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。     

感耦等离子体质谱法（ICP—MS）测定高纯氧化镝中痕量稀土杂质

本文报道用２－乙基己基膦酸单酯萃淋树脂为固定相，ＨＣｌ为淋洗液的萃取色谱法研究了高纯Ｄｙ２Ｏ３中的痕量稀土杂质和Ｄｙ２Ｏ３基体的分离条件，并用ＩＣＰ－ＭＳ法测定了高纯Ｄｙ２Ｏ３中的１４个稀土杂质，稀土元素的测定限为０．００１－０．００５ＩＣＰ－ＭＳ法测定了高纯Ｄｙ２Ｏ３     

电感耦合等离子体质谱法测定高纯氧化镨中稀土杂质

深入考察了ＩＣＰ－ＭＳ法测定高纯氧化镨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Ｐｒ６Ｏ１１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Ｔｂ相结合测定高纯Ｐｒ６Ｏ１１中稀土杂质的ＩＣＰ－ＭＳ分析方法。     

化学分离－质谱法定量分析高纯Dy_2O_3中稀土杂质

以Ｐ_（５０７）萃淋树脂为固定相，ＨＣｌ－ＮＨ４Ｃｌ为淋洗液，研究了９９．９９９％～９９．９９９９％高纯Ｄｙ２Ｏ３中痕量稀土与基体Ｄｙ的分离法，以及火花源质谱法的测定条件。可分析９９．９９９９％超高纯Ｄｙ２Ｏ３中痕量稀土杂质，测定限０．００１～０．１×１０－６，误差３０％。     

2—乙基己基膦酸单（2—乙基己基）酯萃淋树脂分离—火花源质谱法测定…

本文采用萃取色谱法以２－乙基己基膦酸单（２－乙基己基）酯（Ｐ５０７）萃淋树脂为固定相，以ＨＣｌ－ＮＨ４Ｃｌ体系为淋洗液，研究了９９．９９９％￣９９．９９９９％的高纯Ｙｂ２Ｏ３中稀土杂质和Ｙｂ基体的分离条件，将杂质淋洗液富集于复合螯合剂－活性碳上，经灼烧灰化后制成样品电极，进行质谱测定。测定下限达０．０１￣０．０５μｇ／ｇ，可用于高纯Ｙｂ２Ｏ３中杂质的测定。回收率在８０％以上。     

化学分离—质谱法定量分析高纯Dy2O3中稀土杂质

以Ｐ５０７萃淋树脂为固定相，ＨＣｌ－ＮＨ４Ｃｌ为淋洗液，研究了９９．９９９％－９９．９９９９％高纯Ｄｙ２Ｏ３中痕量稀土与基本Ｄｙ的分离法，以及火花源谱法的测定条件。可分析９９．９９９９％超高纯Ｄｙ２Ｏ３中痕量稀土杂质，测定限０．００１－０．１×１０＾－６，误差３０％。     

化学光谱法测定5N氧化钆中14个稀土杂质元素

报道了化学光谱法测定５Ｎ高纯氧化钆中１４个稀土杂质元素，在Ｐ５０７萃淋树脂色层柱上分离氧化钆中稀土杂质元素，分别采用定量分离Ｌａ－Ｓｍ及Ｔｂ－Ｌｕ＋Ｙ和部份分离Ｅｕ的方法，并相应地采用碳粉吸附法和碳粉粉末法进行光谱测定。分离时间为３．５ｈ，测定下限为１．２μｇ／ｇ（ＲＥ）。     

萃取色谱分离—原子发射光谱测定氧化钐,氧化铕,氧化钆中14个稀土杂质

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Ｓｍ２Ｏ３、Ｅｕ２Ｏ３、Ｇｄ２Ｏ３中痕量稀土杂质，可用于纯度为９９９９９９％～９９９９９９９％（不含非稀土杂质）Ｓｍ２Ｏ３、Ｅｕ２Ｏ３、Ｇｄ２Ｏ３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±６４％～±１８４％，分离周期１０～１４ｈ。     

ICP─MS测定高纯钪、钇、钬、铥和镥氧化物中痕量稀土杂质研究

研究了用电感耦合等离子体质谱（ＩＣＰ－ＭＳ）测定高纯钪、钇、钬、铥和镥氧化物中痕量稀土杂质的方法。用内标法有效地校正了基体抑制效应，改善了精密度。与ＩＣＰ─ＡＥＳ分析相比，本法具有灵敏度高、流程简单快速、耗样少等特点。测定下限可降低１─２个数量级。方法可用于９９．９９９％的高纯稀土的分析。     

感耦等离子体质谱法测定高纯氧化镥中14个痕量稀土杂质

本文报道了用感耦等离子体质谱法（ＩＣＰ－ＭＳ）测定高纯氧化镥中１４个稀土杂质的方法。镥基体对测定元素无谱线干扰，但对测定信号产生显著抑制作用。加入内标后有效地补偿了这种基体抑制效应，方法检出限为０．００５～０．０３ｎｇ／ｍＬ。样品加标为０．０１μｇ时，回收率为９０％～１０３％。精密度（ＲＳＤ）为１．４％～４．２％。方法简单，不需分离富集，样品消耗量少（１０ｍｇ）。１４个稀土元素的总测定下限（１０）可达０．５８μｇ／ｇ可直接测定纯度为９９．９％～９９．９９９９％的氧化镥中稀土杂质。     

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。     

在线柱分离ICP-MS测定高纯Eu2O3中Tm

报道了一种在线柱分离ICP－MS快速测定高纯氧化铕中杂质铥的方法，采用一种新型膦酸类萃取剂，大大降低了林洗酸度，洗脱液中的Tm直接进入ICP－MS进行在线测定。整个分离测定周期为40min，方法检出限为0．12ng/mL，加示加收率为91．5％－98％，RSD为4．1％，该方法快速，简便。用于高纯氧化铕中杂质铥的测定，结果满意。     

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).     

2-乙基己基磷酸单(2-乙基己基)酯萃淋树脂分离-火花源质谱法测定高纯氧化镱中痕量稀土杂质

本文采用萃取色谱法以2-乙基已基膦酸单(2-乙基已基)酯(P_507)萃淋树脂为固定相,以HCI-NH_4CI体系为淋洗液,研究了99.999%~99.9999%的高纯Yb_2O_3中稀土杂质和Yb基体的分离条件,将杂质淋洗液富集于复合螯合剂-活性碳上,经灼烧灰化后制成样品电极,进行质谱测定.测定下限达 0.01~0.05 μg/g,可用于高纯 Yb_2O_3中杂质的测定.回收率在80%以上.     

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％。     

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。     

In-situ vaporization and matrix removal for the determination of rare earth impurities in zirconium dioxide by electrothermal vaporization inductively coupled plasma atomic emission spectrometry

A novel method for the determination of trace rare earth impurities in ZrO₂ powder has been developed based on electrothermal vaporization inductively coupled plasma atomic emission spectrometry. A polytetrafluoroethylene slurry was used as a fluorinating reagent to convert both the matrix (Zr) and the analytes (rare earth elements) into fluorides with different volatilities at a high temperature in a graphite furnace. The more volatile ZrF₄ was removed in-situ by selective vaporization prior to the determination of the analytes, removing matrix spectral interferences. Under optimum operating conditions, the absolute detection limits of the analytes varied from 0.04 ng (Yb) to 0.50 ng (Pr) with relative standard deviations less than 5%. The recommended approach has been successfully applied to the determination of trace rare earth impurities (La, Pr, Eu, Gd, Ho and Yb) in ZrO₂ powder and the results were in good agreement with those obtained by pneumatic nebulization inductively coupled plasma atomic emission spectrometry after the separation of the matrix using a solvent extraction procedure.     

Direct determination of rare earth impurities in high purity erbium oxide dissolved in nitric acid by inductively coupled plasma mass spectrometry

A novel method was developed for the direct determination of trace quantities of rare earth elements (REEs) in high purity erbium oxide dissolved in nitric acid by inductively coupled plasma mass spectrometry (ICP-MS) in this work. The mass spectra overlap interferences arose from Er matrix on the neighbouring and monoisotopic analytes of ¹⁶⁵Ho(100) and ¹⁶⁹Tm(100) were eliminated by adjusting instrumental peak resolution value from 0.7 to 0.3 amu. The matrix suppression effect of Er on the ion peak signals of REEs impurities was effectively compensated with spiking In as internal standard element. The limit of quantitation (LOQ) of REEs impurities was from 0.0090 to 0.025 μg g⁻¹, the recoveries of spiked sample for REEs were found to be in the range of 90.3-107% through using the proposed method and relative standard deviation (R.S.D.) varied between 2.5% and 6.7%. The novel methodology had been found to be suitable for the direct determination of trace REEs impurities in 99.999-99.9999% high purity Er₂O₃ and the results obtained from this method keep in good agreement with that acquired from high resolution ICP-MS.     

电感耦合等离子体发射光谱法测定二氧化铀中痕量磷和硅元素

研究了电感偶合等离子体发射光谱法测定二氧化铀(UO2)中痕量磷和硅元素含量的方法。经过对HNO3,H2O等试剂的多级纯化,获得超低空白的高纯试剂。对样品溶解、待测杂质元素与铀基体分离等过程从机理方面进行了研究。在分离铀基体与硅元素时用磷酸三丁酯(TBP)作萃取剂,二甲苯作为稀释剂;在分离铀基体与磷元素时用三辛胺(TOA)作萃取剂,二甲苯作稀释剂。二氧化铀中磷、硅元素检出限分别为0.012,0.078μg/g,加标回收率分别为98%,96%,相对标准偏差小于4%(n=6)。该方法重现性好、检出限低,满足生产和科研检测要求。