28 March 2025, Volume 45 Issue 3
    

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  • Discussion on evolution law of inclusions intire cord steel from billet to wire rod
    WU Yuanyuan, JIN Chuanwei, ZHANG Jiming, MA Han
    Metallurgical Analysis. 2025, 45(3): 1-9. https://doi.org/10.13228/j.boyuan.issn1000-7571.012629
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    Large non-deformable inclusions are one of the main causes of wire breakage for tire cord steels during drawing and stranding.Therefore,it is necessary to study the types and evolution law of inclusions in the tire cord steel.In the paper,the type and morphological evolution law of inclusions in 82A tire cord steel from billet to wire rod were investigated by the means of focused ion beam-electron beam scanning electron microscopy(FIB-SEM),energy disperse spectroscopy(EDS) and three-dimensional reconstruction software.The results showed that the main types of inclusions were MnS,MnS-SiO2 and MnS-SiO2-CaMgAlMnSiO.The planar morphology of MnS inclusions in the billet were mostly elliptical or nearly round,while the morphology of MnS in the wire rod became elongated strip shape.The planar morphology of MnS-SiO2 inclusions in the billet had the core of nearly round SiO2, and the outer layer was wrapped MnS.In the wire rod,its morphology was still maintained in the nearly round SiO2 as the core,but the MnS wrapped on outer layer became long stripes,showing the overall appearance of "eye-shaped".The planar morphology of MnS-SiO2-CaMgAlMnSiO inclusions in the billet was based on SiO2 as the core,which was wrapped with composite oxides enriched in Ca,Mg,Al,Mn,Si and O,and the outermost layer was MnS.In wire rod,the deformation of SiO2 was not obvious,and composite oxides became fragmented. Moreover,MnS was elongated,and the whole morphology showed string-like distribution along the drawing direction.The study on the evolution law of inclusions type and morphology provided process control direction for the analysis of inclusions harm and the development of high-end tire cord steel.
  • Solid waste identification of materials containing metallic elemental substance
    WU Suru, LI Quanbin, ZHANG Qingjian, ZHU Jinbo, MA Hui, YAO Yirong
    Metallurgical Analysis. 2025, 45(3): 10-16. https://doi.org/10.13228/j.boyuan.issn1000-7571.012663
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    The sample declared as "coarse zinc powder and brass powder" belongs to the materials with metallic elemental substance as the main chemical composition.These materials have been reduced and purified significantly,but the quality is still varied and the solid waste identification is difficult.According to the judgment approach of GB 34330-2017,the source inferring of such samples plays an important role in the identification of solid waste attribute.In this study,the solid waste identification of two typical metallurgical products materials,i.e.,zinc powder and brass powder,was conducted by analyzing the characteristics of element content,phase composition,microscopic appearance,and particle size distribution.The important role of microscopic appearance in inferring the source process of samples was discussed,and the method for solid waste identification of materials containing with metallic elemental substances was established.The main phase of zinc powder was metallic zinc followed by zinc oxide and tetrabasic zinc chloride.The microscopic appearance of zinc powder was spherical,which was mainly from the pyrometallurgical volatilization process.The main phases of brass powder were copper-zinc alloy and metallic lead,and it also contained some copper oxide,cuprous oxide and zinc oxide as well as little Cu6Al2(OH)16CO34H2O.Moreover,there was also cotton impurity.Moreover,the microscopic appearance of brass powder was long curl strip shaped like a knife cutting,and it was mainly from the processing techniques of grinding cutting and polishing.Finally,the solid waste attribute of actual sample containing metallic elemental substance was identified using GB 34330-2017 as the basis,which provided technical support for the customs enforcement.
  • Determination of hafnium,niobium,tantalum and zirconium in geochemical exploration sample by inductively coupled plasma mass spectrometry with ammonium fluoride digestion and triethylamine sensitization
    LIU Keke, XIE Yaxiong, MIAO Liang, LI Guoguo, DONG Xueliang
    Metallurgical Analysis. 2025, 45(3): 17-24. https://doi.org/10.13228/j.boyuan.issn1000-7571.012666
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    The accurate determination of high field strength elements(HFSE) in geochemical exploration samples such as hafnium(Hf),niobium(Nb),tantalum(Ta) and zirconium(Zr) is the important prerequisite for achieving information on the diagenetic evolution of rocks.In this study,the solid melt digestion method using ammonium fluoride was combined with the sensitization technology using triethylamine as the matrix modifier.The method for the determination of Hf,Nb,Ta and Zr in geochemical exploration sample by inductively coupled plasma mass spectrometry(ICP-MS) was established.The pretreatment of sample had two steps.Firstly,the sample was melted with ammonium fluoride at 240 ℃ for 2.5 h,where the mass ratio of ammonium fluoride and sample was 6∶1.Then,certain amount of perchloric acid were added to dissolve the sample.After evaporation,the nitric acid and a small amount of hydrochloric acid was added for redissolution-evaporation,realizing the complete digestion of sample.After evaporating the solution to almost dryness,the residue was redissolved with nitric acid.2%(volume fraction,the same below) nitric acid-0.2% hydrofluoric acid was added as the determination medium to avoid the hydrolysis or polymerization of Nb and Ta.10% triethylamine was used as matrix modifier for determination.The normalized signal intensity of Hf,Nb,Ta and Zr increased by 1.8,12.5,2.9 and 3.3 times,respectively.The linear correlation coefficients of calibration curves of elements were all higher than 0.999.The limits of detection of method were between 2.23 and 22.7 μg/kg,and the limits of quantification were between 7.43 and 75.8 μg/kg.The contents of Hf,Nb,Ta and Zr in certified reference materials of soil,rock and stream sediment were analyzed according to the experimental method.Each sample was determined for 12 times in parallel.The results showed that the measured values were basically consistent with the certified values.The logarithmic deviations(ΔlgC) between measurement average and standard value were all less than 0.05.The relative errors(RE) were between -1.7% and 8.0%,and relative standard deviations(RSDs,n=12) were between 1.7% and 9.0%,which could meet the accuracy requirements specified in industry standard DZ/T 0167-2006.Two soil samples from northern area of Henan were determined according to the experimental method and standard method,i.e.,hydrofluoric acid-nitric acid closed dissolution-ICP-MS in GB/T 14506.30-2010.Each sample was determined for 6 times in parallel.The results showed that the measurement values of two methods were basically consistent. The RSDs of analytical results of experimental method were between 1.5% and 6.1%.
  • Determination of gold in copper concentrate by inductively coupled plasma mass spectrometry with methyl isobutyl ketone extraction
    YANG Chunyan, WANG Yanqiu, CHANG Huan, ZHANG Xiuyan
    Metallurgical Analysis. 2025, 45(3): 25-30. https://doi.org/10.13228/j.boyuan.issn1000-7571.012662
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    Gold is a kind of conventional pricing elements in copper concentrate,and the accurate determination of its content has important guiding significance for the smelting,development and factory settlement of copper concentrate.In this study,the sample was dissolved with aqua regia -HF-HClO4 system, and gold in solution was extracted with 20 mL of methyl isobutyl ketone(MIBK). 196.967Au+ was selected as the measuring isotope.The method for the determination of gold in copper concentrate by inductively coupled plasma mass spectrometry(ICP-MS) with MIBK extraction was established.The calibration curve was prepared using the mass concentration of gold as x-axis and using intensity ratio of gold to cesium internal standard as y-axis.The linear correlation coefficient was higher than 0.999.The limit of detection of was 0.039 g/t,and the limit of quantification was 0.13 g/t.The certified reference material and sample of copper concentrate were selected and determined according to the experimental method.For the sample,the fire assay gravimetry was used for the method contrast test.Meanwhile,the standard solution of gold was added into copper concentrate sample for the spiked recovery test.The results showed that the measurement results of certified reference material were basically consistent with the certified values.For the sample,the determination results of experimental method were basically consistent with those obtained by the fire assay gravimetry.The recoveries were between 96% and 109%.The content of gold in two copper concentrate samples were determined according to the experimental method,and the relative standard deviations(RSD, n=10) of determination results were 0.77% and 2.1%,respectively.
  • Effect of electrolysis parameters on electrolytic extraction of precipitated phases in GH4169 superalloy
    XIANG Xuemei, ZHANG Henglei, ZHANG Feifei, XU Qiankun, ZHANG Yueying, YANG Zhongyuan
    Metallurgical Analysis. 2025, 45(3): 31-37. https://doi.org/10.13228/j.boyuan.issn1000-7571.012641
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    Superalloys have high alloying degree and complex composition of precipitated phases.The qualitative and quantitative analysis of precipitated phases in superalloys is of great significance for the service evaluation of superalloys.In this paper,the precipitated phases in GH4169 superalloy were extracted and analyzed by electrolytic extraction.The effects of electrolysis parameters,including electric current density,electrolysis time and temperature,on extraction of precipitated phases were investigated by scanning electron microscope(SEM) observation and X-ray diffraction(XRD).The results showed that the ambient temperature could not exceed 20 ℃ when ammonium sulfate-citric acid solution was used as electrolyte,otherwise it would lead to the hydrolysis of nickel.The time of single electrolysis could not be too long,otherwise it would lead to anode precipitation pollution.The optimum electrolysis conditions for extracting the precipitated phases in GH4169 superalloy were obtained as follows:the electrolyte was 10 g/L ammonium sulfate-10 g/L citric acid solution;the time of single electrolysis extraction was not more than 8 h;the current density was about 0.05 A/cm2;the electrolysis temperature was 17-20 ℃.
  • In-depth analysis of element oxygen K factor in electron probe micro analyzer Oxide ZAF correction method
    YU Junfang, ZHANG Xiaofeng, HU Jinsheng, CHEN Zhenyu, MENG Wenxiang, QIAO Qiao
    Metallurgical Analysis. 2025, 45(3): 38-43. https://doi.org/10.13228/j.boyuan.issn1000-7571.012589
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    When the electron probe micro analyzer(EPMA) is used for the quantitative analysis of oxide minerals,the Oxide ZAF correction method (without measurement of O element K factor, abbreviated as Oxide ZAF method) is usually used instead of Metal ZAF method(measurement of O element K factor).Although the results are very reliable,it is not consistent with the previous understanding of ZAF correction(all elements are required to participate in the analysis especially for the high-content elements).In order to have a deeper understanding on the correction process of Oxide ZAF,and so that the most suitable correction method can be selected for the quantitative analysis of different substances in the future,the ferromagnesia olivine[w(O)=44.00%,w(Mg)=31.41%,w(Fe)=6.27%,w(Si)=18.35%,w(Ni)=0.33%,w(Mn)=0.06%] was taken as the sample in this study,and the two correction methods were used for quantitative analysis and comparison.Then the iterative calculation process was shown by the ZAF simulation program,and the important theory that the K factor of O element in Oxide ZAF method was not measured directly,but it still participated in ZAF correction was verified.In addition,the application range of Oxide ZAF method was discussed,that was,the sample should strictly follow the oxide formula and the chemical valence state of each cation was single.A more widely used CAL quantitative analysis method was proposed.This method could be used for the quantitative analysis of carbonate,water-containing samples and minerals containing F,Cl,OH and Li and Be elements.
  • Determination of total inorganic carbon in organic decarbonization liquid by inductively coupled plasma atomic emission spectrometry with swirling gas-liquid separation
    MA Anju, CHENG Yong, YUAN Jinhong, HE Qiping, WEI Fang
    Metallurgical Analysis. 2025, 45(3): 44-50. https://doi.org/10.13228/j.boyuan.issn1000-7571.012658
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    The capture and adsorption of carbon dioxide in industrial flue gas by organic decarbonization liquid such as alkanolamine is one of the mainstream technologies for carbon compliance.The accurate determination of total inorganic carbon content in the form of inorganic carbonate is crucial for the performance evaluation of decarbonization liquid and the optimization of capture process,while the coexistence of organic matrix will seriously interfere with the determination results.In this study,a swirling gas-liquid separation device for separating inorganic carbon from organic solution was constructed using the original part of atomization transfer system of inductively coupled plasma atomic emission spectrometer(ICP-AES).By online mixing of hydrochloric acid with organic decarburization liquid,the inorganic carbon was converted into gaseous carbon dioxide and then determined.Consequently,a method for the determination of total inorganic carbon in organic decarburization liquid by inductively coupled plasma atomic emission spectrometry was established.The influence of reactor length,carrier gas flow rate and hydrochloric acid concentration on the determination of inorganic carbon and the gas-liquid separation effect was investigated.The optimized determination conditions were obtained as follows:the reaction cell length was 6 cm,the carrier gas flow rate was 0.3 L/min,the reaction agent was hydrochloric acid(1+1),and the analytical line was C 193.030 nm.The calibration curve was drawn with diethanolamine(DEA) as the medium.The results showed that the linear correlation coefficient was higher than 0.999 when the mass concentration of inorganic carbon was in the range of 10-720 mg/L.The limit of detection was 0.039 mg/L.The content of total inorganic carbon in alkanolamine solution sample after absorbing carbon dioxide was determined according to the experimental method.The relative standard deviation(RSD,n=10) was not more than 5.6%,and the recoveries were 98%-105%.The method effectively solved the interference problem of organic matrix with the detection of inorganic carbon,and it could meet the rapid analysis requirement of inorganic carbon in various industrial organic decarbonization liquids.
  • Determination of yttrium and neodymium in wrought magnesium alloyflat ingot by inductively coupled plasma atomic emission spectrometry
    WANG Yueqiang, ZHAO Jianfeng, WANG Binqi, YANG Yongtao
    Metallurgical Analysis. 2025, 45(3): 51-56. https://doi.org/10.13228/j.boyuan.issn1000-7571.012621
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    Yttrium(Y) and neodymium(Nd) are two important alloying elements in wrought magnesium alloy ingot.Therefore,the accurate determination of Y and Nd contents in wrought magnesium alloy ingot is of great significance for the product performance development.In this study,the samples were dissolved with 25 mL of hydrochloric acid(1+1) at room temperature for 5 min.Y 377.433 nm and Nd 401.225 nm were selected as the analytical lines for Y and Nd.The calibration curve was prepared by matrix matching method to eliminate the influence caused by matrix effect.A method for the determination of Y and Nd in wrought magnesium alloy flat ingot by inductively coupled plasma atomic emission spectrometry(ICP-AES) was established.The results showed that the linear correlation coefficients of calibration curves of Y and Nd were both 0.999 9. The limits of detection of Y and Nd were 0.000 84% and 0.000 73%,and the limits of quantification were 0.002 8% and 0.002 4%,respectively.The proposed method was applied for the determination of Y and Nd in magnesium alloy CRMs,the measurement results were consistent with the standard values.The contents of Y and Nd in three wrought magnesium alloy flat ingot samples were determined according to the experimental method,and the precision investigation and spiked recovery experiment were carried out.The relative standard deviations(RSD, n=6) of determination results were between 0.30% and 1.3%.The recoveries were between 94% and 101%.
  • Discussion on decomposition method during the determination of multi-elements in ferroboron by inductively coupled plasma atomic emission spectrometry
    MA Shufeng, LI Yahua, ZHANG Cuimin
    Metallurgical Analysis. 2025, 45(3): 57-63. https://doi.org/10.13228/j.boyuan.issn1000-7571.012601
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    With the development of new technologies,some novel ferroboron alloys with different properties are developed.The contents of different elements in ferroboron determines the properties of alloys.At present,the alkali melting method or acid dissolution slag method is usually used for pretreatment of ferroboron sample before detection of elements.Although the sample can be dissolved completely and the simultaneous determination can be achieved,these methods are cumbersome if some elements are determined separately.Therefore,it is very important to choose the appropriate decomposition method for different elements in consideration of the perspective of economy and time cost.In this study,the certified reference materials(CRM) of ferroboron were digested using various decomposition methods including direct acid dissolution method(nitric acid+hydrofluoric acid+perchloric acid),microwave digestion method,acid dissolution slag method and alkali melting method.Then, the contents of chromium,nickel,vanadium,copper,titanium,manganese,aluminum and phosphorus in the digestion solution using different decomposition methods were determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The results showed that there were few black insoluble matters in the solution when the direct acid dissolution and microwave digestion were used,but the accurate determination of chromium,nickel,vanadium,copper,titanium and manganese was not affected.However,the determination results of aluminum and phosphorus were relatively lower than the certified values or standard values,especially for phosphorus.It indicated that the degree of dissolution of the sample had significant influence on the accurate determination of aluminum and phosphorus.Therefore,for the determination of chromium,nickel,vanadium,copper,titanium and manganese,the four dissolution methods above were all acceptable.However,for the determination of aluminum and phosphorus,the sample must be completely dissolved using acid dissolution slag method and alkali melting method to obtain accurate results.
  • Determination of titanium carbide in titanium carbide slag by X-ray fluorescence spectrometry with fusion sample preparation
    FENG Zongping, YANG Xinneng
    Metallurgical Analysis. 2025, 45(3): 64-69. https://doi.org/10.13228/j.boyuan.issn1000-7571.012623
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    The accurate determination of titanium carbide content in titanium carbide slag(titanium carbide) plays a key role in the guidance of carbonization production process.In this study,the hydrochloric acid-sulfuric acid-hydrofluoric acid system was used to selectively dissolve titanium oxide,realizing the rapid separation of titanium oxide and titanium carbide phases in titanium carbide slag.After separation,the residue and filter paper were ashed and burned at 600-700 ℃ for 20 min,and then burned at 1 100 ℃ for 2-3 min.Lithium tetraborate-lithium carbonate was selected as the flux,and lithium bromide was selected as the release agent.The sample was fused at 1 100 ℃ for 20 min to prepare the transparent bead.A method for the determination of titanium carbide in titanium carbide slag by X-ray fluorescence spectrometry with fusion sample preparation was established.After the titanium carbide slag sample was separated using the hydrochloric acid-sulfuric acid-hydrofluoric acid system,titanium carbide in the residue could be converted to titanium dioxide through burning at high temperature.Therefore,nine samples of spectrally pure titanium dioxide(5.0-80.0 mg) were used to draw the calibration curve.The linear correlation coefficient was r=0.999 98,and the determination range of titanium dioxide was 1.25%-20.0%.The contents of titanium carbide in two titanium carbide slag samples were determined according to the experimental method,and the relative standard deviations(RSD,n=6) of the determination results were not more than 0.5%.Three titanium carbide slag samples were selected and determined according to the experimental method.Then the high-purity titanium carbide was added for the spiked recovery test.The recoveries were between 97% and 102%.The contents of titanium carbide in titanium carbide slag samples were determined by the experimental method and spectrophotometry respectively,and the results were consistent.
  • Determination of mercury in graphite ore by direct mercury analyzer with solid sampling
    SUN Menghua, CHEN Chao, LIU Aiqin, QIAO SongfenRAN Zhuo, TIAN Qing
    Metallurgical Analysis. 2025, 45(3): 70-75. https://doi.org/10.13228/j.boyuan.issn1000-7571.012661
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    The accurately determination of mercury content in graphite ore is of great significance for promoting the processing and comprehensive utilization of graphite ore resources as well as the protection of ecological environment.In this study,the decompositon conditions were optimized through orthogonal experimental method:the sample mass was 0.10 g;the decomposition time was 40 s;the decomposition temperature was 650 ℃.A method for the accurate determination of mercury in graphite ore by direct mercury analyzer with solid sampling was established.The contents of mercury in graphite ore samples were determined by three methods,i.e.,aqua regia water bath digestion-atomic fluorescence spectrometry(AFS),high-temperature and high-pressure microwave digestion-atomic fluorescence spectrometry,and direct mercury analyzer with solid sampling.The comparison results of mercury by different methods showed that the stability of determination results by direct mercury analyzer with solid sampling was good,and the relative standard deviation(RSD) was significantly better than the other two methods.When the mercury content was 1.0-20 ng,the absorbance of mercury showed good linearity with its content with the linear correlation coefficient of 0.999 5.The limit of detection was 1.00 ng/g and the limit of quantification was 3.00 ng/g.Three graphite ore samples with different mercury contents were selected and determined according to the experimental method.In addition,equal amounts of certified reference materials of soil(GBW07427 and GBW07426) and rock(GBW07103) were added for the spiked recovery test.The results showed that the RSD(n=12) of mercury in graphite ore samples were 1.0%-1.9%,and the recoveries were 98%-107%.Eight laboratories were selected for experimental testing.Three graphite ore verification samples were determined for 11 times according to the experimental method in each laboratory.The results provided by the laboratories were statistically analyzed according to GB/T 6379.2-2004.The repeatability limit of this method was r=0.04+0.092 8wHg,and the reproducibility limit was R=0.21+0.123wHg(wHg is the mass fraction of Hg).
  • Preparation of chitosan/sodium polystyrene sulfonate composite microsphere and its adsorption performance for copper(Ⅱ) in wastewater
    ZHANG Yan, LUO Xiaoqiang
    Metallurgical Analysis. 2025, 45(3): 76-83. https://doi.org/10.13228/j.boyuan.issn1000-7571.012651
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    The mass ratio of chitosan to sodium polystyrene sulfonate was controlled at 8∶1,and the mass ratio of chitosan to glutaraldehyde was 3∶1.The chitosan/sodium polystyrene sulfonate composite microsphere was prepared by titration-curing packaging method.The microsphere was characterized by scanning electron microscope(SEM),Fourier transform infrared spectroscopy(FT-IR) and N2 adsorption/desorption isotherm curve.The adsorption performance for copper(Ⅱ) in wastewater was investigated.The results showed that composite microsphere after freeze drying contained chitosan and sodium polystyrene sulfonate.There were many micropores on the surface with large specific surface area.When the mass concentration of composite microsphere was 1.0 g/L,the pH of solution was 6.0,and the temperature was 30 ℃,the saturated adsorption capacity reached to 167.92 mg/g for copper(Ⅱ) after adsorption in 50 mL of 100 mg/L simulated copper-containing wastewater for 12 h.The equilibrium adsorption capacity of composite microsphere was still 89.2 mg/g after five recycles of adsorption-regeneration,indicating the good reusability of this material.The results of adsorption kinetics experiments showed that the adsorption of copper(Ⅱ) was mainly physical absorption when the dosage of composite microsphere was low (0.50 g/L),while it was chemical absorption when the dosage of composite microsphere was relatively high (not less than 1.0 g/L).The adsorption process conformed to the characteristics of Langmuir isotherm absorption model.The prepared chitosan/sodium polystyrene sulfonate composite microsphere had good adsorption performance for copper(Ⅱ),and it was an ideal material for the treatment of wastewater which was polluted by copper(Ⅱ).
  • Determination of antimony in antimony impregnated graphite by ceric sulfate titration after decomposition of sulfuric acid-potassium sulfate-perchloric acid-nitric acid system
    XIAO Liuping, TIAN Ningchen, LIU Wei
    Metallurgical Analysis. 2025, 45(3): 84-89. https://doi.org/10.13228/j.boyuan.issn1000-7571.012656
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    The accurate determination of antimony content in antimony impregnated graphite is of great significance for optimizing production process and improving material performance.The antimony impregnated graphite contains graphite with stable structure,which is difficult to be decomposed completely.In experiments,the sample was decomposed with 20 mL of sulfuric acid-1.0 g of potassium sulfate-1.5 mL of perchloric acid-1.5 mL of nitric acid.If the graphitization degree of sample was too high which could not be decomposed completely at one time,the sample could be fully decomposed by adding 1.5 mL of perchloric acid,1.5 mL of nitric acid for several times.The method for the analysis of antimony in antimony impregnated graphite by ceric sulfate titration was established.2# antimony impregnated graphite sample(the graphitization degree was 98%) was selected as the object of investigation.The sample before decomposition,the residue after the first decomposition,and the solution after adding perchloric acid and nitric acid for four times were characterized by Raman spectroscopy.The results showed that the D peak which represented the lattice defect of carbon atom in residue disappeared after the first decomposition,while the G peak and 2D peak(which represented in-plane telescopic vibration of sp2 hybrid and interlayer stacking,respectively) still existed but the strength was weakened.It indicated that the defective graphite was decomposed firstly,and the residue was non-defective graphite with perfect structure.After adding perchloric acid and nitric acid for four times,the G peak and 2D peak of solution disappeared,indicating that the non-defective graphite could be decomposed completely after adding perchloric acid and nitric acid for several times.The experimental method was applied to the determination of antimony in antimony impregnated graphite samples.The relative standard deviations(RSD,n=7) of determination results were 0.32% and 0.78%,and the recoveries were between 99.5% and 103%.According to the composition of antimony impregnated graphite samples,three simulated samples of antimony impregnated graphite with antimony content in range of 10%-30% were prepared from a certain amount of high purity graphite and antimony powder.The simulated samples were determined according to the experimental method,and the measured results were basically consistent with the theoretical values.
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