改进的等离子体原子发射光谱分析技术在矿产勘查样品中的应用研

1、改进的等离子体原子发射光谱分析技术在矿产勘查样品中的应用研针对矿产勘查样品特点对JA90-750型ICP-AES（Inductively CoupledPlasma-Atomic Emission Spectrometry）进行技术改进，研发出新的测控系统分析软件，利用通用微机系统就可控制ICP-AES进行分析测试，并改善了仪器分析性能，该仪器改进技术具有通用性和可移椊性。建立具有通用性的矿产勘查样品ICP-AES系统分析方法群：ICP-AES技术硅酸盐岩石快速全分析方法，上需要分离同时测定主、次成分的ICP-AES技术硫化物单矿物全分析方法和微波辅助溶样ICP-AES技术生物地球化学样品多元

2、素同时测定的分析方法。采用标准物质法进行ICP-AES测定条件的系统研究，硅酸盐岩石全分析百分总和测量误差在0.03%0.39%之间，微量元素测量误差在0.00%9.68%之间，RSD%在0.54%6.32%之间。单矿物分析应用线性回归理论作为基体元素干扰的校正依据，采用标准溶液基体匹配和干扰系数校正法达到单矿物全分析的目的。以数理统计的方式确定最佳溶样方法，分别建立生物组织微波消解和椊物样品湿法酸消解的分解方法。分析方法均符合矿产勘查样品批量检测要求Application of geochemistry exploration samples analysis methods base on

3、improved inductively coupled plasma-atomic emission spectrometry ICP-AEStechnique. For the research and development purpose of geochemistry explorationsamples analysis, using the updated JA90-750 type spectrometer as operationalplatform. This instrument is improved by adopted advanced currency inter

4、facetechnique and Windows operating system. The modern microcomputer replacePDP-8A computer of old and fall behind. This new computer broadened andstrengthened the function of the ICP spectrometer and improved the whole level ofthe ICP-AES. Development a series of test control system, which is direc

5、tedagainst the old type of ICP spectrometer by import and could be applied on thesame type of spectrometers. Especially, utilizing the results of the new softwarestudy exploit an analytical application software package aiming at the batchquantity analysis of geochemistry exploration samples. Simulta

6、neity using the newsoftware proceed exploratory research for analytic methods. The new analyticmethod of systematical, omni-directional, multi-element simultaneity determinat-ion is build up analysis of minerals exploration samples by ICP-AES. Utilizing newanalytical methods fulfilled samples analys

7、is work of elements determination atsome minerals exploration research work.The detection limits and the precisions of this ICP-AES have amelioration forelements of 2 3 by the instrument technique improved. For example, the detection limits and the precisions have good amelioration for microelements

8、 Cd Co LaMo Nb Ni Pb Zn and macroelements Al Fe Ca Mg Si. The detection limitsobtained inequality lowered from one half to one order of magnitude. General theprecisions increase about one time as old precisions. The detection limits or theprecisions also have commonly amelioration to microelements B

9、 Cr Cu P ThTi V Y Zr. Yet analysis capability of 1 7 elements keep original level. Analyticcapability of the instrument for microelement are improved not only advantage togeochemistry exploration samples analysis but advantage to biogeochemistrysample analysis of elements content lower order.Aimed a

10、t the disadvantage of old ICP-AES analytic software program havenot the function for automatic determination interference correction coefficient,new test control software system add this function for automatic determinationbackground interference correction coefficient and element interference corre

11、ctioncoefficient. Old analysis program is basis measuring result of interference elementsolution for different concentration, manual work calculate processed interferencecorrection coefficient by single element. This calculation mode is a complexoperation work for geochemistry exploration samples an

12、alysis of matrix complexand interference severity. Simultaneity the error of this calculation mode forinterference factor also is not allow ignore. New software to make use of computersuper-strength function have new function of automatic test for background andelement interference correction coeffi

13、cient. The new function can calculate someinterference correction factors by formulation simulation interference samples.Those interference factors at any moment can transfer from analytic program of thenew software by computer in store. This improved technique can settle the problemof interference

14、correction complication. The operation process of interferencecorrection truly reach easily and speedy and accurate. This function is very availfor minerals exploration sample analysis.Dynamic interference correction function of new software developed directedagainst characteristic of main element c

15、oncentration range change larger for geochemistry exploration samples. The method can store many interferencecorrection coefficients in analytic software by determination different concentrationrange of interference elements. In practice analysis, selection suitable interferencecorrection coefficien

16、ts are on the basis of practicable content of interferenceelements in geochemistry exploration samples. This method achieve the purpose ofaccurate determination.Application of ICP-AES technique for sulfide monomineral total analysis, notonly can be used analysis operation easily, but directed agains

17、t characteristic ofmonomineral samples quantity, ICP-AES analytic technique is very propermonomineral analysis because this method has a excellence of consumed a littlesample and simultaneity multielement for testing. For carried gold mineral sulfidemonomineral, its main element are S and also have

18、microelement Au and Ag , theseelements can test simultaneity by ICP-AES. In addition, the background andspectral interference is eliminated by adopted method of matrix matching andinterference coefficient correction. The automatic test interference correction factorfunction increase by technique imp

19、rove for old analytic software. This methodcan greatly reduce chance of analytic error comparatively opposite with the methodof separate and enrichment eliminate interference possibility introduced a ratherlarge analytic error. The method can gain the result of credibility accuracy and highstability

20、1. Technique improved of JA90-750 type ICP spectrometer hardwaresystem for geology samplesThe ICP spectrometer mainly is composed of ICP excitation light source andbeam splitting system and photoelectric incept and enlargement measuring systemand data processing and printing system. The improved of

21、JA90-750 type ICPspectrometer hardware system replace the old PDP-8A computer andLA-120typewrite by the advanced computer control system. The advancedcomputer can control ICP spectrometer by the currency interface technique. The first step of apparatus improvement is the improvement of interfacecirc

22、uit-board. A new currency interface circuit-board replace the old of the primarymachine, which could replace the old PDP-8A computer by the currencymicrocomputer. The next step of apparatus improvement is the improvement of thephotoelectric measuring circuit for data collection system. The method ad

23、opted thedesign of integral circuit to enduringly combine the photoelectric multiplier cell inthe measuring system of the spectrometer and the integral capacitance, which mayeliminate a main electrical leakage and effectively reduce the noise level.Aimed of hardware improvement is using the currency

24、 microcomputer systemto control the ICP spectrometer to analysis and test the mineral exploration samples.In the improvement process, the method designed according to primary propertiesand present state of the JA90-750 type ICP spectrometer, which broadened andincreased the function of the old equip

25、ment. The new interface board adopts is thecurrency high-quality devices, which uses two interface boards instead of the oldthree ones. This improvement could not only diminish the broads area to 1 8 ofthe old ones, but also be applied to all the currency microcomputers, which makesthe repair and re

26、placing of the computers more convenient and fully utilizes theadvanced function of modern microcomputers to carry out the analysis and testingprocedure of ICP. Moreover, the modern microcomputers RAM has supercapability, this is unsurmountable for traditional PDP8A computer of 8 MB EMSmemory. The n

27、ew additional equipments, such as the laser printer, color display,CD-ROM, soft disk, hard disk and USB interface, enable the visual operation,these enhance the whole standard level of the instruments. The method couldcompletely utilize these machines and the usage lives of them are prolonged.2. Dev

28、elopment of JA90-750 type ICP spectrometer analysis softwareThe improvement of the software is mainly the development of real time testand control analysis software of JA90-750 type ICP spectrometer. The newsoftware is under Windows operating system aimed at minerals exploration samples application.

29、 The superstratum interface of ICP real time test and controlsystem software was written by Visual Basic 5.0 language. The dynamic librarywas built up by the mixture program of Visual C+ 5.0 embed assembly languageand this software used dynamic library to accomplish the bottom operation. On thedesig

30、n of the software, it is assimilated the advantages of the software from TJAand PE the international famous American Company and from JY FrenchCompany , and combined the ideas of visualized program, network program,object facing program, modularized program and database program. The softwarecould cl

31、assify the contents of the work according to the great deal of informationgiven. The running process of the software establish the working object bydefinitude their relationships. The new software was added some functionalmodules, such as the visual element tracing, the editing and choosing of repor

32、tprinting format, the offline simulation, the network test and control program andthe usage help, etc., which made the system software multifunctional and easy tohandle. The most important character of the new software is its compatibility ofcomputer system and the strong ability for transplantation

33、.3. Application of quickly total analysis for geochemistry explorationsamples rock soil river system sediment by ICP-AES techniqueFor the application of rock total analysis of geochemistry exploration samplessuch as rock, soil and river system sediment , the method studied and discussedthe disposal

34、technique of silicate rock total analysis samples and the testingcondition of ICP-AES instrument.xThe method used national A standard geological normal substanceGBW07103 GBW07309 to prepare the corresponding waiting behind-testmixture solution, which contained constant element, microelement and trac

35、eelement for testing. The method also systematically studied the testing condition ofICP-AES technology and confirmed the best condition.yThe silicate rock total analysis standard solution, except SiO2, was all prepared by the fusing of artificial synthesized rock and lithium metaborate, andthen add

36、ed every kind of element standard solution as the high-grade standardsolution. The SiO2 high-grade standard solution was prepared by the fusing of rocknormal substance GBW07103 and lithium metaborate.zThe method systematically studied the mineral dissolving technique and thetesting condition, respec

37、tively established the analysis method of the ICP-AESsilicate rock total analytical lithium metaborate fusing system and theHF-HClO4-HCl-HNO3 four acids mixed acid dissolved system. The lithiummetaborate system contains ten main groups, such as silicon, kalium and natrium,and others multi-microeleme

38、nts. The lithium metaborate was fused at 950 for 15minutes and the melting blocks were quenched by ice-water. Then the 5% nitricacid solution at 70 was stirred by the constant temperature induction and wasoff-crucible after ten or twenty minutes. The four acid mixed solution dissolvedsystem was dire

39、ctly used to determine the dissolved samples of more than twentykinds of constant elements, microelements and trace elements in rocks, soils andriver system sediments. This analysis method is quick, sensitive and easy to operate.This method only takes two days to finish a silicate rock total analysi

40、s flow. Themethod solves the technique problem of silicate rock total analysis for testing thegreat batch samples of geochemistry exploration samples analysis. The lower limitof this method satisfies the analysis requirement of minerals exploration samples.The precision and accuracy of the method ar

41、e validated by national A standardsubstance. Testing by the batch samples of minerals exploration, the method hasthe low limit for detection, high precision, fine accuracy and quick analytical speed.The method could completely be up to samples of geochemistry exploration toanalytical methods.4. Appl

42、ication of total analysis for geochemistry exploration samplessingle minerals by ICP-AES technologyWith the development of geology science, it becomes a new way to look for minerals by studying minerals. There are also more and more requirements for thetotal analysis of single minerals presently. Be

43、cause the distribution and groupchange of elements always reflect some latent indiscoverable rules and the groupand ratio of these microelements are especially sensitive indications ofmetallogenic process, the study of single minerals could provide related scienceinformation for metallogenic forecas

44、t and general exploration.ICP-AES technology could simultaneously test many group and consumesonly a few amounts of samples, which has especial advantages for the total analysisof single minerals for limited amount of samples. The method respectivelyestablished the acid dissolved system of pyrite, c

45、halcopyrite, sphaleriteHCl-HNO3 and galenite HCl-NH4Cl- HNO3 and the best testing condition ofinstruments. According to different sample compositions, this method adopted thecombination of computer deducting background method, method of interferingelement correction, matrix element matching method.

46、These methods could deductand overcome the interference of elements and matrix effect. This is established atotal analysis method which could simultaneously test the main and minorcomponents and had no need to separate the tens percent of high-content mainelements.Through the experiment concluded th

47、at the few amounts of sampleconsumption of this method. So this method is more suited for single mineralssample total analysis comparing to other methods. This method has high testingprecision, fine accuracy, fast analysis speed. The analytical quality could satisfy therequest for single minerals sa

48、mples. Especially, the method determine the contentsof main and minor components in sulfide single minerals by ICP-AES technique,this method can get the ideal testing results without any chemical separating means,which not only makes the analytical operation more convenient but also reduces theanaly

49、tical error odds accompanying with the complex operating procedures.5. Application of biogeochemistry samples analysis by ICP-AES technique biogeochemistry provides important proofs for the secret of how the biosphereand the earth cooperated to evolve, how to learn the acting rules between the lives

50、and the environment, and the chemical evolvement of the earth. The growth andsurvival environment of animals and plants affects their metabolism greatly. Thelack of several life elements and the pollution of heavy metal elements can directlyinfluence the growth of plants and animals, and may cause d

51、eath if the situationbecomes severe. Plants play an important role on the biogeochemical circle ofsupergene element. Early in the twentieth century, scientists had already found thatplants had strong abilities to absorb some microelements and thus they utilizedplants to trace and search for minerals

52、. These findings suggest that the action ofenvironment and biogeochemistry has great value in the research of the earthsystem science.ICP-AES technique can simultaneously test more than twenty kinds ofmicroelements in one copy of sample solution only in one time. It has theadvantages of easy operation, low detecting limit, wide linear scope and credibleand accurate results. Our study mainly focused on the pre-preparation meth