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离子交换纤维富集-GFAAS测定痕量铟的研究

Study on Exchange Fiber for Enrichment and Determination of Trace Indium by GFAAS

【作者】 欧阳开

【导师】 龚琦;

【作者基本信息】 广西大学 , 分析化学, 2007, 硕士

【摘要】 本文综述了国内外对稀散元素铟的分离富集方法的现状及进展。根据离子交换纤维分子结构中所含的特殊功能基团,在合适的条件下能选择性地吸附某些金属离子,使它们与其它元素的离子实现分离的特性,研究了将聚丙烯(PP)基阳离子交换纤维、聚丙烯(PP)基阴离子交换纤维、巯基棉(SCF)和黄原酯棉(CCX)作为离子交换剂,用于石墨炉原子吸收法(GFAAS)测定各种基体中痕量铟前的分离富集。1研究了聚丙烯(PP)基阳离子交换纤维富集铟的方法,对铟的富集和洗脱条件进行了优化。含铟富集液在pH=2-4,过柱流速小于16 mL·min-1时,铟被定量富集。其饱和吸附量为32.23 mg·g-1。用10 mL 1.8 mol·L-1的硝酸可将被吸附的铟完全洗脱。该法方法检出限为0.023 ng·mL-1,回收率为96.8%~101%,RSD为0.1%~2.1%,富集倍数为5至3.3×103。测定自来水样,人工合成样,锌精矿和合成地矿样中的痕量铟,得到满意的结果。2研究了聚丙烯(PP)基阴离子交换纤维富集铟的条件,结果表明,在pH=4的HBr介质中,富集液流速在6 mL·min-1以内,铟可被定量富集。其饱和吸附量为1.32 mg·g-1。用6 mL 1.0 mol·L-1的HNO3能很好地洗脱交换柱上的痕量铟。该法能很好地富集自来水样,人工合成样,锌精矿和合成地矿样中的痕量铟。方法检出限为0.08 ng·mL-1,回收率为96%~102%,RSD为0.6%~3.9%,富集倍数为6至251。3研究了巯基棉(SCF)富集痕量铟的条件。结果表明,在pH=4的HNO3介质中,富集液流速为3~4 mL·min-1时,巯基棉能定量富集痕量铟。其饱和吸附量为181μg·g-1。吸附的铟可被10 mL 0.8 mol·L-1的HNO3定量洗脱,该法用于自来水样,人工合成铝,锌基体样品和锌精矿等样品中痕量铟的富集和测定,回收率为92.8%~101%,RSD为0.4%~2.7%,富集倍数在58~4.9×103之间。4研究了黄原酯棉(CCX)富集痕量铟的条件。结果表明,在pH=5的HCl介质中,富集液流速在14 mL·min-1内,黄原酯棉能定量富集痕量铟。其饱和吸附量为433μg·g-1。吸附的铟可被10 mL 0.05 mol·L-1的HNO3定量洗脱,该法用于自来水样、人工合成样、锌焙砂和合成地矿样中痕量铟的测定,回收率为97.4%~112.6%,RSD为0.6%~3.1%,富集倍数为10至68。

【Abstract】 On the basis of a review of the current situation and progress on separationand enrichment methods of indium at home and abroad, according to thecharacteristic that there are special functional groups in the molecule of exchangefiber, they can adsorb some metal ion selectively on right condition, make themseparate from other ions. So, in this paper, use polypropylene based cation ionexchange fiber, polypropylene based anion exchange fiber, sulfhydryl cotton andcotton cellulose xanthate to separate and enrich trace indium form various matrixbefore determination by graphite furnace atomic absorption spectrometer(GFAAS)were investigated.1 A method of enrich trace indium by polypropylene based cation ionexchange fiber was studied. The conditions of enrichment and eluent wereoptimized. When the pH of pregnant solution was 2~4, indium was enrichedquantitatively at the flow rate within 16 mL·min-1.Then it was desorbed from thecolumn completely by 10 mL 1.8 mol·L-1 HNO3. The saturated capacity was32.23mg·g-1. The method was used to enrich trace indium in water samples,artificial samples and.zinc concentrate. The detection limit was 0.023 ng·mL-1, therecovery was 96.8%~101%, the RSD was between 0.1%~2.1%, the enrichmentmultiple was from 5 to 3.3×103.2 The factors for enrichment of trace indium by polypropylene based anionexchange fiber were investigated. The results showed that in HBr solution, whenpH=4 and flow rate within 6 mL·min-1, indium can be enriched quantitatively.Then it was desorbed form the column by 6 mL 1.0 mol·L-1 HNO3. The saturatedcapacity was 1.32 mg·g-1. The method was used to enrich trace indium in watersamples, artificial samples and zinc concentrate. The detection limit was 0.08ng·mL-1, the recovery was 96%~102%, the RSD was between 0.6%~3.9%, the enrichment multiple was from 6 to 251.3 The factors for enrichment of trace indium by sulfhydryl cotton wereinvestigated. The results showed that in HNO3 solution, when pH=4 and flow ratewas 3~4 mL·min-1, indium can be enriched quantitatively. The loaded indium waseluted quantitatively by 10mL 0.8 mol·L-1 HNO3. The saturated capacity was 181μg·g-1. The method was used to enrich trace indium in water samples, artificialsamples and zinc concentrate. The recovery was 92.8%~101%, the RSD wasbetween 0.4%~2.7%, the enrichment multiple was from 58 to 4.9×103.4 The factors for enrichment of trace indium by cotton cellulose xanthatewere investigated. The results showed that in HCl solution, when pH=5 and flowrate within 14 mL·min-1, indium can be enriched quantitatively. The loaded indiumwas eluted quantitatively by 10 mL 0.05 mol·L-1 HNO3. The saturated capacitywas 433μg·g-1. The method was used to enrich trace indium in water samples,artificial samples and zinc samples. The recovery was 97.4%~112.6%, the RSDwas between 0.6%~3.1%, the enrichment multiple was from 10 to 68.

【关键词】 离子交换纤维分离富集石墨炉原子吸收
【Key words】 exchange fiberseparationenrichmentindiumGFAAS
  • 【网络出版投稿人】 广西大学
  • 【网络出版年期】2009年 07期
  • 【分类号】O657.3
  • 【下载频次】110
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