Synthesis and Efficiency of an Epoxy-Urea Chelating Resin for Preconcentrating and Separating Trace Bi,In, Sn,Zr, V And Ti From Solution Samples

Abstract

A new epoxy-urea chelating resin was synthesized from epoxy resin and used for the preconcentration and separation of trace Bi(III), In(III), Sn(IV), Zr(IV), V(V) and Ti(IV) ions from solution samples. The analyzed ions can be enriched at pH 5 at a flow rate of 1–4 ml/min, and can be also desorbed with 10 mL of 2 M HCl +0.1g NH₄F solution from the resin column, with recoveries over 97%. The chelating resin reused 6 times can still adsorb quantitatively the Bi, In, Sn, Zr, V and Ti ions, and eighty to thousand-fold excesses of Ca(II), Mg(II), Cu(II), Zn(II), Al(III), Sb(III), Ni(II), Mn(II) and Fe(III) cause little interference with the enrichment and determination of these ions. The RSDs of the proposed method for the determination of 500–50 ng/ml Bi, In and Sn, 50–5.0 ng/ml Zr, V and Ti were in the range of 0.4 ～ 4.0%, the enrichment factor of the resin for the ions is in the range of 10–100. The recoveries of added standard in waste water are between 96% and 100%, and the concentration of each ion in alloy steel sample determined by the method is in good agreement with the reference value analyzed by a steel plant with average error <2.8%.     

ICP-OES determination of traces of Ru, Au, V and Ti preconcentrated and separated by a new poly(epoxy-melamine) chelating resin from solutions

A new poly(epoxy-melamine) chelating resin is synthesized from epoxy resin and used for the preconcentration and separation of traces of Ru(III), Au(III), V(V) and Ti(IV) ions from sample solutions. The ions analyzed can be quantitatively enriched by the resin at a flow-rate of 2 mL/min at pH 4, and quantitatively desorbed with 10 mL of 1 mol/L HCl + 0.2 g CS(NH₂)₂ at a flow-rate of 1 mL/min with recoveries of over 97%. The chelating resin can be reused 7 times without obvious loss of efficiency. Thousand-fold excesses of coexistent ions caused little interference during the enrichment and determination steps. The RSDs for the determination of 50 ng/mL Ru(III) and Au(III), 5.0 ng/mL V(V) and Ti(IV) were in the range of 1.5–4.5%. The recoveries of added standards in a real sample solution are between 96% and 100%, and the results for the ions analyzed in a nickel alloy sample are in good agreement with their reported values.     

Synthesis of Polyacrylaminothiourea Chelating Fiber and Properties of Concentration and Separation of Trace Noble Metal Ions from Samples

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.     

离子印迹壳聚糖/凹土分离富集-火焰原子吸收光谱测定中药材中痕量Cd(Ⅱ)的研究

建立了离子印迹壳聚糖/凹凸棒石(IICA)分离富集-火焰原子吸收光谱(FAAS)测定中药材中痕量Cd(Ⅱ)的新方法。在动态吸附条件下,系统研究了溶液pH值、流速、洗脱条件和干扰离子对痕量Cd(Ⅱ)分离富集的影响。研究表明,在pH为4.5,上样流速为0.60mL/min条件下,Cd(Ⅱ)能被IICA定量富集;吸附的Cd(Ⅱ)可用1.0mol/L HCl-0.1mol/L甲基异丁酮的乙醇溶液,在流速为0.96mL/min条件下完全洗脱。优化条件下,IICA对Cd(Ⅱ)的动态吸附容量为56.45mg/g。线性范围为0.00097～1.28mg/L,r=0.9994,检出限(3σ,n=11)为0.97μg/L,相对标准偏差为1.32%(n=6,c=0.08mg/L),回收率在96.5%～106.4%之间。该方法操作简便,灵敏度和精密度高,可应用于实际中药材样品中痕量镉的测定。     

ICP-OES determination of traces of Ru, Au, V and Ti preconcentrated and separated by a new poly(epoxy-melamine) chelating resin from solutions

A new poly(epoxy-melamine) chelating resin is synthesized from epoxy resin and used for the preconcentration and separation of traces of Ru(III), Au(III), V(V) and Ti(IV) ions from sample solutions. The ions analyzed can be quantitatively enriched by the resin at a flow-rate of 2 mL/min at pH 4, and quantitatively desorbed with 10 mL of 1 mol/L HCl + 0.2 g CS(NH₂)₂ at a flow-rate of 1 mL/min with recoveries of over 97%. The chelating resin can be reused 7 times without obvious loss of efficiency. Thousand-fold excesses of coexistent ions caused little interference during the enrichment and determination steps. The RSDs for the determination of 50 ng/mL Ru(III) and Au(III), 5.0 ng/mL V(V) and Ti(IV) were in the range of 1.5–4.5%. The recoveries of added standards in a real sample solution are between 96% and 100%, and the results for the ions analyzed in a nickel alloy sample are in good agreement with their reported values. Received: 12 May 1997 / Revised: 1 September 1997 / Accepted: 9 October 1997     

螯合树脂研究——Ⅷ.以聚硫醚为主链的氧杂多乙烯多胺型螯合树脂的合成及其吸附性能

由聚[2′-氯乙基-2,3-环硫丙基醚]和多乙烯声胺反应,合成了四种以聚硫醚为主链的氧杂多乙烯多胺型螯合树脂,它们对贵金属离子Au(Ⅲ)、Pd(Ⅱ)、Pt(Ⅳ)、Ag~+等具有优良的吸附性能。     

以硫醚为主链的螯合树脂研究──Ⅱ．2－氨基噻唑树脂的合成及吸附性能

聚环硫丙烷和环硫氯丙烷与环氧氯丙烷共聚物，在少量二乙烯三胺存在下制得交联聚合物，将交联聚合物与２－氨基噻唑反应，制得二种侧链带有氨基噻唑的新型螯合树脂．它们对贵金属具有优良的吸附性能和高的吸附选择性．通过Ｘ－射线光电子能谱初步探讨了树脂对金属离子的螯合作用．     

巯基葡聚糖凝胶分离富集动力学光度法测定微量铅

研究了动力学分光光度法测定痕量 Pb2 +的新方法。该方法的检出限为1 37× 1 0 -10 g/m L,线性范围为 0～ 2 .0μg/2 5m L,采用巯基葡光度聚糖凝胶分离干扰离子 ,提高了方法的选择性 ,可用于 Pb2 +样品的测定。     

茜素红S螯合树脂分离富集测定地质样品中的痕量金、铂和钯

用螯合树脂对金属进行分离富集及测定,前人已做了许多有意义的研究^[1～4].曾用含键合S双硫腙(P-D)和脱氢双硫腙(P-DT)功能团的离子交换树脂和螯合树脂分离金和铂族金属^[5],用双硫腙负载树脂分离富集Cu(Ⅱ)^[6]。     

键合4-(2-吡啶偶氮)-间苯二酚螯合树脂分离富集-火焰原子吸收法测定蔬菜中痕量镉(Ⅱ)

本文合成了Amberlite XAD-4键合4-(2-吡啶偶氮)-间苯二酚螯合树脂,并考察了其对痕量镉(Ⅱ)的吸附性能。探讨了溶液pH、洗脱剂和干扰离子等对镉(Ⅱ)分离富集的影响。树脂吸附容量为4.7mg/g,吸附的镉(Ⅱ)用5mL 2mol/L HNO3乙醇溶液洗脱,火焰原子吸收法测定。在最佳实验条件下,回收率为94.4%～97.9%,相对标准偏差在1.7%～2.7%之间。方法可用于蔬菜中镉(Ⅱ)的测定。     

贵金属元素电化学分析研究(Ⅻ)——离子交换富集分离阳极溶出伏安法测定微量铱

单独铱与其它贵金属和贱金属的有效分离方法仍属少见^[1,2],作者^[3]采用15%三烷基氧化膦-苯溶液分离过大量铱,可达理想的效果。     

Synthesis of spherical macroporous epoxy-dicyandiamide chelating resin and properties of concentration and separation of trace metal ions from samples

A novel spherical macroporous epoxy-dicyandiamide chelating resin is synthesized simply and rapidly from epoxy resin and use for the preconcentration and separation of trace Ga(III), In(III), Bi(III), Sn(IV), Pb(II), V(V) and Ti(IV) ions from solution samples. The analyzed ions can be quantitatively concentrated by the resin at flow rate of 3.0 ml min(-1) at pH 3, and can also be desorbed with 10 ml of 4 M HCl+0.2 g thiourea from the resin column with recoveries of 97-100%. The chelating resin is reused for eight times, the recoveries of these ions are still over 92%, and a 100-1000 times of excess of Fe(III), Al(III),Ca(II), Mg(III), Ni(II), Mn(II), Co(II), Cu(II), Zn(II), and Cd(II) cause no interference in the determination of these ions by inductively-coupled plasma atomic emission spectrometry. The capacities of the resin for the analytes are in the range of 0.66-4.20 mmol g(-1). The results show the relative standard deviation for the determination of 50.0 ng ml(-1) Ga(III), In(III), Bi(III), Sn(IV) and Pb(II), 5.0 ng ml(-1) V(V) and Ti(IV) are in the range of 1.2-4.0%. The recoveries of a standard added in real solution samples are between 96 and 100%, and the concentration of each ion in mineral sample detected by the method is in good agreement with the certified value.     

同步荧光法同时测定苏丹红Ⅱ和苏丹红Ⅲ

开展了苏丹红的荧光分析研究, 为快速检测苏丹红提供了新的方法. 所建立的恒波长同步荧光法可同时对苏丹红Ⅱ和Ⅲ进行定性定量检测. 荧光方法具有很大的应用前景, 有望成为苏丹红的常规、快速、 简便的检测方法.     

KBr-乙醇-(NH_4)_2SO_4体系析相萃取分离和富集铱的研究

研究了KBr-乙醇-(NH_4)_2SO_4水体系析相萃取分离和富集铱的行为及与一些金属离子分离的条件.结果表明,(NH_4)_2SO_4能使乙醇的水溶液分成两相,在分相过程中,Ir(Ⅳ)与KBr生成的IrBr_6~(2-)与质子化乙醇(C_2H_5OH~(2+))形成的缔合物[IrBr_6~(2-)][C_2H_5OH~(2+)]_2能被乙醇相完全萃取.当乙醇、KBr和(NH_4)_2SO_4分别为体积分数30%、4.0×10~(-3)mol/J L、0.3 g,mL.pH 3时,Ir(Ⅳ)的萃取率达到99.5%以上,Ga(Ⅲ),Al(Ⅲ),Cr(Ⅲ),Mo(Ⅵ),Fe(Ⅲ),Ni(Ⅱ),Zn(Ⅱ),Co(Ⅱ),Mn(Ⅱ),V(Ⅴ),Ag(Ⅰ),Ru(Ⅲ)和Rh(Ⅲ)基本不被萃取,实现了Ir(Ⅳ)与上述金属离子的分离.     

流动注射微柱预富集-火焰原子吸收光谱法测定海水中铅(Ⅱ)

应用流动注射技术,用D412螯合树脂微柱富集海水中的铅(Ⅱ),并与火焰原子吸收光谱法相结合测定海水中铅(Ⅱ)。20mL海水样品以3mL.min-1流量进柱,被树脂螯合吸附富集,以0.2mol.L-1乙酸铵溶液5mL淋洗柱体去除干扰物,以4mol.L-1硝酸溶液4mL为洗脱剂(流量为7mL.min-1),洗脱液直接引入火焰原子吸收光谱仪雾化器,在线检测。当海水样进样20mL时,铅(Ⅱ)测定灵敏度可提高约35倍;检出限(3s)为1.3μg.L-1。实际应用于海水样品分析,加标回收率为94.5%,测定值的相对标准偏差(n=6)为2.2%。     

STUDY ON THE DETERMINATION OF TRACE Fe(Ⅲ) BY THIN LAYER RESIN PHASE SPECTROPHOTOMETRY

A method to determine Fe(Ⅲ) by thin layer resin phase spectrophotometry has been developed in this paper. The colored complex formed by Fe(Ⅲ) and 1,2-benzendiol is concentrated on the 717# resin, then Fe(Ⅲ) can be determined directly by making thin layer. The method is sensitive with a apparent molar absorption of 4.8×104L/mol. cm, which is 16 times higher than that of liquid phase spectrophotometry, most coexisting ions do not influence the determination. The detection limit for Fe(Ⅲ) is 1.47μg/L with the precision of 3.3% [n=6, 7μg/50mL Fe(Ⅲ)]. The calibration curve is linear in the range of 0～25μg/50mL. The preposed method was applied to the determination of Fe(Ⅲ) in water sample with satisfactory results.     

Synthesis of polyacrylaminoimidazole chelating fiber and properties of concentration and separation of trace Au, Hg and Pd from samples

A novel polyacrylaminoimidazole chelating fiber is synthesized simply and rapidly from nitrilon (an acrylonitrile-based synthetic fiber) and used for the preconcentration and separation of trace Au(III), Hg(II) and Pd(IV) ions from solution samples. The analyzed ions can be quantitatively concentrated by the fiber up to a flow rate of 15.0 mlmin(-1) at pH 3 and can also be desorbed with 15 ml of 4 M HCl+3% thiourea from the fiber column, with recoveries of 96.5-100%. The chelating fiber is reused ten times; the recoveries of these ions are still over 92%, and 100-1000 times of excess of Fe(III), Al(III), Ca(II), Mg(II), Ni(II), Mn(II), Cu(II), Zn(II) and Cd(II) causes no interference in the determination of these ions by inductively coupled plasma atomic emission spectrometry. The capacities of the fiber for the analytes are in the range of 1.56-2.92 mmolg(-1). The results show that the relative standard deviations for the determination of 50.0 ngml(-1) each of Au(III), Hg(IV) and Pd(IV) are in the range of 0.7-2.1%. The recoveries of a standard added in real solution samples are between 97 and 99%, and the concentration of each ion in powder sample detected by the method is in good agreement with the certified value.     

Cu（Ⅱ）-H2O2-考马斯亮蓝G250体系催化光度法测定痕量铜

在NH3-NH4Cl缓冲溶液介质中,痕量Cu2+对H2O2氧化考马斯亮蓝G250(CBBG)褪色反应的显著催化作用,建立了催化动力学光度法测定痕量铜的新方法。线性范围为0.02～0.20μg/mL,检出限为1.34×10-9g/mL。考察了20多种共存离子的影响。方法用于发样中痕量铜离子的测定,相对标准偏差小于3.4%,加标回收率为97%～105%。     

流动注射分光光度法快速测定水样中的铬

建立了用流动注射分光光度法快速检测水样中铬含量的方法.测定耗时140 s,测定频率25样/h.本法利用Cr(Ⅵ)和二苯碳酰二肼显色反应,Cr(Ⅵ)标准溶液的质量浓度在0.05～0.8 mm/L之间与吸光度呈线性.该法的检出限是4.0 μg/L,低于国家对Ⅰ类水的相关标准.应用此法分别测定了北京城区一些地表水中铬的含量,加标回收率在90.1%～113%之间.     

螯合树脂研究 ⅩⅩⅤ．环硫（氧）氯丙烷与三（二）乙醇胺钠盐反应合成硫氮杂冠醚型树脂

环硫（氧）氯丙烷，不经过预先聚合，直接与三（二）乙醇胶的钠盐进行反应，制得交联的硫、氮杂冠醚型螫合树脂．提出了可能的反应机理．还研究了这类树脂对一些贵金属和非贵金属离子的吸附性能．比较了相应的含硫、氮和氧氮树脂吸附性能的差别．总的说来合硫氮的树脂对贵金属的吸附性能优于含氧、氮树脂．