American Mineralogist, Volume 64, pages 440445,

1979

andoil immersion staining usingdispersion indexin thin section Measurement of refractive techniques
M. Scornonp Tsoues E. LesrowsKI,De.vID Miami Uniuersily of Geology, Department Oxford, Ohio45056 nNoDoNnLoE. Lnsrowsrt AuhmanHospital Department of Pathology, Ohio447l0 Canton,

Abstract With the aid of a 10X dispersionstaining objectiveadaptedfor apertural and central produced with a cuttingtool, the indexof refractionof and a liquid-graininterface screening, directly.Accuracyof i0.001 is attained. a crystalin thin sectioncan be measured

Introduction Petrographers are commonlyfacedwith the necessity or desirability of obtainingthe indexof refraction yet with no (n) of a specificcrystalin a thin section, the grainfrom the way of doingso withoutremoving thin section,which can be a laborioustask, or by from the rock sample. making a mineral separation that the sepaIn the latter casethereis no assurance rated grains are identical with the specificone of interest in the thin section.The dispersionstaining here,offersa relamethod, described and evaluated tively rapid techniquefor determiningat least one grain in thin section. indexofrefraction for a selected for The procedure is particularlyuseful,for example, obtaining the n of a member of an isomorphous series,which commonly allows chemicalcharacterization of the mineral. Petrographers are familiar with the theory and methodology of index of refraction determination using dispersioncolors (Bloss, 1967).If the n of a grain is closeto a match with that of the oil in which of white light is observed it is immersed, a dispersion which producescolor fringesaround the mineral. Observation of thesecolors can lead to a reasonably precise determination of n. (W. C. Mcstainingobjective A lOX dispersion Illinois)can be usedasan aid in CroneInc.,Chicago, wherethe n of a In cases making this determination. grain and liquid match at one wavelength, but not at staining with the l0X dispersion others,it is possible
00 offi3-ffi4x / 79/ 0304-0440$02.

to makethe grain to appearto havecolored objective is indicativeof the waveborders.The color observed n of the grain and which a match between lengthfor liquid has been obtained (Grabar and Principe, in the aidsmarkedly staining Thus,dispersion 1963). in grainmounts(Lasof minerals rapid identification kowski, 1965). Apertural screeningand central screeningwith a lOX dispersionstaining objective not only in nD of crystals, enables one to determine thin sections. grainmounts, but alsoin petrographic of the hereis to reportan evaluation Our purpose inof refractive method,based on the determination dicesof albite,labradorite,quartz,and microclinein thin section, and to describethe techniquein sufits use. ficient detail to encourage Theory stainingobjectivehas The theory of the dispersion (Cherkasov, 1960; Brown et al., 1963; beendescribed A standardlOx objecGrabar and Principe,1963). tive is fitted with two types of removablescreens placedin the rear focal plane of the objective. Apertural screening is a diaphragmwith an open The aperturescreen This diaphragmis spaceabout 2 mm in diameter. placed in the rear focal plane of the lOX objective for properillumination, (Fig. I ). To adjustthe system the following conditionsare met: l. Nicols uncrossed

LASKOWSKI ET AL.: REFRACTIVE INDEX MEASUREMENT

441

Central screening

Central screening can be usedto definefurther the resultsobtainedin the apertural screening measurement.Thecentral screen is an opaque dot (l-3 mm in diameter)which is mountedon a glassplate.This Aporlure Focol Plone Areo screen is alsoplaced in therearfocalplaneofthe lOX objective(Fig. 2). To adjust the systemfor proper illumination,the followingconditions are met: L Removethe aperturescreen 0bjective Lens 2. Nicols uncrossed 3. High-power condenser out 4. Light intensityhigh 5. Bertrand lensin 6. Insertcentral screen so that the opaque dot is in the centerof the crosshairs 7. Adjust the substage diaphragmof the microscopeso that the radiusof light visiblethroughthe Bertrand lensis equalto theradiusofthe opaque dot on the screen 8. Adjust the opaquedot so that it completely ! Light covers the radiusof light createdin step7 Fig.. l. Schematic diagram showing the effects of apertural 9. Openthe substage diaphragm everso slightlyto screening on dispersed rays of white light as viewed in focus. allow a faint rim of light to be barelyvisiblearound the periphery of the opaquedot 2. High-power condenser out 10. Now take the Bertrandlensout 3. Light source at high intensity ll. The system is now arranged for measurement 4. Bertrandlensin with the centralscreen. 5. Aperturescreen in parallel Figure 2 showsthe systemschematically. 6._ Substage diaphragmof the microscope closed bundles of white light strikethe liquid-grainboundso that the radiusof light visiblethroughthe Ber_ ary and are dispersed into variousrays(A, B, C, D, trand lensis slightlysmallerthan the .udiusof. and E). Wavelength C is not deviated at the liquid-grain locatedwithin, the aperturescreen boundary,thus wavelength C is the wavelength for 7. Now take the Bertrandlensout which the index of refractionof the liquid and the 8. The systemis now arranged for measurement index of refraction of the grain are equal.Wavewith the aperturescreen. Figure I showsthe system parallel schematically. bundles of white light strikethe liquid-grainbound_ ary and are dispersed into variousrays(A, B, C, D, E). Raysof wavelengths A, B, D, and E are deviated at the liquid-grain boundary, but wavelength C is not deviated. As light of wavelength C is not deviated, it is the wavelengrh or color of light for which the liquid and grain have the same refractive index. All the
Table l Colors observ.O;;,:ffi;:."1 screeningand relared

Wevelength

of

liquitl-grain

n natch

Deep Violet Duk RoyeJ. BIue Green Yelfov Yellor YeLlov olange to green Blue Blue green

to violet

Black

Less thm looo Ao !ooo-l+5oo Ao j+6oo-lr8oo Ao l+800-5200 Ao 5zoo-5\oolo Ao 5l+oo-5?od no t?oo-5ooo

to Red red

Red. ormge

5ooo-5200Ao 5zoo-5500 ao creater tbm 6500 Ao

Red orege Red to Bron

42

LASKOI4/SKIET AL.: REFRACTIVE INDEX MEASUREMENT

Ligbt

Blue

to

fihite

Light G!een BIue

Blue

and Hhite

Greater thm lo 55OO-?OOO

?000 Ao

Cenlrol

Focol Plono Areo

Greenish

azue

md

Green

63oo-5500 lo 51oo-5300 Ao 5?oo-6roo lo

Royal

Blue violet

Royel Blue Blue

Blue stl violet

0blsctlYs Lsng

Bl-uish Crinson

Red ed

Ao SZOO-5?OO Sooo-5200no )+l+oo-500o Ao Less thu l+\oo Ao

Light Golden

or@ge yellov

vloLet Falnt

sd Violet GoIal Yeffow

Orege 4d

PaLe Yel1ov

Faint

offwith a sharprazor. Use carefullypry the coverslip glasses is advised. of safety WhiteLighl 2. Selectthe largest grain of a specificmineral which is orientedfor the particularindex despecies Fig. 2. Schematic diagram showing the bffects of central for measurement. sired screening on dispersed rays of white light as viewed in focus. 3. Placethe thin sectionon the cutting apparatus on the mi(Fig. 3), and placethe cuttingapparatus at the liquid- croscopestage.Relocatethe grain desiredfor mealengthsA, B, D, and E are deviated grain boundary.As all of the wavelengths of dis- surementusing a low-powerobjective. 4. Placethe brassguide acrossthe grain to be persedlight are collectedand passthrough the rear and hold the guidefirm with the magnets. focal plane of the objective,they encounterthe cen- measured, blocksout wavelength Make sure the indentationon the brassguide is tral screen. The centralscreen the grain to be measured. A, B, D, and E to passto across C and allowswavelengths and attached slide 5. Take the cutting apparatus Thegrain borders of the crystal thus theimageplane. becomeilluminatedand colored.When viewed in focus,the color at the grain border is relatedto the d RGctongleWllh Gloss (asthe complementary color to the actualwavelength P l ol e C o m n f 6 d T o U n d s r s i d e wavelength) for which the index of refractionof the Sh6ef Melol Perlmslor liquid andthat of thegrainareequal(Table2). When de-focusing, two Beckelines are produced.The colors of theseBeckelines are similarly relatedto the oss Guido wavelength at which the liquid-grainindexmatchis gnt (Table2). obtained in petrographicthin Procedurefor nD measurement section Measurement of an indexof refractionof a specific mineral (in this casenD-beta of an albite will be measured) can be performeddirectlyon the thin secof the determination tion. The followingdescription serves as of the nD for the beta index of plagioclase an example: withl. It is necessary to work with a thin section out a coverslip.If the desiredslide has a coverslip,
lo ngle Cut In Cordboord To Hold Sllde

Fig. 3. Cutting apparatus. A guide which allows one to orient the cutting tool to a selected grain. A slide is placed in the central rectangle, and the assemblageis placed directly on the microscope stage. The slide is viewed with a low-power objective, and a grain for measurement is located. The brass guide is placed across the desired grain and held in place by tlvo magnets. The entire assemblageis then removed from the stage of the microscope for cuttlng.

LASKOWSKI ET AL.: REFRACTIVE INDEX MEASUREMENT

443

off the microscope stageand placeon a flat table. As the rD eachtime liquidsare changed. of acetone 6. Apply three drops of acetone to the slidein the of a given liquid approaches the nD of the grain, grain and rinsewith water. Be dispersion vicinity of the desired visibleat the cut-grain colorswill become carefulnot to disturbthe brassguide. in normal illuminationwith low intensity. boundary 7. Using a high-speed drilling tool fitted with a l- Make surethe grain is in the desired opticalorientainch-diameter carborundum disc,makea vertical cut t l o n . guideacross alongthebrass thegrainto be measured. I L lnsert the aperturescreen and setthe illuminaThis cut must be executed in one downwardmotion tion as previously described. and must penetrate through the rock sectioninto the 12. Place the crosshairsat a point on the grain glass. The idea hereis to createa trough or slit in the where color fringes are observed,and recheckthe grain to be measured. of the screen. centering 8. Removethe slide from the cutting apparatus 13. Recordthe color observed throughthe aperand add one drop of acetoneto the fresh cut with a ture screen, and refer to Table I for the wavelength small pipette.Allow this drop to evaporate partially, for which the indicesof refraction of the grain and then wash the entireslide with water. Dry the slide. liquid areequal.[The albitecrystaldescribed in Table 9. Beforeproceeding, checkto be surethat the cut 3 yieldedgreenbordersas viewedthrough the aperproduced is across the grain in question. when a liquid with nD : 1.532 at 25"C ture screen 10. Placea drop of index liquid (Cargilleliquids was used.This indicated(Table l) a crystal-liquid are preferred)on the cut, making surethat the tem- index match at some wavelength between5200and perature of the liquid is about25'C. A liquid-grain 5400A.1 boundaryhasnow beenestablished. Using successive 14. Removethe aperturescreen and insertthe cenmounts,find a liquid which produces discernable dis- tral screen. illumination for Setthe centralscreening persion colors.Cleanthe cut on the slidewith a drop as previouslydescribed. Perform step 14 without alTable 3. Results of dispersion stainingmeasurements on known crystals
MateriaL Type of uout 4-D liquid Colors observed duing (25oc) screening grain n natch

nD measueCl

Published nD

Apertual
r.508 I.5I2 f.ouo I.5I2 t. oje 1.535 1,608 f.bfz I.544 I.552 l. )4u 1,544 t. >4u 1,544 I. >4o a. >>o 1.532 I.536 L.532 ]-136 r. ))o f . 5b0 f.556 f. >ou f. )o4 I.558 I.56\ I.558 L,520 I.52\ Green Yellov teffov Ormge ureen Yetlov

Central

01ess

I so.

Grain

oruge green red

Violet+0rqge Royal Blue Blue+Red. Blue+Green Violet+0range 81.vio].+Red VioIet+0rmge BI.viol,+Red. Gold+Violet B1.viol.+Red 81.viol+Red Blue+Red 81.Yiol.+Red Blue+Red B1.vio1.+Red Royal Blue Violet+Orege Blue Violet+0range Blue+Red Violet+Ormge Blue Violet+0range Blue Violet+Orange Blue+Red VioIet+0renge Blue+Red. 81.viol.+Red Blue+Red. orng.

52oo Lo 5too A' :too ll 6\00 A"

t.5rl r..5095 r.6396 r.6\67 r.5525 r'l\tr6 1.5\\9 r.ii39 r.53r2 r,i35i 7.5592 t.sig\ r.5617 L.5679 r.5226

t.)r.

rruarglrre./

Glass Arooniu Chloride Sodiw Bronate Low Quutz Lov

I so.

Grain

LOI

(UAg1Ile,/

I so.

craln

green

I so.

Grah

31ue green Green-Ye1. Royal creen uleen Yellov Blue

grn.

orng.

Grain

orng. orng.

:zoo ll ,55o A' :roo l] 5\oo A" )+Too .no 5 3 0 0A ' 53oo.ro 5 8 5 0A " :zoo l! 5 7 o oA " :eoo al 6 1 5 0A 5zoo ll 6200 A" 5 o 5 oA 5eooll 5200 A" :eoo ll 5r5o A" lroo ll 5 o 5 oA " :eoo ll 6 0 0 0A " 6100 A"

1.5392(casilre)
f,olo) (usgalfel

1.553 (B1oss,1957) 1 . 5 ) + l +( B r o s s , r 9 5 ? ) 1.51+l+

Grain Lov Tnln Section rnan beclaon R

Bfue green Yel1ov green Stue gleen leilov orange creen Red orange creen orege ureen Orilge

orng.

Lov

orng.

A-lbtte

Graln Thin Section

q?t-t

q?7

lrarr

toco\

nl :eoo

A.1bite R

yeLlov

r.531-1.t37
f . >)o-f .)oy (trerr, t9>9,

Labradorite

Grain thin Dectlon

real

Labrailorite High Ca Labradorite High Ca Labradorite

Green-Blue grn. Ietfov ormge laue green Yeltov orange creen Yellov-Lt.Ormge Yellov Ormge green

r.558-! .569 r. jj3-r, j69 r.558-r .569

crein Thin Section

Microcline

Thin Section

>:>o,o.l

LASKOWSKI ET AL: REFRACTII/E INDEX MEASUREMENT

tering the position of the slide on the microscope stage,or changing the liquid. 15. Observethe colors produced by central screening, and refer to Table2 for the wavelengthat which the indices of refraction of the grain and liquid are equal. This wavelength or range of possible wavelengths should coincide with the results obtained from apertural screening. [The albite crystal described in Table 3 yielded violet and orange color fringes viewed through the central screen when a l i q u i d w i t h n D : 1 . 5 3 2a t 2 5 o C w a s u s e d .T h i s i n dicated (Table 2) a crystal-liquid index match at some wavelengthbetween5000 and 5200A.1 1 6 . F o r t h e a l b i t ee x a m p l e , s t e p sl 3 a n d l 5 y i e l d e d a crystal-liquid index match at some wavelength within the range of 5200-54004 (step l3) and within the range of 5000-52004 (step l5). These two wavelength ranges overlap at 5200A, thus 52004 was chosen as the wavelength for which the index of refraction ofthe crystal and the liquid (in this casenD : 1 . 5 3 2 a t 2 5 ' C ) a r e e q u a l .I n s o m e c a s e s the results attained from Tables I and 2 will overlap over a range of wavelengths.If this occurs, choose a midpoint within the overlapping wavelengths as the wavelength for which the n of the crystal and the liquid are equal. 17. Plot the liquid (at 25'C) on a graph of n us. wavelength (Fig. a). Plot the match wavelength,attained in step 16, on the liquid curve. For the albite example, the match wavelength attained in step l6 (5200A) was plotted at point ,4 on Figure 4. 1 8 . C l e a n t h e s l i d ew i t h a d r o p o f a c e t o n e r , i n s ei n water, and dry. 19. If a wavelength match of 54004 or less was attained above, choose a higher index liquid for the next measurement. If a wavelengthmatch of greater than 54004 was attained above, choosea lower index liquid for the next measurement. 20. Repeat steps I l-18 with the new index liquid; be sure the crystal is in the same orientation as bef o r e . ( W i t h l i q u i d n D : 1 . 5 3 6a t 2 5 o C , 6 0 5 0 A w a s determinedto be the wavelengthfor which the index of refraction of the albite in Table 3, and liquid rD : 1.536 at 25"C, are equal. This match wavelength is plotted at point B on Figure 4.) 21. Draw a line through the two match points asin Figure 4. This line is an accuraterepresentation of the change in index of refraction of the crystal in the orientation presentwith respectto a changein wavelength. The point on the Y axis where the resulting line intersectsthe sodium D line is the nD of the grain, in the orientation tested(point C on Figure 4).

Discussion measurements Table 3 showsresults of digpersion were All measurements made on varioussamples. conductedat about 25oC. Indicesof refractionof and two optisodiumbromate, ammoniumchloride, (all Cargillestandards) were measured cal glasses using grain mounts and the dispersionstaining Accuracies of equalto described. methodpreviously or better than t0.001 were obtainedin all cases. with accuracies obThese resultsare comparable (1960) and Grabar(1963). tained by Cherkasov for sodiumD light of the The index of refraction zD-betaof rayand rD-omegafor low quartz, epsilon nD-betaof labradorite, afbite, nD-beta of microcline, weremealabradorite and rD-beta of high-calcium In thin sections. sured directly from petrographic grainin a specific was orientation a specific eachcase, for The indexof refraction for measurement. chosen sodium D light of the omegaray and nD-epsilon for low quartz values and L5539measured of 1.5449 comparefavorablywith the valuesgiven by Bloss (1967). for sodiumD light of The indexof refraction in thin section to the betaray for albitewasmeasured gavean A grainmount of the same sample be 1.5355. values fall within a rangeof These nD-betaof 1.5352. (Kerr, 1959) for the albitefield.The indices of values for sodiumD light of thebetaraysfor lowrefraction calcium labradorite and high-calciumlabradorite and 1.5679 weremeasured in thin section to be 1.5594 gave samples respectively. Grain mountsof the same Kerr nD-betasof 1.5592and 1.5677respectively. (1959) placed the labradoritefield at nD-beta : for sodiumD The indexof refraction 1.558-1.569. wasdetermined to light of the betaray of microcline from a thin sectionmount. Bloss(1967) be 1.5226 placedthe microclinefield at nD-beta : 1.522to t.526. is related to nD-betafor the plagioComposition (Chayes, 1952). Using his clasesolid solutionseries graph for nD-beta us. plagioclase composition, the and high-calcium labradorite in albite, labradorite, to have compositions of 8 Table 3 are estimated percent anorthite,53 percent anorthite,and 68 perrespectively. centanorthite In cases discussed above,liquid-grainboundaries were createddirectly on thin sectionslides.Color fringes were produced.To interpret these color (some fringes of them faint) produced in thin section, methodis preferred the dispersion staining overother of the accuracy attained standardmethodsbecause (a color fringe (+0.001),quality of colorsproduced very faint in regularlight is generally which appears

LASKOIYSKI ET AL.: REFRACT,IVE INDEX MEASUREMENT

445

Liquld l* 2

0.1.336ot 25o C

Liquid l* | ll D:t 532 ot

AinA" Fig' 4' Determination of nD of an albite.Liquids I and 2 areplot ted,n us. wavelength, according to values for zF, rD, andnC givenfor eachliquid' Line ACB represents the changein index of refractionof the albite with respect to a change in wavelength. The crystalis orientedto measure the beta index. point c is the nD-beta (1.5355) of the albite crystal.

quite clear when the dispersionstaininglens is em_ ployed),and ease of interpretationof the colorspro_ duced. References
Bloss, F. D. (1967) An Introduction to the Methods of Opticat Crystallography. Holt, Rinehart, and Winston, New york. Brown,K. M., W. C. McCrone,R. Kuhn and L. Forlini (1963) Dispersionstainingpart II-The systematic applicationto the identification of transparent substances.The Microscope and Crystal Front, 14, 39-54. Chayes, F. (1952)Relations between compositions and indices of refraction in natural plagioclase. Am. J. Sci.,BowenVolume.g5_

r05.
Cherkasov, Yu. A. (1960)Applicationof focal screening to measurement of indices of refractionby the immersion method.1zr. Geol. Reu.,2.218-235. Grabar, D. G., and A. H. Principe(1963)Identification of glass fragments by measurement of refractive indexand dispersion. "/. ForensicSci.,8, 54-67. Kerr, P. F. (1959)Optical Mineralogy.McGraw-Hill, New york. Laskowski,D. E. (1965)Chemical microscopy of urinary calculi. Anal Chem., 37, 1399-1404. Manuscript receiued, March 27, 1978; accepted for publication,May 22, 1978.