硼泥、银杏中硼的形态分析法研究

【作者】 顾佳丽；

【导师】 邓桂春；

【作者基本信息】 辽宁大学 ， 分析化学， 2006， 硕士

【摘要】 硼泥是加工硼镁矿制取硼砂或硼酸时排出的工业废渣，它的水浸液呈碱性，堆积占地面积大，所堆积的地方寸草不生，附近农田也因水淋溶使水溶性的硼碱浸入土壤而危害农作物生长。同时，由于长期渗透也会污染地下水。此外，硼泥颗粒小，经自然干燥后，在散落和堆积的地方被风刮起，致使周围环境粉尘飞扬，污染空气。总之硼泥的增多既浪费资源，又占地污染环境。本文简单地分析研究了硼泥中硼的各种存在形态，希望对硼泥的综合治理以及提高经济效益、技术效益，减少环境污染，促进二次资源再生作出贡献。 银杏（Ginkgo bilola L．）系侏罗纪时期植物，是冰川时期存活在地球上的孑遗植物，素有“活化石”之称。因该植物在治疗心脑血管疾病及老年痴呆症等方面的独特疗效，进入八十年代以来，银杏的开发研究热潮风靡全球，国内外对银杏的化学成分、药理作用及其应用等分别进行了大量的研究工作，其提取物和制剂已由单一药用向生物制药、食品、药品、保健品和化妆品等综合应用方向转移。本文鉴于银杏的广泛应用及功能，简单地分析研究了银杏中硼的各种存在形态，希望对提高银杏叶中有效成分的纯度，提高银杏叶综合利用率做出贡献。 本文首先优化了分子荧光法测定硼泥和银杏中硼含量的实验条件，分别就缓冲体系、pH值、变色酸浓度和用量、反应温度、反应时间等对荧光强度的影响进行了条件实验。研究认为以EDTA-NaOH为缓冲体系，酸度在pH6.0～6.5，变色酸浓度为6×10^-4mol／L，用量为0.2mL，室温下反应15min，在λ_ex\λ_em=313nm\380nm处测得硼的荧光强度最大且稳定。实验结果表明：硼的浓度在10～250ng/25mL范围内与荧光强度呈线性相关，回归方程为F=1.0084C_ng/25mL+13.242，相关系数R²=0.9985。加标回收率在90％～108％之间，相对标准偏差≤5％，检出限3.28μg/L。本文还选择用聚四氟乙烯高压密闭消解法和硼酸甲酯蒸馏分离法测定样品中总硼含量，所得结果为：硼泥和银杏中总硼含量分别为4.01g/kg和103.74mg/kg。实验结果与姜黄素光度法测定结果进行比较，结果基本一致。 本实验采用了一种新的形态分析方法—连续浸提法，研究了硼泥和银杏中硼的存在形态，得出结论认为硼泥中各形态的硼量依次为：水溶态＞醋酸溶解态＞螯合态＞盐溶态＞盐酸羟胺溶解态＞残渣态。其中水溶态硼的比例最高，即可作为再生更多还原

【Abstract】 Boron sludge is industry waste residue produced by processing mine of boron-magnesium for making borax and boric acid, its water solution is alkalescence, and occupied a large number of earth, which will not be growed again, and farmland around will also be destroied by water solution boron produced by rain. And at the same time, it pollutes groundwater because of filtering a long time. Besides, after nature drying, the grain of boron sludge which sweeped by wind causes air pollution. In a word, boron sludge not only wastering but also polluting environment. So we ananlysis the boron speciation in boron sludge simply, and hope that this experiment can help fathering boron sludge and improving economy benefit, technic benefit, and decreasing circumstance pullution.Ginkgo bilola L. is the plant of Jurassic, so it aways called "living fossil". Because the specific curative effect in curing disease of heart blood vessel and agedness dementia, its exploiture and investigation is fashionable around the word. Many scholars inside and outside word investigat chemistry element, medicine function and application of the gingkgo, its distillation and preparation is used for producing bioligy preticide, food, medicine, health protection and cosmetic and so on. Because of its abroad application, the speciation of boron in gingkgo is analysed simply, and hope that this experiment can help improving the degree of availability componential and the ratio of utilize of gingkgo.Based on the research of the experiments, a fluorescence spectrophotometric method is used for the determination of boron , experiment conditions are optimized in this paper, and investigated the effect of buffer solution, pH, the concentration and dosage of chromotropic acid, reaction temperature and reaction time on the fluorescence intensity, finally concluded that: under the condition of EDTA-NaOH buffer solution, pH6.0-6.5, dosage of 6×10^-4 mol/L chromotropic acid 0.2 mL, under room temperature, reaction time 15min, and at λ_ex \ λ_em=313 nm \ 380 run, the fluorescence intensity is the most strong and stability. The standard curve indicates that the concentration of boron presents a linear relation with fluorescence intensity between 10-250ng/25mL, the regression equation is F=1.0084C_ng/25ml +13.24, related coefficient（R²） is 0.9985, the recovery is更多还原