四元缔合物体系薄层树脂相分离与光度法联用测定痕量钴

提出了在酸性条件下 (pH=5.0),利用阳离子交换树脂-丁二酮肟-碘-钴四元体系,通过薄层树脂相光度法测定钴的新方法。本法灵敏度高 (e454=1.7105L/molcm),比水相光度法提高14倍,精密度理想 (测定2.0礸/ml Co(II) 6次,RSD=1.3%),选择性好。实测药品VB12及天然水中钴,线性范围0.024~2.0礸/ml (定容50ml),检出限10.4ng/ml。     

薄层树脂相三元缔合体系分光光度法测定痕量Fe(Ⅲ)的研究

在酸性介质中,Fe(Ⅲ)能与硫氰酸盐生成稳定的络离子[Fe(SCN)4]3-,该络阴离子能被碱性717型阴离子交换树脂定量交换,形成阴离子交换树脂(R+)-金属离子(M+)-硫氰酸盐(SCN-)三元配合物体系,该三元配合物体系最大吸收波长为490 nm。通过制作薄层测定了水中Fe(Ⅲ)量。本法具有很高的灵敏度,4ε90=2.4×105L.mol-1.cm-1,线性范围0~0.40μg/mL,检出限为0.12μmol/L。所拟方法用于水中痕量Fe(Ⅲ)的测定,结果与AAS法相吻合。     

薄层离子交换树脂相—反射光度法测定痕量钴的研究

本文提出了一种简单、快速且灵敏的吸附测定钴的分析方法。它是将显色后的有色物质吸附(交换)在离子交换树脂上,直接测定树脂薄层相的反射吸光度。用该方法对国家合金标准样品中钴进行测定,结果令人满意。     

薄层树脂相分光光度法测定痕量钙的研究

利用Na 型732#阳离子交换树脂优先与Ca(Ⅱ)交换缔合,形成二元缔合体系(R- Ca(Ⅱ)),在酸性介质中离子交换树脂负载的Ca(Ⅱ)与乙酰基偶氮羧在树脂上配位显色,形成离子交换树脂 Ca(Ⅱ) 乙酰基偶氮羧三元缔合配位显色体系,该三元体系在720nm波长处有最大吸收,建立了薄层树脂相测定钙的新方法。由于离子交换树脂与Ca(Ⅱ)二元交换缔合和树脂负载Ca(Ⅱ)与乙酰基偶氮羧配位的选择性,使本法选择性极高(EDTA存在下大多数共存离子不影响测定)。由于三元缔合配位体系的形成增大了吸光截面积,扩大了π电子离域空间,加之树脂颗粒变小(孔径为0 074mm以下),晾干浓缩提高了方法灵敏度,表观摩尔吸光系数ε720=9 1×105L·mol-1·cm-1,比水相光度法灵敏度提高15 4倍,测定5 0μgCa(Ⅱ)6次,RSD=2.9%,实测了二次精制盐水中Ca(Ⅱ),线性范围为0～9 0μg/mL,检出限为1 4μg/L。     

甲苯浮选三元配合物光度法测定痕量钴的研究

本文提出了利用甲苯浮选钴－硫氰酸铵－孔雀石绿三元配合物体系痕量钴的方法。本法灵敏度高，精密度较好，除Ｃｕ＾２＋，Ｚｎ＾２＋外其余共存离子基本元干扰，适于水样中痕量钴的测定。     

薄层树脂相光度法测定钇的研究

以溴邻苯三酚红（BPR）为显色剂，建立了以薄层树脂相光度法测定钇的方法。在PH6．5，665nm波长处直接测定钇，表观摩尔吸光系数为6．310^6L.mol^-1.cm^-1，其灵敏度比相庆溶液法提高300倍，方法用于合成矿样中钇的测定。结果满意。     

簿层树脂相吸光光度法测定痕量钴的研究

提出了用薄层树脂相通过光度法测定痕量钴的新方法。本法具有灵敏度高，选择性好，快速等特点。钴离子（Ⅱ）与４－（５－氯－二吡啶）偶氮］－１，３－二氨基苯（简称５－Ｃｌ－ＰＡＤＡＢ）生成有色稳定配合物，将其富集在Ｈ＋型（７３２~＃）。阳离子交换树脂上，制作成薄层直接测定，λ_（ｍａｘ）＝５７１ｎｍ。本法既克服了需特制１ｍｍ比色皿的困难，又提高了测定精密度，使推广树脂相光度法成为可能。用本法实测了天然水中痕量钴，检测限２．８μｇ·Ｌ~（－１），回收率≥９８％。     

薄层树脂相吸光光度法测定痕量铁的研究

本文提出了利用薄层树脂相通过光度法测定痕量铁的新方法。铁离子与硫氰酸钾形成红色络合物，将其富集在Ｈ＋型００１×７阳离子交换树脂上，通过制作成薄层直接测定。本法装皿容易，选择性好，用于天然水和化学试剂中痕量铁的测定，结果满意。     

薄层树脂相吸光光度法测定痕量钴的研究

提出了用薄层树脂相通过光度法测定痕量钴的新方法。本法具有灵敏度高，选择性即，快速等特点。钴离子（Ⅱ）与４－（５－氯－二吡啶）偶氮］－１，３－二氨基苯（简称５－Ｃｌ－ＰＡＤＡＢ）生成有色稳定配合物，将其富集在Ｈ＾＋型（７３２＾＃）。阳离子交换树脂上，制作成薄层直接测定，λｍａｘ＝５７１ｎｍ。本法既克服了需特制１ｍｍ比色皿的困难，又提高了测定精密度，使推广树脂相光度法成为可能。用本法实测了天然水中痕量     

树脂相分光光度法测定水中微量铁

在ｐＨ９６０氨性介质中，巯基乙酸与铁（Ⅲ）生成紫红色络合阴离子，与强碱性阴离子交换树脂交换，将有色络合物富集于树脂相上，用树脂相分光光度法测定微量铁，其最大吸收波长位于５３０ｎｍ；表观摩尔吸光系数ε为６７×１０４Ｌ·ｍｏｌ－１·ｃｍ－１；铁含量在０～１４ｍｇ／Ｌ范围内符合比耳定律；测定内蒙地段黄河水和呼和浩特地区自来水中微量铁，相对标准偏差分别为４６％和３２％。     

Co(Ⅱ)-棉红-H2O2体系测定痕量钴的研究与应用

基于在NH3-NH4Cl缓冲液中,柠檬酸存在下,痕量钴能灵敏地催化H2O2氧化棉红的反应,建立了一种测定痕量钴的新方法。考察了反应的影响因素,研究了该催化反应的最佳条件及动力学参数,探讨了反应机理。该方法线性范围为0~0.025μg/mL,检出限为3.33×10-10g/mL。可用于蜂蜜和维生素B12中钴的测定。     

麦塔喇红催化光度法测定痕量钴的研究

基于在NH3-NH4Cl缓冲液中,柠檬酸存在下,痕量钴能灵敏地催化H2O2氧化麦塔喇红的反应,建立了一种测定痕量钴的新方法。考察了反应的影响因素,研究了该催化反应的最佳条件及动力学参数,探讨了反应机理。线性范围为0~0.050μg/mL,检出限为1.33×10-10g/mL。可用于蜂蜜和维生素B12中钴的测定。     

High performance thin layer chromatographic determination of erythromycin in pharmaceutical preparations

Summary A high performance thin layer chromatographic method was developed for the determination of erythromycin. The drug was separated on a silica gel 60 plate and developed in methanol by means of an automatic multiple development. The chromatogram was sprayed with 10% sulphuric acid solution and heated at 100°C for 10–15 minutes. The area of the spot was quantified by a TLC scanner at a wavelength of 410 nm. A linear calibration curve was established over the range of 4–6 μg in 10μl of erythromycin. The relative standard deviation for five replicate determinations was found to be 1.45% for 5 μg in 10 μl of erythromycin standard. The average percentage recovery was found to be 99.87. The method has been applied to the determination of erythromycin in various pharmaceutical dosage forms. Common excipients in formulations do not interfere. After optimizing the solvent system, it was found that the use of silica gel 60 F₂₅₄ TLC plate with a DVS composed of ethyl acetate, ethanol and 10% sodium acetate pH 9.5 (9:7:8) led to the differentiation and quantitation of erythromycins A, B and C with an R.S.D. of less than 2.0%. The method is simple, precise and inexpensive. It should be used for routine analysis.     

Atomic layer deposition of crystalline molybdenum oxide thin films and phase control by post-deposition annealing

Molybdenum forms a range of oxides with different stoichiometries and crystal structures, which lead to different properties and performance in diverse applications. Herein, crystalline molybdenum oxide thin films with controlled phase composition are deposited by atomic layer deposition. The MoO₂(thd)₂ and O₃ as precursors enable well-controlled growth of uniform and conformal films at 200–275 °C. The as-deposited films are rough and, in most cases, consist of a mixture of α- and β-MoO₃ as well as an unidentified suboxide MoO_x (2.75 ≤ x ≤ 2.89) phase. The phase composition can be tuned by changing deposition conditions. The film stoichiometry is close to MoO₃ and the films are relatively pure, the main impurity being hydrogen (2–7 at-%), with ≤1 at-% of carbon and nitrogen. Post-deposition annealing is studied in situ by high-temperature X-ray diffraction in air, O₂, N₂, and forming gas (10% H₂/90% N₂) atmospheres. Phase-pure films of MoO₂ and α-MoO₃ are obtained by annealing at 450 °C in forming gas and O₂, respectively. The ability to tailor the phase composition of MoO_x films deposited by scalable atomic layer deposition method represents an important step towards various applications of molybdenum oxides.     

协同催化荧光法测定痕量钴的研究

基于在硼酸 硼砂介质中,钴和三乙醇胺协同催化过氧化氢氧化还原型罗丹明6G的反应,建立了协同催化荧光法测定痕量钴的新方法。钴的检出限为0.011ng/mL;测定范围0.016～0.80ng/mL。方法已用于小麦粉,玉米粉,VB12和人尿液等样品中痕量钴的测定。     

Determination of trace amounts of cobalt in water by solid-phase spectrophotometry after preconcentration on a nitroso R salt chelating resin

A sensitive method for the determination of microamounts of cobalt by ion-exchanger spectrophotometry has been developed. The chromogenic agent, Nitroso-R-Salt (NRS), was loaded on an anionic-exchange resin (Amberlite CG-400). The absorbance of the NRS-cobalt complex on the chelating resin was measured at 508 nm. The best conditions for the preconcentration of cobalt on the resin before the spectrophotometric determination were a pH value of 6, temperature of 80 °C, and heating times of 45 or 90 min for 50 and 400 ml of sample, respectively. The detection limits were 27 ng/ml (50-ml samples) and 1.8 ng/ml (400-ml samples). Interference by other metals was investigated. The method is useful for determination of cobalt in natural waters.     

毒鼠强薄层色谱分析的检出限

建立薄层色谱法快速对毒鼠强进行简易分析的方法,利用薄层色谱进行层析分离,采用特殊显色方法,对毒鼠强进行显色,以能正常观察到斑点的色泽状态,辅助GC-MS方法确定检出极限。薄层色谱法分析毒鼠强检出限可达5~10μg。能用此方法对大多数中毒案件提取的检材进行定性分析。