫酸鹽的檢出限為1.25×10~(-3)mg/L,測(cè)試的加標(biāo)回收率均在100%左右。(4)在對(duì)SRB降解硫酸鹽反應(yīng)器中間產(chǎn)物的硫代硫酸根和亞硫酸根測(cè)試中,發(fā)現(xiàn)它們的濃度相對(duì)于硫酸根的還原量很小,平均只有0.16mg,幾乎可以忽略不計(jì)。其各含硫組分含量順序?yàn)镾~(2-)S~0H_2SSO_3~(2-)/(S_2O_3~(2-))。大約70%的產(chǎn)物是以硫化物形式存在的,10%是以單質(zhì)硫形式存在的,其余的硫是以SO_3~(2-),S_2O_3~(2-),S_2O_5~(2-),S_2O_4~(2-)等形式存在。摻入針鐵礦的反應(yīng)器中發(fā)現(xiàn)有17.2%的硫損失,主要以FeS,FeS_2及有機(jī)硫等形式損失。
[Abstract]:There are many methods for the measurement of sulfur in the atmosphere and in water, but there are still many uncertain factors (such as sulfides, thiosulfate, sulfite, sulfate and elemental sulfur) for sulfur conversion in anaerobic environment, which lead to the accuracy of the determination. Reliability is subject to certain limitations. In this paper, the species of various sulfur components (including sulfides, thiosulfate, sulfite, sulfate and elemental sulfur) are analyzed and quantitatively tested. At the same time, we have independently designed a variety of detection methods (S0 / so _ 3 ~ (2-) and S _ 2O _ 3 ~ (2-),) to sum up the extraction and test methods of different forms of sulfur by using the methods of extraction of elemental sulfur. The dissolved elemental sulfur was determined by high performance liquid chromatography (HPLC). The thiosulfate and sulfite in sediment were analyzed and tested by using DTNB as derivative. So the overall change trend of sulfate products was analyzed in (SRB) biofilm reactor combined with other sulfur components test. The following conclusions are obtained: (1) acetone is selected as extractant on the basis of comparative experiments, and after 10 minutes of ultrasonic extraction, simple sulfur can be extracted stably and efficiently. (2) A new method for the determination of sulfur is designed. The detection limit of elemental sulfur is 1.25 脳 10 ~ (-3) mg/L (2.5 脳 10 ~ (-3) 渭 g/kg) and the detection limit is 4.18 脳 10 ~ (-3) mg/L (8.36 脳 10 ~ (-3) 渭 g/kg). The concentration of sulfides in anaerobic fermentation products is all within the range of detection, so we can use this method to detect the elemental sulfur in fermentation products. (3) in the study of the determination method of thiosulfate and sulfite, DTNP is chosen as the derivative reagent. The method of multi-step gradient elution and the suitable operating conditions of liquid chromatography can obtain better test results. The detection limit of thiosulfate is 1.25 脳 10 ~ (-3) mg/L, sulfite, and the detection limit is 1.25 脳 10 ~ (-3) mg/L,. It is found that their concentration is very small relative to sulfate, with an average of only 0.16 mg, which is almost negligible. The order of the content of sulfur components is S ~ (2-) S ~ (2) H _ (2SO) _ 3 ~ (2-) / (S _ 2O _ 3 ~ (2-).) About 70% of the products are in the form of sulfide, 10% of the products are in the form of simple sulfur, and the rest of the sulfur is in the form of SO_3~ (2-) S2O3- (2-) S _ 2O _ 5- / S _ 2O-S _ 2O _ (4-), etc. In the reactor mixed with goethite, 17.2% of sulfur loss was found, mainly in the form of FeS,FeS_2 and organic sulfur.
【學(xué)位授予單位】：合肥工業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：X703;X830

【參考文獻(xiàn)】

相關(guān)期刊論文 前10條

1 閆春輝;徐凌云;馬泓冰;張勇;孫宏枚;;離子色譜法測(cè)定甲基亞磺酸鈉中的氯離子和硫酸根離子[J];化學(xué)試劑;2017年03期

2 晁輝;李花;戴興德;;自動(dòng)電位滴定法標(biāo)定硫代硫酸鈉溶液和碘鹽碘含量測(cè)定[J];中國衛(wèi)生檢驗(yàn)雜志;2016年19期

3 張光建;;Excel在校準(zhǔn)曲線估算方法檢出限及測(cè)定下限中的應(yīng)用[J];中國衛(wèi)生檢驗(yàn)雜志;2016年07期

4 羅剛;黃兆龍;賴夢(mèng)書;;絡(luò)合滴定法間接測(cè)定硫酸根濃度的條件研究[J];紅河學(xué)院學(xué)報(bào);2016年02期

5 鄒洪濤;凌堯;于洋;張玉玲;虞娜;張玉龍;;包膜肥料用改性聚乙烯醇膜材料降解性的研究（英文）[J];光譜學(xué)與光譜分析;2015年11期

6 畢思峰;崔香梅;;重量法與分光光度法測(cè)鹽湖鹵水中硫酸根[J];鹽業(yè)與化工;2015年10期

7 郭愛華;王瑋;袁佗;高洋洋;李曄;;離子色譜法同時(shí)測(cè)定飲用水中11種無機(jī)陰離子[J];化學(xué)分析計(jì)量;2015年04期

8 王金霞;林江麗;鹿毅;王吉德;;熒光衍生化法測(cè)定新疆特色葡萄干中總亞硫酸鹽含量[J];食品科學(xué);2016年04期

9 任華忠;封家福;伍朝君;;離子色譜法測(cè)定注射用硫代硫酸鈉中的亞硫酸鹽和硫酸鹽[J];華西藥學(xué)雜志;2015年01期

10 張春紅;蔡足根;;EDTA-Ba容量法快速測(cè)定地下水中硫酸根[J];廣州化工;2014年18期

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