光电直读光谱法测定高速工具钢中多元素

利用美国贝尔德公司生产的ＢＡＩＲＤＳＰＥＣＴＲＯＶＡＣ２０００（ＤＶ－５，ＨＲ－４００光源）光电直读光谱仪测定高速工具钢（Ｗ１８Ｃｒ４Ｖ）中硅，锰，磷，硫，铬，钒，镍，钨和钼，以铁元素做内标，对谱线进行基体和干扰校正，所得分析结果基本与标准值一致，其相对标准偏差为０．２％～５．６％。     

ICP-AES 法测定 RZnAl5RE 合金中的镧、铈、铁、铝、铅、镉

采用ＩＣＰ－ＡＥＳ测定了ＲＺｎＡｌ５ＲＥ合金中的Ｌａ、Ｃｅ、Ｆ３、Ａｌ、Ｐｂ、ＣＤ元素含量。考察了基体及无机酸浓度对６种元素线强度的影响。选择了仪器工作条件,检出限在０．０３～１．００μｇ／Ｌ之间,加标回收率为９３％～１０８％,相对标准偏差小于１２．６８％（ｎ＝１０）。     

聚乙烯吡咯啉酮对稀土变色酸双偶氮类试剂显色反应的褪色作用

研究了非离子型表面活性剂聚乙烯吡咯啉酮（ＰＶＰ）、（ＮＨ４）２ＳＯ４对ＲＥ（Ⅲ）、Ｆｅ（Ⅲ）、Ｚｒ（Ⅳ）、Ｔｈ（Ⅳ）、Ｃｕ（Ⅱ）等离子与变色酸双偶氮类试剂显色反应的影响。建立了大量稀土存在下测定微量Ｆｅ（Ⅲ）的新方法。纯稀土中Ｆｅ（Ⅲ）的测定，回收率在９８．０％～１０１．０％；对矿样测定，６次测定ＲＳＤ为１．７９％。     

稀土取代的复合氧化物Eu_（0．5）RE_（0．5）Fe_（0．5）Mn_（0．

利用固相反应合成了稀土取代的复合氧化物Ｅｕ_（０．５）ＲＥ_（０．５）Ｆｅ_（０．５）Ｍｎ_（０．５）Ｏ_３（ＲＥ＝Ｌａ，Ｐｒ，Ｎｄ，Ｓｍ，Ｇｄ，Ｔｂ，Ｄｙ，Ｈｏ，Ｅｒ，Ｔｍ，Ｙｂ）．测量了这些化合物的ＸＲＤ和ＸＰＳ谱。在ＸＰＳ研究中发现，稀土取代而使稀土元素本身的结合能相对于其倍半氧化物中的有所降低；在取代的复合氧化物中，随着ＲＥ离子半径的减小，Ｆｅ、Ｍｎ的结合能随之增加。     

示波极谱法快速测定食品用橡胶制品,铝制品中的锌

根据在０．０６８￣０．２３８ｍｏｌ／Ｌ乙酸底液中,锌在滴汞电极上产生一灵敏的极谱还原波,峰电位（Ｅ）为－１．０９Ｖ（ｖｓ,ＳＣＥ）建立了单扫示波极谱法,用于快速测定食品用橡胶制品,铝制品中的锌,该法的回收率为９０．６％￣１０６％,相对标准偏差（ＲＳＤ）为１．０％￣４．３％。     

一种在线液—液萃取微型多用分相器的设计和应用：IV.流动注射液— …

设计了在线液－液萃取多用重分布相器及相应流动注射流路系统与ＩＣＰ－ＡＥＳ法联用。具有良好的分析性能，通过对矿石中某些重稀土元素在硝酸介质中被ＴＢＰ萃取的应用研究表明钇，镱，铒的检出限（３σ）分别为６．８ｎｇ／ｍＬ，０．２ｎｇ／ｍＬ和１．５ｎｇ／ｍＬ，精密度（ＲＳＤ％）分别为０．２４，０．４７和１．８，进样频率为２５－３０个／ｈ。     

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。     

新型液晶／高聚物复合富氧膜的富氧性能及结构表征Ⅰ．液晶／高聚物复合膜的富氧性能研究

研究用烃橡胶（ＳＢＲ、ＰＢ）和聚二甲基硅氧烷（ＰＤＭＳ）分散α，ω－对乙氧羰氧基苯甲酸聚乙二醇酯（ＰＥＥＣＢ）而得到聚合物分散液晶复合膜（ＰＤＬＣＭ）．用这种复合膜进行富氧分离，当ＰＥＥＣＢ－４．０５（４．０５为聚醚软段的数均聚合度ＤＰ）的含量超过某一临界值（约２３．０％ｗｔ）时，室温下ＳＢＲ／ＰＥＥＣＢ－４．０５／ＰＤＭＳ体系膜的氧气透过系数Ｐｏ２值达７０～６３４ｂａｒｒｅｒ），增加约６０倍，分离系数仍较高（αｏ２／Ｎ２＝３．４７～２．５９）．考察了各种影响因素对膜透气性能的影响．     

一种在线液-液萃取微型多用分相器的设计和应用 Ⅳ.流动注射液-液萃取电感耦合等离子体原子发射光谱法测定矿石中稀土元素

设计了在线液－液萃取多用重力分相器及相应流动注射流路系统与ＩＣＰ－ＡＥＳ法联用，具有良好的分析性能．通过对矿石中某些重稀土元素在硝酸介质中被ＴＢＰ萃取的应用研究表明钇、镱、铒的检出限（３σ）分别为：６．８ｎｇ／ｍＬ、０．２ｎｇ／ｍＬ和１．５ｎｇ／ｍＬ．精密度（ＲＳＤ％）分别为０．２４、０．４７和１．８．进样频率为２５～３０个／ｈ．     

注射用舒尔哌酮的高效液相色谱分析

建立了高效液相色谱法分离与测定复方制剂舒尔哌酮中斯巴坦及头孢哌酮的含量。采用Ｃ_（１８），１０μｍ，４．６ｍｍ×２５０ｍｍ（大连化物所Ｓｐｈｅｒｉｓｏｒｂ）柱，以０．２５％三乙胺溶液（用磷酸调ｐＨ６．０）＋乙腈（８６．５＋１３．５）为流动相，在紫外检测器２１０ｎｍ波长处进行检测，线性范围０．０５～０．６ｍｇ／ｍＬ，γ＝０．９９９９（ｎ＝５），精密度：斯巴坦及头孢哌酮的日内平均ＲＳＤ分别为０．６％及０．７５％（ｎ＝１８），日间平均ＲＳＤ分别为０．８６％及０．８７％（ｎ＝１２）。     

阳离子交换树脂分离富集-ICP-AES法测定地质样品中15种稀土元素

样品用四酸(盐酸+硝酸+高氯酸+氢氟酸)溶解,经阳离子交换树脂分离富集后用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定其中的15种的稀土元素。选用HCl(1.2mol/L)作平衡液和淋洗液,HCl(4.0mol/L)作洗脱液进行实验,测量时选择最佳的分析谱线从而避开杂质峰的干扰。各稀土元素的方法检出限均低于1.5μg/g,相对标准偏差小于11%。经标准物质验证结果可靠,适合地质样品中稀土元素的同时测量。     

ICP-AES直接测定氯化稀土中稀土元素

以电荷耦合器件为检测器的ＩＣＰ－ＡＥＳ光谱仪直接测定了混合稀土中的十五种稀土元素。考察十五种稀土元素的五十余条灵敏线的谱图,分析稀土元素之间的干扰并选取了合适的分析线,利用多组分谱图拟合方法扣除了空白及稀土元素间的谱线干扰,试验了最佳的溶液酸度及仪器工作参数,方法回收率为９８．４％￣１０１．７％,相对标准偏差小于２％。     

电荷注入检测器电感耦合等离子体光谱仪测定铂族元素的性能

研究了用电荷注入检测器等离子体光谱仪测定铂族元素的分析性能。结果表明铂族元素有较好的检出限和10^4以上的线性动态范围，铂族元素间光谱干扰很少，在元素浓度＞1mg/L时测量精度可优于1％，钠对铂族元素的影响是轻微的。     

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.     

热带海洋生物稀土元素生态化学特征分析研究

于中国南海南沙海域采集了30种鱼类、5种贝类和4种甲壳类热带海洋生物,以HNO3-H2 O2为消解体系,利用微波消解进行前处理,并用电感耦合等离子体质谱测定了生物体中稀土元素( Rare earth elements, REE)的含量,分析了稀土元素的生态化学特征。结果表明,微波消解-ICP-MS方法测定稀土元素,各元素的线性关系良好(r=0.9997~1.0000),检出限可达ng/L,准确度高和精密度较好,相对标准偏差(RSD, n=3)<5.0%,各稀土元素回收率在91.5%~106.7%之间。鱼类、贝类和甲壳类生物样品中稀土总量(∑REE)变化范围分别为5.02~34.8μg/kg,30.4~1481μg/kg和103~863μg/kg,3类生物对各稀土元素的富集平均含量为甲壳类>贝类>鱼类,14种稀土元素在鱼类/贝类/甲壳类内含量存在明显正相关性(r>0.80);生物体内轻稀土元素( La~Eu)含量高于重稀土元素( Gd~Lu)含量,从稀土配分模式看出,鱼类/贝类/甲壳类中REE分布模式基本一致, Gd均出现负异常,轻重稀土元素之间有明显的分馏;生物体中δEu值出现负异常,δEu值与相应海域沉积物中δEu值相近,而δCe值出现正异常;同时研究了稀土元素在生物体中的富集和沉积物沉降过程中相关性等。本研究得出的关于热带海洋鱼类/贝类/甲壳类稀土元素的含量和分配规律,可为研究南海水体环境中稀土元素的含量水平和迁移富集提供基础资料。     

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.     

An ICP-AES method for the determination of heavy rare earth elements (Eu-Lu) in high purity yttrium oxide

Traces of heavy rare earth elements (Eu-Lu) were determined in high purity yttrium oxide by inductively coupled plasma atomic emission spectrometry. The yttrium oxide samples were dissolved in nitric acid and the solutions analyzed with a plasma produced by a 56 MHz RF generator at an output power of 1.5 kW. Using a high resolution sequential monochromator, interference-free spectral lines for Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu could be found for calibration. The detection limits for the above elements have been found to be slightly higher in the presence of yttrium matrix, than in aqueous solution. This could be attributed to background enhancements due to the presence of yttrium. The mean RSD of the method varied between 2.3% and 6.3% in the concentration range 0.01 and 0.5 g/ml. The percentage recovery ranged from 84 to 106 for the different rare earth elements.     

离子吸附型稀土矿中浸出相稀土元素含量的浸取方法研究

将风化壳离子吸附型稀土矿原矿样品加工至0.149 mm,使用35 g/L硫酸铵溶液(pH为4.0)作为浸取剂,提取浸出相稀土元素. 考察了提取浸出相稀土元素时,样品粒度、浸取剂浓度及用量、浸取剂酸度、浸取方式、浸取时间等条件的影响,确定最佳试验条件,利用电感耦合等离子体质谱法(ICP-MS)测定样品溶液中浸出相稀土的总量及分量. 试验结果表明:采用静态浸取方式浸取30 min,固液比为1∶10,能有效提取浸出相稀土元素. 各稀土元素的方法检出限为0.006 5~0.160 0 μg/g,测定下限为0.035~0.520 μg/g,精密度为1.34%~5.65%,加标回收率为96.0%~102.0%. 结果准确可靠,方法完全满足矿产地质勘查要求.     

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。     

Determination of Rare Earth Elements in Acid Mine Drainage by Inductively Coupled Plasma Mass Spectrometry

A method was developed for the direct determination of 14 naturally occuring rare earth elements (REE, La–Lu) by means of inductively coupled plasma mass spectrometry in seepage waters caused by acid mine drainage. The analytical procedure includes the additional determination of oxide and hydroxide formation by Ba and REE. The determined polyatomic ion formation can be used to correct spectral interferences of oxides and hydroxides of Ba and the light REE on middle and heavy REE. The total REE content in the acidic seepage waters investigated is up to 220µgL^–1. The concentration of the REE normalized to Post Archean Australian Shale (PAAS) is shown, and fractionation of the REE is discussed. The PAAS-normalized REE-patterns feature an enrichment of middle and heavy REE as opposed to the light ones. For one seepage water sampled over a period of about half a year, the REE patterns show very high reproducibility. The accuracy of the method was demonstrated by the analysis of two water samples containing certified concentrations of REE.