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本文报道了钯与4-(2-吡啶偶氮)间苯二酚(PAR=H_2R,下同)和四苯钟离子形成离子缔合物的化学条件,经氯仿萃取后,建立了一种测定微量钯的萃取光度法。萃取的最佳pH为4.4,络合物的化学式为[(C_6H_5)_4As~+,PdClR~-],其最大吸收峰波长为532nm,表观摩尔吸光系数e_(532)=3.3×10~4L·mol~(-1)·cm~(-1),10mL萃取液中钯量在0~25μg内遵守比耳定律。方法简便,选择性好,用于催化剂中钯的测定,结果满意。 相似文献
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萃取阻抑光度法间接测定痕量硫脲 总被引:2,自引:0,他引:2
研究了在pH 4.5的柠檬酸盐缓冲溶液介质中, 利用硫脲对钒(Ⅴ)催化溴酸钾氧化邻氨基酚显色反应的阻抑作用, 用萃取平衡控制反应时间和水相中邻氨基酚的浓度及反应程度, 通过测量424 nm下有机相的吸光度, 建立了萃取催化光度法测定痕量硫脲的新方法。在最佳实验条件下, 测定硫脲的线性范围为0.020~1.20μg/mL,检出限为1.4×10-8 g/mL。对1.00μg/mL硫脲进行11次平行测定的相对标准偏差为3.8%。用于水样中硫脲的测定, 结果满意。 相似文献
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新显色剂邻磺酸基苯偶氮若丹宁合成及与钯的光度法研究 总被引:2,自引:1,他引:2
报道了新显色剂邻磺酸基苯偶氮若丹宁(o-SBAR)的合成及其与钯显色反应的性能。在2.4mol· L~(-1)磷酸介质中,试剂与钯形成 1: 1的桔红色配合物,在 520nm波长处配合物有最大吸收,表观摩尔吸光系数为6.65×10~4,反应速度快,选择性高,应用于钯碳催化剂中钯的测定,结果满意。 相似文献
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5-Br-PADAB分光光度法测定钯 总被引:8,自引:0,他引:8
研究了4-(5-溴-2-吡啶偶氮)-1,3-二氨基苯(简称5-Br-PADAB)分光光度法测定微量钯的反应,在乙酸介质中Pd(Ⅱ)与5-Br-PADAB生成紫红色络合物,确定了分光光度法测定钯的新体系。在实验条件下试剂的最大吸收峰位于438nm处,络合物的最大吸收峰位于564nm处,表观摩尔吸光系数ε=5.20×10-4L/mol.cm,用等摩尔连续变化法、摩尔比法测得络合比n(Pd(Ⅱ))∶n(5-Br-PADAB)=1∶1,钯离子的量浓度在4.27×10-8~1.54×10-5mol/L时,服从Beer定律。试验了30种离子在一定量下不干扰测定。 相似文献
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萃取分离—苯芴酮分光光度法测定茶叶中锗的含量 总被引:8,自引:0,他引:8
对苯芴酮分光光度法测定微量锗时的干扰情况进行了考查,发现在H3PO4和HClO4共存体系中,以CCl4萃取Ge,并在显色测定时加入乙酰丙酮作掩蔽剂,能有效地消除干扰,本实验还对茶叶样品的处理方法进行了比较,灰化法时间短,操作简单,Ge损失小。 相似文献
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双波长分光光度法同时测定贵金属钯和锇 总被引:4,自引:0,他引:4
本文提出了在对羟基苯基荧光酮和溴化十六烷基三甲烷基甲胺存在下,双波长分光光度法同时测定微量和锇的新方法,在pH=7.6~8.0的磷酸盐介质中,钯和锇的对羟基苯基荧光酮-CTMAB配合物吸收光谱相互重叠,选择测定钯配合物的波长对为580.5nm与530.5nm,测定锇配合物的波长对为553.5nm与604.5nm,钯含量在0~7.0μg/10mL范围内,锇含量在0~9.0μg/mL范围内,与ΔA值呈 相似文献
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研究了抗坏血酸与磷钼钨三元杂多酸的显色反应,提出了借磷钼钨杂多蓝测定抗坏血酸的分光光度法.最大吸收波长为730nm,抗坏血酸在0.08~10mg/L范围内线性良好.回归方程为A=1.05×104C+0.017,线性相关系数γ=0.9995,表观摩尔吸光系数ξ730=1.05×104L·mol-1·cm-1,方法检出限为0.04mg/L,回收率为94~102%,相对标准偏差≤1.5%(n=8).本方法由于钨钼的混合配位增强了氧化能力,较之二元杂多酸的方法,省去了水浴加热等操作,只需在室温下反应30min,吸光值至少可稳定6h.过量的黄色杂多酸可加入适量的氢氧化钠溶液分解,从而获得色泽纯正的高灵敏度显色体系. 相似文献
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磷钼钨三元杂多酸光度法测定药物中的抗坏血酸 总被引:2,自引:0,他引:2
研究了抗坏血酸与磷钼钨三元杂多酸的显色反应,提出了借磷钼钨杂多蓝测定抗坏血酸的分光光度法。最大吸收波长为730nm,抗坏血酸在0.08~10mg/L范围内线性良好。回归方程为A=1.05×104C+0.017,线性相关系数γ=0.9995,表观摩尔吸光系数ξ730=1.05×104L·mol-1·cm-1,方法检出限为0.04mg/L,回收率为94~102%,相对标准偏差≤1.5%(n=8)。本方法由于钨钼的混合配位增强了氧化能力,较之二元杂多酸的方法,省去了水浴加热等操作,只需在室温下反应30min,吸光值至少可稳定6h。过量的黄色杂多酸可加入适量的氢氧化钠溶液分解,从而获得色泽纯正的高灵敏度显色体系。 相似文献
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《Analytical letters》2012,45(11):827-834
Abstract A sensitive and selective method has been developed for the spectrophotometric determination of antimony in the tervalent oxidation state. It was found that antimony (III) reacts with mandelic acid to form a complex anion extractable into chlorobenzene with malachite green in weak acidic media (pH 2.2 to 3.5) at room temperature and is determined indirectly by measuring the absorbance of malachite green in the extract at 628 nm. The calibration graph is linear for antimony (III) over the range 0.088–1.8 mg 1?1 (7.2 × 10?7–1.5 × 10?5 mol 1?1) with the apparent molar absorptivity ε × 6.9 × 104 1 mol?1 cm?1. Antimony (V) was slightly extracted in the presence of phosphate buffer with ε × 2.7 × 103 1 mol?1 cm?1. 相似文献
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《Analytical letters》2012,45(1-2):25-36
Abstract Solvent extraction spectrophotometric and atomic absorption spectrophotometric methods for the determination of selenium(IV) in microgram quantities are described. The selenium(IV) forms yellow colored complex with N-phenylbenzohydroxamic acid (PBHA) extractable into chloroform from 7 M HClO4. Se-PBHA complex has maximum absorbance at 345 nm with a molar absorptivity 1.5 × 105 1 mol?1 cm?1 and Sandell's sensitivity 0.000526 μg /cm2. Effect of molarity, reagent concentration, diverse ions on the extraction of selenium complex were studied. The selenium is determined in presence of tellurium. 相似文献
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This work aims to achieve a determinate characterization of compound formation and to find out the resolution to overcome chemical interferences in atomic absorption spectrophotometric (AAS) determination of palladium. The effect of flame composition in producing a neutral palladium atoms was investigated. A new analytical procedure has been elaborated for the determination of palladium. 相似文献
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《Analytical letters》2012,45(20):2349-2357
Abstract A sensitive and selective method for the extraction and spectrophotometric determination of Zr(IV) with N-p-chlorophenyl-3,4-,5-trimethoxycinnamohydroxamic acid (PTCHA) has been developed. The binary complex of Zr(IV)-PTCHA is extracted from 2–6 M HCl into chloroform, having a maximum absorbance at 385 nm; molar absorptivity 2.1 × 104 1 mol?1 cm?1. A ternary complex with xylenol orange (Zr-PTCHA-XO) have been studied in chloroform-ethanol media, which absorbs at 540 nm; molar absorptivity 4.3 × 104 1 mol?1 cm?1. The present method is applied for the analysis of zirconium in standard samples. 相似文献
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《Analytical letters》2012,45(7):531-534
Abstract The sulfate ion is extracted into toluene with nonionic surfactant span 20 and crystal violet. A linear calibration curve was obtained between the absorbance due to crystal violet in the extract and sulfate concentrations over the range 2.5 × 10?5 to 2.5 × 10?4 mol 1?1 (2.4 to 24 ppm) in the aqueous phase. 相似文献
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微波消解和固相萃取光度法测定氰化渣中痕量钯 总被引:7,自引:0,他引:7
根据 2_(2_喹啉偶氮 )_5_二甲氨基苯甲酸 (QADMAB)与钯的显色反应及C18固相萃取小柱对显色络合物的固相萃取 ,并结合微波消解样品 ,建立了一种测定氰化渣中痕量钯的方法。即在pH为 3 5的HAc_NaAc缓冲介质中 ,溴化十六烷基三甲胺 (CTMAB)存在下 ,QADMAB与钯反应生成 2 1稳定络合物 ,该络合物可被C18小柱萃取富集 ,富集的络合物用乙醇洗脱后用光度法测定 ,在乙醇介质中体系λmax=63 0nm ,ε=1 2 0× 1 0 5L·mol-1·cm-1。钯含量在 0 0 1~ 1 5mg L内符合比尔定律 ,方法用于氰化渣中钯含量的测定 ,结果令人满意。 相似文献
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《Analytical letters》2012,45(12):2360-2373
Abstract A selective, sensitive, and economical derivative spectrophotometric method has been developed for the determination of trace amount of Cu(II) and Pd(II) with MDTC as a reagent in the presence of CTAB, a solubilizing agent. The molar absorption coefficient and analytical sensitivities of the 1:2 Cu(MDTC)2 and Pd(MDTC)2 complexes are 2.467×104 and 2.989×104 l mol?1, respectively. The developed derivative procedure, is applied for the rapid and selective simultaneous determination of Cu(II) and Pd(II) in the range of 0.2–15 and 0.1–10 µg/ml, respectively. Complex matrices, including alloys, biological samples, pharmaceutical samples and synthetic mixtures have been successfully analyzed for trace amounts of two metal ions. 相似文献