催化光度法测定城市污泥中的痕量镍

利用Ni2 对还原型罗丹明B(RRhB)与KClO3显色反应的催化作用,对城市污泥中痕量Ni2 进行测定。结果表明,在pH 5.3的HAc-NaAc缓冲溶液中具有高灵敏的显色反应,其催化程度与Ni2 含量在0~0.07 mg/L范围内符合比耳定律。方法的检出限为4.3×10-8g/L,加标回收率为98.5%~104.6%(n=6)。本法结合萃取分离,用于测定城市污泥中的痕量镍,结果满意。     

痕量汞的气热提取应用于现场快速分析污水

为测定污水中汞含量,取约25mL水样,加入硫酸亚锡和氨基磺酸的混合物(质量比3∶1)0.40g,反应15min,使汞(Ⅱ)还原为气态单质汞,以0.3L·min~(-1)流量将汞蒸气引入由碘酸钾和硫酸氢铵的混合物(质量比1∶4)0.20g,约5 mL去离子水和1 mol·L~(-1)硫酸溶液0.100mL组成的吸收液中,使单质汞氧化成汞(Ⅱ),随即向此溶液中加入含有镉试剂的汞检测剂0.10g,使汞(Ⅱ)反应显色,2min后进行测定。显色反应时,所加入的汞检测剂中含有氢氧化钠和四硼酸钠组成的缓冲剂(相当于2mol·L~(-1)氢氧化钠溶液0.1mL和四硼酸钠0.04g),曲拉通X~(-1)00(相当于体积分数为10%的曲拉通X~(-1)00溶液30μL)和镉试剂(相当于1g·L~(-1)镉试剂乙醇溶液60μL)。按上述操作流程结合使用便携式专用仪器可在20min内完成一次测定,方法的检出限(3s/k)为2μg·L~(-1)。分别对0.050,0.500mg·L~(-1)汞标准溶液进行精密度试验,测定值的相对标准偏差(n=6)分别为3.6%,5.1%。方法用于废水样品的分析,并进行加标回收试验,测得回收率为92.0%～103%。     

紫外脉冲荧光法测定微量铀的研究

紫外脉冲荧光法是一种通过液体激光来直接测定微量铀的方法。在采用紫外脉冲荧光法分析面包酵母吸附放射性核素铀后溶液剩余铀浓度之前,研究了荧光增强剂、pH 值、以及温度对微量铀浓度工作曲线的影响。结果表明:当pH > 3时,400 μL 荧光增强剂可以充分缓冲溶液,不同pH 值下测得的荧光计数基本保持恒定,即待测溶液pH值不会影响铀浓度的测量;随着温度的升高,荧光计数近似线性下降,并在室温23.6℃时得到了铀质量浓度范围为0:120 μg/L 的工作曲线。在此基础上研究了酵母菌对放射性核素铀的吸附作用,为使吸附剂达到最高效利用,对溶液pH 值、吸附速率进行了批次实验,并通过紫外脉冲荧光分析法进行测量, 发现达到吸附平衡所需的最短时间为180 min,吸附的最佳溶液pH 值为5.8 左右。The method of pulse ultraviolet fluorescence was employed to analyze the concentration of radioactive nuclide uranium after adsorbed by baker’s yeast. Influences of fluorescent enhance reagent, pH value, and temperature on measurement of the concentration of trace uranium were investigated. The results showed that 400 μL fluorescent enhance reagent was greatly enough to buffer the solution when pH > 3 and the counts of fluorescence kept constant with the variation of pH, which indicates that the pH of solutions doesn’t affect the determination of uranium concentration, moreover, the counts of fluorescence declined linearly as the increase of the temperature. In addition, the working curve of the determination of uranium concentration within 0.1 20 μg/L was obtained when the temperature was 23.6 ℃. On this basis, the adsorption of uranium by baker’s yeast was studied. For the adsorption of radioactive nuclides of uranium by baker’s yeast to achieve the best use, the batch experiments were carried out on the rate of adsorption and pH of solutions. The method of pulse ultraviolet fluorescence was used to measure and found that the minimum time required to reach adsorption equilibrium was 180 min and the optimum pH value of solutions was about 5.8.     

超声萃取-免疫亲和柱净化-柱后光化学衍生高效液相色谱法同时测定蜂房药材中4种黄曲霉毒素

建立超声萃取-免疫亲和柱净化-柱后光化学衍生高效液相色谱同时测定蜂房药材中黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2含量的分析方法。样品经粉碎，过孔径为120μm筛后，采用70%甲醇溶液超声处理30 min，经免疫亲和柱净化、高效液相色谱分离、光化学柱后衍生，通过荧光检测器测定4种黄曲霉毒素的含量。黄曲霉毒素B1的线性范围为0.010 4～0.052 0 ng，相关系数为0.999 9；黄曲霉毒素B2的线性范围为0.003 8～0.019 0 ng，相关系数为0.999 8；黄曲霉毒素G1的线性范围为0.010 8～0.054 0 ng，相关系数为0.999 8；黄曲霉毒素G2的线性范围为0.003 8～0.019 0 ng，相关系数为0.999 8。4种黄曲霉毒素检出限分别为0.42、0.15、0.43、0.15μg/kg，测定结果的相对标准偏差不大于2.5%(n=6)，样品加标回收率为92.9%～96.9%。该方法操作简便，灵敏度高，可用于蜂房中黄曲霉毒素含量的测定。