波长色散X射线荧光仪器进展

本文叙述了自１９９０年以来波长色散Ｘ射线荧光光谱仪及分析技术的最新进展，介绍分为波长色散Ｘ射线荧光分析仪的整机特点，设计思想的发展，新技术应用，计算机及软件发展和定性定量分析等部分。     

X射线荧光光谱法测定橄榄岩主次痕量元素

本文采用熔融玻璃片和粉末压片法制样，用理论ａ系数和散射线内标法校正元素间的效应，     

波长色散X射线荧光光谱仪的内部校准

根据波长色散X射线荧光光谱仪检定规程制定了内部校准作业指导书,对PANalytical Axios 4.0型X射线荧光光谱仪的外观、精密度（RSD）、稳定性（RR）、探测器分辨率（流气正比计数器、闪烁计数器、封Xe正比计数器）和仪器的计数线性进行了性能测试和内部校准.     

波长色散X射线荧光光谱仪的性能测试方法介绍

介绍澳大利亚国家标准和中国国家计量检定规程中关于波长色散型 X射线荧光光谱仪的性能测试方法 ,并对 SRS34 0 0型 X射线荧光光谱仪进行了性能测试和计量检定。     

土壤重金属铅元素的X射线荧光光谱测量分析

在实验室条件下,利用NITON XLt793型便携式X射线荧光光谱重金属分析仪测量并分析土壤中铅元素的X射线荧光光谱特性。分别以铅的L_α(10.55 keV)和L_β(12.61 keV)特征谱线作为分析线,分析了不同基体元素对分析线的影响;测定在不同铅浓度下的特征谱线强度变化。结果表明铅的质量分数在10×10-6～1 800×10-6范围内,元素的光谱强度与浓度之间呈现较好的线性关系;建立了铅元素的定标曲线,并计算得到铅的检出限为7.89×10-6。     

X射线荧光光谱快速分析地质物料主、次元素

本文建立了X射线荧光光谱分析地质、化探扫面样的快速方法，掌握各元素的分析特征，选择适宜的条件，从而缩短分析时间，降低其成本，达到快速、简便的目的。     

应用X射线荧光光谱法测定过磷酸钙中主量元素

磷肥是农业生产中最常用的肥料之一。文章通过X射线荧光分析技术测定了过磷酸钙中九种成分的含量,各元素的测定精度都在0.20%～0.005%之间,所以X射线荧光光谱法是一种测定过磷酸钙肥料有效成分和其他元素的快速、有效的方法。通过磷肥中各种成分的含量分析可以得出如下结论：(1)选用的过磷酸钙中有效P₂O₅≥16%(18.101%),不是假磷肥;所以X射线荧光光谱分析技术可以识别磷肥真假;(2)所测定磷肥中SiO₂,TFe₂O₃,MgO, CaO和K₂O含量比较高,分别是16.954%, 1.495%, 1.580%, 21.428%和1.585%,所以以过磷酸钙作为肥料时可以起到微肥的作用,但是研究磷元素作用时应当注意这几种成分对磷肥效果的干扰作用;(3)Al₂O₃的含量为3.225%,长期使用磷肥应当注意Al毒的发生。     

X射线荧光光谱法同时测定煤灰中的12种成分

采用熔融制样法,用X射线荧光光谱法同时测定煤灰中的常量、少量和微量成分SiO₂,Al₂O₃,Fe₂O₃,CaO,SO₃,TiO₂,K₂O,Na₂O,P₂O₅,Mg_O,MnO,BaO。选用混合熔剂并加入氧化剂的方式降低熔融温度,解决了硫的准确测量问题。同时通过选用土壤等标准样品解决了煤灰成分标准样品不足的问题。应用可变理论α系数及固定α系数法进行基体效应校正,所得结果与化学法的分析结果相符合。     

Application of total reflection X-ray fluorescence spectrometry for trace elemental analysis of rainwater

Applicability of total reflection X-ray fluorescence (TXRF) spectrometry for trace elemental analysis of rainwater samples was studied. The study was used to develop these samples as rainwater standards by the National University of Singapore (NUS). Our laboratory was one of the participants to use TXRF for this study. The rainwater sample obtained from NUS was analysed by TXRF and the trace elements Mn, Fe, Ni, Cu, Zn, V and Pb were determined as required by the NUS. The average precision was found to be within 16% and the TXRF-determined elemental concentrations of these elements were below 20 μg/l. The average deviation of TXRF-determined values from the certified values were 20% (excluding the deviation for Fe and V which were comparatively high). Apart from the above elements, S, K, Ca, Rb, Sr, Ba and Br were also determined by TXRF and were found to be in the range of 0.2 to 191 μg/l. TXRF-determined values of our laboratory played an important role in the certification of concentration of seven elements in this rainwater sample which was later developed as a rainwater standard.     

Determination of elements in some lichens growing in Giresun and Ordu province (Turkey) using energy dispersive X-ray fluorescence spectrometry

The concentration of five different elements in six lichens species of different regions in Giresun and Ordu (Turkey) was determined using the energy dispersive X-ray fluorescence method. A radioisotope excited X-ray fluorescence analysis using the method of multiple standard addition is applied to the elemental analysis of lichens. An annular 50 mCi ²⁴¹Am radioactive source and an annular 50 mCi ⁵⁵Fe radioactive source were used for excitation of characteristic K X-rays. An Si(Li)detector which has a 147 eV full-width at half-maximum for 5.9 keV photons was used for intensity measurements. A qualitative analysis of spectral peaks showed that the samples contained potassium, calcium, titanium, iron, and barium.     

Evaluation of the dose received in the tissues of the neck during quantification of iodine in the thyroid by X-ray fluorescence spectrometry

The determination of the iodine content in the thyroid is of great interest for many investigations of this gland. The conventional scintigraphic method, using radionuclides, is efficient but delivers a significant dose to the patient. The X-ray fluorescence spectrometry could give information about the iodine content in the thyroid. The measured signal is obtained after stimulation of the stable iodine contained in the gland by X-rays. The advantage of this technique is the complete absence of radioactive isotope injected into the patient body. By applying this, a decrease in effective dose to the patient should be obtained. In this work, the study of the dose received by a thyroid phantom (surrounded by the different tissues of the neck) was performed. The phantom is made of PLA. The dose is measured in optimised conditions defined for the analytical technique. A total head-neck phantom was also used in order to consider the absorbed dose in each different tissues and organs as spinal cord or eyes. Thermo-luminescence dosimeters were chosen for their small size, their sensitivity and the easy positioning on the surface of the phantom but also inside of it to evaluate dose to internal organs. Those LiF 100 dosimeters have been calibrated within the X-ray beam also used for the analysis of iodine. The repeatability and reproducibility of the method has been evaluated. The influence of parameters as concentration of iodine in the thyroid, distance between the X-ray generator and the neck, thickness of the tissues surrounding the thyroid, has been investigated in terms of modifying parameters of the dose received by different tissues situated in the neck and the head.     

Application of X-ray fluorescence spectrometry in plant science: Solutions,threats, and opportunities

X-ray fluorescence (XRF) spectrometry is a nondestructive, rapid, simultaneous multi-elemental imaging methodology for plant materials. Its applications are broad and cover most of the elements with varying concentration below the parts per million (ppm). XRF is a well-established atomic spectrometric technique that is also being used as a field portable instrumentation. In recent decades, XRF has been considered a very versatile tool for plant nutrition diagnosis due to its fast and multi-elemental analytical imaging response directly from a solid sample. In this review, we have mainly focused on the recent developments and advancements in XRF spectrometry to analyze plant materials. We have also included the fundamental aspects and instrumentation for XRF spectrometry for its use in plants imaging. We have also covered the use of XRF for vegetal tissues and plant leaves. Mainly, we have briefly focused on some features of sampling procedures and calibration strategies regarding the use of XRF for plant tissues. Microchemical imaging applications by XRF, μ-XRF, μ-SRXRF, and TXRF have been covered for a wide variety of plant tissues such as leaves, roots, stems, and seeds.     

Detection and quantification of heavy metal elements in gallstones using X-ray fluorescence spectrometry

Gallbladder cancer, which is associated with the heavy metal toxicity, is one of the most dangerous malignancies. High occurrence of gallstones in the gallbladder is a well-recognized risk factor for gallbladder cancer. Accumulation of heavy and toxic metals in the biliary system is one of the main causes of gallstone formation and leads to gallbladder cancer if it remains untreated. In this work, we investigate heavy and toxic metals in gallstones to identify their association as potential risk factors for gallbladder cancer. Detection and quantification of the heavy and toxic chemicals present in gallstones are important to define etiopathogenic factors that, in turn, are useful to identify preventive and therapeutic strategies. We quantified the heavy metals in gallstones collected from patients of different age groups and dietary habits. We carried out chemical composition studies of trace and heavy metal elements present in gallstones by applying Fourier transform infrared (FTIR) spectroscopy and wavelength-dispersive X-ray fluorescence (WD-XRF) spectrometry. We also compared our experimental results with the results obtained from atomic absorption spectroscopy, as well as values previously reported in literature. These findings demonstrate the potential of WD-XRF spectrometry and FTIR spectroscopy as important emerging diagnostic tools in the field of gastroenterology.     

K X-ray fluorescence cross-sections for some light elements excited by keV photons

K and K X-ray fluorescence cross-sections have been experimentally determined for the elements Cu, Se, Y, and Mo at excitation energies 23.62, 24.68, 36.82, 43.95, 48.60, and 50.20keV using an X-ray tube with a secondary exciter system as the excitation source. The X-ray tube with a secondary target arrangement was used to obtain high intensity with high degree of monochromatization. Experimental values were compared with the theoretical values using tabulated I ratios based on Hartree-Fock and Hartree-Slater theories calculated by Scofield. The experimental values for all the elements at various excitation energies are in good agreement with the theoretical values.     

内标法在土壤重金属镍元素X荧光分析中的应用研究

利用能量色散型XRF重金属实验平台,在实验室自然大气环境下获取土壤的X射线荧光,通过X射线荧光光谱法定量分析了国家标准土壤样品中元素Ni的含量。实验研究了土壤中Ni元素的X荧光特征分析谱线,采用加入内标法测定了Ni元素定标曲线,并依据实验结果分析了内标元素选取方法。实验结果表明,对土壤样品进行内标法分析时,可选取基体中适宜元素作为内标元素;使用Pb的Lα线,Cu和Fe的Kα线作内标线时相对标准偏差(RSD)分别为6.24%,5.24%和5.22%,说明选择合适基体主量元素的特征谱线作为内标线,可有效提高测量结果的准确性。     

便携式X射线荧光光谱分析仪测定土壤中重金属

应用NITON XL3t600型便携式X射线荧光谱分析仪对土壤中主要重金属污染物Cu,Zn,Pb,Cr和As进行了测试。结果表明,Cu,Zn,Pb,Cr和As元素的最低检出限分别为:23.96,11.69,8.58,19.23,6.24mg.kg-1;对土壤成分分析标准物质GSS-5进行5次重复测定,准确度在96%～102%之间,RSD在1.0%～7.6%范围内,表明仪器对于土壤中较高浓度重金属检测准确度和精密度良好;田间进行原位检测,相对标准偏差均小于20%,与国标方法检测结果相比,准确度在55%～119%之间。通过实验室测试和田间原位检测,验证了便携式X射线荧光谱分析仪检测土壤中重金属元素有较好的准确度和精密度,适用于土壤中重金属的快速检测。     

Measurement of L X-ray fluorescence cross sections and relative intensities for some elements in the atomic range 78 ≤ Z ≤ 92

The L X-ray fluorescence cross sections (σ_Ll, σ_Lα, σ_Lη, σ_Lβ, σ_Lβ6, σ_Lβ2,₄, σ_Lβ1,₃, σ_Lβ9,10, σ_Lγ, σ_Lγ1, σ_Lγ2,3, σ_Lγ4 and σ_Lγ5) and relative intensities (I_Lα, I_Ll, I_Lη, I_Lβ, I_Lβ6, I_Lβ2,4, I_Lβ1,3, I_Lβ9,10, I_Lγ, I_Lγ1, I_Lγ2,3, I_Lγ4 and I_Lγ5) for some elements in the atomic range 78 ≤ Z ≤ 92 have been measured at 59.54 keV photons energies from an Am-241 point source. The L X-rays emitted by samples have been counted by a Si(Li) detector. The L X-ray fluorescence cross sections and relative intensities have been also calculated theoretically by using atomic parameters. The measured values have been compared with the theoretical values.     

Qualitative and quantitative analysis of pathological and non-pathological human bone using radioisotope X-ray fluorescence technique

Pathological and non-pathological human elbow bone samples were collected from one male human patient and one female human patient who were undergoing treatment in our University Research Hospital. Pathological and non-pathological human elbow bone samples were analyzed by means of energy-dispersive X-ray fluorescence spectrometry by using standard additions method. Experimental results are presented and discussed in this work.