X射线荧光光谱法测定钒铁合金中主次元素含量

用熔融制样法将钒铁合金样品在铂金坩埚中与四硼酸锂和偏硼酸锂熔融,熔体在铂金坩埚中自动成型,用X射线荧光光谱法测定钒铁合金中钒、硅、锰、铝和磷等主次元素含量。经试验求得熔融时,四硼酸锂、混合溶剂(四硼酸锂∶偏硼酸锂=67∶33)和样品的最佳质量比为30比5比1。各元素的检出限在12.4～51.2μg.g-1之间。方法用于标准样品分析,测定值与认定值相符。     

熔融制样-X射线荧光光谱法测定锰铁中硅、锰、磷、铬、镍和铜

采用熔融制样-X射线荧光光谱法测定锰铁中硅、锰、磷、铬、镍和铜的含量。样品以四硼酸锂为熔剂,在300℃下加热15min,慢速升温至1 100℃,熔融15min,冷却后制成玻璃片,用于X射线荧光光谱分析。6种元素在一定的质量分数范围内与其信号强度呈线性关系,方法的检出限在15~59μg·g-1之间。方法用于锰铁样品的分析,测定值的相对标准偏差(n=11)在0.16%~3.6%之间。     

直读光谱法测定生铁中硅锰磷

提出了采用HK 200型磨样机制样,直读光谱法测定生铁中硅、锰和磷的含量。探讨了基体效应、狭缝位置、分析条件和制样方法等影响因素。在优化的试验条件下,3种元素的相对标准偏差(n=11)均小于5%。方法用于生铁试样分析,测定结果与X射线荧光光谱法和分光光度法的测定结果基本一致。     

X射线荧光光谱法快速测定锰矿石中的主次组分

采用粉末压片法制样,使用ZSX Primus Ⅱ X射线荧光光谱仪实现了对锰矿样品中锰元素及杂质组分钠、镁、铝、硅、磷、钾、钙、铁的快速测试。虽然方法在分析准确度上不及化学法或熔融制样—X射线荧光光谱法,但方法的精密度好,测试范围广,分析结果与标准值和比对值基本吻合。方法简便、快速,可满足实验室对锰矿石批量检测的要求。     

X射线荧光光谱法同时测定锰锌铁氧体材料的主量组分

用熔融制样法将样品在铂金坩埚中与四硼酸锂熔融,熔体倒入铂金专用模具中成型为玻璃态块样。用X射线荧光光谱法测定锰锌铁氧体样品中氧化铁、四氧化三锰及氧化锌含量。经试验求得熔融时样品和无水四硼酸锂熔剂的最佳质量比为1比17.5。采用基体参数法和理论α系数法对基体效应及谱线重叠的干扰予以校正。此法用于锰锌铁氧体材料分析,3种组分的日间和日内相对标准偏差(n=7)分别小于3.5%和4.0%;用于标准样品的分析,3种组分的测定值与标准值之间的绝对误差在-0.15%~0.02%之间。     

熔融制样-X射线荧光光谱法测定工业硅中总硅、二氧化硅和其他杂质组分

将四硼酸锂内衬坩埚熔融制样方法应用于X射线荧光光谱法测定工业硅中总硅、二氧化硅和其他杂质组分(铝、铁、钙、镁、钛)。在熔融制样前,样品(1.000 0g)经直接灼烧(700～750℃)计算灼减量并除去样品中碳。称取上述灼烧后的样品0.200 0g,与碳酸锂1.700g和600g·L~(-1)硝酸铵溶液0.1～0.3mL混匀后移入四硼酸锂内衬坩埚中,于710～720℃预氧化10～12min。将此经预氧化的混合物及其内衬坩埚一起转移至预置有3.000g硼酸的铂金坩埚中,加入400g·L~(-1)溴化铵溶液0.1～0.4mL,于熔样机中静置熔融8min,摇动熔融12min,冷却,脱模后即得样品的玻璃片。选取测定元素的氧化物,按0.200 0g称样量模拟制备了5个校准样片,各组分的质量分数在一定范围内与其对应的X射线荧光强度呈线性关系,提出了样品中二氧化硅含量的计算公式。方法用于5个工业硅样品的分析,测定结果与湿法分析测定值相符。     

X荧光玻璃熔片法分析铁矿石

使用无水四硼酸锂作为溶剂，在1050℃熔融制样，以X荧光光谱法测定铁矿石中铁、硅、铝、钙、镁、锰、钛、磷、硫等元素，其分析结果的精密度和准确度可与化学法相比。     

熔融制样-X射线荧光光谱法测定直接还原铁中主次元素含量

应用熔融制样-X射线荧光光谱法测定了直接还原铁中主次元素的含量。样品置于铂金坩埚中,以四硼酸锂和偏硼酸锂为熔剂于1 050℃熔融20min,将熔化的样品倒入铂金模具中,所制得的片样用于X射线荧光光谱分析。以铁矿石标准物质GBW 07221等25种标准物质制作校准曲线,以固定理论α影响系数法校正基体效应。方法用于实际样品的分析,所得结果与其他方法测定值相符。测定值的相对标准偏差(n=10)在0.31%~16%之间。     

熔融制样-X射线荧光光谱法分析铝合金

提出了用X射线荧光光谱法测定铝合金中镁、硅、钛、锰、铁、镍、铜、锌、铅等9种元素。样品0.2000g置于聚四氟乙烯杯中用200g·L~(-1)氢氧化钠溶液5mL溶解后,加硝酸10mL酸化,将溶液移入已盛有4.000g熔剂(四硼酸锂、偏硼酸锂与氟化锂以4.5比1比0.4的质量比混合)的铂金坩埚中,低温蒸干,并加热熔融制成厚度为2.5mm的玻璃状熔片,供X射线荧光光谱法分析用。该方法可适用于不同牌号、不同铸造或锻造热处理状态的铝合金样品分析。按该方法分析了4个标准样品,其测定结果与标准值相吻合。用一个铝合金标准物质(牌号ZLD 108)制备10个样片并测量,各元素相对标准偏差在0.62%～2.7%之间。     

X射线荧光光谱法测定萤石中氟化钙

采用X射线荧光光谱仪可以快速准确测定萤石中总钙的含量.但测定其中氟化钙含量时,一方面,由于样品中碳酸钙计入钙量,从而造成氟化钙测定结果准确性较差.另一方面,铜、锌等金属元素在熔融制样时对铂金坩埚腐蚀较大,因此需要进行酸处理除去碳酸钙及铜、锌等金属元素.然而,样品经过酸处理后,质量会发生变化,造成熔剂与样品的比例不一致,从而影响测定结果.对样品前处理条件、XRF分析中熔片和仪器工作条件等进行了优化,建立了熔融制样、X射线荧光光谱法（XRF）准确测定萤石中氟化钙含量的方法.方法干扰少,具有良好的准确度和精密度,操作简单,提高了分析效率.     

X射线荧光光谱法测定洗衣粉中硅、铝、磷、硫的初步研究

用X射线荧光光谱法测定了洗衣粉中硅，铝，磷，硫的含量，并与化学法进行了比较。结果表明，本法样品处理简单，分析速度快，可用于快速确定洗衣粉的化学成分。     

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。     

X-射线荧光光谱法测定钛铁中的硅、锰、磷、铝

介绍用X-射线荧光光谱仪测定钛铁中Si、Mn、P、Al含量的方法,通过试验确定了合适的研磨时间、压力和保压时间,用压片法制样,建立了各元素的工作曲线,各元素的测定范围分别为Si3.00%～6.00%,Mn1.00%～3.00%,P0.030%～0.070%,Al5.00%～9.00%。通过强度测量得到测定Si、Mn、P、Al的相对标准偏差分别为0.074%、0.308%、0.383%、0.040%,精密度满足测试要求。将该方法测定结果与化学法比对,准确度满足国家标准方法分析误差的要求。     

Combined non-destructive XRF and SR-XAS study of archaeological artefacts

We report on a non-destructive study of Sicilian ceramic fragments of cultural heritage interest, classified as “proto-majolica” pottery and dating back to the twelfth to thirteen centuries AD. The analytical approach used is based on the employment of two totally non-invasive spectroscopic techniques: X-ray fluorescence (XRF), using a portable energy-dispersive XRF analyser, and X-ray absorption spectroscopy, using synchrotron radiation as a probe (SR-XAS). XRF measurements allowed us to collect elemental and spatially resolved information on major and minor constituents of the decorated coating of archaeological pottery fragments, so providing preliminary results on the main components characterizing the surface. In particular, we assigned to Fe and Mn the role of key elements of the colouring agent. With the aim of obtaining more detailed information, we performed SR-XAS measurements at the Fe and Mn K-edges at the Italian BM08 beamline at the European Synchrotron Radiation Facility (Grenoble, France). The experimental data were analysed by applying principal component analysis and least-squares fitting to the near-edge part of the spectra (X-ray absorption near-edge structure) to determine the samples’ speciation. From the overall results, umber, a class of brownish pigments characterized by a mixture of hydrated iron and manganese oxides, has been ascribed as a pigmenting agent.     

X射线荧光光谱熔融法测定锶永磁铁氧体中各组分含量

本文使用自制标准样品,采用混合熔剂熔融样品,用X射线荧光光谱法(XRF)测定锶永磁铁氧体半成品中Fe,Sr,Si等元素的含量.熔融制样有效地消除了矿物效应,并降低了基体效应的影响.实验结果表明,本法准确度高,重现性好,平行测定11次相对标准偏差(RSD)可达到0.1%.该方法用于实际样品分析,其结果与传统化学分析方法结...     

Determination of Sr,Zn, Cu and Fe in Licorice by X-ray Fluorescence Spectrometry

Few persons determine the trace elements in the licorice by X-ray fluorescence spectrometry (XRF), because there is no standard samples of the licorice. This paper describes the method to determine Sr,Zn,Cu and Fe in licorice using XRF. The samples are ashed and then determined with the powder process. The measured results are corrected by artificial standard samples.     

Use of geologically biased enrichment factors (EF) as indicators of natural air pollutants

Airborne samples representing dustfall, street, and household dusts of Aswan were collected; and ten elements (Si, Ti, Fe, Mn, K, Al, Ca, Mg, Na, and P) were chemically analysed by means of instrumental activation analysis (INAA), inductively coupled plasma (ICP), and X-ray fluorescence (XRF). The puzziling differences in the values of the enrichment factors (EF) and obvious contradiction with the mineralogy of the dustfall samples both indicate that this method of calculation could help to establish models of dust matrices in different geological and industrial regions rather than considering it only as a tool for assessing the source rocks.     

熔融法X射线荧光光谱测定岩石主成分含量

选用国家一级标准物质,采用X射线荧光光谱法对岩石样品中的二氧化硅、氧化铝、氧化钙、氧化镁、氧化钾、氧化钠、三氧化二铁、五氧化二磷、氧化钛、氧化锰10种主要组分进行测定,分析结果和标准值或化学值相吻合,各组分测定结果的相对标准偏差小于2％（n=12）。     

Comparison between X-ray fluorescence and inductively coupled plasma atomic emission spectrometry in the analysis of sediment samples

Two multielemental analytical techniques, X-ray fluorescence analysis (XRF) and inductively coupled plasma atomic emission spectrometry (ICP-AES) were used for the analysis of the elemental composition of sediment samples from a marsh and standard reference materials. The sediment samples were pretreated with different methods which are widely used in practice. A comparison was made not only between the concentrations obtained by the different methods, but also between the statistical conclusions derived from the processing of the experimental results. Good agreement was found for some elements, e.g. Mn, Zn and Sr, while the concentrations and the statistical conclusions were shown to depend on the analytical method used in the case of other elements, e.g. Fe and Zr.