新试剂6-溴-2-苯并噻唑重氮氨基偶氮苯的合成及其与汞(Ⅱ)的显色反应

报道了6 溴 2 苯并噻唑重氮氨基偶氮苯(BBTDAA)的合成及其与汞(Ⅱ)的显色反应。在TritonX 100存在下,于pH10.8的Na2B4O7 NaOH缓冲体系中,Hg(Ⅱ)与BBTDAA形成1∶4的红色配合物,试剂与配合物的最大吸收波长分别为430nm和515nm,表观摩尔吸光系数为1.88×105L/mol·cm。汞在0～0 32μg/mL范围内符合比尔定律。用拟定的方法测定了湖水和废水中的汞。     

新试剂苯并噻唑重氮氨基偶氮苯与锌的显色反应的研究

研究了新显色剂苯并噻唑重氮氨基偶氮苯(BTDAB)与锌的显色反应.结果表明,在TritonX-100存在下,于pH11.0～11.8的硼砂-氢氧化钠介质中,该试剂与锌可形成稳定的橙红色络合物,其最大吸收波长位于525nm处,表观摩尔吸光系数为1.6×10~5L·mol~(-1)·cm~(-1),锌量在0～12μg/25ml范围内符合比耳定律.     

新显色剂2,4,4''''-三硝基苯基重氮氨基偶氮苯的合成及其与汞的显色反应

合成了新试剂2,4,4'-三硝基苯基重氮氨基偶氮苯(简称TNBDAA),并研究了在Triton X-100存在下其与汞的显色反应. 在pH 9.0的Na2B4O7-HCl缓冲介质中,Hg(Ⅱ)与试剂形成12的红色络合物,最大吸收波长为553 nm,表观摩尔吸光系数为1.69×105 L·mol-1·cm-1,汞质量浓度在0～0.7 μg/mL范围内服从比尔定律. 方法已用于废水中微量汞的直接测定.     

6-Br-苯并噻唑重氮氨基偶氮苯的合成及其与镉(Ⅱ)的显色反应研究

合成了新三氮烯类试剂——６－Ｂｒ－苯并噻唑重氮氨基偶氮苯。通过红外光谱和元素分析等验证了其结构,研究了试剂与镉（Ⅱ）的显色反应。结果表明,该试剂是测定微量镉（Ⅱ）的高灵敏显色剂之一,其ε值达２．２３×１０５Ｌ·ｍｏｌ－１·ｃｍ－１,并且有较好的选择性。用拟定的方法测定了废水中的微量镉,结果令人满意     

汞与邻羟基苯基重氮氨基偶氮苯显色反应的研究

研究了汞与邻羟基苯基重氮氨基偶氮苯(HBDAB)的显色反应。在Na2B2O7-Na2CO3缓冲溶液中有OP乳化剂存在下,Hg(Ⅱ)与HBDAB形成1:3橙红色配合物,其最大吸收峰位于515nm波长处,表观摩尔吸光系数为1.36×105L·mol-1·cm-1,Hg(Ⅱ)在0～20μg/25ml范围内符合比耳定律,方法应用于中草药中痕量汞的测定,结果满意。     

4,4'-对偶氮苯重氮氨基偶氮苯与汞(Ⅱ)的显色反应及其应用

废水中镉、汞的含量是环境污染最重要的指标,镉、汞离子及其盐均是致癌物质,因此,简单、快速、准确地测定环境废水中镉、汞的含量具有十分重要的意义.     

对硝基重氮氨基偶氮苯与汞的显色反应

在表面活性剂吐温-60存在下,于pH 8.05的盐酸-硼砂缓冲溶液中,汞对硝基重氮氨基偶氮苯该试剂形成稳定橘红色配合物,其最大吸收波长位于480 nm处,表观摩尔吸光率为1.54×10~5L·mol~(-1)·cm~(-1),汞量在0.7 mg·L~(-1)以内符合比耳定律。方法用于废水样中汞的测定,所得结果与二苯硫腙光度法测得结果相符合。     

对氯苯重氮氨基偶氮苯分光光度法测定微量汞

研究了对氯苯重氮氨基苯偶氮苯 (p -CBDAA)与Hg (Ⅱ )的显色反应 ,在非离子表面活性剂OP存在下 ,在pH 9 5的硼砂缓冲介质中 ,Hg (Ⅱ )与P -CBDAA形成 1∶2的橙红色稳定络合物 ,其λmax=5 3 0nm ,ε=1 2 0× 1 0 5L·mol- 1·cm- 1,汞含量在 0～ 0 8μg/mL范围内遵守比尔定律。方法用于废旧钮扣电池和自来水中汞的测定 ,结果令人满意。     

新显色剂4—甲基—2—磺酸基苯基重氮氨基偶氮苯的合成及与镉的显色反？…

报道了新显色剂４－甲基－２－磺酸基苯基重氮氨基偶氮苯的合成及其与Ｃｄ（Ⅱ）的显色反应。实验表明,在非离子表面活性剂Ｔｒｉｔｏｎ Ｘ－１００存在下,于ｐＨ１０．８的氨水－氯化铵缓冲介质中,试剂与Ｃｄ（Ⅱ）形成３：１的红色络合物,最大吸收波长位于５２２ｎｍ处,Ｃｄ（Ⅱ）含量在０～２０μｇ／２５ｍＬ范围内符合比耳定律,表观摩尔吸光系数为２．０５×０５＾５Ｌ·ｍｏｌ＾－１·ｃｍ＾－１。已直接用于废水中微量     

对氯苯重氮氨基偶氮苯与银（I）显色反应的研究及其应用

研究对氯苯重氯氨基偶氯苯在TritonX-100存在下与银(Ⅰ)的显色反应:在pH=11.0的硼砂-氢氧化钠缓冲溶液中,对氯苯重氮氨基偶氮苯与银(Ⅰ)形成1:1的橙红色配合物,其最大吸收波长为504nm,表观摩尔吸光系数ε=6.20×10~4L/(mol·cm),银(Ⅰ)的浓度在0～10.0μg/(25 mL)范围内符合比耳定律,线性回归方程为,A=0.0228c 0.00188,相关系数r=0.9997。方法应用于实验室废液和银锌组扣电池液中银的测定,加标回收率分别为97％、102％,相对标准偏差分别为4.6％、2.5％。     

钒与新显色剂 1,4-双肼酞嗪显色反应的研究及应用

研究了钒与新显色剂 1,4-双肼酞嗪的显色反应.在 pH 5.8 的 HAc-NaAc 缓冲溶液中,加入溴化十六烷基三甲铵于 60℃加热 10 min,钒与 1,4-双肼酞嗪形成稳定的螯合物,λmax=422nm,ε422=1.32×104 L·mol-1·cm-1,钒的浓度在 0 μg/25 mL～20 μg/25 mL 范围内符合比耳定律,检出限为 15 ng/mL,已用于测定钢样中的微量钒.     

新试剂2,6-二甲基苯基重氮氨基偶氮苯测定化妆品中微量汞

通过对新试剂2,6 二甲基苯基重氮氨基偶氮苯与汞的显色反应的研究,建立了直接测定化妆品中微量汞的光度分析方法。在氨水介质中,2,6 二甲基苯基重氮氨基偶氮苯和汞发生灵敏的显色反应,生成配合比为3∶1的红色配合物。配合物的最大吸收峰位于516nm,表观摩尔吸收系数为1.5×105L·mol-1·cm-1;在25mL溶液中,汞量在0～18μg之间符合比耳定律。此外,该显色反应具有良好的选择性,绝大多数金属离子不干扰汞的测定,它的选择性好于目前所用的其它重氮氨基偶氮苯试剂,用于化妆品中微量汞的测定,结果与原子吸收光谱法相一致。     

新试剂对甲基偶氮羧与钡显色反应的研究及其应用

合成了对甲基偶氮羧新显色剂 ,经研究发现 ,在柠檬酸介质中 ,对甲基偶氮羧与钡发生高灵敏的显色反应 ,生成蓝色配合物 ,它的最大吸收峰位于 72 0nm。Ba(Ⅱ )在 0 μg/2 5mL～ 1 0 μg/2 5mL符合比耳定律 ,配合物的表观摩尔吸光系数达 2 1 8× 1 0 5L·mol- 1 ·cm- 1 ,检测限为 1 5ng·mL- 1 。该试剂已用于钛酸钡烧结物中游离钡的测定     

Synthesis of a new carbbenzyloxymethylenetriparatolylphosphorane ylide and study of its reaction with mercury(II) halides: Spectral and structural characterization

A new carbbenzyloxymethylenetriparatolylphosphorane ylide (BTPY), {(p-tolyl)₃PCHCOOCH₂C₆H₅},was synthesized and characterized with elemental analysis as well as various spectroscopic techniques. The reactions of the title ylide with mercury(II) chloride, mercury(II) bromide and mercury(II) iodide in equimolar ratios using dry methanol as solvent have yielded [BTPY · HgCl₂]₂ (1), [BTPY · HgBr₂]₂ (2) and [BTPY · HgI₂]₂ (3), respectively. Single crystal X-ray analysis of 2 reveals the presence of a centrosymmeteric dimeric structure containing the ylide and HgBr₂. The analytical data, IR and ¹H, ¹³C and ³¹P NMR data for the latter compound are similar to those of 1 and 3, indicating similar structures. The theoretical studies indicated that, for all three compounds, the observed trans-like structure for compound 2, is more stable than the possible cis-like structure in each case.     

Synthesis of a novel bistriazene reagent 4,4′-bis[3-(4-phenylthiazol-2-yl)triazenyl]biphenyl and its highly sensitive color reaction with mercury(II)

We report the synthesis of a novel bistriazene, 4,4′-bis(3-(4-phenylthiazol-2-yl)triazenyl)biphenyl (BPTTBP), and its highly sensitive color reaction with Hg²⁺. The new reagent was synthesized in good yield by coupling 2-amino-4-phenylthiazole with 4,4′-biphenyldiamine bisdiazonium salt. Using a blend of surfactants N-cetylpyridinium chloride (CPC) and polyethylene glycol n-octanoic phenyl ether (OP) as a micelle sensitizer, the red colored reagent assembles with Hg²⁺ in pH 9.8 borate buffer according to a 1:1 stoichiometry, forming a blue oligomeric/polymeric chelating complex with a high apparent stability constant (1.1 × 10⁸ M⁻¹). Whereas the maximum absorption of reagent occurs at 510 nm with an extinct coefficient of 1.35 × 10⁴ M⁻¹ cm⁻¹, the complex absorbs at 611 nm, with an apparent extinct coefficient of 1.04 × 10⁵ M⁻¹ cm⁻¹. Beer's law is obeyed in the range of 0-15 μg/25 mL Hg²⁺, and Sandell's sensitivity is 1.92 × 10⁻³ μg/cm². In the presence of thiourea and Na₄P₂O₇ as masking agents, the method was found free from interferences of foreign ions commonly occurring with mercury. The optimized protocol has been successfully applied to spectrophotometric determination of mercury in waste water samples. The features of the new reagent associated with its special structure were discussed, and an unprecedented “domino effect” was proposed to account for its unique chelating stoichiometry with Hg²⁺.     

Spectrophotometric flow-injection analysis of mercury(II) in pharmaceuticals with p-nitrobenzoxosulfamate

A new, simple and rapid spectrophotometric FI method for the accurate and precise determination of Hg(II) in pharmaceutical preparations has been developed. The method is based on the measuring the decrease of absorbance intensity of p-nitrobenzoxosulfamate (NBS) due to the complexation with Hg(II). The absorption peak of the NBS, which is decreased linearly by addition of Hg(II), occurs at 430 nm in 2×10⁻⁴ mol l⁻¹ HNO₃ as a carrier solution. Optimization of chemical and FI variables has been made. A micro column consisting of several packing materials applied instead of reaction coil was also investigated. A background level of Fe(III) maintained in reagent carrier solution with NBS was found useful for sensitivity and selectivity. Under the optimized conditions, the sampling rate was over 100 h⁻¹, the calibration curve obtained were linear over the range 1-10 μg ml⁻¹, the detection limit was lower than 0.2 μg ml⁻¹ for a 20 μl injection volume, and the precision [S_r=1% at 2 μg ml⁻¹ Hg(II) (n=10)] was found quite satisfactory. Application of the method to the analysis of Hg(II) in pharmaceutical preparations resulted a good agreement between the expected and found values.     

新显色剂三甲氧基苯基荧光酮光度法测定锗

研究了新试剂三甲氧基苯基荧光酮光度测定锗的方法。在 3mol/ m LH3PO4 介质中 ,当 Triton X- 1 0 0存在时 ,锗与三甲氧基苯基荧光酮形成 1∶ 2橘红色络合物 ,最大吸收在 5 0 5 nm波长处 ,摩尔吸光系数为 1 .7× 1 0 5L· mol-1·cm-1且具有高的选择性。当锗含量在 0～ 6μg/ 2 5 m L范围内符合比尔定律。已用于大蒜与枸杞子中锗的测定