聚乙烯醇存在下锇(Ⅱ)-氯化亚锡-结晶紫体系超高灵敏显色反应的研究

本文研究了聚乙烯醇存在下锇(Ⅱ)-氯化亚锡-结晶紫体系的超高灵敏显色反应。反应物λ_(max)=555nm,ε_(555)=1.52×10~6L·mol~(-1)·cm~(-1)。锇含量为(0～4.8)μg/25ml时符合比尔定律。对共存离子的干扰和分离进行了实验,拟定的方法可用于矿石和一些含低品位锇物料的分析。     

Spectrophotometric methods for the determination of labetalol hydrochloride in pure and dosage forms

Simple and sensitive Spectrophotometric methods for the determination of labetalol hydrochloride are described. The first two are based on the oxidative coupling reaction of labetalol hydrochloride withp-N,N-dimethyl-phenylenediamine dihydrochloride (method A, _max 685 nm) and 3-methyl-2-benzothiazolinone hydrazone hydrochloride (method B, _max 545 nm) in the presence of sodium hypochlorite and eerie ammonium sulphate as oxidants, respectively. The third depends on the formation of an ion-association complex of labetalol hydrochloride with suprachen violet 3B at pH 1.3, which is extracted into chloroform (method C, _max 565 nm). The methods obey Beer's law and the precision and accuracy of the methods were checked against the B.P. reference method and the relative standard deviations were in the range 0.35–0.52%. These methods are applied to the determination of labetalol in dosage forms.     

Adsorption of fast green and erythrosin-B to montmorillonite modified with crystal violet

Adsorption of erythrosin-B (EB) and fast green (FG) to a non-charged organosmectite based on crystal violet adsorbed up to 100% of the cation exchange capacity (CEC) was tested. Adsorption isotherms of EB and FG were prepared at 3, 24 and 50°C. All isotherms are of H-type reaching loads of approximately up to 20% of the original CEC of the crude montmorillonite (up to 0.15 and 0.10 mol dye kg^–1 clay for EB and FG, respectively). Adsorption decreases with temperature, indicating an exothermic process. Enthalpy was evaluated using van’t Hoff equation, yielding approximately –20 kJ mol^–1 for both dyes.     

稳定回归法用于复方氯丙嗪片的测定

本文应用稳定回归法用于紫外重叠光谱的分析。以复方氯丙嗪为例,不经分离,测定了盐酸氯丙嗪和盐酸异丙嗪的含量。与最小二乘回归法比较,提高了测定结果的准确度和精密度。结果满意。     

司帕沙星与茜素红荷移反应的研究

采用紫外分光光度法研究了π电子受体茜素红与电子给予体司帕沙星的荷移反应。确定了反应条件,建立了一种快速简便灵敏准确测定司帕沙星的荷移分光光度法。结果表明,司帕沙星与茜素红在(4+6)乙醇-水介质中,室温条件下即可形成1∶1稳定的荷移络合物,该络合物的最大吸收波长为530 nm,表观摩尔吸光系数为4.8×103L.mol-1.cm-1,司帕沙星药物质量浓度在6~160mg/L范围内服从比尔定律,r=0.9991。当该法用于片剂中司帕沙星的测定时,回收率为99.75%~100.00%,相对标准偏差为1.4%(n=10)。     

流动注射-结晶紫-磷钼杂多酸离子缔合体系光度法测定水中痕量正磷酸盐

在一定的酸度条件下,结晶紫与磷钼杂多酸离子缔合物的流动注射分光光度法可直接测定痕量磷.灵敏度高,重现性和选择性好.水中常见离子不干扰痕量磷的测定,工作曲线的线性范围为0～500μg·L~(-1)的磷,检出下限达1.0μg·L~(-1),以120h~(-1)采样频率,对各种天然水样进行测定,回收率为92.5%～105.0%,相对标准偏差为0.1%～6.7%.     

双显色剂高灵敏协同显色反应的研究——钴(Ⅲ)-亚硝基R盐-结晶紫体系

在水溶液中钴(Ⅱ)与亚硝基R盐所形成的配合阴离子可以与有机碱阳离子(结晶紫)缔合形成中性缔合分子。在聚乙烯醇存在下,配合物可稳定存在于水溶液中。钴(Ⅲ)-亚硝基R盐-结晶紫配合物在510nm处有一最大吸收,摩尔吸光系数ε_(510)=1.47×l0~5L·mol~(-1)·cm(-1)。配合物中各组分的摩尔比为:Co:R:CV=1:3:6。反应具有较高的选择性,采用双峰双波长法测定钴可使灵敏度得到进一步提高,相应的摩尔吸光系数ε_(510-640)=4.09×10~5L·mol~(-1)·cm~(-1)。方法用于合成试样中钴的测定,结果满意。     

Influence of CTAB/alkanol/cyclohexane w/o microemulsions on the basic hydrolysis of crystal violet

The basic hydrolysis of crystal violet has been studied in w/o microemulsions of the CTAB/alkanols/cyclohexane system (alkanols: 1-butanol and 1-hexanol). The reaction can be considered to occur in the water phase of the droplets and from the rate constant the apparent dielectric constant of the water phase was determined. The cyclohexane incorporation in the system produces a decrease in the effective dielectric constant of the water phase and in the specific conductivity.     

离子交换树脂相分光光度法测定水中痕量铋

利用离子交换树脂相通过光度法测定痕量铋。铋离子在碱性介质中与邻苯二酚紫形成紫色络合物将其富集在苯乙烯阴离子交换树脂上,通过制作成薄层直接光度法测定。本法操作简便,装皿容易,选择性好,精密度高(测定5μgBi3 5次,RSD=3.8%),铋浓度在0~10μg(50ml)时与吸光度呈线性关系,线性回归方程为A=0.010 0.075C(μg/50ml),相关系数r=0.9997,铋的回收率为98%~99%,检出限为3.2μg/L,用于水中痕量铋的测定,结果满意。     

Study of the concentration and separation of cadmium with microcrystalline phenolphthalein modified by crystal violet

A new method for cadmium separation and concentration with microcrystalline phenolphthalein modified by crystal violet (CV) was developed in the paper. In the presence of potassium iodide (KI) and CV, cadmium are quantitatively absorbed on microcrystalline phenolphthalein in the pH range 1.0-6.0 as the forms of water-insoluble ion-associated complexes (CdI₃⁻)·(CV⁺) and (CdI₄²⁻)·(CV⁺)₂. Effect of different parameters such as phenolphthalein amount, stirring time, the concentration of CV and KI, various salts and metal ions was studied in detail. During the present study, a significant enhancement of the extraction of cadmium was observed. Cd(II) can be completely separated from Zn(II), Fe(II), Co(II), Ni(II), Mn(II), Cr(III) and Al(III) in this microcrystalline system and well concentrated without the interference of these metal ions at high level. The possible reactive mechanism of cadmium concentration has been discussed. Analytical results obtained by this new method were very gratifying.