大气及污染源排放气体中苯系物气相色谱测定

建立了气体样品中不同浓度的苯系物的分析方法,优化了测定的操作条件,提出了保证测定质量的技术关键。方法已用于污染源及环境空气中苯系物的气相色谱测定。     

毛细管气相色谱法测定12种农药的有效成分

 建立了毛细管气相色谱法测定速克灵、戊唑醇等 12种农药中有效成分的方法。采用SE 3 0大口径毛细管柱和火焰离子化检测器 (FID) ,内标法定量 ,气相色谱 /质谱法定性确证 ,样品加标的平均回收率为 99 2 0 %～10 2 4 4 % ,相对标准偏差为 0 0 7%～ 5 4 9%。该方法简单快速 ,结果准确 ,可作为测定单样、复配样农药或同时测定多种农药有效成分的通用方法     

溴酸钾滴定法测定铜冶炼烟尘中的砷含量

研究了测定铜冶炼烟尘中砷含量的溴酸钾滴定方法。对测定体系中的各共存元素进行研究,探讨了测定方法的各项测定条件,方法的相对标准偏差RSD为0.13%～0.61%,样品加标回收率在99.5%～100%,方法精密度高,准确度好,适用于铜冶炼烟尘中砷含量为1.00%～50.00%的测定。     

Determination of Iridoids in Gentiana rigescens by Infrared Spectroscopy and Multivariate Analysis

Gentiana rigescens is a famous herbal medicine in China for treatment of convulsion, rheumatism, and jaundice. Here, the infrared determination of gentiopicroside, swertiamarin, sweroside, and loganic acid in G. rigescens from different areas and varieties was presented for the first time. Reference information for the iridoids were obtained by high-performance liquid chromatography. Partial least squares was used to characterize the relationship between spectra matrix and concentration vector for the determination of the analytes. For determination of gentiopicroside, the appropriate performance of partial least squares model was acquired with coefficient of determination of calibration and coefficient of determination of prediction values of 0.965 and 0.868. The root mean square error of estimation (RMSEE), root mean square error of cross validation (RMSECV), root mean square error of prediction (RMSEP), and residual predictive deviation (RPD) values were 2.612, 5.292, 5.239?mg g^?1, and 2.701, respectively, based on the first derivative and multiplicative scatter correction. For determination of the total iridoids, the best results were obtained using the coefficient of determination of calibration and coefficient of determination of prediction of 0.943 and 0.834, RMSEE, RMSECV, RMSEP and RPD of 3.896, 7.536, 6.543?mg g^?1 and 2.438, respectively, based on the first derivative. Both models were reliable and robust. The results demonstrated that infrared spectroscopy provided a rapid, low-cost tool to monitor the quality of G. rigescens by the determination of the iridoids.     

ICP-MS测定高纯氧化铒中稀土杂质的研究

从同位素的选择、基体效应,内标元素的选择及仪器工作等方面对实验参数进行了优化,重点研究了等离子体功率及仪器分辩率的改变对铒基体所形成的氢化物多原子离子干扰的影响。通过提高等离子体功率、改变仪器分辨率及数学方程校正等方法,减小和剔除了ErH对Ho和Tm测定的干扰。实验中选取Cs为内标元素,测定了不同含量的高纯氧化铒样品。分析结果与标准加入法结果进行了比较,之间无显著性差异。     

Kinetic spectrophotometric determination of sulfide, using in-cuvette mixing and titration techniques with computerized data acquisition

In-cuvette mixing and titration techniques have been used for the kinetic determination of sulfide based on its inhibition effect on the oxidation of indigo carmine with hexacyanoferrate(III) in the presence of silver. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of indigo carmine at 612 nm. Both initial rate and fixed-time methods were applied to the in-cuvette technique. Using in-cuvette mixing, sulfide up to 1800 ng was determined and detection limit and relative standard deviation for the determination of 120 ng of sulfide were calculated as 23.0 ng and 1.59%, respectively. On the basis of the titration technique, the upper limit of determination was 25 μg of sulfide and detection limit and average relative standard deviation for the determination of 1 μg of sulfide were 0.025 μg and 4.95%, respectively. The effect of foreign ions on the sulfide determination was studied. The proposed methods were applied to the determination of sulfide in water.     

Determination of chromium by on-line preconcentration on a poly (hydroxamic acid) resin in flow-injection atomic absorption spectrometry

A series of poly(hydroxamic acid) resins were used for the preconcentration and determination of chromium(III). Conditions were optimized for the determination of chromium(III) and its separation from multi-component mixtures. A flow manifold was developed for the on-line preconcentration and determination of chromium(III) by atomic absorption spectrometry.     

电感耦合等离子体质谱法测定地质样品中银研究进展

应用电感耦合等离子体质谱（ICP-MS）测定地质样品中银时,锆、铌等元素干扰银的测定,造成准确度低、测定偏差大。采用银的富集、王水偏提取和化学分离法等方法可对干扰元素预分离,从而准确测定样品中银;而应用干扰校正方程及碰撞/反应池（CRC-ICP-MS）、膜去溶（DSN-ICP-MS）、激光剥蚀（LA-ICP-MS）和高分辨质谱（HR-ICP-MS）等新技术,能够更加方便、准确测定地质样品中银。     

Na2EDTA滴定法测定铜冶炼烟尘中铋含量

研究了测定铜冶炼烟尘中铋含量的Na_2EDTA络合滴定方法。对测定体系中的各干扰元素进行了研究,探讨了测定方法的各项测定条件。方法的相对标准偏差为0.40%～0.67%,样品加标回收率在99.9%～100%,方法精密度高,准确度好。适用于铜冶炼烟尘中铋含量为5.00%～16.00%的测定。     

微波消解原子发射光谱法测定鲍鱼中微量元素的含量

用硝酸-过氧化氢作消解液,用微波消解法处理样品,采用电感耦合等离子体原子发射光谱法测定了鲍鱼中锌、铁、锰和铜的含量。测定结果的相对标准偏差RSD<4%,加标回收率在97.4%~105.0%之间,检出限在0.764~1.539μg/L之间。该法快速、稳定、准确,结果令人满意。