能量色散X荧光分析仪分析钒钛烧结矿中SiO2、CaO和TFe

在烧结矿生产中，SiO2、CaO、TFe的准确含量是烧结成球造粒的最为重要指标，其分析准确与否直接关系到烧结矿的物化性能以及高炉产量。目前，国内外分析行业主要采用波长色散X荧光分析仪，很少使用能量色散X荧光分析仪。本法使用CIT-3000SJ钙硅铁能量色散X荧光分析仪，该仪器分析速度快、准确度高、操作简单、使用方便，能同时分析钒钛烧结矿中的SiQ、CaO、TFe等含量，分析结果完全达到了炼铁厂生产对分析的要求。     

能量色散一X荧光能谱法同时测定工业硅中铝钙铁硅

研究了能量色散-X荧光法测定工业硅的方法，提出以硼酸作外壳，粉末直接压片测定，应用于实际测定，速度快、准确度高，与国家标准方法比较，无显著性差异。     

能散X荧光分析仪分析烧结矿

根据西核FJ－2810G能散X荧光分析仪在水泥行业的成功使用经验，用XRF法对烧结矿化学成分进行了研究，绘制了标准曲线，并进行了数学校正，经过试验，已成功地用于烧结生产控制分析。     

能量色散型X荧光分析仪测定生铁样品

目前 ,国内钢铁企业生铁样品分析大多采用传统的化学分析方法 ,分析速度慢 ,难以满足生产需要 ,部分企业采用进口的波长色散型X荧光分析仪 ,但因其价格昂贵 ,很多企业难以接受。而采用能量色散型X荧光分析仪 (简称EDXRF)测定生铁样品 ,国内还未见报道。本文试验了国产X荧光仪分析生铁样品的方法 ,成功地应用于炼铁化验室生产分析 ,为国内炼铁化验手段的更新换代作了有益的探索。1　试验部分1.1　仪器及性能WISDOM 80 0 0型能量色散X荧光分析仪 (上海精谱仪器有限公司 )分析范围 :同时分析元素周期表中由钠到铀之间的全部元素。高压发…     

X射线荧光光谱法测定钨铁合金（粉末）中的钨,铁,硅,锰,铜

介绍Ｘ射线荧光光谱法定量测定钨铁合金（粉末）中的Ｗ，Ｆｅ，Ｓｉ，Ｍｎ，Ｃｕ。试样经粉碎过筛后选取直径为５３～６３μｍ的粉末压制成型，对部分元素作基体校正，此方法快捷、准确、可靠，能满足生产上对快速分析的要求。     

X射线荧光光谱(XRF)法测定绿泥石中镁、铝、硅、磷、钾、钙、钛、铁元素含量

建立了X射线荧光光谱法测定绿泥石中镁、铝、硅、磷、钾、钙、钛、铁元素含量的快速分析方法。以标准物质及标准物质与基准试剂氧化镁、氧化钙人工混合配制标样的方法建立标准工作曲线,重点讨论了熔剂和脱模剂的选取。最佳熔样条件：采用8.0g四硼酸锂和偏硼酸锂混合熔剂(质量比67: 33)+0.8g样品并添加溴化锂作为脱模剂,熔样温度1100℃,熔样时间10min。该方法相对标准偏差(n=12)均小于5.57%,绿泥石样品测定结果与化学法一致,硅酸盐标准物质测定结果均满足不确定度要求。     

X射线荧光光谱法快速测定生铁中硅锰硫磷钛

高炉生铁化验项目为硅、锰、硫、磷、钛五元素，其中硅、锰、硫、磷是基本分析元素，钛是高炉使用后期为了护炉加入钛球而需要分析的元素。自进行X射线荧光光谱仪测定生铁试验以来，由于受高炉冶炼影响，一时无法收集到所需的样品，作者采用自制样品先建立一条基本曲线，用于日常分析，然后在仪     

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。     

粉末压片X射线荧光光谱法测定铌铁合金中 铁、铌、硅、铝、磷

为提高铌铁合金检验效率,替代繁琐的化学湿法分析,采用粉末压片制样,利用X荧光光谱法对铌铁合金中Fe、Nb、Si、Al、P 5种主要成分进行测定。选用定值过的生产样品作为内控标准样品,主要研究制样细节对分析结果的影响,确认合适的试样粒度和压片参数,通过曲线拟合建立校准曲线。测定结果与化学湿法和电感耦合等离子体原子发射光谱法测定结果比较,各组分精密度相对标准偏差为0.48%～1.9%,准确度满足国标分析要求。     

ICP-AES法测定氧化铝粉中硅、钙、铁、钛、钒和锌

采用高压盐酸消化，电感耦合等发射光谱法测定氧化铝中硅、钙、铁、钛、钒和锌等6元素，研究了铝基体对被测元素的影响，并选择了最佳工作条件，被测元素的检出限为0．34－52ng/mL，样品加标回收率为95．7％－108．6％。     

Surface acidity and basicity of functionalized silica particles

Tetraethoxysilane has been co-hydrolyzed with functionalized organosilanes in a modified Stöber process to produce silica particles with amino, carboxylate or dihydroimidazole groups on the surface. The effects of reaction conditions and the loading of the functionalized organosilane on particle size was examined by TEM. Fluorescence spectroscopy of the surface amino groups covalently modified with fluorescamine, and the surface carboxylate groups with 4-bromomethyl-6,7-dimethoxycoumarin, demonstrated that these functional groups were accessible for further reaction. Changes in surface acidity and basicity caused by the presence of functional groups (amine, dihydroimidazole, carboxylate) on the particle surface were determined using an indicator titration technique. Particles with surface imidazole and amine groups and particles with surface carboxylate groups have enhanced basicity and acidity, respectively. Dihydroimidazole-modified silica had greater surface basicity than the amine-modified silica. The effect on basicity and acidity increases as the amount of added functionalized silane increases. However, this increase is nonlinear with respect to the increase in added functionalized silane. Particles with both surface dihydroimidazole and carboxylate groups demonstrated reduced surface basicity and acidity.     

A comparison of X-ray fluorescence spectrometric (XRF) techniques for the determination of metal traces,especially in plastics

A comparative study of energy-dispersive X-ray fluorescence techniques (without and with polarized radiation) and a wavelength-dispersive technique was carried out in order to investigate their sensitivity for the quantitative determination of 3d transition metal traces in plastic materials. For this purpose, liquid calibration samples in paraffin oil for the elements Cr, Mn, Co, Ni and Cu were prepared. Calibration lines in the concentration range of 1–100 g/g were evaluated for commercially available XRF-instruments and the results were critically compared. Limits of detection (LOD) ranged from 0.1 to 0.7 g/g for wavelength-dispersive XRF and energy-dispersive XRF with polarized radiation. The LOD's for energy-dispersive XRF without polarized radiation ranged from 0.9 to 8.6 g/g for elements in the same atomic number range between 24 and 29. The application of these optimized methods to the quantitation of wear and corrosion phenomena in plastic extruders and in a relevant model test apparatus, the annular slit tribometer, is elucidated.     

Application of radioisotope XRF for the determination of noble metals in aqueous solutions

Radiometric methods of determination of platium and palladium (0.1 to 5% of Pt and 0.1 to 2% of Pd), gold and indium (0.01 to 1% of Au and 1 to 4 g In/l) and of platinum and rhodium (0.1 to 9% of Pt and 0.05 to 1% of Rh) in aqueous solution has been worked out. A suitable measuring device has been designed and constructed. The methods are based on the measurement of characteristic radiation of the L_α line for gold and platinum and of the K-series for indium, palladium and rhodium, as well as on the measurement of scattered radiation from a²³⁸Pu source. The r.m.s. error of the determination varies from 0.01 to 0.10% of Pt, 0.002 to 0.01% of Au and 0.01 to 0.15% of Pd depending on the concentration. In the case of Rh and In the errors are 0.008% and 0.04 g In/l, respectively.     

Development of a method for direct determination of solids as thin films by energy dispersive X-ray fluorescence analysis

Solid samples can be analysed as without a prior decomposition step, if they are pulverized and then embedded in a thin layer of a cold-setting polymer. This method is very appropriate for materials which are difficult to decompose or which can be easily contaminated. The sample components are evenly distributed in a thin layer, which improves considerably the signal-tonoise-ratio, and this leads to a decrease of the limits of detection. The reproducibility of the method was tested with cobalt oxide and yttrium oxide and also a mixture of these with silver oxide and manganese dioxide. Between 20 and 60 ng of these elements can be determined without difficulty, with a precision of ± 2–4%. The correlation coefficients found for the calibration graphs were between 0.994 and 0.999.     

藉L-半胱氨酸包覆的ZnS纳米粒子的共振光散射定量分析蛋白质

合成和表征了功能性L-半胱氨酸包覆的ZnS纳米粒子。在pH5．12的NaAc-HAc溶液介质中,L-半胱氨酸包覆ZnS纳米粒子于波长308．0nm处出现共振光散射峰。一定量蛋白质的加入能明显增强体系的共振光散射,且峰强度增加值与蛋白质浓度间存在良好线性关系,据此建立了一种灵敏的测定微量蛋白质的方法。用L-半胱氨酸包覆ZnS纳米粒子作为探针,不仅克服了有机染料可能出现的光漂白等缺点,而且本身不具毒性。该法用于人血清试样中总蛋白的测定,其结果与临床数据一致。     

Application of XRF and field portable XRF for environmental analysis

The aim of the present review is to evaluate, on the basis of published papers, the real potential of XRF technique for environmental analysis. Special attention is given for the determination of heavy metal pollution in water. Results of numerous papers for various samples are presented. Some details of the technique and preconcentration methods employed are also discussed. This revised version was published online in July 2006 with corrections to the Cover Date.     

Application of l-cysteine-capped nano-ZnS as a fluorescence probe for the determination of proteins

Nanometer-sized l-cysteine-capped ZnS particles have been synthesized and used as a fluorescence probe to investigate the effect of proteins on fluorescent intensity. With =190 nm, maximum and constant synchronous fluorescence enhancement was produced at 267 nm and pH 5.12 in the presence of proteins. A highly sensitive synchronous fluorescence method for the rapid determination of proteins has been developed. Under optimum conditions, calibration graphs are linear over the range 0.03–8.0 g mL^–1 for bovine serum albumin (BSA), 0.01–6.0 g mL^–1 for human serum albumin (HSA), 0.05–8.0 g mL^–1 for -globulin (-G), and 0.04–4.0 g mL^–1 for ovalbumin, respectively. The relative standard deviations of seven replicate measurements were 1.75% for 1.0 g mL^–1 BSA, 1.90% for 1.0 g mL^–1 HSA, 1.65% for 1.0 g mL^–1 -G, and 2.32% for 1.0 g mL^–1 ovalbumin.     

Brilliant cresyl blue as a new red region fluorescent probe for determination of nucleic acids

A fluorescence quenching method was developed for determination of microamounts of nucleic acids by using brilliant cresyl blue (BCB) as a new red region fluorescent probe. In aqueous hexylmethylene tetramine solution, BCB showed maximum excitation and emission wavelengths at 626 and 670 nm, respectively, and the fluorescence of BCB could be greatly quenched by DNA (or RNA). Under optimal conditions, the calibration graphs are linear over the range of 0.02–0.80 μg/ml for SM DNA and 0.25–1.5 μg/ml for yeast RNA. The corresponding detection limits are 7 ng/ml for SM DNA and 25 ng/ml for yeast RNA, respectively. SM DNA can be determinated in the presence of 40% (w/w) RNA, and the relative standard deviation of six measurements is 2.5% for 500 ng/ml SM DNA. The result of the determination of golden staphylococcus DNA by this method was satisfactory.     

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。