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Ion Microprobe Techniques and Analyses of Olivine and Low-Ca

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Ion Microprobe Techniques and Analyses of Olivine and Low-Ca American Mineralogist, Volume 66, pages 526-546, l98l Ion microprobetechniques and analysesof olivine and low-ca pyroxene I. M. SreBrE, R. L. HnRvIc, I. D. HurcHEoN AND J. V. Snanu Department of Geophysical Sciences, (Iniversity of Chicago Chicago, Illinois 60637 Abstract Experimentalconditions for major, minor, and trace elementanalysis of olivine and low- Ca pyroxene are describedand analytical accuracy tested using suites of natural samples spanninga wide range of Mg/Fe. Special attention was given to sample cleanlinessto avoid contamination, instrumental vacuum to eliminate hydrides in the secondaryion spectrum,and samplepreparation to give good precisionin measuredintensities. Especially bothersome were molecular interferences in the secondaryion spectrumwhich were separatedfrom analytical peaksusing massresolu- tion (M/AM) over 3000.Careful analysisof the secondaryion spectrumallowed choiceof ei- ther high or low massresolution depending on the presenceof interferences.Lithium (0.005), F (l?), Na (0.01),Mg, Al (0.1),Si, P (5), K (0.05),Mn (0.1),Fe, and Co (l) were analyzedat low resolutionwith detectionlimits (ppm) in parentheses.Elements requiring high resolution includeCa (l), Sc (l), Ti (l), V (l), Cr (l) and Ni (5). The secondary-ionintensities for Mg and Si do not correlate linearly with composition whereasFe is nearly linear. The simple relation of the Mgl(Mg + Fe) ratio to the measured secondaryion ratio Mg*/(Mg* + Fe*) enabled major element determination to within +l mol% of forsterite or enstatitecontent. The yield of Mg and Fe secondaryions is a complex function of composition,and Mg*/Si* and Fe*/Si* are not simply related to atomic ratios in the target. To test accuracyof minor elementdetermination as a function of major elementvariation, secondary-ioniatensities were compared with compositionsbased on electron probe mea- surements.Some elements (Al, Cr, Ti, Mn) give a linear relationshipwith no obvious matrix eflect,but Ni, and possiblyCa and Co, definitely dependon the matrix. The linear relation- ship allows compositiondetermination to within tl\Vo of the amount presentby referenceto known standards.A major efort is required to calibrateLi, K, Na, F, v and Sc for which few reliable standardsexist. Introduction analysis)are available for analysisof trace elements, but most of them require mechanical separation of The development of the electron nicroprobe in the material to be analyzed.The ion microprobe was 1960-1970brought about a revolutionin the studyof recognizedaround 1970to be a potential "chemical rocks and minerals: indeed, it could be called a microscope"for many trace elements,and qualitative "chemical microscope" becauserapid non-destruc- analysesrapidly became routine especially in the tive analyses possible became at spotsselected by op- study of metals and doped semiconductors.Quan- tical study. It was no longer necessaryto separate tification of analysesof materials has posed severe minerals for analysesof major and minor elements practical and theoretical problems. Although these with atomic number (Z) greaterthan 10, and chem- problems are not fully solved,we now describeana- ical zoning could be studiedwith a spatial resolution lytical techniquesfor.reliable ion microprobe analy- near I ;.rm.However, light elementscould not be ana- sesof various trace elementsin olivine and low-Ca lyzed, and the continuous X-ray spectrum placed a pyroxene.Particular emphasisis placedon the useof detectionlimit near 40 ppm (2o) for elementswith Z high massresolution for identification and separation > 10. Many techniques(e.g., spark-sourceand iso- of massinterferences. tope-dilution mass spectrometry;neutron activation The ion microprobe utilizes a focusedprimary ion oo03-004x/ 8 | /0506-0526$02.00 526 STEELE ET AL.: ION MICROPROBE ANALYSES OF OLIVINE AND PYROXENE 521 beam to sputter a small volume of material from a Sampleselection and preparation targeUsome sputtered atoms are ionized and these secondaryions (SI) are analyzedwith a mass spec- Natural olivines lie very close to the binary join trometer. The extremely low background in a SI (Mg,Fe)rSiOo,but severalelements including Ni, Ca massspectrum allows analysisof trace elements,and and Mn are at high enough levels for comparisonof the focusedbeam can be positioned carefully on the ion and electron probe analyses.Low-Ca pyroxenes samplesurface. Although the potential of this analyt- lie fairly close to the binary join (Mg,Fe)SiO' and ical tech-niquehas been discussed(e.9., Evans, 1972; severalelements, especially Al, Ca, Mn, Cr and Ti Liebl, 1975;Werner, 1975),relatively little has ap- are readily measuredwith an electron microprobe. pearedregarding its potential for analysisof geologi- Chemically-analyzedlow-Ca pyroxeneswere usedby cal materials. To provide a fundamental test of the Howie and Smith (1966)to test correctionprocedures technique with typical applications, we have em- for the electron microprobe, and a selectedsuite of barked on a systematic study of important rock- thesepyroxenes was mounted for ion probe analysis. forming minerals using an AEI IM-20 ion probe with Olivines were selectedfrom those analyzedby Sim- high mass-resolution(Banner and Stimpson, 1975). kin and Smith (1970) and Smith (1966). Several Thesespecific studies follow severalyears devoted to other homogeneousolivines were used as well as an instrument developmentand to practical experience extensive suite of Mg-rich olivines and ortho- in analysisof geologicsamples. pyroxenes from mantle-derived peridotites which By far the greatesthindrance to measurementof had been carefully analyzed with the electron probe raw SI intensity dzta are molecular interferences (Hervig, 1980).Choice of sampleswas basedmostly which often are far more intensethan an analytical on grain size and absenceof visual inclusions. Be- peak. For example,in mafic silicates24Mgt6O+ occurs cause only six one-inch diameter samples can be at the samenominal mass(: 40) as the most abun- placed in the sample chamber of the ion probe and dant Ca isotope.Thus measurementwith a massres- becauserapid sampleexchange is not feasibleif vac- olution sufficient only to separateadjacent nominal uum is to be maintainedat <10-'torr, grain mounts masseswill give incorrect intensity data. with up to 36 samplesin each sample holder were Two contrastingtechniques are currently available prepared. A second important consideration in to reducethe effectsof molecular interferences.Her- choosing this mounting method is that the relative zog et al. (1973)and Shimizu et al. (1978) described ion intensitiesappear to be sensitiveto the physical application of energy filtering to increasethe signal environment(holes, cracks, etc.) rn the vicinity of the to interferenceratio while Bakale et al. (1975) and analysispoint; thus a rather large insulating surface Steeleet a/. (1980)described use of high massresolu- with few defects is required. Sample mounts were tion to separateanalytical peaks from interferences. preparedby scribing a grid of 2 mm squareson one Becausethe AEI Itvt-20ion microprobe allows only side of a l-inch diameter fused silica disk in a 6 x 6 limited energyfiltering (Steeleet al.,1977a), we pre- array. A thin layer of epoxy was placed on the non- fer to use high mass resolution when interferences scribedside of the silica disk, and grains were placed are present. within individual squaresduring observation with The precision and accuracy of measuremenJsis transmitted light under a stereomicroscope.Each crucial to use of the ion microprobe. Central thereto grain was checked for visual defects while in the is the influence of the mineral matrix on the sput- epoxy, and removed if necessary.With practice, 36 tered ion intensitiesand any systematicinstrumental sampleseach of -5 grains were mounted in a two effects.To attempt to answerthis questionwe assem- hour period. Each mount was ground to thin-section bled a suite of natural samplesof olivine and low-Ca thickness and polished. To avoid possible surface pyroxene to span nearly the entire range of Mg/Fe. contamination (seebelow), diamond polishing com- After careful electron-probeanalysis for all detect- pound was made by mixing gradeddiamond powder 'Aaselins". able elements we systematically examined the SI with commercial fill commercial dia- spectrumto determineanalytical conditions for each mond pasteswere found to have high levelsof K, Na, element as well as other elementsnot detectedwith CL Si, F, Ca and other elements.Commercial vase- the electron probe. We then compared ion-probe line was found to be contaminant-free at detection count rates against electron-probemeasurements to levelsof the electronmicroprobe. Because of possible test the quantitative ability of the ion-probe tech- hydrocarbon contamination and degassingunder nique. high vacuum, thick epoxy mounts were not used; STEELE ET AL.: ION MICROPROBE ANALYSES OF OLIVINE AND PYROXENE standardthin sectionsdo not noticeably degradethe cies derived from the duoplasmatronitse$ and vacuum. A reflected light photograph was taken of from possibleleaks, but at the expenseof a re- each sample and any particular featuressuch as in- duced intensity. clusionsand exsolutionlamellae were noted. (2) The primary beam has an impact energy of Before analysisby the ion probe, selectedgrains of 20kV; higher potentialsmight increasethe sput- each sample were analyzed with an ARL-EMx-sM tering and ion yields but are more susceptibleto electronprobe. Operatingat 25 kY, with a high beam electricalbreakdown. current
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