载PMBP泡沫塑料吸附粉末进样电感耦合高频等离子体光谱法测定岩石中稀土元素

以溶液进样电感耦合高频等离子体光谱法测定单一稀土元素已有报导。为了防止溶液进样系统堵塞,提高分析灵敏度,降低氩气的消耗量和酸性溶液对摄谱仪尤其是对光栅的腐蚀,本文试验了载PMBP泡沫塑料吸附,粉末进样电感耦合高频等离子体光谱法测定岩石中15个稀土元素。采用本法15个单一稀土元素含量在0.0001-0.03％时,经25次测定相对标准偏差为4.8-12.1％。本法具有相对灵敏度高、准确度好、成本低等优点,经一年多生     

微波消解样品-电感耦合等离子体质谱法测定植物灰分中微量元素

应用电感耦合等离子体质谱法(ICP-MS)同时测定植物灰分中21种微量元素和15种稀土元素.用微波消解样品,对微波消解植物灰分样品的条件进行了试验.其优选微波消解条件为:微波压力为2 MPa,消解时间为10 min,以硝酸、盐酸、氢氟酸、高氯酸(体积比为6比2比1比1)的混合酸消解样品,对0.100 0 g植物标准物质(GBW 07603)进行10次平行测定,微量元素测定结果的相对标准偏差(n=10)在0.87%～5.96%之间,稀土元素测定结果的相对标准偏差(n=10)在2.14%～8.00%之间.     

电感耦合等离子体质谱法测定高岭土中的15种稀土元素

样品经硝酸-氢氟酸-硫酸三酸消解后,以103 Rh为内标,采用电感耦合等离子体质谱法测定高岭土中的15种稀土元素。采用标准物质制备工作溶液绘制校正工作曲线消除质谱干扰,通过控制样品的稀释因子消除非质谱干扰。各元素的线性范围为0.20~200mg·kg~(-1),检出限在0.03~0.09 mg·kg~(-1)之间。方法用于分析岩石标准物质,测定值与认定值的相对误差在-6.7%~8.3%之间,相对标准偏差(n=5)在0.70%~5.9%之间。实际样品中15种稀土元素的测定值的相对标准偏差在3.8%~12%之间。     

电感耦合等离子体质谱法测定高岭土中的15种稀土元素北大核心CSCD

样品经硝酸-氢氟酸-硫酸三酸消解后,以103 Rh为内标,采用电感耦合等离子体质谱法测定高岭土中的15种稀土元素。采用标准物质制备工作溶液绘制校正工作曲线消除质谱干扰,通过控制样品的稀释因子消除非质谱干扰。各元素的线性范围为0.20~200mg·kg^(-1),检出限在0.03~0.09 mg·kg^(-1)之间。方法用于分析岩石标准物质,测定值与认定值的相对误差在-6.7%~8.3%之间,相对标准偏差(n=5)在0.70%~5.9%之间。实际样品中15种稀土元素的测定值的相对标准偏差在3.8%~12%之间。     

碱熔-电感耦合等离子体质谱法(ICP-MS)直接测定高纯稀土荧光粉中微量杂质元素

建立了一种碱熔样-电感耦合等离子体质谱法(ICP-MS)直接分析稀土荧光粉中微量杂质元素(非稀土杂质和稀土杂质元素)的新方法。采用Na2CO3-H3BO3混合熔剂对样品进行分解,熔块由HNO3(2+3)提取后定容,优化了最佳的熔融温度和熔样时间。用ICP-MS标准曲线法直接测定。方法的检出限非稀土元素为0.007~0.952μg/g,稀土元素为0.001~0.057μg/g,相对标准偏差(RSD)12%。方法预处理简单、检出限低、重现性好,为高纯稀土荧光粉成品的质量控制提供了可靠的分析手段。     

超痕量稀土元素测定的等离子体质谱法研究

研究了超声波雾化去溶进样电感耦合等离子体质谱法(ICP-MS)测定地质样品中超痕量稀土元素含量的方法,稀土元素的检出限低达0.3～4pg/ml,能检测稀土总量为ng/g级的固体样品中的15个稀土分量。     

落叶松与白桦树中微量及稀土元素的ICP-MS检测方法研究

利用微波消解法处理植物灰分样品,讨论了混合酸组成、混酸配比、固液比和微波消解时间对样品制备结果的影响.优选微波消解方案:微波压力(MPa)0.5、1.0、1.5、2.0,消解时间(min)4、3、3、10的微波程序,混合酸体系HNO3-HCl-HF-HClO4(体积比为6 ∶ 2 ∶ 1 ∶ 1).在此条件下, 进行了方法准确度实验和测量结果重复性实验, 该方法经植物国家标准物质(GBW07603)验证,微量元素测试结果的相对误差为1.06% ～5.60%,相对标准偏差为0.87% ～5.25%;稀土元素测试结果的相对误差为1.82% ～10.2%,相对标准偏差为2.14% ～8.00%.应用电感耦合等离子体质谱法(ICP-MS)同时测定植物灰分中21种微量元素和15种稀土元素.结果表明, 微波消解法处理植物灰分样品, 具有快速、简便、节省试剂、消解完全等特点, 测定结果的准确度和精密度令人满意.     

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。     

193nm激光器与电感耦合等离子体质谱仪联用条件优化研究

激光剥蚀电感耦合等离子体质谱仪( LA-ICP-MS)是采用激光剥蚀固体进样方式构建的新型等离子体质谱分析仪器.由于受激光产生原理-“脉冲式激发”的限制,样品的剥蚀进样过程属于间歇模式.因而激光剥蚀系统与电感耦合等离子体质谱仪联机分析结果的相对标准偏差( RSD)通常达10％以上,影响数据的分析精度.本设计在激光剥蚀系...     

萃取分离电感耦合等离子体原子发射光谱法测定钢中的微量稀土元素

本文采用苯甲酰苯胲(BPHA)-甲基异丁基酮(MIBK)溶剂萃取方法将钢中基体元素Fe,Ti,Mo,V等大量非稀土元素萃入有机相中,稀土元素留于水溶液中.由电感耦合等离子体原子发射光谱(ICP-AES)仪直接测定水溶液中的微量稀土元素La,Ce,Pr,Nd.Sm,Y和Gd,实验结果与推荐值基本相符,方法的回收率为96％～108％,相对标准偏差低于5％.     

电感耦合等离子体质谱法测定三水铝土矿中的15种有效稀土元素

建立电感耦合等离子体质谱法测定三水铝土矿中15种有效稀土元素的分析方法。参考三水铝土矿中有效铝的概念,提出了有效稀土元素的概念,并对三水铝土矿中稀土元素的回收利用的可行性进行了评价。模拟低温拜耳法生产氧化铝的工艺,对三水铝土矿中稀土元素溶出过程中的氢氧化钠浓度、溶出温度及时间等条件进行了试验,采用90 g/L氢氧化钠结合微波消解技术对三水铝土矿进行分解,用ICP-MS法测定有效稀土元素,有效稀土元素测定结果的相对标准偏差为0.92%~7.40%(n=7),回收率为98.6%~101.2%。该方法可用于测定三水铝土矿中有效稀土元素,能够对三水铝土矿中稀土元素的回收利用价值进行评价。     

茶叶中稀土元素的萃取分离-ICP-AES法测定

采用1-苯基-3-甲基-4-苯甲酰基-5-吡唑酮(PMBP)苯溶液萃取分离-ICP-AES法同时测定茶叶中15种稀土元素,消除了基体的干扰,并对样品前处理方法、萃取分离条件进行了考查.方法回收率为: 92.3%～112%,相对标准偏差＜2.5%.在最佳工作条件下,测定了茶叶标准物质(GBW07605)中稀土元素,结果与标准值吻合.     

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.     

Determination of rare earth elements in the biological reference materials Pine Needles and Spruce Needles by neutron activation analysis

Instrumental neutron activation analysis was applied to determine La, Ce, Nd, Sm, Eu, Tb, Yb, Lu and Sc in two biological reference materials: NIST 1575 Pine Needles and BCR-CRM 101 Spruce Needles. The purpose was to contribute to the reference data for these two reference materials. The results were obtained with a good precision (relative standard deviations less than 15%). For the Pine Needles reference material there are already some proposed values and our results showed, in general, a good agreement with the data published. The contribution of uranium fission products to La, Ce, Nd and Sm was evaluated and considered in the determination of these elements. Interferences in the determination of rare earth elements in biological materials are also discussed.     

Direct determination of trace rare earth elements in high purity Y2O3 using fluorination assisted electrothermal vaporization inductively coupled plasma atomic emission spectrometry with slurry sampling

A new method for the determination of trace amounts of 14 rare earth elements in high purity Y₂O₃ using fluorination assisted electrothermal vaporization inductively coupled plasma atomic emission spectrometry with slurry sampling was developed. A polytetrafluoroethylene (PTFE) emulsion was used as a fluorinating reagent to promote the vaporization of the analytes from graphite furnace. The main factors affecting analytical signals were investigated systematically. The interference of matrix could be minimized in the presence of PTFE. Under optimum conditions, the detection limits for rare earth elements were 0.032 ng～2.52 ng and the relative standard deviations were in the range of 1.4% to 4.3%. The proposed method was applied to the direct analysis of high purity Y₂O₃ powder with satisfactory results.     

Determination of the rare earth elements in natural waters by isotope-dilution mass spectrometry

A method is described for the determination of ten rare earth elements (La, Ce, Nd, Sm, Eu, Gd, Dy, Er, Yb, Lu) in natural waters by isotope-dilution mass spectrometry. A 1-l sample is used for sea water, and proportionately less for other natural waters. The rare earth elements are extracted by co-precipitation with hydrated iron (III) oxide and purified on a single cation-exchange column, with hydrochloric and nitric acids as eluents. Final measurements are from a triple Re/ Ta filament in the mass spectrometer, run automatically under computer control. Relative standard deviations are better than 4% for the analysis of standard solutions, with accuracy in the same range. The analytical blank is low ( <0.03 pmol, 4 pg, for Nd) producing a sample/blank concentration ratio greater than 100 for all ten rare earth elements when determined in a 1-l seawater sample. Concentration depth profiles are given for an ocean water and normalised abundance patterns for three natural waters.     

电感耦合等离子体质谱法测定三七粉中痕量稀土

建立电感耦合等离子体质谱法测定三七粉中15种痕量稀土元素的方法。样品以硝酸–过氧化氢–氢氟酸混酸体系进行微波消解,以铑、铼为内标物,在优化后的仪器条件下进行测定。镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥、钇的质量浓度在0.5~50μg/L范围内线性良好,相关系数r^2>0.999 9,检出限分别为3.11,2.32,1.70,2.51,1.84,1.22,1.99,1.46,2.62,2.56,1.27,2.18,1.16,1.66,1.28μg/kg。测定结果的相对标准偏差为1.88%~18.7%(n=6),回收率为86.0%~104.0%。该方法样品处理简单快速,检出限低,准确度和精密度高,适合于三七粉中15种痕量稀土元素的测定。     

Direct determination of trace rare earth elements in high purity Y2O3 using fluorination assisted electrothermal vaporization inductively coupled plasma atomic emission spectrometry with slurry sampling

A new method for the determination of trace amounts of 14 rare earth elements in high purity Y₂O₃ using fluorination assisted electrothermal vaporization inductively coupled plasma atomic emission spectrometry with slurry sampling was developed. A polytetrafluoroethylene (PTFE) emulsion was used as a fluorinating reagent to promote the vaporization of the analytes from graphite furnace. The main factors affecting analytical signals were investigated systematically. The interference of matrix could be minimized in the presence of PTFE. Under optimum conditions, the detection limits for rare earth elements were 0.032 ng∼2.52 ng and the relative standard deviations were in the range of 1.4% to 4.3%. The proposed method was applied to the direct analysis of high purity Y₂O₃ powder with satisfactory results. Received: 19 June 1999 / Revised: 10 December 1999 / Accepted: 16 December 1999     

惰气熔融-红外吸收光谱法测定镧铈稀土钢中氧含量

高品质稀土钢要求进行精确低氧含量控制,而依据现有GB/T11261-2006标准进行氧含量测定,检测结果具有较大的不准确性。本研究以具有不同镧、铈稀土元素含量的稀土钢为对象,以其氧含量精确测定为目标,基于惰气熔融-红外吸收法,开展了分析功率、助熔剂和称样量对镧铈稀土钢中氧含量分析结果的影响研究。结果表明,对于不同镧、铈元素含量的稀土钢,需要采用不同的分析方法：当稀土钢中的镧、铈含量较低时,通过降低分析功率即可较为精确的测定稀土钢中的氧含量;对于镧、铈含量较高的稀土钢,在调控分析功率（分析功率在4000W～4500W）的基础上,需同时采用锡作为助熔剂,并将助熔剂与样品比例设定为1:1（称样量为0.3g～0.6g）,即可实现氧含量的精确测定。精密度验证实验结果显示,采用本研究所建立的方法,氧含量测试结果相对标准偏差（RSD）小于8.0%;采用钢标样进行回收率实验,回收率值在97%～108%,而加标回收率略有升高的原因在于助熔剂Sn降低了合金熔点,使少量难熔氧化物中的氧得到更充分释放。本研究所建立的分析方法可准确测定不同镧、铈元素含量稀土钢中的氧含量。     

Determination of trace rare earth elements by inductively coupled plasma atomic emission spectrometry after preconcentration with multiwalled carbon nanotubes

A new method has been developed for the determination of trace rare earth elements (REEs) in water samples based on preconcentration with a microcolumn packed with multiwalled carbon nanotubes (MWNTs) prior to their determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). The optimum experimental parameters for preconcentration of REEs, such as pH of the sample, sample flow rate and volume, elution solution and interfering ions, have been investigated. The studied REEs ions can be quantitatively retained by MWNTs when the pH exceed 3.0, and then eluted completely with 1.0 mol L⁻¹ HNO₃. The detection limits of this method for REEs was between 3 and 57 ng L⁻¹, and the relative standard deviations (RSDs) for the determination of REEs at 10 ng mL⁻¹ level were found to be less than 6% when processing 100 mL sample solution. The method was validated using a certified reference material, and has been successfully applied for the determination of trace rare earth elements in lake water and synthetic seawater with satisfactory results.