ICP-AES法测定高纯氧化铕中稀土杂质元素

研究了锌粉还原 5709萃淋树脂分离富集 ICP AES法测定高纯氧化铕中14个稀土杂质元素的方法,用ICP AES法测定稀土元素工作曲线下限为(以氧化物计)镧为0.05mg·L-1,铈、镨、钇为0.25mg·L-1,钕、钐、铽、镝、钬为0.1mg·L-1,铒、铥、镱、镥、钇为0.05mg·L-1,回收率为90%～106%。方法简便、准确、快速,可用于99.99%氧化铕中14个稀土杂质元素的测定。     

微柱分离-ICP-MS测定高纯氧化钆中14种稀土杂质

研究了采用自制微柱分离装置分离Gd2O3基体的条件。99．9％以上基体被分离，分离周期为36min。建立了高纯Gd2O3中分离Gd后测定Yb、Lu以及内标补偿法直接测定其它12种稀土杂质的ICP—MS分析方法.定量下限为0．08～0．80μg／g，加标回收率为85％～115％，相对标准偏差为1．1％～8．5％、方法可满足快速测定99．999％ Gd2O3中14种稀土杂质的要求。     

微柱分离-ICP-MS测定高纯氧化钐中稀土杂质

研究了微柱分离 ICP MS测定高纯氧化钐中痕量Dy,Ho,Er,Tm的方法,方法基于采用Cyanex272负载树脂微柱,选定上述杂质与大量基体分离的实验条件,分离周期为32min。最终建立了微柱分离Sm后测定Dy,Ho,Er,Tm,其他稀土杂质用内标补偿ICP MS法直接测定的分析方法。方法测定下限为0.1～5.0μg·g-1,加标回收率为90%～115%,相对标准偏差为0.9%～5.1%。本法可满足快速测定99.999%氧化钐中14个稀土杂质的要求。     

电感耦合等离子体质变法测定高纯氧化铕中Cr,Mn,Co,Ni,Cu,Cd和Pb

报道敢用电感耦合等离子体质谱直接测定高纯氧化铕中Ｃｒ，Ｍｎ，Ｃｏ，Ｎｉ，Ｃｕ，Ｃｄ，Ｐｂ等杂质的方法，选择了仪器工作条件，讨论了谱干扰和基体效应。采用Ｒｈ作内标，减小了基体的影响。本法检出限为０．１２－２．２８μｇ／Ｌ，加标回收率为８８．６％－１０８．３％，相对标准偏差为３．２－７．９％，方法简便，快速。     

ICP-MS 法测定高纯氧化铕中稀土杂质的研究

深入考察了ＩＣＰ－ＭＳ法测定高纯氧化铕时基体对稀土杂质测定的影响,研究了Ｐ５０７萃淋树脂分离大量基体Ｅｕ２Ｏ３的实验条件,建立了采用内标补偿直接测定大部分稀土杂质和经Ｐ５０７萃淋树脂分离基体后测定被干扰离子Ｔｍ相结合的高纯Ｅｕ２Ｏ３中稀土杂质的ＩＣＰ－ＭＳ分析方法。方法检出限为０．００５～０．０２１μｇ／Ｌ,加标回收率为８４％～１１２％。ＲＳＤ为１．４％～８．１％。本法适用于质量分数为９９．９９％～９９．９９９９％的高纯Ｅｕ２Ｏ３中稀土杂质的分析。     

电感耦合等离子体质谱法测定农产品土壤中痕量稀土元素

建立了电感耦合等离子体质谱法（ICP-MS）测定农产品土壤中15个稀土元素的分析方法．研究了溶样体系用量、标准溶液配制、质谱干扰、内标元素的选择．采用HNO3-HF—H2O2体系电热板溶解样品,稀土元素的溶出率较高．用ICP—MS同时测定土壤中的钇、镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥．以Rh、Re双内标在线校正,有效地降低了信号漂移对分析结果的影响．方法检出限为0．0012—0．0071ng／mL．对实际样品进行连续7次测定,方法精密度为0．2％～4．7％,回收率为97％-114％．经国家标准物质验证,结果与标准值相符．方法弥补了微波消解法的不足,且快速、准确,适合于大批量土壤样品分析．     

等离子体质谱法测定高纯氧化铥中痕量稀土杂质元素的研究

本文提出了ＩＣＰ－ＭＳ内标补偿校正法直接测定５Ｎ－６高纯氧化铥中１４种痕量稀土杂质的方法，研究了ＩＰＣ－ＭＳ测定的谱干扰和基体效应。     

高纯氧化铒中镨、钐、镝、钬、铥和钇的电感耦合等离子体原子发射光谱分析

本文采用PGS-2型2米平面光栅光谱仪和ICP光源联用,样品溶液以乙醇预去溶方式引入ICP,直接同时测定了高纯氧化铒中6个痕量稀土杂质。当样品溶液中Er_2O_3的浓度为5mg/ml时,测定下限为镨和钐为0.0010％,镝、钬、和铥为0.0020％,钇为0.00080％。分析结果令人满意,其相对标准偏差为4.4～6.8％。     

微型柱分离-ICP-MS法测定高纯氧化铽中14个稀土杂质元素

研究了微型柱分离 电感耦合等离子质谱法(ICP MS)测定高纯Tb4O7中痕量Lu的方法,采用Cyanex272负载树脂微型分离柱,选定了分离大量Tb4O7基体的实验条件,分离周期为40min。建立了微型柱分离Tb后测定Lu以及内标补偿法直接测定其它稀土杂质的高纯Tb4O7中14个稀土杂质元素的ICP MS分析方法。方法检出限为0.003～0.10μg g,加标回收率为86.6%～114%,相对标准偏差为1.1%～18%。方法可满足快速测定99.999%Tb4O7中14个稀土杂质元素的要求。     

化学光谱法测定6N氧化铕中14个稀土杂质元素

本文利用有铕易被还原的特性，将铕还原为二价进行预分离，继以Ｐ５０７萃淋树脂柱进行二次分离，光谱测定富集物中１４个稀土杂质元素，本方法富集倍数高达２０，０００倍，化学光谱测定了下限为０．６５μｇ／ｇ（∑ＲＥ）可满足６氧化铕产品分析的要求。     

膜去溶-ICP-MS法测定高纯Eu_2O_3中14种痕量稀土杂质

研究了不需基体分离,膜去溶-ICP-MS法直接测定高纯Eu2O3中的14种痕量稀土杂质的分析方法。讨论了Eu基体产生的多原子离子对被测元素的质谱干扰。使用膜去溶后,待测元素灵敏度提高3倍左右,EuO/Eu产率从去溶前的0.016%降低为0.0007%。建立了Tm的数学校正方程,通过膜去溶结合数学校正可将Eu基体对Tm干扰完全消除。14种稀土杂质的检出限和(∑RE)为70 ng/L,测定下限和(∑RE)为0.54μg/g。对6N高纯Eu2O3样品进行了分析,样品回收率为96%~109%,RSD小于10%。所建立的方法对Eu2O3标准样品的测定结果与国家标准方法测定结果相一致。     

Determination of rare earth impurities in high purity gadolinium oxide by inductively coupled plasma mass spectrometry after 2-ethylhexylhydrogen-ethylhexy phosphonate extraction chromatographic separation

A method was developed for the determination of rare earth impurities in high purity Gd(2)O(3) by inductively coupled plasma mass spectrometry (ICP-MS). The matrix suppression effect of Gd(2)O(3) on signals of rare earth impurities was compensated for by Re internal standardization. The spectra overlap interferences from GdH, GdO, GdOH(n) (n=1-3) on Tb, Tm, Yb and Lu were eliminated by 2-thylhexylhydrogen-2-ethylhexy phosphonate (EHEHP) extraction chromatographic separation. The detection limits for REEs were 0.005-0.017 ng ml(-1) in solution and 0.002-0.05 mug g(-1) in solid. Recoveries of spiked sample for REEs were from 88 to 121% with the precision of 1.0-7.5% RSD. Determination of trace REEs in two Gd(2)O(3) samples were performed. The method can be applied to analysis of 99.99-99.9999% high purity Gd(2)O(3).     

高纯氧化镨中痕量稀土杂质的ICP-MS测定

本文研究了用等离子质谱法测定高纯氧化镨中十三个稀土杂质。确定了仪器最佳工作条件，试验了功率，雾化器流量对基体抑制效应的影响，考察了镧、铈、镨氧化物离子及氢氧化物离子的干扰，选择了测定同位素，用标准加入法校正基体的抑制作用，以改善测量精度。通过加料回收及实际分析，认为本法具有耗样少、灵敏度高、操作简单的优点，可用于４Ｎ～６Ｎ纯度的氧化镨的分析。     

高纯氧化铕中微量稀土杂质的化学光谱测定

将高纯Ｅｕ２Ｏ２通过Ｐ５０７萃淋树脂分离富集，分离掉大量基体Ｅｕ２Ｏ３剩下微量稀土杂质用碳粉吸附，加ＫＢＨ４作载体进行光谱测定，本方法可测定９９．９９９９％，纯度的Ｅｕ２Ｏ３中微量稀土杂质。     

高纯氧化钬的电感耦合等离子体原子发射光谱分析及光谱干扰的校正

本文提出了以PGS-2型平面光栅摄谱仪与Plasma Therm ICP-5000D射频发生器联用,乙醇溶液预去溶进样方法,直接同时测定高纯氧化钬中5个稀土杂质元素的方法,并讨论了基体浓度对分析方法检出限的影响和光谱干扰及其校正。当样品溶液中稀土总浓度为5mg/ml时,测定下限分别为铽0.003％,镝、铒和铥0.002％,钇0.0003％。其相对标准偏差为2.8％～7.4％。     

Carbon Nanofibers as Solid‐Phase Extraction Adsorbent for the Preconcentration of Trace Rare Earth Elements and Their Determination by Inductively Coupled Plasma Mass Spectrometry

Abstract

Systematic investigations were carried out into the sorption of rare earth elements (REEs) on carbon nonofibers (CNFs) by inductively coupled plasma mass spectrometry (ICP‐MS). The experimental parameters for preconcentration of REEs, such as pH, sample flow rate and volume, eluent concentration, and interfering ions on preconcentration of REEs have been examined in detail. The studied metal ions can be adsorbed quantitatively on CNFs in a pH range from 2.0 to 5.0, and then eluted completely with 0.5 mol l^?1 HNO₃. Based on the above facts, a novel method using a microcolumn packed with carbon nanofibers as an adsorption material was developed for the separation and preconcentration of REEs prior to their determination by ICP‐MS. The proposed method has been successfully applied to the determination of light (La), medium (Eu and Gd) and heavy (Yb) rare earth elements in real sample with the recovery more than 90%. In order to validate this method, two certified reference materials of tea leaves (GBW 07605) and mussel (GBW 08571) were analyzed, and the determined values are in good agreement with the certified values.     

镉基体分离及纯镉中杂质成分的ICP-MS法测定

研究了用阴离子交换树脂分离纯镉中铜、锌、铅、铁的条件，所得优化分离条件为：717型阴离子交换树脂柱，样品溶液为2mol/L HCl溶液；三段淋洗液依次为2mol/L HCl溶液、0．2mol/L HBr 0．25mol/L HNO3的混合酸溶液及3mol/L HNO3溶液。经ICP-MS测定证明，95％以上的镉得到分离，95％以上的铜、锌、铅、铁可以分离测定，有效地降低了ICP-MS测定纯镉中铜、锌、铅、铁时镉基体的干扰。     

Determination of trace metallic impurities in high-purity quartz by ion chromatography

A method has been developed for the determination of relevant trace impurities (alkali, alkaline and transition metals) in high purity quartz by ion-chromatography. In situ reagent (HF) purification and simultaneous sample dissolution was achieved in a multichannel vapour phase digestion assembly. Twenty-one samples can be digested at a time in this vapour phase system. Significant decrease in the process blank levels for all the analytes was observed. Drastic reduction (250 times) of NH4+ blank was achieved in the described vapour phase digestion, which enables the determination of trace concentration of sodium in high purity quartz. After volatilisation of the matrix and unreacted HF, the clear water leached solutions were injected into an ion-chromatograph equipped with conductivity detector for the determination of alkali and alkaline earth metals. In the case of transition metals, the trace residues were leached with 10 mM HCl and after separation on a mixed bed analytical column (IonPac CS5) were detected by spectrophotometry after post column derivatisation using 4-(2-pyridylazo)resorcinol (PAR). The accuracy of the result was checked by their comparison with those obtained by independent methods like inductively coupled plasma (ICP) MS and ICP atomic emission spectrometry. The achievable detection limits are between 0.4 ng/g (Li) and 22 ng/g (Mn). The application of the method to the determination of the above trace metals in two high-purity-grade quartz samples is demonstrated.     

萃取色谱分离-原子发射光谱测定超高纯氧化铥、氧化镱和氧化镥中痕量稀土杂质

用２－乙基己基膦酸单２－乙基己酯萃取色谱分离－原子发射光谱测定超高纯Ｔｍ２Ｏ３、Ｙｂ２Ｏ３、Ｌｕ２Ｏ３中痕量稀土杂质，可用于纯度为９９．９９９９％～９９．９９９９９％（不含非稀土杂质）Ｔｍ２Ｏ３、Ｙｂ２Ｏ３、Ｌｕ２Ｏ３的纯度分析，１４个稀土杂质的回收率在６７％～１３３％之间；相对标准偏差 ５．１％～２３．２％；分离周期 １０～１３ ｈ。