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基于同位素分析法的氮识别技术及迁移规律研究
The Identify and the Migration of Nitrogen on Isotopic Analysis Method
【作者】 王丽丽;
【导师】 吴俊森;
【作者基本信息】 山东建筑大学 , 环境工程, 2012, 硕士
【摘要】 本文研究了适应鹊山水库水体中硝酸盐氮稳定同位素分析的预处理方法。即用阴离子交换方法富集硝态氮和凯氏蒸馏法将硝态氮还原为氨态氮,研究确定了最佳实验条件,同时结合鹊山水库库区的实际情况,监测了引黄条渠和鹊山水库水中硝酸盐氮的丰度值,根据丰度值判断该库区硝酸盐氮的来源。实验结果表明阴离子交换方法的最佳实验条件是:选用OH型阴离子交换树脂(anion exchanger (Ion exchanger Ⅲ, Merck)),该种树脂吸附和洗脱效果均很稳定,不会产生同位素分馏,因此作为富集硝酸盐氮的载体。针对水库水体,交换柱装填的树脂高度为3cm;吸附过程中过柱流速控制在800~900mL/min左右,洗脱时采用浓度为2mol/L的KCl溶液40mL作为洗脱液,洗脱速率控制在15mL/h,洗脱率可以达到95%以上。由于原水中的杂质较多,在经过阴离子交换树脂前,先用Al2O3柱处理水样,结果表明处理后的水样吸附和洗脱效果均较好。因此该方法能够适用于引黄水库的大部分水体中硝酸盐氮的富集。实验结果表明凯氏蒸馏法的最佳实验条件是:最佳定氮合金量为0.7g,最佳蒸馏时间为50min,最佳沸石量为75mg,吸附的最佳环境是15mL0.003mol/L的HCl。实验还研究了3A型沸石分子筛和改性沸石对氨氮的吸附能力和最佳吸附条件,实验结果表明75mg改性沸石的吸附率能够达到95%以上,不会产生同位素分馏。文中结合鹊山水库附近的实地情况,研究了鹊山水库库区硝酸盐氮的来源和迁移规律。水体中硝酸盐氮经条渠沉砂,水库的沉淀等过程,硝酸盐氮的含量逐渐降低,经过水厂的过滤消毒等工艺后,能够达到合格饮用水标准;同时分析研究了鹊山水库水中硝酸盐氮的主要来源,实验结果表明水库水中硝酸盐氮主要来源于生活污水和化肥源,可能也存在土壤矿化有机氮的作用,该问题有待进一步研究。本文对控制鹊山水库水中硝酸盐氮的来源提出了控制措施,对研究中存在的不足和发展方向做了总结。
【Abstract】 The pretreatment method which was adapted the stable isotope of nitrate nitrogen in the reservoir of Queshan was studied in this paper. The method was that the nitrate was enriched with anion exchange method, Kjeldahl distillation method was used to the nitrate reduction to ammonia,the best experimental conditions was deterimined in the study and combined with the actual situation in the reservoir of Queshan, the abundance values of nitrate nitrogen isotope in the canal of Yellow River and the reservoir of Queshan was monitored, the source of nitrate nitrogen in the area was judged according to the abundance value.The results showed that the best experimental conditions of anion exchange method:OH anion exchange resin (anion exchanger (Ion exchanger III, Merck)) was selected,the resin which was very stable in the effect of adsorption and elution,and no isotopic fractionation, so it was used to concentrate the carrier of nitrate nitrogen. For the reservoir water, the exchange column packing of the resin height was3cm; the flow rate through column was controlled in800-900mL/min in the adsorption process,2mol/L40mL of KCl solution was used as the eluent, the elution rate was controlled in15mL/h, elution rate could be reached more than95%.Because of more impurities in raw water, before the anion exchange resin, the water samples were treated with the Al2O3columns, the results indicated that the adsorption and elution of the treated water samples were both better. Therefore, this method could be applied to nitrate nitrogen enrichment in most of the Yellow River Reservoir.The results showed that the optimum experimental conditions of the Kjeldahl distillation method:the optimum amount of alloy’s was0.7g, distilled time was50min, the amount of zeolite was75mg, and the best environment of the adsorption was15mL0.003mol/L of HCl. 3A zeolite and modified zeolite for the adsorption capacity of ammonia and the best adsorption conditions was also studied in the experiments, the experiment result showed that the adsorption rate of75mg modified zeolite can be reached more than95%, and no isotope fractionation.Combining with the actual situation near the reservoir of Queshan, the sources of nitrate nitrogen and migration regularity in the reservoir of Queshan were studied. The nitrate nitrogen of the water through by desilting in the Article Drainage, and the sedimentation in the reservoir, the content of nitrate nitrogen decreased, after filtration and disinfection process of the water treatment plant, it can be reached the required standards for drinking water; and analysed that the source of nitrate nitrogen in Queshan reservoir water, the result of the experiment showed that the nitrate nitrogen of the reservoir water came mainly from sewage and fertilizer source. There also may be the role of organic nitrogen in soil mineralization, the problem needed further study. The paper was proposed the control measures for controlling the source of nitrate nitrogen in the reservoir of Queshan, and summarized the shortcomings in the research and development direction.
【Key words】 nitrogen isotope; preparation method; the reservoir of Yellow River; the regular of migrate;