A method was developed for content determination of Na, Mg, A1, Si, P,S, C1, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Nb, Zr, Y, Sr, Rb, Ba, La and Ce etc. covering 26 major, minor, and trace elements in marine sedim...A method was developed for content determination of Na, Mg, A1, Si, P,S, C1, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Nb, Zr, Y, Sr, Rb, Ba, La and Ce etc. covering 26 major, minor, and trace elements in marine sediment samples using fused glass disc by X-ray Fluorescence spectrometry. Calibration was made using marine sediment certified reference materials and the synthetic standard samples prepared by mixing several marine sediments with stream sediment and carbonate standard samples in different proportions. The matrix effect was corrected using theoretical alpha coefficients, experience coefficients and the scattered radiation as the internal standard （for the trace elements）. The accuracy of the method was evaluated by analysis of certified reference materials GBW07314, GBW07334 and GSMS6. The results are in good agreement with the certified values of the standards with RSD less than 2.60%, except for Y, Cr, Ga, Ce, La, Nb, Rb, and V with RSD less than 9.0% （n=12）.展开更多
Although laser-induced breakdown spectroscopy(LIBS),as a fast on-line analysis technology,has great potential and competitiveness in the analysis of chemical composition and proximate analysis results of coal in therm...Although laser-induced breakdown spectroscopy(LIBS),as a fast on-line analysis technology,has great potential and competitiveness in the analysis of chemical composition and proximate analysis results of coal in thermal power plants,the measurement repeatability of LIBS needs to be further improved due to the difficulty in controlling the stability of the generated plasmas at present.In this paper,we propose a novel x-ray fluorescence(XRF) assisted LIBS method for high repeatability analysis of coal quality,which not only inherits the ability of LIBS to directly analyze organic elements such as C and H in coal,but also uses XRF to make up for the lack of stability of LIBS in determining other inorganic ash-forming elements.With the combination of elemental lines in LIBS and XRF spectra,the principal component analysis and the partial least squares are used to establish the prediction model and perform multi-elemental and proximate analysis of coal.Quantitative analysis results show that the relative standard deviation(RSD) of C is 0.15%,the RSDs of other elements are less than 4%,and the standard deviations of calorific value,ash content,sulfur content and volatile matter are 0.11 MJ kg,0.17%,0.79% and 0.41%respectively,indicating that the method has good repeatability in determination of coal quality.This work is helpful to accelerate the development of LIBS in the field of rapid measurement of coal entering the power plant and on-line monitoring of coal entering the furnace.展开更多
The structure around Ti^(4+) in Bao-SiO_2 -B_2O_3-TiO_2 had been studied by X-ray fluorescence spectra. The results show that the Ti^(4+) mainly exists in the [TiO_4] and enters the network of [SiO_4]. [TiO_4] has the...The structure around Ti^(4+) in Bao-SiO_2 -B_2O_3-TiO_2 had been studied by X-ray fluorescence spectra. The results show that the Ti^(4+) mainly exists in the [TiO_4] and enters the network of [SiO_4]. [TiO_4] has the tendency to change to [TiO_6] with the increase of TiO_2 con-tent. When the TiO_2 content increases to about 20mol% the tendency reaches its maximum.展开更多
<span style="font-family:Verdana;">A simple </span><span style="font-family:Verdana;">portable X-Ray Fluorescence (</span><span style="font-family:;" "=&qu...<span style="font-family:Verdana;">A simple </span><span style="font-family:Verdana;">portable X-Ray Fluorescence (</span><span style="font-family:;" "=""><span style="font-family:Verdana;">XRF) spectrometer was successfully used for </span><i><span style="font-family:Verdana;">in-situ</span></i><span style="font-family:Verdana;"> and nondestructive identification of the painting materials in two 15</span><sup><span style="font-family:Verdana;">th</span></sup><span style="font-family:Verdana;"> century icons from the Onufri Museum in Beart, Albania. </span></span><span style="font-family:Verdana;">The spectrometer is based on a low power X-ray tube, a thermoelectrically cooled Si PIN detector and the spectrum acquisition system. It was assembled and adjusted at our laboratory for the investigation of the icons. </span><span style="font-family:Verdana;">A small number of pigments were clearly identified by </span><span style="font-family:Verdana;">X-Ray Fluorescence (</span><span style="font-family:Verdana;">XRF) measurements in both icons. This include</span><span style="font-family:Verdana;">s</span><span style="font-family:;" "=""><span style="font-family:Verdana;"> Lead white for the white color, gold and yellow ochre for the yellow color, red lead, cinnabar and red ochre for the red color, as well as cooper based pigments for the green color. At the same time, the investigation raised some new questions that need further investigations by </span><span style="font-family:Verdana;">the use of additional analytical techniques. The results show that in both</span><span style="font-family:Verdana;"> icons are used similar pigments, which are in accordance with the Byzantine icon painting tradition.</span></span>展开更多
Separation of target elements or minerals from their host rock or ore is essential to successful mining operation. The inevitable loss of a portion of the desired material that accompanies each step in the extraction ...Separation of target elements or minerals from their host rock or ore is essential to successful mining operation. The inevitable loss of a portion of the desired material that accompanies each step in the extraction process must be documented to develop the operational protocol. Superposition of the characteristic X-ray fluorescence spectra of head (crushed rock ore particles, pre-processing) and tail (post-processing particles) samples provides a direct visual comparison of relative peak sizes, and thereby the relative concentrations, of elements of interest. If the head and tail peaks are identical, none of the element was recovered in the extraction process. At the other extreme if the tail peak “flat lines”, i.e., there is no peak, there was 100% recovery of that element. Standardless visual comparison is valid if the same mass of identical starting material is incorporated into the head and tail sample analysis pucks, and XRF analytical conditions are identical. The considerable time and expense of acquiring and calibrating the standards associated with XRF analysis of 75 or more elements are avoided, a significant advantage during initial broad screening of an experimental extraction procedure. Full quantitation by XRF or an alternate technique can proceed at a later project stage, if desired. The approach retains and presents all features of the original data, thus eliminating questions about data quality, standards and their calibration, and data manipulation in processing from raw counts to concentrations in printout tables. This form of display is ideal for both the mining professional and such less technical groups as corporate staff, investors, regulators, and the public. Examples presented herein are for heap leaching;the protocol can be applied as well to any of the other traditional ore processing and beneficiation procedures, e.g., gravity concentration, magnetic and electrical separation, froth flotation, and ore sorting.展开更多
用电感耦合等离子体质谱（inductively coupled plasma mass spectrometry,ICP-MS）测量某海滨城市50例胎儿脐血中铅（Pb）质量浓度,发现Pb超标（＆gt;100μg/L）为8%.根据婴儿母体是否常食用海产品,将50例样品分为常食用海产品（A组）...用电感耦合等离子体质谱（inductively coupled plasma mass spectrometry,ICP-MS）测量某海滨城市50例胎儿脐血中铅（Pb）质量浓度,发现Pb超标（＆gt;100μg/L）为8%.根据婴儿母体是否常食用海产品,将50例样品分为常食用海产品（A组）、偶尔食用海产品（B组）和极少食用海产品（C组）,用X射线荧光光谱分析（X-ray fluorescence,XRF）测量这3组婴儿毛发中的Pb质量分数,发现婴儿毛发中Pb质量分数具有显著性差异,由高至低依次为A组＆gt;B组＆gt;C组,其相应的脐血Pb质量分数也具有相同特征.同时对婴儿中的溴（Br）质量分数也进行了测量,发现Pb质量分数高的婴儿,其Br质量分数也显著偏高,由于海产品中Br质量分数远高于淡水产品,从另一方面说明,常食用海产品组的婴儿Pb质量分数偏高与母亲食用海产品有关.此外,对同一海滨城市393例儿童（2～11岁）血液中Pb质量分数进行统计学分析,得出Pb超标（〉100μg/L）为8.9%,说明海滨城市Pb污染仍对儿童具有一定的威胁.最后,通过对环境中常见的铅源（PM2.5、大气、油漆和海产品等）及人体摄入状况进行分析比较,认为食用铅污染的海产品是造成海滨城市胎儿铅超标的主要原因之一.展开更多
基金Supported by China Ministry of Science and Technology (2000DEB20081)China Ocean Mineral Resources R&D Association (COMRA) (No.DY105-05-01-05)+1 种基金China Ministry of Education(No.205089)China National Natural Science Foundation (No.40076015)
文摘A method was developed for content determination of Na, Mg, A1, Si, P,S, C1, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Nb, Zr, Y, Sr, Rb, Ba, La and Ce etc. covering 26 major, minor, and trace elements in marine sediment samples using fused glass disc by X-ray Fluorescence spectrometry. Calibration was made using marine sediment certified reference materials and the synthetic standard samples prepared by mixing several marine sediments with stream sediment and carbonate standard samples in different proportions. The matrix effect was corrected using theoretical alpha coefficients, experience coefficients and the scattered radiation as the internal standard （for the trace elements）. The accuracy of the method was evaluated by analysis of certified reference materials GBW07314, GBW07334 and GSMS6. The results are in good agreement with the certified values of the standards with RSD less than 2.60%, except for Y, Cr, Ga, Ce, La, Nb, Rb, and V with RSD less than 9.0% （n=12）.
基金supported by National Energy R&D Center of Petroleum Refining Technology of China(RIPP,SINOPEC)National Key Research and Development Program of China(No.2017YFA0304203)+5 种基金Changjiang Scholars and Innovative Research Team in University of Ministry of Education of China(No.IRT_17R70)National Natural Science Foundation of China(Nos.61975103,61875108,61775125 and 11434007)Industrial Application Innovation Project(No.627010407)Scientific and Technological Innovation Project of Shanxi Gemeng US-China Clean Energy R&D Center Co.,Ltd111 Project(D18001)Fund for Shanxi‘1331KSC’。
文摘Although laser-induced breakdown spectroscopy(LIBS),as a fast on-line analysis technology,has great potential and competitiveness in the analysis of chemical composition and proximate analysis results of coal in thermal power plants,the measurement repeatability of LIBS needs to be further improved due to the difficulty in controlling the stability of the generated plasmas at present.In this paper,we propose a novel x-ray fluorescence(XRF) assisted LIBS method for high repeatability analysis of coal quality,which not only inherits the ability of LIBS to directly analyze organic elements such as C and H in coal,but also uses XRF to make up for the lack of stability of LIBS in determining other inorganic ash-forming elements.With the combination of elemental lines in LIBS and XRF spectra,the principal component analysis and the partial least squares are used to establish the prediction model and perform multi-elemental and proximate analysis of coal.Quantitative analysis results show that the relative standard deviation(RSD) of C is 0.15%,the RSDs of other elements are less than 4%,and the standard deviations of calorific value,ash content,sulfur content and volatile matter are 0.11 MJ kg,0.17%,0.79% and 0.41%respectively,indicating that the method has good repeatability in determination of coal quality.This work is helpful to accelerate the development of LIBS in the field of rapid measurement of coal entering the power plant and on-line monitoring of coal entering the furnace.
文摘The structure around Ti^(4+) in Bao-SiO_2 -B_2O_3-TiO_2 had been studied by X-ray fluorescence spectra. The results show that the Ti^(4+) mainly exists in the [TiO_4] and enters the network of [SiO_4]. [TiO_4] has the tendency to change to [TiO_6] with the increase of TiO_2 con-tent. When the TiO_2 content increases to about 20mol% the tendency reaches its maximum.
文摘<span style="font-family:Verdana;">A simple </span><span style="font-family:Verdana;">portable X-Ray Fluorescence (</span><span style="font-family:;" "=""><span style="font-family:Verdana;">XRF) spectrometer was successfully used for </span><i><span style="font-family:Verdana;">in-situ</span></i><span style="font-family:Verdana;"> and nondestructive identification of the painting materials in two 15</span><sup><span style="font-family:Verdana;">th</span></sup><span style="font-family:Verdana;"> century icons from the Onufri Museum in Beart, Albania. </span></span><span style="font-family:Verdana;">The spectrometer is based on a low power X-ray tube, a thermoelectrically cooled Si PIN detector and the spectrum acquisition system. It was assembled and adjusted at our laboratory for the investigation of the icons. </span><span style="font-family:Verdana;">A small number of pigments were clearly identified by </span><span style="font-family:Verdana;">X-Ray Fluorescence (</span><span style="font-family:Verdana;">XRF) measurements in both icons. This include</span><span style="font-family:Verdana;">s</span><span style="font-family:;" "=""><span style="font-family:Verdana;"> Lead white for the white color, gold and yellow ochre for the yellow color, red lead, cinnabar and red ochre for the red color, as well as cooper based pigments for the green color. At the same time, the investigation raised some new questions that need further investigations by </span><span style="font-family:Verdana;">the use of additional analytical techniques. The results show that in both</span><span style="font-family:Verdana;"> icons are used similar pigments, which are in accordance with the Byzantine icon painting tradition.</span></span>
文摘Separation of target elements or minerals from their host rock or ore is essential to successful mining operation. The inevitable loss of a portion of the desired material that accompanies each step in the extraction process must be documented to develop the operational protocol. Superposition of the characteristic X-ray fluorescence spectra of head (crushed rock ore particles, pre-processing) and tail (post-processing particles) samples provides a direct visual comparison of relative peak sizes, and thereby the relative concentrations, of elements of interest. If the head and tail peaks are identical, none of the element was recovered in the extraction process. At the other extreme if the tail peak “flat lines”, i.e., there is no peak, there was 100% recovery of that element. Standardless visual comparison is valid if the same mass of identical starting material is incorporated into the head and tail sample analysis pucks, and XRF analytical conditions are identical. The considerable time and expense of acquiring and calibrating the standards associated with XRF analysis of 75 or more elements are avoided, a significant advantage during initial broad screening of an experimental extraction procedure. Full quantitation by XRF or an alternate technique can proceed at a later project stage, if desired. The approach retains and presents all features of the original data, thus eliminating questions about data quality, standards and their calibration, and data manipulation in processing from raw counts to concentrations in printout tables. This form of display is ideal for both the mining professional and such less technical groups as corporate staff, investors, regulators, and the public. Examples presented herein are for heap leaching;the protocol can be applied as well to any of the other traditional ore processing and beneficiation procedures, e.g., gravity concentration, magnetic and electrical separation, froth flotation, and ore sorting.
