环境中痕量铜、钴、镍的检测新方法研究
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摘要
1.在0.18mol/L硫酸介质中,通过高压汞灯照射,铜能强烈催化异丙醇还原钼酸铵生成同钼多蓝的反应,据此建立了光化学催化动力学显色法测定痕量铜的新方法。铜离子浓度(Cu~(2+))在0.01~0.50μg /mL范围内,体系吸光度变化(ΔA)与其呈现良好的线性关系,线性回归方程为:△A=1.1053ρ(μg/mL)+0.133 (r=0.9993);检出限为6.43ng/mL;相对标准偏差为1.1~3.2%。用于水样中痕量铜的测定,样品加标回收率98.3~102.0%。
2.研究了Co~(2+)与1-(2-噻唑偶氮)-2-萘酚(TAN)、十二烷基苯磺酸钠(SDBS)作用的共振光散射光谱。在pH8.0的BR缓冲溶液中,Co~(2+)的加入导致体系共振光散射的增强,在342nm处存在一最大散射增强峰,其增强强度与Co~(2+)的浓度呈线性关系,据此建立了一种测定Co~(2+)的共振光散射法。该法的线性范围为7.5~600ng/mL,相关系数为γ=0.9990,检出限为2.25ng/mL,将该法用于人发、茶叶、维生素B12中钴的测定,加标回收率为97.8~105.4%。
3.在碱性条件下,Ni(II)和1-(2-吡啶偶氮)-2-萘酚(PAN)形成聚合物,对PAN的共振光散射有增强作用,加入十二烷基苯磺酸钠(SDBS)进一步敏化该体系。共振光散射增强强度(ΔI)与Ni(II)浓度呈良好的线性关系,据此建立了测定Ni(II)的共振光散射分析方法。在优化的实验条件下,体系的最大散射波长位于545nm处,方法的线性回归方程为ΔI_(RLS)=4502.9ρ(μg/mL) + 271.82;线性范围为15.2~500ng/mL;相关系数γ=0.9975;检出限为4.57 ng/mL。对Ni(II)分别为50ng/mL、200ng/mL、400ng/mL低、中、高三个浓度进行11次平行测定,其相对标准偏差分别为:3.5%、3.0%和1.7%。
4.研究了多元线性回归法(MLR)、K-矩阵法和主成分回归法在浊点萃取分光光度法同时测定钴和镍的应用。该法基于非离子表面活性剂TritonX-100的浊点现象,当体系加热至浊点时,溶液分为两相——富胶束相和水相,Co和Ni与PAN形成的疏水性螯合物进入富胶束相,从而达到预富集的目的。对影响浊点萃取的主要因素进行了详细的研究。借助于多元线性法、K-矩阵法和主成分回归法三种多元校正法解析了两种物质光谱的重叠问题,用Matlab7.0软件自编程序处理数据,从而建立了同时测定钴和镍的新方法——浊点萃取多元校正分光光度法。校正集对检验集的预测结果:MLR法中Co和Ni平均回收率分别为99.6%和93.2%;K-矩阵法进行预测Co和Ni平均回收率分别为105.0%和95.5%;主成分回归法中Co和Ni平均回收率分别为100.5%和97.8%。MLR法、K-矩阵法、PCR法预测Co和Ni回收率的相对标准偏差依次为:12.2%和4.0%,2.6%和3.7%,1.2%和2.1%。
1. In 0.18 mol/ L H2SO4 medium, trace copper can significantly catalyze the reaction of ammonium molybdate with iso-propyl alcohol to produce molybdenum blue by the irradiation of high-press mercury lamp. Based on this, a novel method for the determination of trace copper with photochemical catalytic spectrophotometry has been developed. In this method, ?A is linear to the concentration of Cu~(2+) in the range of 0.01~0.50μg/mL with the correlation coefficient of 0.9993, the linear equation is△A=1.1053ρ(μg/mL) +0.133 and the detection limit is 6.43 ng/mL. The method has been used to determine trace copper in river water with the recovery of 98.3~102.0% and the relative standard deviation of 1.1~3.2%.
2. The resonance scattering spectra of Cobalt with 1-(2-thiazolylazo) -2-naphathol (TAN) and sodium dodecyl benzene sulfonate (SDBS) have been studied. The RRS of the system is greatly enhanced with the increasing of Cobalt in pH 8.0 BR buffer solution, the maxmium scattering wavelength is located at 342nm, the enhanced intensity of RRS is proportional to the concentration of Cobalt. Thus, a method of RRS for the determination of Cobalt is established. The linear range is 7.5~600ng/mL with a correlation coefficient of 0.9990. The detection limit is 2.25ng/mL. This method has been applied to the determination of Cobalt in human hair, teas and vitamin 12 with the recovery of 97.8~105.4%.
3. A resonance light scattering (RLS) enhancement method is developed for the determination of nickel. The proposed method is based on the enhanced effect on the resonance light scattering of PAN after the formation of Ni-PAN complex in the presence of SDBS which acted as sensitizer in the alkaline medium. The maximum RLS wavelength is located at 545nm. Under optimal conditions,ΔI is proportional to the concentration of Ni~(2+) in the range of 15.2~500ng/mL, the linear regress equation isΔI_(RLS)= 4502.9ρ(μg/mL) + 271.82(γ=0.9975), the detection limit is 4.57ng/mL, the relative standard deviation is 3.5%, 3.0% and 1.7% for the Ni~(2+)concentration of 50ng/mL, 200ng/mL and 400ng/mL, respectively.
4. The application of multivariate linearity regress (MLR), K-matrix method and principal component regression method(PCR) for the simultaneous determination of cobalt and nickel in mixture system by spectrophotometry coupled with cloud point extraction(CPE) has been studied. The method is based on cloud point phenomenon of nonionic surfactant TritonX-100. The formation of two distinct phases——a surfactant-rich phase and an aqueous phase occurs, when the temperature of the system reachs the cloud point of TritonX-100. The ion-associated complex of Co-PAN and Ni-PAN are extracted into the surfactant-rich phase. The main effects of influencing on CPE are studied detailedly. The overlapped spectra are resolved by multivariate calibration such as MLR, K-matrix and PCR. The data are dealt with Matlab 7.0 program written by ourselves. Thus, a new method for the simultaneous determination of cobalt and nickel——multivariate calibration spectrophotometry coupled with cloud point extraction is developed. The recoveries and the relative standard deviations are 99.6% and 93.2%, 12.2% and 4.0% for cobalt and nickel in the MLR method, 105.0% and 95.5%, 2.6% and 3.7% in the K-matrix method, 100.5% and 97.8%, 1.2% and 2.1% in the principal component regression method.
2.研究了Co~(2+)与1-(2-噻唑偶氮)-2-萘酚(TAN)、十二烷基苯磺酸钠(SDBS)作用的共振光散射光谱。在pH8.0的BR缓冲溶液中,Co~(2+)的加入导致体系共振光散射的增强,在342nm处存在一最大散射增强峰,其增强强度与Co~(2+)的浓度呈线性关系,据此建立了一种测定Co~(2+)的共振光散射法。该法的线性范围为7.5~600ng/mL,相关系数为γ=0.9990,检出限为2.25ng/mL,将该法用于人发、茶叶、维生素B12中钴的测定,加标回收率为97.8~105.4%。
3.在碱性条件下,Ni(II)和1-(2-吡啶偶氮)-2-萘酚(PAN)形成聚合物,对PAN的共振光散射有增强作用,加入十二烷基苯磺酸钠(SDBS)进一步敏化该体系。共振光散射增强强度(ΔI)与Ni(II)浓度呈良好的线性关系,据此建立了测定Ni(II)的共振光散射分析方法。在优化的实验条件下,体系的最大散射波长位于545nm处,方法的线性回归方程为ΔI_(RLS)=4502.9ρ(μg/mL) + 271.82;线性范围为15.2~500ng/mL;相关系数γ=0.9975;检出限为4.57 ng/mL。对Ni(II)分别为50ng/mL、200ng/mL、400ng/mL低、中、高三个浓度进行11次平行测定,其相对标准偏差分别为:3.5%、3.0%和1.7%。
4.研究了多元线性回归法(MLR)、K-矩阵法和主成分回归法在浊点萃取分光光度法同时测定钴和镍的应用。该法基于非离子表面活性剂TritonX-100的浊点现象,当体系加热至浊点时,溶液分为两相——富胶束相和水相,Co和Ni与PAN形成的疏水性螯合物进入富胶束相,从而达到预富集的目的。对影响浊点萃取的主要因素进行了详细的研究。借助于多元线性法、K-矩阵法和主成分回归法三种多元校正法解析了两种物质光谱的重叠问题,用Matlab7.0软件自编程序处理数据,从而建立了同时测定钴和镍的新方法——浊点萃取多元校正分光光度法。校正集对检验集的预测结果:MLR法中Co和Ni平均回收率分别为99.6%和93.2%;K-矩阵法进行预测Co和Ni平均回收率分别为105.0%和95.5%;主成分回归法中Co和Ni平均回收率分别为100.5%和97.8%。MLR法、K-矩阵法、PCR法预测Co和Ni回收率的相对标准偏差依次为:12.2%和4.0%,2.6%和3.7%,1.2%和2.1%。
1. In 0.18 mol/ L H2SO4 medium, trace copper can significantly catalyze the reaction of ammonium molybdate with iso-propyl alcohol to produce molybdenum blue by the irradiation of high-press mercury lamp. Based on this, a novel method for the determination of trace copper with photochemical catalytic spectrophotometry has been developed. In this method, ?A is linear to the concentration of Cu~(2+) in the range of 0.01~0.50μg/mL with the correlation coefficient of 0.9993, the linear equation is△A=1.1053ρ(μg/mL) +0.133 and the detection limit is 6.43 ng/mL. The method has been used to determine trace copper in river water with the recovery of 98.3~102.0% and the relative standard deviation of 1.1~3.2%.
2. The resonance scattering spectra of Cobalt with 1-(2-thiazolylazo) -2-naphathol (TAN) and sodium dodecyl benzene sulfonate (SDBS) have been studied. The RRS of the system is greatly enhanced with the increasing of Cobalt in pH 8.0 BR buffer solution, the maxmium scattering wavelength is located at 342nm, the enhanced intensity of RRS is proportional to the concentration of Cobalt. Thus, a method of RRS for the determination of Cobalt is established. The linear range is 7.5~600ng/mL with a correlation coefficient of 0.9990. The detection limit is 2.25ng/mL. This method has been applied to the determination of Cobalt in human hair, teas and vitamin 12 with the recovery of 97.8~105.4%.
3. A resonance light scattering (RLS) enhancement method is developed for the determination of nickel. The proposed method is based on the enhanced effect on the resonance light scattering of PAN after the formation of Ni-PAN complex in the presence of SDBS which acted as sensitizer in the alkaline medium. The maximum RLS wavelength is located at 545nm. Under optimal conditions,ΔI is proportional to the concentration of Ni~(2+) in the range of 15.2~500ng/mL, the linear regress equation isΔI_(RLS)= 4502.9ρ(μg/mL) + 271.82(γ=0.9975), the detection limit is 4.57ng/mL, the relative standard deviation is 3.5%, 3.0% and 1.7% for the Ni~(2+)concentration of 50ng/mL, 200ng/mL and 400ng/mL, respectively.
4. The application of multivariate linearity regress (MLR), K-matrix method and principal component regression method(PCR) for the simultaneous determination of cobalt and nickel in mixture system by spectrophotometry coupled with cloud point extraction(CPE) has been studied. The method is based on cloud point phenomenon of nonionic surfactant TritonX-100. The formation of two distinct phases——a surfactant-rich phase and an aqueous phase occurs, when the temperature of the system reachs the cloud point of TritonX-100. The ion-associated complex of Co-PAN and Ni-PAN are extracted into the surfactant-rich phase. The main effects of influencing on CPE are studied detailedly. The overlapped spectra are resolved by multivariate calibration such as MLR, K-matrix and PCR. The data are dealt with Matlab 7.0 program written by ourselves. Thus, a new method for the simultaneous determination of cobalt and nickel——multivariate calibration spectrophotometry coupled with cloud point extraction is developed. The recoveries and the relative standard deviations are 99.6% and 93.2%, 12.2% and 4.0% for cobalt and nickel in the MLR method, 105.0% and 95.5%, 2.6% and 3.7% in the K-matrix method, 100.5% and 97.8%, 1.2% and 2.1% in the principal component regression method.
引文
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