X荧光光谱法测定硫精矿中硫元素

建立波长色散X荧光光谱法测定硫精矿中硫元素的含量。将样品研磨成粒径为75μm粉末,压片压力设置为30 t,保压时间20 s。方法测定硫元素的检出限为3.05μg/g。用该法对10个硫精矿样品中的硫元素进行测定,测定结果与传统化学分析法测定结果相一致,同一样品测定结果的相对标准偏差为0.42%(n=11)。该方法简便、准确,可用于硫精矿中硫元素的快速分析。     

X射线荧光光谱法测定锶铁氧体半成品中铁、锶、硅

将样品在玛瑙研钵中与淀粉混合研磨,然后倒入压样机钢环模具中,在30 t压力下,采用粉末压片制样法压制成型。用X射线荧光光谱法测定锶铁氧体半成品中铁、锶、硅的含量。经试验验证压片时样品与黏合剂淀粉的最佳质量比为5比1。此法用于锶铁氧体半成品样品分析,3种元素的相对标准偏差(n=11)分别为0.06%,0.14%,0.70%,测定值与常规方法测定值相一致。     

X射线荧光光谱法测定农田底泥中8种元素

建立X射线荧光光谱法测定农田底泥样品中砷、铬、铜、锰、镍、铅、锌、铁8种元素含量的分析方法.以塑料环粉末压片法制样,选用50种土壤、水系沉积物标准物质拟合校准曲线,探讨各元素的测定条件.当待测样品与建立校准曲线的标准样品粒径均小于75μm时,能够有效减少矿物效应和粒度效应的影响,从而提高检测准确度;各元素在各自的含量范...     

X射线荧光光谱法测定新研制土壤标准物质中11种元素的含量北大核心CSCD

用粉末压样机将5.0 g经105℃烘干的样品制成样片,采用X射线荧光光谱法(XRF)测定其中铅、砷、铜、锌、铬、镍、钴、钒、锰、锡和钼等11种元素的含量。以经验系数法和康普顿散射内标法校正基体效应和谱线重叠干扰,选择65种土壤、沉积物及岩石国家标准物质用于绘制校准曲线。结果显示,11种元素的质量分数在一定范围内与其对应的荧光强度呈线性关系,检出限(3s)为1.0~3.9μg·g^(-1),测定值的相对标准偏差(n=10)为0.64%~9.2%。对新研制的30个农用地土壤成分标准物质进行测定,按照HJ 780-2015的质量控制标准评估各元素的测定准确度,结果表明:铅、铜、锌、铬、镍、钒、锰的测定合格率均为100%,说明XRF可用于土壤中这7种元素的测定;钴的测定合格率为93.3%,这是由于样品中高含量铁的影响;砷的测定合格率为80.0%,当砷的质量分数小于13μg·g^(-1)时准确度较差;锡、钼的测定合格率不足50.0%,因此不建议用XRF测定土壤中锡和钼的含量。     

X射线荧光光谱法测定石油焦中主量元素硫和痕量元素的含量

提出了粉末压片制样-X射线荧光光谱法测定石油焦样品中硫、钠、镁、铝、硅、磷、氯、钾、钙、钡、钛、钒、铬、锰、铁、镍、铜和锌等18种元素含量的方法。将粒径小于0.076mm的石油焦粉末经105℃烘干后置于模具中,以160MPa压力制成厚度小于4mm的样品。以经验系数法和康普顿散射线内标法校正基体效应和元素间的谱线重叠干扰。对石油焦样品连续11次测定,各元素测定值的相对标准偏差均小于8%。方法用于标准样品的分析,测定结果与认定值相符。     

粉末压片—X射线荧光光谱法测定土壤中的铜铅锌砷锑钴铬镍等重金属元素

采用粉末压片法制样,使用ZSX PrimusⅡ型X射线荧光光谱仪,对土壤样品中与生命健康和环境污染有直接影响的重金属元素Cu、Pb、Zn、As、Sb、Co、Cr、Ni进行同时测定.选用土壤国家标准物质、以国家标准物质为基体自制校准物质绘制标准曲线,解决了相关标准不足的问题,拓宽了元素测定范围(10~20 000μg/g),重点探讨了As、Sb的测量条件.虽然As、Sb的检出限和准确测定下限较高,但对于土壤质量的评价有重要的参考意义.方法快速、简便、准确.     

土壤样品ICP-AES多元素同时分析

电感耦合等离子体发射光谱法(ICP-AES)应用于土壤及环境样品的分析,多有报道。我们用HClO_4-HNO_3-HF混酸分解土壤样品,利用元素间干扰系数法修正土壤样品中基体元素对微量元素测定的干扰,测定了土壤标准参考物质中16种元素,其测定结果均能满足欲测元素定值要求。     

XRF法快速测定粉饼化妆品中Pb

讨论了粉饼类化妆品的成分配比,通过添加分析纯Pb粉末,采用硼酸镶边垫底的粉末压样法,制备了用于X射线荧光分析的粉饼类化妆品Pb元素的标准样品,保证了标样和待测样品基体大致相同。在XRF分析过程中选择Pb Lβ作为分析线,建立了粉饼类化妆品Pb元素的工作曲线,其线性相关系数为0.9977,检出限为2.30μg/g。对市售5款粉饼化妆品进行了Pb含量检测,样品加标回收率为106%;待测样品RSD为2.7%(n=11);5款样品中有2款Pb含量略高于当前国标限值。     

微波消解ICP-OES法测定土壤样品中22种元素

采用微波消解辅助混酸(盐酸-硝酸-氢氟酸-高氯酸),讨论了加入草酸、柠檬酸、酒石酸、EDTA二钠盐等络合剂对土壤样品进行前处理的影响,根据加标回收实验和国家标准物质(GSS-1)验证实验,采用电感耦合等离子体发射光谱法(ICP-OES)同时分析土壤样品中的22种元素。结果表明:加入4 mL 10%的酒石酸络合剂的效果最好,22种元素测定结果的相对标准偏差在0.06%~4.0%范围内;检出限为0.024~0.846μg/mL;回收率良好。该方法可用于土壤样品前处理技术及土壤中元素含量测定。     

混酸消解-电感耦合等离子体质谱法（ICP-MS） 同时测定土壤样品中10种重金属元素

建立了盐酸、硝酸、氢氟酸、高氯酸四酸消解-电感耦合等离子体质谱体系,对土壤环境样品中的铜、铅、锌、镍、镉、铬、钴、铊、锰、锑等重金属的测定进行了研究与讨论。优化了样品前处理条件和电感耦合等离子体质谱仪的相关参数,并利用内标元素45Sc、103Rh、209Bi校正土壤基体效应干扰。实验结果表明,各元素标准曲线的相关系数R均在0.9996之上,方法检出限（3σ）在0.007-0.325ug/g之间,加标回收率为92.5%-108.2%,相对标准偏差为0.2%-4.2%。研究过程中选用国家一级土壤成分分析标准物质进行质量控制,其测定值与标准值基本相符,从而为土壤中重金属元素提供了真实有效的检测依据,可用于大批量土壤中重金属元素的测定。     

溶液-粉末压片法XRF分析NdFeB磁性材料的成分

结合化学酸溶方法制备样品和使用X射线荧光（XRF）光谱测量试样,建立了NdFeB合金常见主量和痕量杂质元素的快速定量分析方法。同时自制一套参考标样。方法简单。流程短,可以满足准确定量的要求。     

X射线荧光光谱法测定红土镍矿中多种元素

分别研究了采用压片、熔片两种制样方法,用X射线荧光光谱法(XRF)测定了红土镍矿中的9种元素。压片法重点研究了基体效应校正,经散射线作内标和经验系数法校正后,可准确测定除二氧化硅、氧化镁外的7种元素,方法简便、快速;而熔片法着重研究了熔剂和熔样温度的选择,经基体效应校正,各分析元素的结果准确度完全可与化学法相媲美,其相对标准偏差(RSD)在0.50%～3.00%间。     

辉光放电质谱法测定核级石墨粉中痕量杂质

建立了直流辉光放电质谱法(DC-GDMS)测定核级石墨粉中痕量杂质元素的方法。用一定的压力将石墨粉镶嵌在高纯铟片上,形成一个直径约为5 mm的圆形石墨薄层,用铟片辅助石墨粉放电,实现了粉状样品直接检测。优化的实验条件为放电电流0.8 mA,放电电压1.2 kV,放电气体流速0.437 mL/min。用石墨粉标准样品(19J T61029)单点校准了仪器相对灵敏度因子,消除基体效应,实现15个关键杂质元素定量分析。方法检出限为5.0 ng/g,在单侧0.05显著性水平下,利用Student's t检验,方法测定结果t值均小于临界值,与标准值无显著性差异。相对标准偏差(RSD)均小于10%。本方法与电感耦合等离子体光谱法测定结果比较,相对误差在2.4%~17.4%之间。     

Determination of Trace Elements in Different Powdered Samples by Atomic Emission Spectrometry with Spectral Excitation in a Two-Jet Arc Plasmatron

The effects of operating parameters and easily ionized additives on the analytical signal in the region before the confluence of plasmatron jets were studied. It was shown that the effective atomic excitation temperature in this region is independent of the concentration of NaCl (0–50%) in the graphite powder. A method was proposed for the direct atomic emission determination of trace elements in powdered samples. In this method, multielement analysis of various samples, such as graphite concentrates of trace impurities, soils, bottom sediments, plants, and humic acids can be performed under unified conditions using a unified set of reference samples without sample mineralization and dissolution. At the stage of sample preparation, a finely divided sample is mixed with a spectroscopic buffer (graphite powder doped with NaCl). The detection limits for several dozen elements in their direct determination varied from 10^–6 to 10^–4 wt % at a relative standard deviation (RSD) of no worse than 15%.     

Total reflection X-ray fluorescence analysis of Mongolian coals

Coal samples were analysed for trace elements using total reflection X-ray fluorescence with monochromatic excitation. The procedure involved direct irradiation of the sample with the incoherent peak as internal standard. A new method for spectrometer sensitivity determination and sample quantification, was evaluated. Variable amounts of several trace elements were obtained in the analysis of coal from eight different deposits of Mongolia. The accuracy of the procedure was verified with the analysis of a coal standard.     

Application of RF GDMS for trace element analysis of nonconducting La0.65Sr0.3MnO3 ceramic layers

Radio-frequency glow discharge mass spectrometry (RF GDMS) has been applied to the determination of trace elements in ceramic perovskite layers (La_0.65Sr_0.3MnO₃) using synthetic standards. For the preparation of these standards high-purity powder of the basic material (La_0.65Sr_0.3MnO₃) was doped with trace elements in concentrations from 20 to 500 μg/g and the mixture was pressed to compact samples. The resulting calibration curves and the calculated relative sensitivity factors (RSF) differed only from 0.4 to 2 for different elements. For nearly all elements the standard deviations in the determination of trace elements in La_0.65Sr_0.3MnO₃ were better than 15% and detection limits (using the 3σ-criterion) were below 10 μg/g. Changes of the discharge parameters (RF power, pressure of the discharge gas (Ar) in the RF glow discharge) have no significant influence on the sensitivity to elements.     

X射线荧光光谱法测定灰岩中14种主次量元素

采用X射线荧光光谱法对灰岩中的Ca,Mg,Si,K,Na,Fe,Al,Ti,P,S,Mn,Sr,Ba,Cl等14种元素进行同时测定,采用硼酸镶边垫底的粉末压样法,优化了测量条件。对比较轻的元素,采用经验影响系数法校正基体效应,对于较重的元素,采用理论α影响系数法校正基体效应。分析标准参考物质GBW 07132,各元素的精密度(RSD)为0.1%~5.9%,分析标准参考物质GBW 07130,各元素的测定值与标准值相符,该方法对各元素的测定范围宽、速度快。     

Direct analysis of glass powder samples by radio frequency glow discharge atomic emission spectrometry (rf-GD-AES)

A method is described for the elemental analysis of glass powder samples by rf-GD-AES. Glass powder samples were pressed without binder to form sample disks. A brass sample holder was designed to hold the pellet onto the source and provide a good vacuum seal. Sample preparation conditions and particle sizes are shown to influence spectral characteristics and plasma stabilization times. The discharge operating parameters were optimized based on both raw analyte signal intensity (S) and signal-to-background ratio (S/B), the latter was found more useful in terms of sample-to-sample precision and quantification. A NIST Standard Reference Material (SRM 89 Lead-Barium Glass) was used to evaluate the method. The limits of detection for trace components ranged from 1–10 g/g for several elements, depending on the concentrations of the analytes in the SRM. Sample-to-sample reproducibilities were better than 10% RSD and linear calibration curves were obtained using either the Si (I) optical emission as an internal standard or the individual analyte's S/B characteristics.     

Determination of refractive and volatile elements in sediment using laser ablation inductively coupled plasma mass spectrometry

Wet-milling protocol was employed to produce pressed powder tablets with excellent cohesion and homogeneity suitable for laser ablation (LA) analysis of volatile and refractive elements in sediment. The influence of sample preparation on analytical performance was also investigated, including sample homogeneity, accuracy and limit of detection. Milling in volatile solvent for 40 min ensured sample is well mixed and could reasonably recover both volatile (Hg) and refractive (Zr) elements. With the exception of Cr (−52%) and Nb (+26%) major, minor and trace elements in STSD-1 and MESS-3 could be analysed within ±20% of the certified values. Comparison of the method with total digestion method using HF was tested by analysing 10 different sediment samples. The laser method recovers significantly higher amounts of analytes such as Ag, Cd, Sn and Sn than the total digestion method making it a more robust method for elements across the periodic table. LA-ICP-MS also eliminates the interferences from chemical reagents as well as the health and safety risks associated with digestion processes. Therefore, it can be considered as an enhanced method for the analysis of heterogeneous matrices such as river sediments.