Determination of trace elements in maifanite by outer cover electrode atomic emission spectrometry

Maifanite is a nature medicinal stone used in many fields for long time. Theresearch on it showed that there are many trace elements in maifanite. In this paper, 36 traceelements in maifanite were determined by outer cover electrode atomic emission spectrometry, and thedetermination conditions were studied systematically. The results show that the concentrations ofelements, which are beneficial to human health, are higher, and the elements harmful to peoplehealth such as As, Cd, Hg, Cr, and Pb are tiny in maifanite. The precision and the accuracy werealso discussed.

Simultaneous determination of some trace metal impurities in high-purity sodium tungstate using coprecipitation and inductively coupled plasma atomic emission spectrometry

A method based on the combination of coprecipitation with inductively coupledplasma atomic emission spectrometry (ICP-AES) was developed for the determination of impurities inhigh-purity sodium tungstate. Six elements (Co, Cu, Fe, Mn, Ni, and Pb) were coprecipitated bylanthanum hydroxide so as to be concentrated and separated from the tungsten matrix. Effects of somefactors on the recoveries of the analytes and on the residual amount of sodium tungstate wereinvestigated, and the optimum conditions for the coprecipitation were proposed. Matrix-matchingcalibration curve method was used for the analysis. It is shown that the elements mentioned abovecan be quantitatively recovered. The detection limits for Co, Cu, Fe, Mn, Ni, and Pb are 0.07, 0.4,0.2, 0.1, 0.6, and 1.3 μg·g^(-1), respectively. The recoveries vary from 92.5% to 108%, and therelative standard deviations (RSDs) are in the range of 3.1%-5.5%.

电感耦合等离子体原子发射光谱(ICP-AES)法测定真空精炼镁合金物料中铁、铜、镍

真空精炼是目前镁金属提纯的重要工艺,工艺原料及真空精炼提纯镁金属过程残留物中Fe、Cu、Ni含量的准确测定对工艺参数的优化及调整具有重要的指导作用。传统测定方法中以邻二氮杂菲分光光度法、新亚铜灵分光光度法、丁二酮肟分光光度法测定三种元素含量,结果准确,但操作繁琐,周期较长,难以满足工业生产中高效、快速测定的需要,且方法中所需的有机萃取剂对环境污染较大。选择电感耦合等离子体发射光谱(ICP-AES)法测定真空蒸馏精炼镁合金物料中Fe、Cu、Ni,系统探究溶解酸、溶解温度、溶解时间对物料溶解和测定的影响,选择盐酸(1+1)和过氧化氢溶解体系,200℃加热条件下反应20 min为最佳消解镁合金原料条件;选择王水溶解体系,200℃加热条件下反应25 min为真空精炼残留物最佳溶解条件。并探讨ICP-AES测定过程中各元素的检出限和测定下限以及共存元素的干扰情况,建立了ICP-AES法测定真空精炼提纯镁合金物料的方法。测定结果的相对标准偏差(RSD,n=11)为Fe 5.9%~11.5%、Cu 2.6%~11.8%、Ni 3.4%~11.5%,各元素加标回收率为Fe 96.4%~102%、Cu 101%~108%、Ni 103%~105%;按照建立的方法测定镁合金原料、真空精炼残留物中的铁、铜、镍,并与国家标准方法测定结果进行对比,结果相一致。实现了ICP-AES法快速、准确测定真空蒸馏精炼镁合金物料中铁、铜、镍含量,对及时、高效、准确评估真空精炼提纯镁工艺及产品具有重要意义。

电感耦合等离子体原子发射光谱(ICP-AES)法测定石煤钒矿石中钒、铁、钛的含量

研究一种快速准确测定石煤钒矿石中钒、铁、钛含量的方法对石煤钒矿检测行业的发展和石煤钒矿资源的开发利用、综合评价具有重要的意义。试样经过氧化钠在650℃完全熔融后保持1~3 min,取出冷却,热水浸提,盐酸酸化,定容稀释,选择V 292.402 nm、Fe 259.940 nm、Ti 334.941 nm为分析谱线,利用电感耦合等离子体原子发射光谱法(ICP-AES),建立了石煤钒矿石中同时测定钒、铁、钛含量的方法。优化了钒、铁、钛元素的分析谱线和背景校正模式,采用全程序样品空白稀释配制的校准曲线消除盐度钠基影响;研究了坩埚、熔剂种类、直接碱熔与灼烧-碱熔前处理方式、酸度效应的影响。结果表明:方法检出限为0.009%~0.019%,定量限为0.027%~0.057%;铁、钛、钒3种元素浓度在0.10~30.0μg/mL时,校准曲线线性回归方程的相关系数均大于0.9999;采用国家一级标准物质(GBW07876、GBW07877、GBW07878)进行验证,相对标准偏差(RSD,n=12)为0.49%~0.87%,且测定值与标准值吻合。方法具有快速简便、精密度好、准确度高、同时测定钒、铁、钛等优点,满足石煤钒矿石化学分析检测需求,且可为石煤钒矿化学分析标准方法的建立提供技术支撑。

Determination of Ni, Ca, Mg, Cu and Pb in Wolfram byInductively Coupled Plasma Atomic Emission Spectrometry

The method for the determination of Ni, Ca, Mg, Cu and Pb in wolfram wire by ICP AES was studied. Results showed that perhydrol affects the intensities of elements (Ni, Ca, Mg, Cu, Pb) and this effect can be compensated by internal reference element. It is also showed that the stability of plasma caused by perhydrol matrix was effectively improved. The replicate experiment and recovery experiment revealed perfect precision and accuracy. Results got by two methods were just the same.

Determination of Carbon by Means of Microwave Plasma Torch Atomic Emission Spectrometry

The determination of carbon by means of microwave plasma torch atomic emission spectrometry(MPT-AES) was studied. Aqueous samples were introduced with a pneumatic nebulization system. The detection limit for carbon was 0. 047μg/mL.The method was applied to the analysis for tap water and results were satisfactory.

A Study on Determination of Some Trace Nonmetals by Microwave Induced Plasma Atomic Emission Spectrometry

In general, atomic emission spectrometry (AES) is an excellent technique for determination of metal elements. However, its capability of determining nonmetals has not been developed well. The major reasons are the resonance lines of most nonmetals lie in the vacuum ultraviolet spectral region and the ionic lines of these elements are difficult to be used because the ionization potentials of the elements are very high. And furthermore only He plasma can efficiently excit those ionic resonance lines. The practical application of HeICP-AES to determining the nonmetals is also difficult because its operating and perchace costs are very high. In contrast to HeICPAES, the costs of He microwave induced plasma (MIP)-AES are relatively low, HeMIP has a high excitation capability which can excite ionic lines of various nonmetals and the nonmetals can be determined by HeMIP-AES with a high sensitivity.

Studies on Combination of Flow Injection and Microwave Plasma Torch-Atomic Emission Spectrometry

Although the flow injection(FI) as a sample introduction technique has been extensively applied to atomic spectrometry, such as ICP-AES and AAS, very little has been done so far on coupling FI to microwave plasma systems. Gehlausen et al. determined aqueous fluorine by coupling flow injection analysis (FIA) with HeMIP

On Line Anion Exchange Preconcentration in Microwave Plasma Torch Atomic Emission Spectrometry

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CORRECTION OF WING INTERFERENCE WITH KALMAN FILTERING IN INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETRY

A Kalman filter was developed for correction of wing interference in ICP-AES.Modeling wing interference theoretically instead of experimentally, the filter can compensate the shift in wavelength position in scans, and therefore reduce the effect of the interference on detection limit.

电感耦合等离子体原子发射光谱(ICP-AES)法与EDTA滴定法联用测定含白云岩矿石中氟化钙

氟化钙的测定目前较多采用的是国家标准方法GB/T 5195.1—2017和DZG93-05非金属矿萤石分析规程两种方法,前者测定范围≥60%,后者测定范围>3%。两种方法各有优缺点,然而却都无法满足矿石中含有白云岩时的测定。对于萤石矿与白云岩共存样品,直接采用国家标准方法,测定结果偏高,行业标准方法测定的精密度和准确度也很难达到要求。通过对方法进行优化,在样品中加入含钙冰乙酸分离碳酸钙,过滤残渣用混合酸分解后,直接取澄清液在Ca 317.933 nm处,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定氟化钙含量,根据测定结果,将氟化钙质量分数大于15%的样品用EDTA滴定法再次测定。按照实验方法测定实际样品,两种方法测定结果的相对标准偏差(RSD,n=11)分别为1.9%和0.77%,加标回收率为97.9%~102%,可满足含白云岩矿石中氟化钙的准确测定。

湿法消解-电感耦合等离子体原子发射光谱(ICP-AES)法测定水凝胶中Mg的含量

为了准确测定水凝胶样品中的金属元素含量,以Mg为例,通过优化电感耦合等离子体原子发射光谱(ICP-AES)仪参数,考察硝酸及硝酸-高氯酸湿法消解以及硝酸-微波消解法对于样品消解程度的不同,建立了湿法消解-ICP-AES法测定水凝胶中Mg绝对含量的方法。结果表明,在110℃下用硝酸消解2 h与硝酸-高氯酸(1∶1)以及硝酸-微波消解得到的溶液相比,Mg含量几乎没有明显差别。在选定条件下,方法的日内和日间精密度良好,相对标准偏差(RSD,n=3)分别为0.38%和1.2%;加标回收率为97.6%~98.2%。方法准确、适用、可靠,适用于水凝胶中Mg的绝对含量测定,可为水凝胶中金属元素的定量分析提供一种借鉴。

电感耦合等离子体原子发射光谱法(ICP-AES)测定GH3128中钨、钼、铬、锆的含量

研究了快速准确测定GH3128中4种元素(W,Mo,Cr,Zr)的分析方法。样品利用盐酸、硝酸低温加热进行溶解。采用电感耦合等离子体原子发射光谱法(ICP-AES)测定所得溶液中4种元素的含量,选择的分析谱线分别为W207.912 nm、Mo202.031 nm、Cr284.325 nm、Zr343.823 nm,选择了合适的光谱仪工作参数等检测条件。采用基体匹配法消除基体组分的影响制作工作曲线。各元素检出限(3s)为6.3、5.6、2.5、1.9μg·m L^(-1)之间,相对标准偏差(n=10)在1.1%~3.1%之间。按上述方法分析GH3128标准物质,测定值与认定值一致。

碱熔-标准物质法-电感耦合等离子体原子发射光谱(ICP-AES)法测定硅酸盐岩中10种主量元素

硅酸盐岩元素的准确测定是其地球化学分析研究的基础,其主量元素含量通常可以采用电感耦合等离子体原子发射光谱(ICP-AES)法测定,但其测定方法的系统性研究相对缺乏,尤其是样品前处理和基体干扰的有效消除两方面。前处理过程中,考察不同熔剂用量对硅酸盐岩样品的分解能力,发现当熔剂与样品比例达到6∶1后,熔珠为纯色透明,经稀硝酸提取后溶液澄清,确定了硅酸盐岩前处理时熔剂与样品的最佳配比。测定过程中,通过考察基体匹配法和标准物质法两种基体干扰消除方法对测定结果的影响,发现当采用与岩性一致或者接近的标准物质绘制校准工作曲线时,基体干扰消除效果更好,更适用于测定硅酸盐岩10种主量元素含量。据此,建立了硅酸盐岩经偏硼酸锂熔融,稀硝酸振荡提取处理,以标准物质法绘制校准工作曲线,采用ICP-AES法同时测定SiO_(2)、Fe_(2)O_(3)、Al_(2)O_(3)、CaO、K_(2)O、MgO、Na_(2)O、TiO_(2)、P_(2)O_(5)、MnO 10种成分含量的方法。对岩石标准物质GBW07107进行分析测定,方法的相对标准偏差(RSD)为0.17%~0.75%,方法检出限为0.001%~0.016%,满足硅酸盐岩样品元素定量分析的要求,而且操作简单快速,环境污染小,适用于大批量样品分析。

ICP-AES测定稀土强化黑色二氧化钛中镧铈钇的方法研究

采用HF-HNO_(3)混合酸作为消解试剂,选择Y(360.073 nm)、La(408.672 nm)、Ce(413.380 nm)为分析线,建立了电感耦合等离子体原子发射光谱法测定稀土强化黑色二氧化钛中La、Ce、Y这3种稀土元素的方法。通过系列实验,探讨了样品消解条件、基体效应、共存元素干扰,分析谱线选择等对待测元素测定的影响。结果表明:当试样溶液中待测元素浓度低于5.0 mg/L时,基体钛对待测元素有影响,须采用基体匹配消除影响;共存元素干扰实验表明,当各共存元素溶液低于200 mg/L时,互不干扰测定。各元素方法检出限如下:La为0.0009%,Ce为0.0013%,Y为0.0004%,回收率为97.8%~102.6%,变异系数CV值为0.56%~3.19%;该方法用于测定稀土强化黑色二氧化钛中各稀土元素测定结果与理论值基本一致,测定结果准确可靠。

ICP-AES法测定焊锡中金属银的研究分析

本文综述了电感耦合等离子体-原子发射光谱法在测定焊锡中金属银元素的工作原理,文章从待测样品前处理方法、样品制备过程、实验条件、以及数据分析方法四个方面分析了影响电感耦合等离子体-原子发射光谱法检测结果准确度的因素,并提出了相应的提高准确度的改进措施,并在高级算法方面对电感耦合等离子体-原子发射光谱法测定焊锡中金属银的未来发展进行了展望。

ICP-AES法检测脂肪乳注射液中铝元素杂质的含量

目的:建立测定脂肪乳注射液中铝元素杂质含量的电感耦合等离子原子发射光谱(ICP-AES)法。方法:样品稀释后,采用电感耦合等离子原子发射光谱法进行测定,以标准曲线法计算铝元素含量。结果:铝元素在0~200μg·L^(-1)范围内线性关系良好(r=0.99993),重复性试验结果RSD为2.0%,方法检出限为1.22μg·L^(-1),方法定量限为4.07μg·L^(-1),加样回收率平均值为107.7%,RSD为2.7%(n=6)。结论:该方法操作简单、灵敏,准确度高、重现性好,适用于脂肪乳注射液中铝元素杂质含量的测定。

ICP-AES法测定含铝预熔性渣洗料中钙、镁、硅、铝氧化物

研究使用电感耦合等离子体发射光谱法测定炼钢含铝预熔性渣洗料中钙、镁、硅、铝氧化物的分析条件以及处理样品的方式方法,为便于区别金属铝和三氧化二铝,创建了一种新型的仪器分析方法。由于试样中金属铝的存在,采用先酸溶再碱融的处理方式,并采用配置相似基体的方法消除基体干扰。研究了渣洗料的溶样过程、仪器分析参数的选择、基体的干扰消除等对分析结果影响,在优化仪器分析参数和分解试样实验过程中,试样分析结果相对标准偏差远小于1.0%,分析结果准确度和精密度都很高。因此,该方法可取代化学分析法,是一种准确、快速的仪器分析方法。

A Perspective of Laser Sampling for Inductively Coupled Plasma-Atomic Emission Spectro metry for Rock and Mineral Analysis

The development of laser sampling for optical emission spectrometry is reviewed . Advantages and limitations of pulsed laser sampling are compared with those of continuous laser sampling . A novel method of laser sampling of liquid samples for inductively coupled plasma -atomic emission spectrometry has been proposed , and its analytical performance investigated.Experimental results showed that,as a method of sample introduction , laser vaporization of liquid samples enjoyed certain advantages , e.g.,much higher sensitivity, much lower detection limit and reduced sample volume , over solution nebulization . A perspective of the application of laser sampling-inductively coupled plasma - actomic emission spectrometry for rock and mineral analysis is estimated as well.

ICP-AES法测定天水核桃青龙衣及4种特色水果中矿质元素的含量

核桃青龙衣是核桃的外层果皮,内含丰富的人体必需的微量元素成分,具有较高的药用价值。本实验选取了天水特色坚果核桃的青龙衣为研究对象,经过微波消解仪对试样进行了前期预处理,再利用电感耦合等离子体-原子发射光谱法(Inductively Coupled Plasma-Atomic Emission Spectrometry,ICP-AES)测定天水核桃青龙衣以及具有地方特色的4种水果中的Zn、Fe、Mn、Ca、Na、Cu、K和Mg 8种矿质元素的含量。结果表明,天水核桃青龙衣中钾、钙和镁3种矿质元素含量远远高于4种地产特色水果,为利用天水核桃副产物开发营养保健功能性产品提供了技术支撑。