流动注射催化光度法测定微量钒

采用流动注射与催化动力学光度法相结合,研究了在H3PO4介质中微量钒(Ⅴ)催化溴酸钾氧化吡啶偶氮变色酸试剂-2-(5-硝基-2-吡啶偶氮)-1,8-二羟基萘-3,6二磺酸(简称5-NO2-PACA)褪色反应,建立了测定微量钒的新方法。该方法线性范围为0.02~0.20μg/mL,线性回归方程为:ΔA=-0.004 2.63ρ(μg/mL),相关系数r=0.9988,检出限为:4.1×10-6g/L。方法已用于水样中微量钒的测定。     

催化动力学光度法测定青霉素G及其机理研究

研究了在青霉素G存在下双氧水氧化苋菜红的褪色反应,建立了催化动力学光度法测定微量青霉素G的方法.方法线性范围为0.20～4.00μg/mL,回归方程y=-0.015p(μg/mL)+0.311,r=0.9998;方法线性范围为4.00～50.0μg/mL,回归方程y=0.001p(μg/mL)+0.280,r=0.99...     

流动注射催化光度法测定微量Sb(Ⅲ)

基于在B-R缓冲溶液介质中,Sb(Ⅲ)对H2O2氧化孔雀石绿褪色反应具有催化作用,建立了流动注射催化动力学光度法测定微量元素Sb(Ⅲ)的新分析方法,该方法的线性范围为0.010～2.0μg/mL,检出限为7.8×10-3μg/mL,r=0.9996。对0.1μg/mL Sb(Ⅲ)测定的RSD=0.97%n=11,进样频率为22.8次/h。用于环境水样中微量Sb(Ⅲ)的测定,回收率为97.3%～97.7%。     

酸性铬兰K催化光度法测定水中的氟含量

研究了稀硫酸介质中,游离的F-对溴酸钾氧化酸性铬兰K褪色反应具有催化作用,基于此建立了测定微量F-的催化光度分析的方法。结果表明,有色溶液的最大吸收波长为523 nm,测定的线性范围为0.2～6.0μg/mL,检出限为0.1031μg/mL。方法用于水中微量F-的测定,相对标准偏差为0.65%～0.76%,回收率99.5%～105%。     

双波长双指示剂催化动力学光度法测定微量铬(Ⅵ)

基于在pH=4.5的HAc-NaAc缓冲介质中,微量铬(Ⅵ)催化过氧化氢氧化混合指示剂(中性红和亚甲基蓝)褪色的指示反应,建立了双波长双指示剂催化动力学光度法测定微量铬(Ⅵ)的新方法。方法的线性范围为0.005～0.3μg/mL,检出限为8.7×10-4μg/mL。该方法操作简单,灵敏度高,选择性好,用于环境水样中微量铬(Ⅵ)的测定,回收率在98.5%～102.5%之间,结果满意。     

丽春红2R-高碘酸钾催化动力学体系光度法测定痕量铁

在硫酸介质中,微量铁(Ⅲ)能显著催化高碘酸钾氧化丽春红2R(PR)的褪色反应。研究了该指示反应的最佳反应条件和动力学参数,建立了一个测定痕量铁的新的催化动力学分析方法。方法的线性范围为0.010～1.0μg/25mL,检出限为1.18×10-9g/mL。用本法测定了中草药及食品中铁的含量,结果满意。     

流动注射催化动力学光度法测定碘的研究

本文采用流动注射技术,利用微量碘离子催化铁的硫氰酸配合物与亚硝酸钠的褪色反应,实现水中微量碘离子的催化动力学光度测定。该法测定碘离子的线性范围是1．0～7．0μg／mL,检出限为0．5μg／mL,相对标准偏差为5．0％。方法用于实际水样中微量碘离子的测定,结果令人满意。     

孔雀石绿-H_2O_2体系动力学光度法测定微量溴化物

基于在NH3-NH4Cl介质中, Br-对H2O2氧化孔雀石绿的褪色反应有催化作用的特性, 建立了高灵敏度测定痕量溴化物的催化动力学光度分析法新体系. 讨论了酸度、试剂用量、温度、干扰离子等因素的影响. 研究了反应的最佳条件, 测定了一些动力学参数, 非催化反应和催化反应的的表观活化能分别为为52.85和19.53 kJ/mol. 方法的线性范围为0.10～1.2 μg/mL Br-, 检出限为 0.081 μg/mL. 方法用于水样中溴化物的测定, 结果与国标分析法所得结果相吻合.     

丁基罗丹明B-溴酸钾催化动力学体系光度法测定痕量铬

在硫酸介质中,微量铬(Ⅵ)能显著催化溴酸钾氧化丁基罗丹明B褪色.研究了该指示反应的动力学行为,建立了测定痕量铬的新的催化动力学分析方法.方法的线,性测定范围为0.04～2.0μg/25 mL,检出限为9.68×10-10g/mL.本法用于电镀废水中Cr(Ⅵ)的测定,结果满意.     

阻抑动力学分光光度法测定痕量碘

研究了在稀H3PO4介质中,痕量碘离子对NO-2催化溴酸钾氧化吖啶橙的阻抑作用,建立了测定痕量碘离子的阻抑动力学光度分析的新方法。测定碘离子的线性范围为0～0.40μg/mL,检出限为7.3×10-9g/mL。已用于食品中的微量碘的测定。     

溴值法测定加氢石油树脂不饱和度局限性分析

探讨了国内现行行业标准《HG2231-91石油树脂(PR)溴值试验方法》在测定深度加氢石油树脂不饱和度时存在的局限性. 实验结果表明, 在测定不饱和度较低的加氢石油树脂的溴值时, 应采用浓度为0.1 mol/L的Br标准滴定溶液, 加入量为6～7 mL;碘化钾的加入量应为假设溴值为零时的理论用量, 这样在测定不饱和度较低的石油树脂的溴值时, 才能保证碘化钾过量, 得到可靠的溴值.     

Preconcentration and determination of 2‐mercaptobenzimidazole by dispersive liquid–liquid microextraction and experimental design

A method was developed to determine 2‐mercaptobenzimidazole in water and urine samples using dispersive liquid–liquid microextraction technique coupled with ultraviolet–visible spectrophotometry. It was essential to peruse the effect of all parameters that can likely influence the performance of extraction. The influence of parameters, such as dispersive and extraction solvent volume and sample volume, on dispersive liquid–liquid microextraction was studied. The optimization was carried out by the central composite design method. The central composite design optimization method resulted in 1.10 mL dispersive solvent, 138.46 μL extraction solvent, and 4.46 mL sample volume. Under the optimal terms, the calibration curve was linear over the range of 0.003–0.18 and 0.007–0.18 μg/mL in water and urine samples, respectively. The limit of detection and quantification of the proposed approach for 2‐mercaptobenzimidazole were 0.013 and 0.044 μg/mL in water samples and 0.016 and 0.052 μg/mL in urine samples, respectively. The method was successfully applied to determination of 2‐mercaptobenzimidazole in urine and water samples.     

火焰原子吸收分光光度法测定维血康颗粒中总铁

建立火焰原子吸收分光光度法测定维血康颗粒中总铁的含量,火焰类型选择空气–乙炔,测定波长为248.3 nm,测定时间为4.0 s,燃气流量为0.9 L/min,以氘灯作为背景校正。铁的质量浓度在2.4~28.8μg/mL范围内与吸光度呈良好的线性,线性相关系数r~2=0.999 8。6次测定结果的相对标准偏差小于1.0%,样品加样回收率为93.89%,方法检出限为0.011 3μg/mL。该方法具有准确度高,稳定性、重复性好等优点,可用于维血康颗粒中总铁含量的测定。     

火焰原子吸收光谱法测定红花中的Cu、Fe、Zn

采用火焰原子吸收光谱法和表面增敏的方法测定了红花中Cu、Fe、Zn的含量。实验表明,使用表面活性剂十二烷基硫酸钠(SDS),可使Zn的吸光度增感34.91%,使Cu增感37.39%,Fe增感232.10%。该法的检测限分别为Zn1.85×10-3μg/mL;Fe1.50×10-2μg/mL;Cu3.50×10-2μg/mL,加标回收率在99.37%~104.23%之间。该法灵敏度高,结果准确,可用于红花等中草药中Cu、Fe、Zn的同时测定。     

On-Line Flow-Injection Chemiluminescence Determination of Bovine Serum Albumin Using Surfactant-Enhanced Dichlorofluorescein-Hypochlorite System

A flow injection technique combined with a chemiluminescence method was established for the determination of bovine serum albumin (BSA). Strong chemiluminescence was observed when BSA-dichlorofluoresce (DCF) complex was oxidized by sodium hypochlorite (NaClO) in an alkaline medium and in the presence of cetyltrimethylammonium bromide (CTAB). The reaction conditions of the chemiluminescence were carefully optimized. Under the optimal conditions, the method had a linear range of 0.01–20.0 μg/mL, with a detection limit of 0.007 μg/mL for BSA (3σ). The relative standard deviation of 1.0 μg/mL BSA (n = 8) is 1.4%. The method was applied to determine BSA in milk samples and it worked well.     

Quantitation of native and forced degraded collagens by capillary zone electrophoresis: Method development and validation

A new capillary zone electrophoresis method for collagen quantitation was developed and validated according to the International Council for Harmonization guideline Q2 (R1). The Sircol collagen assay and ultraviolet spectrometry were employed as reference methods. Capillary zone electrophoresis enables specific, simple, and fast determination within 9 min. It is less user-dependent and more automated than the Sircol collagen assay. With a limit of detection of 18.0 μg/mL, the new method is less sensitive than the Sircol collagen assay, which has a limit of detection of 6.5 μg/mL. Nonetheless, capillary zone electrophoresis covers a wider linearity range (50-400 μg/mL) compared to the Sircol collagen assay (5-80 μg/mL), with similar precision. Additional advantages of capillary zone electrophoresis are the ability to gain information on collagen integrity and to simultaneously determine native and denatured collagens. This approach represents a modern and legitimate alternative to the Sircol collagen assay. The developed method has been successfully applied to the study of three collagen products and samples from forced degradation.     

STUDY ON THE DETERMINATION OF TRACE Fe(Ⅲ) BY THIN LAYER RESIN PHASE SPECTROPHOTOMETRY

A method to determine Fe(Ⅲ) by thin layer resin phase spectrophotometry has been developed in this paper. The colored complex formed by Fe(Ⅲ) and 1,2-benzendiol is concentrated on the 717# resin, then Fe(Ⅲ) can be determined directly by making thin layer. The method is sensitive with a apparent molar absorption of 4.8×104L/mol. cm, which is 16 times higher than that of liquid phase spectrophotometry, most coexisting ions do not influence the determination. The detection limit for Fe(Ⅲ) is 1.47μg/L with the precision of 3.3% [n=6, 7μg/50mL Fe(Ⅲ)]. The calibration curve is linear in the range of 0～25μg/50mL. The preposed method was applied to the determination of Fe(Ⅲ) in water sample with satisfactory results.     

Sensitive determination of phenothiazines in pharmaceutical preparation and biological fluid by flow injection chemiluminescence method using luminol-KMnO4 system

A flow injection chemiluminescence method was described for the determination of four phenothiazine drugs, namely, chlorpromazine hydrochloride, perphenazine hydrochloride, fluphenazine hydrochloride and thioridazine hydrochloride. Strong Chemiluminescence (CL) signal was produced when above-mentioned drug was injected into the mixed stream of luminol with KMnO₄. The linear ranges of the method were 0.0020-1.0 μg/mL chlorpromazine hydrochloride, 0.0040-3.0 μg/mL perphenazine hydrochloride, 0.0020-5.0 μg/mL fluphenazine hydrochloride and 0.0050-1.0 μg/mL thioridazine hydrochloride. The detection limits were 0.4 ng/mL chlorpromazine hydrochloride, 0.7 ng/mL perphenazine hydrochloride, 2 ng/mL fluphenazine hydrochloride and 0.7 ng/mL thioridazine hydrochloride. The proposed method was applied to the determination of chlorpromazine hydrochloride in injections and in mental patient's urine samples and the satisfactory results were achieved. The possible CL reaction mechanism was also discussed briefly.     

高效液相色谱法测定洗手液中水杨酸和对氯间二甲苯酚

建立高效液相色谱仪同时测定洗手液中水杨酸和对氯间二甲苯酚含量的方法。采用Shim-pack Scepter C18柱(250 mm×4.6 mm,5 μm),流动相为甲醇–0.1%磷酸水溶液(体积比为70∶30),流量为1.0 mL/min,柱温为室温,检测器为岛津SPD–M20A二极管阵列检测器,检测波长为280 nm。水杨酸和对氯间二甲苯酚与色谱峰面积呈良好的线性关系,线性范围分别为40~400 μg/mL,20~200 μg/mL,相关系数均为r^2=0.999 9。方法的检出限为0.1 μg/mL,水杨酸和对氯间二甲苯酚测定结果的相对标准偏差分别为0.79%,1.39%(n=5),加标回收率为96.9%~99.8%。该方法方法简便、快速、灵敏度高、重现性好,能同时准确检测洗手液中水杨酸和对氯间二甲苯酚的含量。     

极谱法和原子吸收光谱法快速分析矿石中的锑

建立了用极谱法和原子吸收光谱法测定矿石中含锑量为0.00X%~XX%的锑的快速分析方法,使锑在H2SO4(2%)-HCl(10%)体系中,既可以用极谱法测定,也可用原子吸收光谱法测定,两种方法测锑的定量线性范围均为:0~30μg/mL;检出限(3 N/S):极谱法为0.01μg/mL,原子吸收法为0.1μg/mL。方法加标回收率在98%~110%;相对标准偏差RSD(n=6)在1.5%~5.0%。方法快速简便,高效准确,已用于锑矿的采、选、冶生产过程控制分析,效果良好。