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《Analytical letters》2012,45(13):2805-2820
ABSTRACT The preconcentration and separation of platinum and palladium from weakly acidic solution (pH=4) were done on microcolumn packed with Cellex-T resin. Selective platinum elution from the column was performed with 0.01 mol/l glycine solution at pH=12, while for palladium elution 1.2 mol/l thiourea (pH=0.5) or 4.0 mol/l potassium thiocyanate (pH=1) may be used. As the detection technique was used either FAAS or GFAAS, depending on the concentration of studied metals in the eluate. 相似文献
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离子交换法提纯钯的优化工艺条件 总被引:1,自引:0,他引:1
钯由于其独特的物理和化学性能,目前广泛地用于航空、航天、微电子技术、石油化工、废气净化及冶金工业等领域.但它在自然界中含量少,二次资源中钯的含量反而大大高于原矿中的含量.钯的提纯方法有沉淀法、溶剂萃取法和色谱分离法[1,2]等.其中以氯钯酸铵沉淀法[3]和二氯二氨络亚钯法最为常用.但其工艺复杂,过程损失大.本文研究了离子交换法分离提纯钯,并用二次通用旋转组合设计法[4]对分离提纯的条件进行了优化.结果表明,该法工艺简单,分离提纯效果好,成本低.取732型阳离子交换树脂(粒度为0-6~1-25mm… 相似文献
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Abraham Warshawsky 《Separation & Purification Reviews》2013,42(2):95-130
A process for concentration and separation of platinum group metals (PGM) by a combination of ion exchange and liquid-liquid extraction is presented. First the PGM metals are dissolved by HC1/C11 and then passed through an isothiouronium anion exchange resin, where specific absorption occurs. The thiourea eluate from the resin is converted to the chloride complexes. Further hydrolysis (conditioning) yields an aqueous feed to a liquid-liquid extraction step, with Alamine-336. Platinum and palladium are very well extracted, while most of the other PGM are rejected in the aqueous phase. The liquid-liquid extraction can be used by itself, if the level of the base metals does not exceed the concentration of the PGM ions. Platinum and palladium are now separated from each other by the selective stripping of palladium with thiourea, and platinum with thiocyanate. The paper discusses the extraction chemistry of all the steps, and provides also experimental pilot-plant results. 相似文献
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Low concentrations of Pt and Pd in industrial (µgg–1 level) and environmental samples (ngg–1 level) together with the complexity of the matrix causing many interferences during the determination of noble metals often require elaboration and application of pre-concentration/matrix separation procedures before detection of the analyte. Different pre-concentration/matrix separation procedures applied prior to the determination of Pt and Pd by atomic spectrometric techniques are reviewed and critically compared taking into account potential interferences. The methods studied are divided into 5 groups including precipitation and coprecipitation, liquid–liquid extraction, solid phase extraction, electrochemical pre-concentration and biosorption. The main analytical problems occuring during sample preparation and storage are discussed. 相似文献
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C-410树脂分离富集-电感耦合等离子体质谱法测定地质样品中的金、铂、钯 总被引:20,自引:1,他引:20
研究了地质样品中超痕量Au,Pt和Pd的测定方法。采用C-410阴离子交换树脂在1.5mol/L HCl条件下对Au,Pt,Pd的吸附率分别为91.2%、100.0%、95.7%。共存离子除Ge^4 ,Cr^6 ,Ti^4 外,无显著性干扰,用ICP-MS测定Au,Pt,Pd的检出限分别为0.27、0.40和0.19μg/L。当n=8时,Au的RSD为19.2%;Pt的RSD为28.1%;Pd的RSD为15.6%。 相似文献
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双硫腙螯合形成树脂分离富集地质样品中的微量金,铂,钯及其测定 总被引:17,自引:0,他引:17
研究了双硫腙螯合形成树脂的合成及其分离富集地质样中Au,Pt,Pd的条件。于pH1.5的HCl介质中,Au,Pt,Pd定量吸附于H2DZ形成树脂上与大量贱金属分离。用0.6mol/L的硫脲-0.1mol/LHCl洗脱贵金属,回收率均在94%-106%之间。铁也部分上柱,用磺基水杨酸与酒石酸1:1联合掩蔽除去。 相似文献
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双硫腙萃取双波长系数倍率法测定铂和钯的研究及应用 总被引:4,自引:0,他引:4
在1mol/L盐酸溶液中,当氯化亚锡存在时,用双硫腙溶液同时萃取铂和钯,双波长系数倍率法测定。测定铂时,λ_1为600nm、λ_2为710nm,K=7,测定钯时,λ_1为720nm。λ_2为638nm,K=3.5。铂和钯均在0~1.0μg/ml浓度范围内符合比尔定律,表观摩尔吸光系数分别为2.01×10~5L·mol~(-1)·cm~(-1)和1.10×10~5L·mol~(-1)·cm~(-1)。本文还探讨了氯化亚锡在萃取反应中的作用机理。方法简便、选择性好,用于地质样品中痕量铂和钯的测定,可获得满意的结果。 相似文献
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反相离子对色谱法—电化学检测测定亚硝酸根,硫氰酸根,苯胺 总被引:4,自引:0,他引:4
本文采用反相离子对色谱法(安培检测)对影响NO^-2、SCN^-、C6H5NH2容量因子的各因素进行了研究,建立了分离测定这三种组分的最佳色谱条件。方法快速、灵敏、选择性高。 相似文献
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Radiochemical separation methods have been applied for the neutron activation analysis of impurities in four high-purity refractory metals, Ta, Nb, W and Mo. Impurities in the metals of Ta, Nb and W can be separated into groups using anion exchange resin with HF and/or a mixture of HF acid and HCl, but those in Mo is done using both anion and cation exchange resins. The coprecipitation of U with Th in HF media is also investigated. 相似文献
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显色剂N-间甲苯基-N''''-(氨基对苯磺酸钠)硫脲光度法测定微量铂(Ⅳ) 总被引:3,自引:0,他引:3
研究了新试剂-N间甲苯基-N’-(氨基对苯磺酸钠)硫脲(MMPT)与铂(Ⅳ)的显色反应,结果表明,在 pH 3.7~4.4的 HAc-NaAc缓冲体系中,Pt(Ⅳ)与 MMPT形成 1:3的绿色水溶性络合物,最大吸收波长位于 754.4 nm,表观摩尔吸光系数ε754.4=8.58 × 104·mol-1·cm-1,铂含量在0~1.28 mg/L的范围内服从比尔定律。本法灵敏度高、选择性好、操作简便、测定结果准确可靠。将其用于矿石和催化剂中铂的测定,结果令人满意。 相似文献
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建立了离子色谱法测定硫脲中钙离子的方法。采用CS12A阳离子交换色谱柱,以甲基磺酸(16mmol/L)作为淋洗液,测定了硫脲样品中的钙离子,通过分析5批不同的样品,分别得到其钙值在270~410μg/g,加标回收率在97.2%~102.3%。方法无需复杂的样品前处理,分析方法干扰小,测定结果令人满意。 相似文献
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Neudachina L. K. Kholmogorova A. S. Puzyrev I. S. Galieva Z. R. 《Russian Journal of Physical Chemistry A, Focus on Chemistry》2018,92(11):2309-2314
Russian Journal of Physical Chemistry A - A polysiloxane with attached groups of rubeanic acid is proposed for the extraction of silver(I), platinum(IV) and palladium(II) from dilute aqueous... 相似文献
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用浸渍法分别将铂、钯负载在铝柱撑蒙脱石载体上,制备了铂、钯负载铝柱撑蒙脱石催化剂。运用X射线衍射(XRD)、原子吸收光谱(AAS)、透射电镜(TEM)等分析方法对样品的性能和结构进行了表征,并考察了不同铂、钯负载量的催化剂对一氧化碳的催化氧化性能。结果表明,铂、钯均以高度分散的纳米粒子状态均匀分布在载体表面,并表现出良好的CO催化氧化活性。铂、钯在铝柱撑蒙脱石载体表面的有效负载率在70%~76%之间,在相同的设计负载量条件下,铂的实际负载量和有效负载率均略大于钯。CO催化氧化试验结果表明,相对于负载前,负载后催化剂的催化活性明显增加,且其催化活性随着铂、钯负载量的增加而不断增强。在相同温度和负载量条件下,钯负载型催化剂的催化活性明显高于铂负载型催化剂。 相似文献
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离子色谱法测定乳品中硫氰酸钠含量 总被引:2,自引:0,他引:2
采用离子色谱法测定乳品中硫氰酸钠的含量。样品用5 mL乙腈沉淀蛋白质,上清液过C18柱净化,所得的产物采用离子色谱法测定,外标法定量。结果表明,通过流动相以及前处理方法的改进,硫氰酸钠质量浓度在0.10~4.00 mg/L范围内与色谱峰面积呈良好的线性,相关系数r2=1,方法的检出限为0.01 mg/L。在牛奶样品中加入硫氰酸钠标准溶液进行回收试验,测得回收率为95.0%~101.0%,测定结果的相对标准准偏差为1.8%~2.8%(n=7)。该方法操作简便,能有效避免假阳性的发生,测定结果准确,适合于乳品中硫氰酸钠的检测。 相似文献
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用阳离子交换树脂柱上交换法将试样中硫酸根与稀土离子分离.交换柱上流出溶液再经AS 9阴离子分离柱(250 mm×4 mm)分离,用9.0 mmol·L-1碳酸钠溶液作流动相.定量测定中采用电导检测器和标准曲线法,该方法的检出限为0.05 mg·L-1,测定下限为0.03%.对硫酸根质量分数为3.19%的试样作精密度试验,测得相对标准偏差(n=11)为1.63%,回收率试验的结果在94.2%~112.6%之间. 相似文献
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