离子色谱非梯度洗脱法同时测定7种稀土元素的研究

研究了离子色谱非梯度洗脱法同时测定7种稀土元素的方法，用草酸一元淋洗液，采用非梯度洗脱方式，以PAR为显色荆，在520nm处对7种稀土元素同时进行检测。考察了淋洗液的组成、浓度、pH及流量等因素对被测组分分离和测定的影响，选择了显色剂的浓度、流量和检测波长，并进行了干扰实验，在选定的最佳分离测定条件下，测定了7种稀土元素的线性回归方程、检出限0．04～0．20mg／L，回收率在94．3％～101．5％之间。本方法已用于稀土氧化物的高温氯化产物中稀土元素的测定。     

Zeeman效应AAS中元素的吸收线分裂行为的研究

本课题包括三方面内容: 1.绘制了周期系Ⅰ-Ⅷ族元素吸收线的Zeeman分裂谱图,以往文献只见过51条线15幅图,稀土元素zeeman谱图是空白。本工作列出包括稀土元素在内的250条线97幅Zeeman图。结合谱图对灵敏度的影响的统计趋势的实验研究,第一次给商品ZAAS使用者提供系统、完整有半定量概念的Zeeman谱图。     

2-乙基已基膦酸单(2-乙基已基)酯萃淋树脂分离-火花源质谱法测定高纯氧化钐中痕量稀土杂质

1引言火花源质谱法是测定高纯稀土的方法之一，具有灵敏度高、基体影响小、谱线干扰少等优点。对于单同位素的超高纯稀土元素，通常可以利用火花源质谱法直接测定，但对于99．9999％的超纯Sm3O3，由于Sm有7个同位素，晕轮背景干扰，谱线干扰以及大量基林元素存在，严重影响火花源质谱法灵敏地测定痕星稀土元素，必须分离富集，以P507萃林树脂为固定相、HCl-NH4Cl为淋洗液研究了大量基体Sm和其它14个痕量稀土杂质元素的分离方法，结合资合剂-活性碳柱富集淋洗液中14个痕量稀土元素，成功的建立了化学分离-火花源质谱法分析高纯氧化衫的方…     

珍珠中痕量稀土元素的ICP-MS测定及其分布特性

探讨了等离子体质谱(ICP-MS)分析珍珠样品中稀土元素的基体效应及多原子离子干扰,并采用干扰校正因子进行有效的校正,以In-Rh双内标校正体系进行分析信号动态漂移的监控和补偿,建立了珍珠样品中稀土元素的ICP-MS分析方法。方法的定量检出限为0．1～0．5ng／g,RSD≤15％(n=5)。所建立的方法用于标准物质Gui-1、Gui-2、Gui-3及人工养殖珍珠的分析。珍珠中稀土元素的分布与分馏特性与其生长环境密切相关。     

ICP－AES半智能直接测定稀土氧化物

本文报道了一种用ＩＣＰ－ＡＥＳ直接测定稀土氧化物的半智能方法，稀土基体对某一稀土分析谱线的光谱干扰被预先扫描并存于谱图集中。在实际测定中，相应的干扰谱图被调用，参加扣除干扰谱线影响的校正计算。结果表明该法令人满意。     

ICP—AES半智能直接测定稀土氧化物

本文报道了一种用ＩＣＰ－ＡＥＳ直接测定稀土氧化物的半智能方法，稀土基体对某一稀土分析谱线的光谱干扰补预先扫描并存于谱图集中，在实际测定中，相应的干扰谱图被调用，参加扣除干扰谱线影响的校正计算。结果表明该法令人满意。     

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。     

X-荧光α系数法测定稀土氧化物中15个稀土元素

采用粉末稀释直接压片,在PW1400顺序式X-荧光光谱仪上测定了 15个稀土元素。通过电子计算机采用干扰系数扣除严重的谱线干扰,应用α系数校正复杂的基体效应,取得满意的结果。本文研究重点是选择了最佳仪器测量条件;测量出元素间的干扰系数及校正了背景影响;比较了三种基体校正数学模型的效果。分析精度:当含量小于2％时,优于 5％;含量大于2％时,优于?2％。分析速度较文献[5]提高三倍。     

电荷注入检测器电感耦合等离子体光谱仪的稀土元素分析性能

研究了电荷注入检测器电感耦合等离子体发射光谱（ＣＩＤ－ＩＣＰＥＳ）测定稀土元素的分析性能。结果表明,在稀土元素常用谱线波段内（２６０～４４０ｎｍ）光谱背影发射强度低于４０ＣＰＳ（计数／秒）,ＲＳＤ〈０．６％。研究了谱线强度和相对标准偏差的关系,当谱线强度高于５ＣＰＳ时,对于任何稀土元素谱线的ＲＳＤ均低于０．６％。谱线强度降低时,ＲＳＤ逐渐增大。文中给出了稀土元素常用分析谱线的强度值、线背比、背影等     

稀土高氯酸溶液导数光谱的研究及其在分析中的应用——Ⅲ.导数分光光度法测定混合稀土中的镨、钕、钐、铕、镝、钬、铒、铥

本文探讨了共存稀土离子及温度对镨、钕、钐、铕、镝、钬、铒、铥等稀土离子的高氯酸溶液的二阶导数吸收光谱的影响。在所选定的分析峰位,共存稀土离子或不干扰或仅存在轻微干扰,而对于待测稀土离子导数峰的这种轻微干扰及温度的影响,都可用校正系数法消除。文中提出了一种在混合稀土(十五个稀土元素共存)中直接、快速测定上述八个稀土元素的导数光度法,并在合成样品及实际样品分析中获得了满意的结果。     

ICP-AES法直接测定金属钕、氧化钕中的稀土和非稀土杂质元素

建立了金属钕和氧化钕中24个杂质元素的高频感耦等离子体原子发射光谱直接测定的方法。配制了3组可混听多元素标准溶液，采用基体匹配法和多组分光谱拟合（MSF）技术以消除基体光谱干扰。测定元素的回收率为96．8％－104．0％，精密度为0．92（Ti)%-6.9(Ca)%.     

ICP emission spectrometric analysis of rare earth elements in permanent magnet alloys

An analytical method for the determination of rare earth elements (REE) in a NdFeB permanent magnet alloy by ICP emission spectrometry is described. Spectral interferences, arising from overlapping, as well as matrix effects have been studied. Considering spectral interferences, sensitivities of spectral lines, background intensities and the chemical composition of the sample investigated, optimum spectral lines for each REE have been selected. Because of an unfavourable concentration ratio in samples of a NdFeB permanent magnet alloy, a preliminary separation of matrix elements from rare earth elements by ion chromatography is necessary. Different modes of elution (isocratic and gradient) with -hydroxy-isobutyric acid and different columns (NUCLEOSIL, SULFOPROPYL SI-100, DIONEX HPIC-CS3) have been tested. Optimum separation conditions have been chosen for each element and the separation efficiency at equal or different concentrations of the selected elements have been established. Although the separation of REEs resulted in partly overlapping peaks, the ratio between analyte and interferent is improved and the spectral interferences are diminished. The results obtained are in good agreement with certified values.     

Spectral Interferences of Rare Earth Elements in ICP-AES with a High Resolution Sequential Spectrometer-Spectral Interferences of Eu and Gd on Other Rare Earth Elements

The important function and status of the rare earth elements are well known. Being a powerful tool for elemental analysis, inductively coupled plasma atomic emission spectroscopy (ICP-AES) has been extensively applied in the purity analysis of REEs due to its high performance. However, the spectral interferences are the major obstacle in the analysis of REEs because of the rich spectral lines of REEs. In spite of many reports about the spectral interferences of REEs, all-inclusive information is not enough to satisfy the needs of the analysis of REEs.     

ICP－AES法测定氧化铕中14种数量稀土杂质

采用ＩＣＰ－ＡＥＳ单道扫描光谱仪详细考察了十四种被测稀土杂质元素的４７条灵敏分析线的谱线轮廓及基体Ｅｕ的背景谱线轮廓，从而选定基体干扰小，灵敏度高的分析线及扣除背景的合适位置；试验了酸度，载气流量，观测高度，射频发生器功率等对信号强度和基体干扰程度的影响，采用基体匹配法校正基体对测定的影响，建立了氧化铕中１４种稀土杂质的直接测定法。已用于出口产品的分析和标准试样的定值测定，得到了满意的结果。     

High-resolution spectra of selected rare earth elements and spectral interferences studied by inductively coupled plasma-atomic emission spectroscopy (ICP-AES)

The rare earth elements (REEs) play very important roles in industrial manufacturing, technology development and biological processes. Due to their complex emission spectra, trace levels of REEs are difficult to analyze by conventional ICP-AES techniques. The present study investigates possible spectral interferences of matrices (rare earth oxides of Ce, Pr, Nd, Sm and Dy) on the analytical lines (± 0.1 nm) of a target REE. Detailed and well-resolved spectra for selected REEs are presented, and procedures used to rectify the problem of spectral interferences caused by REE matrices are discussed. A computer-assisted system (CAS) for spectral recognition has been developed and used to assist in the study of matrix interference. To determine directly trace rare earth elements in REE matrices without sample pre-separation, the application potential is demonstrated with a one meter sequential instrument retrofitted with a 3600 grooves/mm grating.     

稀土对茶叶中稀土结合糖蛋白的组成及活性的影响

应用电感偶合等离子体质谱（ＩＣＰ－ＭＳ）、气相色谱（ＧＣ）、氨基酸分析仪及动力物模型,研究了喷施稀土对茶叶中稀土结合糖蛋白（ＲＥＥ－ＴＧＰ）组成及活性的影响,成品茶中有稀土结合糖蛋白;稀土对单糖种类及组成没有明显影响,但ＲＥＥ－ＴＧＰ中羟脯氨酸（Ｈｙｐｒｏ）及丝氨酸（Ｓｅｒ）含量增加明显,而谷氨酸（Ｇｌｕ）含量则比对照区的低,稀土处理区茶叶制得的ＲＥＥ－ＴＧＰ中Ｌａ含量增加了１９３％;ＲＥＥ－ＴＧＰ具有明显的降血糖效果和增强免疫作用等活性。     

Spectral interferences in the determination of traces of scandium, yttrium and rare earth elements in “pure” rare earth matrices by inductively coupled plasma atomic emission spectrometry: Part VII — Terbium, Dysprosium, Holmium and Thulium

This article is the seventh part of a series of papers discussing the spectral interferences of rare earth elements (REEs) in ICP-AES. Radial viewing 27.12 MHz inductively coupled plasma atomic emission spectrometry (ICP-AES) was used in the determination of scandium, yttrium and rare earth elements in Tb₂O₃, Dy₂O₃, Ho₂O₃ and Tm₂O₃ as “pure” rare earth matrices. The quantification of the interferences in terms of Q-values for line interference Q_I(_a) and wing background interference Q_W(Δλ_a) were used in accordance with Boumans and Vrakking [Spectrochim. Acta Part B 43 (1988) 69]. The “best” analysis lines from point of view of spectral interferences were selected. The true detection limits by using the “best” analysis lines were calculated.     

交流电弧中共存稀土元素对光谱线强度影响的研究

本工作较系统地研究了在交流电弧中不同量的共存稀土元素镝、钬，饵，铥和镱对某些被测稀土元素光谱线强度的影响。用交流电弧激发溶液干渣样品，其样品是在固定量的被测元素溶液中各自分别加入不同量的共存元素镝、钬、铒、铥和镱，摄谱后测量各被测元素的光谱线强度对共存元素在溶液中各个不同浓度作关系曲线。