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1.
Synthesis of Polyacrylaminothiourea Chelating Fiber and Properties of Concentration and Separation of Trace Noble Metal Ions from Samples 总被引:1,自引:0,他引:1
A novel polyacrylaminothiourea chelating fiber was synthesized simply and rapidly from nitrilon (an acrylonitrile-based synthetic fiber), which was applied to preconcentrate and separate of trace amount of Au(Ⅲ),Pt(Ⅳ),Pd(Ⅳ) and Ir (Ⅳ) ions from solution of samples.The analyzed ions can be quantitatively concentrated by the fiber up to a flow rate of 20.0mL/min at pH2, and can also be desorbed with 15 mL of 4mol/L HCl 3% thiourea from the fiber column with recoveries of 96.5%-100%.The chelating fiber can be reused for ten times,the recoveries of these ions are still over 92%,and hundred to thousand times of excess of Fe(Ⅲ),Al(Ⅲ),Ca(Ⅱ),Mg(Ⅱ),Ni(Ⅱ),Mn(Ⅱ),Cu(Ⅱ),Zn(Ⅱ),and Cd(Ⅱ) cause no interference on the determination of the analyzed ions by inductively-coupled plasma atomic emission spectrometry (ICP-AES).The static saturation adsorption capacities of the fiber for the analytes are in the range of 1.15-2.80mmol/g.The relative standard deviations for the determination of 20.0ng/mL each of Au(Ⅲ),Pt(Ⅳ),Pd(Ⅳ)and Ir(Ⅳ) are in the range of 0.7%-3.0%.The recoveries for test from standard additions to real solution samples are between 96% and 100%.The concentration of each ion in powder sample detected by the method is in good agreement with the certified value. 相似文献
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A new spherical macroporous epoxy-polyamide chelating resin was synthesized from epoxy resin by simple and rapid means and used for the preconcentration and separation of trace noble metal ions from solution samples. The acidity, flow rate, reusability, capacity and interference with the adsorption of ions on the resin as well as the conditions of desorption of these ions from the resin are discussed. The results show that the relative standard deviations for the determination of 50ng mL–1 Au(III), Pt(IV) and Pd(IV) by inductively coupled plasma atomic emission spectrometry are in the range of 0.5–3.6%. The procedure was applied to determine metal smelter samples with satisfactory results. 相似文献
3.
An ICP-OES method using a new poly (acrylphenylamidrazone-phenylhydrazide-acylphenylhydrazine) chelating fiber to preconcentrate
and separate trace In(III), Zr(IV), Tl(I), V(V), Ga(III) and Ti(IV) ions from solution samples has been established. The new
chelating fiber was synthesized using polyacrylonitrile fiber as a starting material and the structure of the chelating fiber
was determined by FT infrared spectrometry. The acidity, adsorption rate, re-use, capacity and interference on the adsorption
of ions on the chelating fiber as well as the conditions of desorption of these ions from the chelating fiber were investigated
by means of inductively coupled plasma optical emission spectrometry (ICP-OES). The results show that the relative standard
deviations for the determination of 10 ng/ml In, Tl, Ga and 1 ng/ml Zr, V, Ti were lower than 2.5%. The results obtained for
these ions in real solution samples by this method were basically in agreement with the given values with average errors of
less than 4%.
Received November 29, 2000. Revision May 22, 2001. 相似文献
4.
A flow injection analysis system incorporating a microcolumn of nanometer-sized TiO2 loaded with 1-(2-pyridylazo)-2-naphthol (PAN) has been used for the development of an on-line multi-element method for simultaneous separation and preconcentration and subsequent determination of Cu2+, Co2+, Cr3+, Y3+, Yb3+ and Bi3+ by ICP-AES. Effects of pH, sample flow rate and volume, elution conditions, adsorption capacity and interfering ions on analyte recovery were examined. The adsorption capacity of nanometer-sized TiO2 loaded with PAN was 4.73, 18.57, 3.81, 6.14, 4.52 and 20.35mgg–1 for Cu2+, Cr3+, Y3+, Yb3+, Co2+ and Bi3+, respectively. The method has been applied to the analysis of trace elements in standard reference biological samples, and the results are in good agreement with the certified values. 相似文献
5.
Krystyna Pyrzynska 《Mikrochimica acta》2006,153(3-4):117-126
Donnan dialysis has been demonstrated to be a useful technique for the preconcentration and recovery of metal ions. The chemical
composition of both the sample and receiver solutions in terms of concentration and ionic compounds has a significant influence
on the mass transfer efficiency. Illustrated by examples, approaches have been reviewed that can be used to obtain higher
selectivity of metal ion transport across ion-exchange membranes. Practical applications in analytical procedures are also
discussed. 相似文献
6.
建立了双硫腙修饰纳米TiO2分离富集-石墨炉原子吸收光谱法测定水样中痕量镉、铬和铅的新方法,优化了纳米TiO2-双硫腙对试样中这3种痕量物质的吸附和解吸条件。结果表明,在pH 5.0时,镉、铬和铅可被定量吸附,静态饱和吸附容量分别为13.3、5.5、21.8 mg/g。吸附的各种金属离子可用5 mL 0.1mol/L的硝酸完全洗脱。该方法对Cd2+、Cr3+和Pb2+的检出限(3σ,n=11)分别为0.18、0.51、1.92 ng/L,相对标准偏差分别为2.8%、2.3%和1.0%,加标回收率为96%~101%。该方法已成功应用于环境水样中镉、铬和铅的测定。 相似文献
7.
作者等就多年来在萃淋树脂及螯合树脂在金属元素分离及试剂纯化方面所取得的经验和成果作了总结。在萃淋树脂方面,概要地叙述了此类树脂的制备方法,其选择性及应用等内容。就螯合树脂方面几种突出实例,如Chelex 100树脂应用于从碱金属及碱土金属离子溶液中选择性地分离两价重金属;Amberlite 743硼选择性树脂用于选择性分离以BO33-或BF4-形式存在的硼(Ⅲ)离子;LZ 85树脂用于制备高纯度含钴试剂及353E树脂用于吸附分离金属离子与氰根形成的络合离子如Au(CN)4-、Ag(CN)2-等作了介绍。此外,还对应用阴离子交换树脂,如Dowex 1-X8,分离金属离子与氯离子生成的络阴离子,如[AuCl6]3-、[FeCl4]-等;对阳离子交换树脂用于制备高纯铀等特例作了简述。 相似文献
8.
Efficient Separation of Ar and Kr from Environmental Samples for Trace Radioactive Noble Gas Detection 下载免费PDF全文
Radioactive noble-gas isotopes, 85Kr (half-life t1/2=10.8 y), 39Ar (t1/2=269 y), and 81Kr (t1/2=229,000 y), are ideal tracers and can be detected by atom trap trace analysis (ATTA), a laser-based technique, from environmental samples like air and groundwater. Prior to ATTA measurements, it is necessary to efficiently extract krypton and argon gases from samples. Using a combination of cryogenic distillation, titanium chemical reaction and gas chromatography, we demonstrate that we can recover both krypton and argon gases from 1-10 L "air-like" samples with yields in excess of 90% and 98%, respectively, which meet well the requirements for ATTA measurements. A group of testing samples are analyzed to verify the performance of the system, including two groundwater samples obtained from north China plain. 相似文献
9.
A new poly(acryl-p-nitrophenylamidrazone-p-nitrophenylhydrazide) chelating fibre was synthesized from polyacrylnitrile fibre, and the structure of the chelating fibre was determined with the help of the FT-IR spectrum. The parameters influencing the efficiency of the fibre for concentrating trace amounts of Bi3+, In3+, Sn4+, Ga3+ and Ti4+, including sample acidity during enrichment, flow rate, adsorptive capacity, re-usability, interfering ions and desorption conditions were investigated. Trace Bi3+, In3+, Sn4+, Ga3+ and Ti4+ were enriched and separated from real sample solutions and detected using inductively coupled plasma optical emission spectrometry (ICP-OES) with satisfactory results. The experiments show that the method is rapid, precise, simple and convenient to use. 相似文献
10.
Ning Lian Xijun Chang Hong Zheng Sui Wang Yuemei Cui Yunhui Zhai 《Mikrochimica acta》2005,151(1-2):81-88
A new method using dithizone-modified TiO2 nanoparticles (nanometer TiO2-DZ) as solid-phase extractant has been developed for the simultaneous preconcentration of trace amounts of chromium and lead prior to their measurement by inductively coupled plasma atomic emission spectrometry (ICP-AES). The preconcentration conditions of the analytes, including the effects of pH, sample flow rate and volume, elution conditions and interfering ions on the recovery of the analytes were investigated. At pH 5, the adsorption capacity of the nanometer TiO2-DZ was found to be 5.8 mg g−1 and 22.5 mg g−1 for Cr and Pb, respectively. According to the definition of IUPAC, the detection limits (3σ) of this method for Cr and Pb were 0.38 and 1.72 ng mL−1, respectively. The proposed method was applied to the determination of trace chromium and lead in foodstuffs, plants and water samples with satisfactory results. 相似文献
11.
A very stable calixarene-based polymeric chelating resin has been synthesized by covalently linking calix[4]arene-o-vanillinthiosemicarbazone through its lower rim to Merrifield resin. It was characterized by FT IR, 1H NMR and elemental analysis. The resin was efficiently employed to separate and preconcentrate toxic metal ions such as Cu(II), Cd(II) and Pb(II) in a column prior to their determination by UV-Vis spectrophotometry and atomic absorption spectrophotometry (GFAAS) with a relative standard deviation ranging between 1.0–1.4%. Various physico-chemical parameters such as pH, concentration of eluting agents, flow rate, total sorption capacity, metal-ligand stoichiometry, exchange kinetics, preconcentration factor, distribution coefficient, breakthrough capacity, resin stability, effect of electrolytes and associated metal ions have been studied. Uptake and stripping of these metal ions on the resin were fast, indicating better access of the metal ions to the chelating sites. Detection limits (3B) of 4.22µgL–1, 11.89µgL–1 and 19.61µgL–1, along with preconcentration factors of 100, 125 and 111 for Cu(II), Cd(II) and Pb(II), respectively, were achieved. The proposed method was successfully applied to the separation and trace determination of Cu(II), Cd(II) and Pb(II) from natural water samples of Ahmedabad city. 相似文献
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金橙G螯合形成树脂分离富集地质样品中的微量贵金属 总被引:10,自引:0,他引:10
主要研究了金橙G螯合形成树脂分离富集地质样品中金、铂、钯的最佳实验条件。在柱高大于16cm,0.1mol/L HCl介质的样品溶液以小于或等于0.5mL/min流速过柱,用0.1mol/L HCl的3%硫脲溶液以小于或等于0.5mL/min流速洗脱金、铂、钯(和铑),都能同时定量富集。用火焰原子吸收光谱法测定,回收率均在95% ̄110%之间。经地质样品加标准回收实验,结果令人满意。证明这种以磺酸基 相似文献
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交联壳聚糖富集分离冷原子吸收分光光度法测定环境水样中痕量无机汞 总被引:9,自引:1,他引:9
报道了采用不溶于酸碱的交联壳聚糖,以EDTA为络合剂性富集分离,冷原子吸收分光光度法直接测定环境水样中痕量无机汞的方法,并发分析的最佳条件进行了探讨。地分析实际水样,回收率为94%-98%;检测下限为7.8ng/L;相对标准偏差小于6%。 相似文献
17.
贵金属(Au, Ag, Pt等)纳米簇通常指的是由几个到约一百个原子组成的分子聚集体, 具有生物相容性好、超小尺寸(<2 nm)以及优异的物理化学性质, 尤其是能发出较强荧光等特点引起了人们的广泛关注. 目前多种贵金属纳米簇的合成方法已相继被报道, 且已应用于生物荧光成像、电化学发光、生物传感器以及细胞标记等多个领域. 本文共分为五部分, 首先重点介绍近几年兴起的以蛋白和多肽为模板来合成纳米簇的方法及优点, 并随后总结列举了文献中所采用的蛋白以及自主设计的多肽组分序列的类别, 随后探索了蛋白和多肽中的特定氨基酸与合成的贵金属纳米簇的荧光波长、量子产率、粒径之间的联系. 本文最后总结阐述了蛋白和多肽为模板成功合成贵金属纳米簇的先决条件并对其生物医学应用前景进行了展望. 相似文献
18.
交联聚苯乙烯树脂经研磨、分选后便可得到粒度均匀的小颗粒树脂(5~15μm)。我们用分选后的树脂合成了一种亚胺基二乙醛肟树脂,将其吸附Cu~(2+)后用作定位金属离子亲和色谱固定相,以甲醇氨溶液为流动相分离胺类化合物。本文详细讨论了胺类化合物在柱上的保留机制以及氨的浓度对样品洗脱的影响。 相似文献
19.
报道了色谱301固载硫杂杯芳烃树脂分离预富集-火焰原子吸收光谱法测定痕量银的新方法。探讨了固载硫杂杯芳烃树脂对银的吸附原理与最佳条件。将含Ag^+试液在pH=10、温度为23±2℃的条件下恒温震荡10min,静置10min,Ag^+可被树脂定量富集被吸附的Ag^+可用5mL酸性硫脲(0.15mol/L HCl+0.15mol/L硫脲)完全洗脱,洗脱液中的银用火焰原子吸收光谱法测定。该法对银的检出限为0.17μg/L(3σ,n=11);线性范围为0.006—3mg/L。对0.18mg/L的Ag^+标液进行7次测定,RSD=1.53%。回收率在99.9%-105.0%之间。用于“二次资源”锌矿渣和环境水样中痕量银的测定,结果满意。 相似文献
20.
固载硫杂杯芳烃树脂分离富集-火焰原子吸收法测定痕量银 总被引:5,自引:0,他引:5
报道了色谱301固载硫杂杯芳烃树脂分离预富集-火焰原子吸收光谱法测定痕量银的新方法。探讨了固载硫杂杯芳烃树脂对银的吸附原理与最佳条件。将含Ag 试液在pH=10、温度为23±2℃的条件下恒温震荡10min,静置10min,Ag 可被树脂定量富集被吸附的Ag 可用5mL酸性硫脲(0.15mol/LHCl 0.15mol/L硫脲)完全洗脱,洗脱液中的银用火焰原子吸收光谱法测定。该法对银的检出限为0.17μg/L(3σ,n=11);线性范围为0.006~3mg/L。对0.18mg/L的Ag 标液进行7次测定,RSD=1.53%,回收率在99.9%~105.0%之间。用于“二次资源”锌矿渣和环境水样中痕量银的测定,结果满意。 相似文献