You are on page 1of 11

The Polarized Light Microscope: Should We Teach the use of a

19th Century Instrument in the 21st Century?


Mickey E. Gunter Department of Geological Sciences, University of Idaho, Moscow, Idaho
83844-3022, mgunter@uidaho.edu

ABSTRACT computer-based instruments (e.g., X-ray diffractometers


and electron microscopes). The overarching theme is that
The polarizing light microscope (PLM) has no doubt students, and researchers, must understand the
contributed more to our knowledge of minerals and limitations of the various instruments and be able to
rocks than any other single instrument. Then why is the select the most appropriate one for the problem at hand.
use of the PLM, and the teaching of optical mineralogy in Also, equally important, we should teach how to
general, decreasing? Probably one of the main reasons is integrate several different analytical methods to answer
educators seek to present the newest, most the question at hand.
technologically advanced techniques and methods to The PLM is one of the few instruments students will
their students. Also, the geoscience curriculum has ever get to use independently. This itself warrants its
changed to include environmental geology, essentially teaching as we strive for more interactive methods of
hydrogeology. However, in presenting these newer instruction. No other single instrument provides
materials, or new courses, we must exclude something, chemical, structural, and morphological information on
and it appears that one of the things excluded is a single sample and with so little sample preparation,
instruction in use of the PLM. Another possibility is the albeit the chemical and structural data are found
professors teaching these courses do not have an indirectly. It is this “indirect method” of inferring
adequate understanding of optical mineralogy. chemical and structural data that is the double-edged
Excluding the subject of optical microscopy will be sword for the use of the PLM. Microscopists must infer
the biggest mistake we ever make in the geosciences this information based on their experiences. When data
curriculum. This statement is justified because of the are misinterpreted, it is often (incorrectly) the
fundamentally important concepts presented in optical microscopic techniques and not the microscopist who is
mineralogy: 1) three-dimensional visualization, 2) blamed.
inquiry-based learning, and 3) hands-on use of an Clearly, the PLM cannot directly determine a
analytical instrument. No other single course in our material’s crystal structure or chemical composition;
curriculum provides so many of these fundamental skills diffraction methods are commonly used for the former
to our students. An example of inquiry-based learning is and spectroscopic methods for the latter (e.g., energy
determining the best technique to identify a mineral. For dispersive spectroscopy in an electron beam instrument).
example, powder X-ray diffraction provides a diffraction However, once the structure and composition are
pattern searchable in a database, but the result might not known, generally speaking, they can be related to some
be correct. In the past 20-30 years, the spindle stage has feature that is observable or measurable with a PLM. For
allowed for more detailed single crystal studies than ever instance, refractive index is related to compositional
before. Optical techniques are also used to study such variation and optical class is related to crystal system.
diverse mineralogical problems as cation-diffusion in Students can quickly confirm the identity of a mineral if
zeolites and asbestos identification, or they may be they are taught how to use oil immersion and grain
incorporated into other areas of research, such as mounts. For example, the refractive index can provide
synchrotron experiments on oriented single crystals. the species of a plagioclase feldspar much easier than
Also, any serious petrologic study must begin with a using power X-ray diffraction, which is difficult
thorough examination of the samples by PLM, before interpret. Also, chemical information from an electron
other types of characterization can proceed. A diversity microscope cannot differentiate among kyanite,
of employment opportunities exist for students who are sillimanite, and andalusite, or between quartz and opal.
trained in use of the PLM, such as in the fields of Working with minerals in thin sections, there are even
forensics, material science, manufacturing, the food simpler optical properties such as color, relief, twinning,
industry, medical technology, and the emerging field of mineral associations, and alteration that give qualitative
environmental mineralogy. chemical information and guide the pertologist in
further characterization of the rocks. The examples are
numerous, and several more will be presented below.
Most importantly, the PLM excels in determining sample
INTRODUCTION morphology, for instance to aid in differentiating
amphibole from amphibole-asbestos in grain mounts or
Our understanding of minerals and rocks is attributed the textural relationships of minerals in rocks. The
more to use of the polarized light microscope (PLM) than significance of these relationships could be expanded
any other single instrument. With the PLM, we can almost endlessly. And the cost of maintaining a PLM
quickly identify and characterize minerals and versus that of an X-ray diffractometer or electron-beam
determine textural relationships in rocks, including instrument is several orders of magnitude less. This
microstructures used in petrofabric analysis. Why, then, lower cost allows institutions with modest budgets to
are we abandoning teaching these skills to our students still teach the use of the PLM, while the maintenance on
in favor of other subject matter? One of the main other instruments may be cost prohibitive.
problems using a PLM, though, is the answers do not Mineralogists often only think of using the PLM for
come from a computer but must be determined by the geological materials, but the uses outside of our
user. Thus, more education and experience are required discipline often have important societal implications.
to use the PLM correctly than what is required for Again, the examples are numerous, and several will be

34 Journal of Geoscience Education, v. 52, n. 1, January, 2004, p. 34-44


presented. Despite this, other disciplines have also It was not until 1856 that the first true PLM was built, and
discontinued instruction of the PLM. We not only should a theoretical understanding of how light interacts in a
continue teaching polarized light microscopy but better mineral was quickly developed. Advances were made
integrate its use into our research, both in the study of both in the immersion and thin section methods until the
geology and other areas. early 1900’s, when these techniques were basically
Probably the main reason for the decline in the perfected. Little has changed in their use since. The
teaching of optical mineralogy, and in fact mineralogy in immersion methods allow for a fairly rapid identification
general, is that many geologists view this discipline as a of single crystals, while thin section methods permit not
surrogate to igneous and metamorphic petrology, or only mineral identification but also the study of textural
geochemistry. That is to say, that mineralogy is not a relationships of minerals in rocks. Currently, thin section
stand-alone discipline but merely leads to more techniques are more commonly taught than the
“important areas” in the field of geology. Unfortunately immersion methods. This is probably because thin
by thinking like this they ignore the geological section techniques can be applied to the study of rocks,
information gained by consideration of the crystal whereas the immersion method is basically used for
chemical aspects of a mineral. A close corollary is that identification of minerals. Also, many scientists
because so many petrologists have been trained in the incorrectly believe the commercially available refractive
field of optical petrography (i.e., using thin sections to index liquids in use today contain PCB’s and are
study rock texture), they teach optical mineralogy carcinogenic; this was true of formulations used decades
courses without a full understanding of the power of ago but not the newer formulations.
optical mineralogy outside of the field of petrology (i.e., In the early 1900’s, the PLM was the main instrument
they would always favor “cutting a thin section” to used by mineralogists and petrologists to study minerals
examine a rock over using the immersion method to aid and rocks. The discovery of X-rays in 1912 led to a major
in identification of a mineral). This is also unfortunate breakthrough by which the crystalline properties of
because geological information could be gained by single minerals could be directly studied by X-ray diffraction,
crystal optical studies of, for instance, the structure state instead of indirectly studied by the interaction of light
of feldspars (Su et al.,.1984). with a mineral. The development of X-ray diffraction led
This paper will provide a brief history of the PLM many mineralogists to abandon use of the PLM, because
and its historical uses in mineralogy and geology, now they could use powder diffraction to aid in the
followed by a review of some basic optical methods (e.g., identification of minerals and single crystal X-ray
what can be measured with a PLM with the aid of a diffraction to determine the crystal structures. Electron
spindle stage). Next, a series of mineralogical examples beam instruments were also being developed in the
will be given, some of which could only be solved with a middle 1900’s, but it was not until the invention of the
PLM. Finally, several examples of on-going integration microprobe in 1959 that these instruments became a
of optical techniques to study the orientational dominant force in the field of mineralogy and petrology.
dependence of physical properties of minerals will be In the 1960’s, the chemical composition of micron-sized
highlighted. It is not the intention of this paper to discuss minerals could be determined with an electron
all the uses of the PLM but rather to concentrate on the microprobe. This replaced the laborious technique of
author’s research in an attempt to show the evolution of using larger size samples and performing wet chemical
his work and how he has incorporated classical optical analysis. Mineralogists then had at their disposal
mineralogy into newer analytical methods in instrumentation capable of directly studying the atomic
mineralogy. This paper is based on a seminar the author arrangement of atoms in minerals and precisely
gave as a Mineralogical Society of America distinguished determining the chemical composition of minerals.
lecturer.
MAJOR USES OF THE PLM
BRIEF EVOLUTION OF THE USE OF THE
PLM Identification and characterization of minerals -
Mineral samples are identified based on their structural
The main impetus for development of the PLM was to and chemical characteristics. X-ray and electron
study crystalline materials. In the 1800’s, scientists diffraction techniques directly provide data about the
studying minerals noted light interacted with minerals in atomic structure of a mineral. Diffraction occurs when
unique ways. They determined that certain minerals X-ray radiation or electrons pass through and interacts
would cause light to become polarized, and they also with the atoms of a crystalline material. Analysis of
observed that light traveled at different speeds in diffraction patterns are used to determine structural
different directions for some minerals, while for others properties such as space group, unit cell parameters, and
the speed of light was the same regardless of propagation positions of atoms. Energy dispersive spectroscopy
direction. They attributed these differences to varying (EDS) and wavelength dispersive spectroscopy (WDS)
crystal structures of minerals and sought ways to study directly provide information about the chemistry of a
this in more detail. The PLM would become their main sample. A sample is placed in the path of a high-energy
tool for studying minerals for the next hundred years. electron beam. These electrons collide with the inner
For a complete discussion of the development of the PLM shell electrons of the atoms comprising the sample, eject
and many of the accessories associated with it (e.g., the an inner shell electron, and create a vacancy. Outer shell
U-stage for study of petrofabrics) see Kile (2003). electrons move into the vacant inner shell and, in the
Two separate methods were developed to study process, release energy in the form of X-ray radiation.
minerals. One was the immersion method, where
crystals of minerals were crushed and placed in a liquid The specific energy, or wavelength, of X-ray radiation
then observed with a microscope. This was first done in produced by an atom is characteristic of each element.
1815 using water as the liquid. The other method was EDS methods determine the energy of these X-rays, and
development of thin sections, first crudely done in 1831. WDS determines the wavelengths of the X-rays. By using

Gunter - The Polarized Light Microscope 35


resolution of a light microscope. Second, the
distinguishing characteristic of asbestos is its
morphology, which is fibrous. It could be argued that the
emerging filed of environmental mineralogy has its roots
in the use of the PLM for asbestos identification and
characterization. (For an overview of the asbestos issue
in the U.S.A. refer to Gunter, 1994.) A material could
have the exact same chemical composition and X-ray
diffraction pattern and in one case its morphology might
be fibrous and the other case it might be non-fibrous. So
the only method to distinguish between fibers and
non-fibers is the morphology, which can be observed in
the magnification range of that for a PLM. For example,
Figure 1 shows amphibole samples from Libby,
Montana, in an oil immersion mount. Clearly, the
particle on the left, labeled fragment, is non-fibrous and
the particle on the right is fibrous. This distinction can
only be made based on morphology. Chemical analysis
Figure 1. A photomicrograph of amphibole and of these two materials would be identical, and if we were
amphibole-asbestos from Libby, Montana showing to perform a powder X-ray diffraction experiment, the
differing morphologies. (The photo was taken in diffraction patterns would also be identical.
plane-polarized light with 1.58 refractive index Asbestos regulations are currently being revised in
liquid; the scale bar is 1 mm.) the U.S.A. This is mainly the result of the amphibole and
amphibole asbestos minerals occurring in the former
EDS or WDS, it is possible to determine the quantity of vermiculite mine near Libby, Montana (Bandli et al.,
each element in a sample. EDS is more rapid and requires 2003; Gunter et al., 2003). The first change in the
less sample preparation than WDS; however, WDS regulations will no doubt be to regulate amphiboles
produces more precise and accurate quantitative based on group name and not species name. This is
chemical analysis. Often, the correct identification of a necessary because the amphiboles at Libby are winchites
mineral requires that both structural and chemical and richterites which, as of this time, are non-regulated
information be obtained. but are just as harmful as the regulated amphibole
Structural and chemical characteristics can also be minerals. At first this seems like a fairly simple
indirectly observed using polarized light microscopy. modification to the regulations. However, the issue will
Structural properties are obtained by the correlation of a then become how to distinguish asbestos from
mineral’s optic class to its crystal system. Optical non-asbestos amphiboles. Many of the regulatory
classification of minerals is based on whether they are agencies have used the aspect ratio to make this
distinction. For instance, if an amphibole particle has a
isotropic or anisotropic. If a sample is isotropic, it has length-to-width ratio greater than 3, it would be
only a single refractive index value and belongs to the considered a fibrous particle. Thus, what would clearly
isometric crystal system, or it is amorphous. If a sample is be a non-fibrous sample (Figure 1) would, based on this
anisotropic, it is further classified based on its optic class. aspect ratio rule, become regulated as an asbestos
Anisotropic minerals can be either uniaxial, which material. Clearly, to regulate these materials correctly
belong to either the hexagonal or tetragonal crystal there must be close interaction between those
system, or biaxial, which belong to the orthorhombic, individuals trained in polarized light microscopy and
monoclinic, or triclinic crystal system. Both of these the regulatory agencies.
classes are further divided into positive and negative Today there are many more jobs in asbestos
groups based on the relationship of refractive indices identification laboratories and in regulatory agencies
and their principal vibration directions. than there are qualified microscopists to fill them. This
Chemical characteristics of minerals can be related to scarcity of trained microscopists has occurred because
the optical properties of the minerals (e.g., refractive we have stopped teaching classical optical mineralogy in
indices, 2V, sign of elongation, extinction, pleochroism, our geology curriculum. The void has been filled in the
etc.). A century’s worth of careful optical and chemical private sector with one-week short courses in polarized
measurements has provided many empirical light microscopy, optical mineralogy, and asbestos
relationships, whereby a quick check of refractive index identification. For instance, the McCrone Research
or a determination of 2V can provide an approximation Institute in Chicago has trained hundreds of
of chemical composition often required for mineral microscopists in the past 20 to 30 years. If the private
identification. Thus, chemical data of minerals are found sector is teaching these courses because of a nationwide
indirectly by measurement of some basic optic property, demand, it would be logical for us to include them as part
usually the refractive index. of our curriculum. Any geology student successfully
completing a semester long course in optical mineralogy
SOME IMPORTANT SPECIFIC USES OF could be practically guaranteed a job in one of these labs.
THE PLM The spindle stage - One of the major advances in optical
characterization of minerals has been the refinement of
Asbestos - Without a doubt the most important use of spindle stage techniques by Bloss and coworkers (for
the PLM for the past 20 to 30 years is in the identification example, Bloss, 1982; Bloss 1999; Gunter et al., 1988;
of asbestos. This is true for two reasons. First, the size Gunter and Twamley, 2001; Su et al., 1987). The spindle
range of concern for identification of asbestos fits the stage, which is basically a one-axis rotation device, is a

36 Journal of Geoscience Education, v. 52, n. 1, January, 2004, p. 34-44


Figure 3. Photographs of three different types of
spindle stages: Supper, detent, and poster board. The
figure shows the X-ray goniometer head (with an
affixed crystal) mounted onto the Supper spindle
stage and the oil cell supplied with this spindle stage.
The oil cell for the poster board and detent spindle is
also shown.

a thorough discussion of spindle stage techniques, see


Bloss (1981; 1999).
The basic design for the spindle stage is a single
crystal mounted on a glass fiber, or sewing needle, that is
placed on the rotation device (i.e., the spindle stage). The
crystal can be placed in an immersion liquid, and routine
optical measurements and observations can be made.
Figure 2 is a photograph of three different spindle stages.
The Supper spindle stage is often used for research
purposes, while the small detent spindle stage (Bloss,
1999) and poster board spindle stage (Gunter, 1997) can
be used for teaching purposes. In all cases, however, the
setup is the same: small (50 to 200 mm) single crystals are
mounted on the end of the spindle stage and placed on a
PLM. Figure 3 shows the materials required to mount
single crystals. Commonly, a single crystal is mounted,
with the aid of a binocular microscope, on the end of a
glass fiber with fingernail polish. The glass fiber is, in
turn, placed in a 3 mm diameter brass pin, which is
inserted into an X-ray goniometer head. Next, the X-ray
goniometer head is screwed onto the Supper spindle
Figure 2. A) The necessary “equipment” to mount
stage shown in Figure 3. Now the crystal can be
single crystals for optical examination with a spindle immersed in refractive index liquid contained in the oil
stage. Under a binocular microscope, a small single cell mounted on the spindle stage. Figure 3B and C show
crystal (ca. 50-200 mm) is glued with fingernail polish an amphibole crystal affixed to the end of a glass fiber
to a (ca.) 100 mm glass fiber. Then the glass fiber is and immersed in refractive index oil. The crystal has
placed in a brass pin that fits into the X-ray been rotated 90° between B and C.
goniometer head, also pictured. Acetone can be used Figure 4A shows the spindle stage X-ray goniometer
to remove the crystal for further study if desired. B & head combination mounted on the stage of a PLM. Also
C) Photomicrographs of an amphibole single crystal shown in this image is a temperature-controlled oil cell
mounted on a glass fiber. The sample has been used to record and change the oil’s temperature. At the
rotated 90° on the spindle axis between B & C, thus same time, the wavelength of light can be changed with a
allowing three-dimensional viewing of the single monochrometer. By changing both temperature and
crystal. (The photos were taken in plane-polarized wavelength, the refractive indices of a material are
light with a 1.58 refractive index liquid; the scale bar measured to within plus or minus two to five in the
is 100 mm.) fourth decimal place by the double-variation method
(Bloss, 1981; Su et al., 1987).
microscope attachment that aids in obtaining large One of the major advances of Bloss and coworkers is
amounts of optical data quickly and efficiently. A brief the ability to orient biaxial minerals easily on the spindle
introduction to the spindle stage and its uses follows; for stage with the aid of the computer program EXCALIBR
(Bloss, 1981; Gunter et al., 1988). All that is required is

Gunter - The Polarized Light Microscope 37


Figure 4. Photographs of three different experimental
setups for single crystal study; in all cases, an X-ray Figure 5. Sketches showing the optical orientation
goniometer head is used and thus the same crystal for andalusite and “Mn-andalusite.” Note that for
can be easily moved between experimental setups. A) andalusite the small refractive index (X) is parallel to
The Supper spindle stage, with goniometer head, is the long dimension of the crystal, while for
mounted on the rotating stage of a PLM to observe Mn-andalusite the optical orientation has changed
crystal morphology in three dimensions and to and Z (the largest refractive index) is parallel to c. The
measure optical properties (e.g., refractive index, lower part of the figure is a polyhedral representation
pleochroism, 2V, orientation of the indicatrix, etc.). of the structure of andalusite. The main structural
B) A goniometer head mounted on a single-crystal unit is an edge-sharing chain of octahedral parallel to
diffractometer used to obtain structural data (e.g., the c crystallographic axis.
unit cell parameters, crystal structure, orientation of
the crystallographic axes, etc.). C) A modified spindle
stage placed in a synchrotron beam source for studies
of the orientational dependence of absorption
spectra.

38 Journal of Geoscience Education, v. 52, n. 1, January, 2004, p. 34-44


Figure 6. Relationship between refractive indices and Mn + Fe content for 20 andalusite samples (modified
from Gunter and Bloss, 1982). Because there is a change in the optical orientation as a function of Mn + Fe
content (x+y on graph), the refractive index curves are labeled n||a, n||b, and n||c to correspond to the
refractive index directions in the a, b, and c crystallographic directions, respectively. Note that when the
curves cross, a sample of that composition would appear isotropic.

extinction measurements are determined for different and Fe substitute for Al in the M1 site that form
spindle stage settings. A mathematical relationship edge-sharing chains of octahedrons parallel to the c
exists between these extinction data and the optical crystallographic axis. Notice how the structure of
indicatrix. In other words, given extinction andalusite controls its morphology; these edge-sharing
measurements, a computer program will provide the chains are the main structural unit, thus elongating
microscopist the spindle stage and microscope stage andalusite parallel to its c crystallographic axis.
settings to place the crystal so any of its three principal Gunter and Bloss (1982) obtained a suite of
refractive indices can be directly determined without approximately 50 andalusite samples and selected 20 of
appreciable error due to misorientation. Another major varying compositions. For each of these 20 samples, we
advantage of this method is that all refractive indices are precisely measured the refractive indices with the PLM
determined on the same crystal. This, in turn, lends itself and spindle stage, cell parameters by X-ray diffraction,
to studies whereby the optically characterized single and chemical composition by electron microprobe. These
crystal can also be used for X-ray diffraction or chemical different measurements were made on the same single
analysis. All the physical properties of a mineral can be crystals; thus, the change in the optical orientation could
determined on the same single crystal. be tracked as a function of chemical composition. We
found that the refractive index direction parallel to the c
Isotropic andalusite - An example of an integrated crystallographic axis was the smallest of the refractive
optical, X-ray, and chemical study was performed on indices for pure andalusite; however, it increases at a
andalusites with varying compositions (Gunter and greater rate than the other two refractive indices with
Bloss, 1982). Andalusite, Al2SiO5, can have appreciable substitution of Mn and Fe for Al. Upon close examination
substitution of Mn and Fe for the six-coordinated Al in its of Figure 6, notice a void in our data in the area where
structure. There is also a change in the optical orientation these three curves of refractive index values cross. Two
in andalusite as this substitution occurs (Figure 5). Figure reasons were postulated for this: that samples of this
5 also shows a polyhedral representation of a portion of composition do not exist in nature (although this did not
the structure of andalusite. Andalusite is an orthosilicate seem reasonable to us), and that andalusites with this
mineral and the isolated Si tetrahedron is shown in composition had been overlooked in thin section because
Figure 5. There are two Al sites: a five-coordinated site they would appear isotropic, or near isotropic. Shortly
labeled M2 and a six-coordinated site labeled M1. Mn after our work was published, Grambling and Williams

Gunter - The Polarized Light Microscope 39


Figure 7. Relationships of the refractive of the fibrous Figure 8. Photomicrographs of an approximately 500
zeolites - natrolite, mesolite, and scolecite (modified mm long natrolite sample capped with mesolite taken
from Gunter and Ribbe, 1993). This graph was in both plane-polarized and cross-polarized light. The
produced from data synthesized from the literature – crystal is mounted on a glass fiber and immersed in
no data were collected. Based on this graph, it is easy index-matching fluid for natrolite. In the plane-
to distinguish between these three samples by their polarized photo, the mesolite tip has higher relief
sign of elongation. than the natrolite portion of the crystal. In the
cross-polarized photo, the mesolite tip appears near
(1985) found andalusites in this compositional range that isotropic because of the lower birefringence of
indeed appeared isotropic. mesolite (Figure 7).
While this discovery may seem like a mere optical
curiosity (i.e., that orthorhombic minerals may appear increases at a lower rate than the refractive indices
isotropic), it has significance to the metamorphic parallel to the a and b crystallographic axes (Figure 7).
petrology community. Grambling and Williams (1985) Thus, natrolite has its largest refractive index direction
showed how changes in the triple point for the parallel to its long dimension, mesolite has its
aluminosilicates could be related to the Mn and Fe intermediate refractive index direction parallel to its long
contents of those andalusites, thus helping to account for direction, and scolecite has its smallest refractive index
some of the variability in location of the triple-point in parallel to its elongation. It is simple to distinguish these
the aluminosilicate phase diagram. three minerals in thin section or grain mount based upon
their sign of elongation.
Retardation and optical orientation of natrolite group Figure 7 also shows that the retardation for natrolite
zeolites - Based upon my previous work on andalusite, I and scolecite, while being low, would still appear
searched the literature for other possible effects of anisotropic in thin section or grain mount. Mesolite, on
changes in optical orientation that could provide the other hand, exhibits very low retardation and would
worthwhile information. Also, in general, a portion of appear isotropic, or near so. During the preparation of
my research is directed toward the understanding of Gunter and Ribbe (1993), we collected samples of fibrous
how the optical properties of materials are related to zeolites from a nearby basalt flow (Gunter et al., 1993).
their crystal structure and chemical composition. I first Figure 8 shows one of these fibrous zeolites affixed to a
investigated zeolites because of their many industrial glass fiber. In the plane-polarized light photograph, the
applications and wide-spread geologic occurrences. refractive index fluid matches natrolite, so it exhibits
Also, zeolites have low birefringence because they are very low relief. Mesolite has a slightly higher refractive
framework silicates; thus, a small change in some index and thus stands out in higher relief at the tip of the
structural or chemical property may cause a large change crystal. In cross-polarized light the photomicrograph
in the easily observable retardation. reveals how the retardation clearly shows an anisotropic
Gunter and Ribbe (1993) collected optical data from crystal, but because the retardation for mesolite is so low,
the existing literature for the natrolite group zeolites it appears isotropic. The study again shows how subtle
(natrolite, mesolite, and scolecite). After some obvious changes in chemistry can cause large effects on the
corrections to the optical orientations incorrectly retardation. Because retardation is so easily observable, it
provided in some of the standard reference books, a plot can be used for other purposes than simply to identify
of the refractive indices for these three minerals could be minerals in thin section or grain mount.
made as a function of their Ca and Na content. In a
similar manner to andalusite, the rate of change of the Cation diffusion in heulandite group zeolites - In
refractive indices were different for the different another study by Gunter et al. (1994) on Pb-exchange
crystallographic directions. In this mineral group, the heulandite group zeolites, we used optical data to aid in
refractive index direction parallel to the c determining the extent of Pb exchange. Pb substitution
crystallographic axis, which corresponds to chains of increases the birefringence, and thus the retardation.
tetrahedrons parallel to the c crystallographic axis, Figure 9A shows a non-exchanged sample exhibiting

40 Journal of Geoscience Education, v. 52, n. 1, January, 2004, p. 34-44


were able to determine the diffusion coefficients for Na,
K, Rb, and Cs by making simple observations in changes
of optical properties with a PLM. No other single method
available could be used as easily and efficiently to
qualitatively observe exchange in zeolites or to
quantitatively determine their diffusion coefficients.

EXAMPLES OF CURRENT RESEARCH


A major theme in this paper is the orientational
dependence of refractive indices and morphology of
minerals. And, as discussed in detail above, the spindle
stage is the perfect tool to study this dependence. What
follows are three examples of how we have recently
integrated the spindle stage into other analytical
methods with the underlying theme to characterize the
directional dependence of various physical properties.

Single-crystal X-ray diffraction and optical orienta-


tion - The optical orientation of minerals relates the crys-
tallographic axes to the optical indicatrix. It is also useful
to identify the mineral either in immersion mounts or in
thin section and is an important physical property of the
Figure 9. A series of images of natural and mineral. While X-ray diffraction is used to locate the
Pb-exchanged heulandite zeolites showing changes in crystallographic axes, it cannot be used to locate the opti-
retardation (in the PLM images) and back-scattered cal directions. Thus if one wants to collect spectroscopic
electron (BSE) intensity (in the BSE images) as a data along the optical directions of a mineral, the spindle
function of Pb exchange (modified from Gunter et al., stage is used to determine these orientations. The optical
1994, which are in color). (All scale bars are 100 mm.) orientation is basically nonexistent for isotropic minerals
A) PLM image of a natural sample exhibiting low and trivial for uniaxial minerals. However, for biaxial
retardation. B) PLM image of a fully Pb-exchanged minerals the relationship is harder to determine, espe-
sample showing a drastic increase in retardation. C)
BSE image of a partially Pb-exchanged sample; the Pb
cially for monoclinic and triclinic minerals. Determining
has only diffused into the edges of the sample. D) PLM the optical orientation of these minerals requires an inte-
image showing how increased retardation can be used grated study using both X-ray diffraction to locate the
to monitor Pb exchange around the edges of the crystallographic axes and the PLM to determine the ori-
crystal; the greatest exchange is in the lower right entation of the biaxial indicatrix.
hand corner of the grain. E) BSE image of a partially This entire process can be simplified by using a
Pb-exchanged sample, with Pb diffusing in along the spindle stage equipped with an X-ray goniometer head
edge and cracks in the grain. F) PLM image showing (Figure 4A). The X-ray goniometer head, with crystal
Pb diffusion along the edges and cracks in a sample as affixed, can be transferred between the spindle stage and
shown by increases in retardation. an X-ray diffractometer (Figure 4B). Also, as described
above, the orientation of the biaxial indicatrix can be
first-order grey retardation, and Figure 9B shows a fully determined with the measurement of extinction
Pb-exchanged sample exhibiting second-order red positions and use of the computer program EXCALIBR.
retardation. (A color rendition of this figure can be found Thus, the orientation of the biaxial indicatrix is found
in Gunter et al., 1994.) and cast into the coordinate system of the microscope.
Another method that can be used to determine Next, the goniometer head is transferred to the X-ray
whether exchange has occurred, or to measure diffusion diffractometer and the orientation matrix is obtained.
of Pb into the structure, is backscattered electron imaging The orientation matrix contains information on the
(BSE) with a scanning electron microscope. Figure 9C orientation of the crystallographic axes a, b, c cast into the
shows a BSE image where the Pb has diffused a few tens coordinate system of the X-ray diffractometer. Next, to
of microns on the rim of the grain. Figure 9D shows a fully determine the optical orientation, these two
similar grain except this time as observed with a PLM. coordinate systems are transformed into each other and
Note the high order retardation on the lower right the relationship of the biaxial indicatrix and the
portion of the grain; this indicates Pb has diffused into crystallographic axes mathematically determined
this portion of the mineral. Pb not only diffuses into the (Gunter and Twamley, 2001). This entire process takes
rims of these minerals, but also through cracks. Figure 9E about one hour, as compared to older methods that
is a BSE image showing areas of Pb diffusion, and Figure might require several days.
9F is a PLM image showing areas of Pb diffusion. Thus,
again, in this study optics is very sensitive in Synchrotron radiation and absorption spectroscopy
determining chemical changes and much more efficient - The advent of synchrotrons with their high-energy
than performing a chemical analysis with an electron white X-ray beams have created a major new analytical
beam instrument to see spatial variation in chemistry. technique with which to examine minerals. X-ray
A natural extension of this project was to measure absorption spectroscopy is one of many techniques that
diffusion rates of different cations in heulandite group requires synchrotron radiation. In this method, the
zeolites by observing changes in optical properties. In a energy of the X-ray beam is changed in such a way as to
series of exchange experiments by Yang et al. (1997), we encompass the absorption-edge of an element of interest.

Gunter - The Polarized Light Microscope 41


Figure 11. Photographs showing integration of
spindle stage methods with a scanning electron
microscope (SEM). A) Stage of SEM with a 3 mm brass
pin used for crystal mounting in a goniometer head
Figure 10. X-ray absorption near-edge spectroscopy (Figure 3A) inserted into a normal SEM sample holder.
(XANES) spectra of a garnet and olivine with the B) Photomicrograph of an acicular amphibole particle
polarized synchrotron beam parallel to each of the mounted on the end of a glass fiber. C) SEM image of
three crystallographic axes. For garnet, all spectra the same sample in B in approximately the same
exhibit the same features, while for olivine they vary orientation. D) SEM image of a bundle of amphibole
as a function of orientation. Thus, the X-ray fibers mounted on a glass fiber. E) Magnified and
absorption indicatrix is similar to the optical reoriented image of the white box area in D to better
indicatrix. observe the morphology of the amphibole. (Images
modified from Bandli and Gunter, 2001.)
For example, for Fe absorption the energy of the X-ray
beam is scanned over the main absorption edge at 7111
eV. Information about the coordination, valence, and to ascertain the orientational dependence of these
other bonding characteristics can be obtained from absorption spectra by using oriented thin section
interpretation of these spectra. The majority of the work minerals. There are technical difficulties with this
in this area has been on millimeter-scale powders of method, along with a considerable amount of time being
minerals, as well as on single crystals of similar size. Our required for sample preparation. For instance, study of
current research (Dyar et al., 2002a, b) is exploring new an orthorhombic mineral would require at least two
ways to make these measurements on micron-sized oriented samples.
single crystals. However, one of the concerns in this area To study the orientational dependence of the spectra
of research is the orientational dependence of the and fully characterize them on a 100 micron-size crystal,
absorption spectra. Some previous researchers have tried we modified a spindle stage so it could be placed in a

42 Journal of Geoscience Education, v. 52, n. 1, January, 2004, p. 34-44


polarized synchrotron beam (Figure 4C). We could then
place an X-ray goniometer head on the spindle CONCLUSIONS
stage/synchrotron combination and make the required
measurements. To test the system we developed, we I hope I have convinced the reader that the answer to the
made measurements on samples that should show no question posed in the title is “yes.” From the teaching
preferred orientation (e.g., an isotropic mineral, such as perspective, the main reason we should continue
garnet) and samples that should show orientational teaching polarized light microscopy is that it is one of the
dependence (e.g., an orthorhombic mineral, such as few hands-on, interactive methods of learning about
olivine). The garnet was oriented using X-ray diffraction analytical instrumentation students get to participate in.
as described above. The olivine was oriented using the From an employment perspective, there is no other
spindle stage as described above. Based on the spectra in single course students can take that will secure them a job
Figure 10, it is clear there is no orientational dependence as rapidly as one that teaches the use of a PLM in
of the absorption spectra for garnet, as would be environmental applications, especially in the field of
predicted, and there is an orientational dependence of asbestos identification. In mineralogical research, there
the absorption spectra for the olivine, as also would be are still many new discoveries and innovations waiting
predicted based on the analogy with the behavior of the to be made using well-established, existing methods in
minerals and polarized light. Prior to the collection of optical mineralogy, and efforts should be made in the
these spindle stage assisted spectra, it was unclear what mineralogical community not to lose sight of these
the orientational dependence of the spectra would be. methods in favor of the latest instrumentation, which
Thus, integration of the methods of classical optical may not provide the best and most accurate data.
mineralogy aids in understanding these new analytical
methods and provides for better data collection methods. ACKNOWLEDGMENTS
Scanning electron microscope and three-dimen- I would like to thank Emeritus Professor F.D. Bloss, VPI
sional imaging - When higher magnifications are re- & SU, for his major contributions to the field of optical
quired, the scanning electron microscope (SEM) can be mineralogy as a textbook author, teacher, and researcher,
used in lieu of, or in conjunction with, a PLM. It is also and for mentoring me in the field of optical mineralogy. I
possible to obtain chemical information directly if the would also like to thank the MSA (Mineralogical Society
SEM is equipped with an energy dispersive detector. The of America) for inviting me to be a distinguished lecturer
SEM has a greater depth of field at similar magnifications in 2002-03; this paper was based on a seminar presented
when compared to a PLM. Standard sample preparation in that series. I would like to thank Professor Osamu
for the SEM is placement of mineral grains on an alumi- Tamada of Kyoto University for providing a visiting
num stub or glass slide. With this type of mount, professorship, which enabled me to contemplate the
two-dimensional imaging of the sample is possible. significance of polarized light microscopy in the
However, if a single crystal is affixed to the brass geoscience curriculum and work on my MSA lecture.
pin/glass fiber combination that fits into the X-ray Lastly, I would like to thank Professor Charles Guidotti
goniometer head, as used on the spindle stage, this brass of the University of Maine for a thorough review of this
pin can be placed in the sample holder stage of the SEM manuscript, providing suggestions for how to improve
(Figure 11A) to achieve three-dimensional imaging of the it, and confirming my views of the importance of
particle (Bandli and Gunter, 2001). Combined optical and teaching the use of the PLM. This work was partially
scanning electron microscope studies can be performed supported by funds from the National Science
on the same single crystal; this is a great aid in identifica- Foundation (NSF-CCLI 0127191).
tion of the sample because chemical information can also
be obtained. It is also a very useful method to handle REFERENCES
100-micron size particles without losing them. Once a
crystal has been affixed to a glass fiber and observed in Bloss, F.D., 1981, The spindle stage: principles and
the PLM (Figure 11B), it can then be easily transferred to practice, Cambridge University Press, Cambridge,
the scanning electron microscope (Figure 11C). England, 340 p.
The main advantage of this method is to be able to Bloss, F.D., 1999, Optical crystallography, Mineralogical
manipulate the crystal in the SEM to gain morphological Society of America, Washington, D.C., 239 p.
information in different directions. Figure 11D shows a Bandli, B.R. and Gunter, M.E., 2001, Identification and
bundle of amphibole asbestos fibers affixed to the end of characterization of mineral and asbestos particles
a glass fiber. In Figure 11E the sample has been using the spindle stage and the scanning electron
manipulated to view approximately down the long axis microscope, The Libby, Montana, U.S.A.
of the fibers. In this orientation the crystal faces of the Amphibole-asbestos as an example, The Microscope,
amphibole particle can be seen. If the sample were v. 49, p. 191-199.
mounted on a flat surface, one would not be able to Bandli, B.R., Gunter, M.E., Twamley, B., Foit, F.F., Jr., and
manipulate it to observe the morphology in different Cornelius, S.B., 2003, Optical, compositional,
directions. In the case of amphibole minerals, different morphological, and X-ray data on eleven particles of
surfaces may have an impact on the minerals’ health amphibole from Libby, Montana, U.S.A., Canadian
effect. For instance, amphibole asbestos particles tend to Mineralogist, v. 41, p. 1241-1253.
expose the 100 surface, amphibole cleavage fragments Dyar, M.D., Gunter, M.E., Delaney J.S., Lanzarotti, A.,
expose the 110 surface, and small single crystals of and Sutton, S.R. 2002a, Use of the spindle stage for
amphibole expose the 100 surface. Clearly, from a orientation of single crystals for microXAS: Isotropy
mineralogical perspective these different surfaces would and anisotropy in Fe-XANES spectra, American
have different reactivities. Using the SEM with a spindle Mineralogist, v. 87, p. 1500-1504.
stage style sample mount helps to characterize the
morphology of these particles.

Gunter - The Polarized Light Microscope 43


Dyar, M.D., Gunter, M.E., Delaney, J.S., Lanzarotti, A., Gunter, M.E., Knowles, C.R. and Schalck, D.K., 1993,
and Sutton, S.R., 2002b, Systematics in the structure Composite natrolite-mesolite crystals from the
and XANES spectra of pyroxenes, amphiboles, and Columbia River Basalt Group, Clarkston,
micas as derived from oriented single crystals, Washington, Canadian Mineralogist, v. 31, p.
Canadian Mineralogist, v. 40, p. 1347-1365. 467-470.
Grambling, J.A. and Williams, M.L., 1985, The effects of Gunter, M.E., Armbruster, T., Kohler, T., and Knowles,
Fe3+ and Mn3+ on aluminum silicate phase reactions C.R., 1994, Crystal structure and optical properties of
in North-Central New Mexico, U.S.A., Journal of Na- and Pb-exchanged heulandite group zeolites,
Petrology, v. 26, p. 324-354. American Mineralogist, v. 79, p. 675-682.
Gunter, M.E., 1994, Asbestos as a metaphor for teaching Gunter, M.E., Dyar, M.D., Twamley, B., Foit, F.F.Jr., and
risk perception, Journal of Geological Education, v. Cornelius, S.B., 2003, Composition, Fe3+/ΣFe, and
42, p. 17-24. crystal structure of non-asbestiform and asbestiform
Gunter, M.E., 1997, Laboratory exercises and amphiboles from Libby, Montana, U.S.A., American
demonstrations with the spindle stage, In Teaching Mineralogist, v. 98, p. 1870-1942.
Mineralogy, Mineralogical Society of America, Kile, D.E., 2003, The petrographic microscope: evolution
editors J.B. Brady, D.W. Mogk, and D. Perkins III, p. of a mineralogical research instrument, Mineralogi-
309-318. cal Record, special publication number 1.
Gunter, M.E. and Bloss, F.D., 1982, Andalusite-kanonaite Su, S.C., Bloss, F.D., Ribbe, P.H., and Stewart, D.B., 1984,
series: Lattice and optical parameters, American Optic axial angle, a precise measure of Al,Si ordering
Mineralogist, v. 67, p. 1218-1228. in T1 tetrahedral sites of K-rich alkali feldspars,
Gunter, M.E. and Ribbe, P.H., 1993, Natrolite group American Mineralogist, v. 69, p. 440-448.
zeolites: correlations of optical properties and crystal Su, S.C., Bloss, F.D., and Gunter, M.E., 1987, Procedures
chemistry, Zeolites, v. 13, p. 435-440. and computer programs to refine the double
Gunter, M.E. and Twamley, B., 2001, A new method to variation method, American Mineralogist, v. 72, p.
determine the optical orientation of biaxial minerals: 1011-1013.
A mathematical approach, Canadian Mineralogist, Yang, P., Armbruster, T., Stoltz, J., and Gunter, M.E.,
v. 39, p. 1701-1711. 1997, Na, K, Rb, and Cs exchange in heulandite
Gunter, M.E., Bloss, F.D., and Su, S.C., 1988, EXCALIBR single-crystals: Diffusion kinetics, American
revisited, American Mineralogist, v. 73, p. 1481-1482. Mineralogist, v. 82, p. 517-525.
Gunter, M.E., Bloss, F.D., and Su, S.C., 1989, Computer
programs for the spindle stage and double-variation
method, The Microscope, v. 37, p. 167-171.

44 Journal of Geoscience Education, v. 52, n. 1, January, 2004, p. 34-44