This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D2798 − 11a (Reapproved 2019)

Standard Test Method for

Microscopical Determination of the Vitrinite Reflectance of
Coal1
This standard is issued under the fixed designation D2798; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope 3.2 Abbreviations:

1.1 This test method covers the microscopical determination 3.2.1 Romax—mean maximum reflectance measured in oil.
of both the mean maximum and mean random reflectances 3.2.2 Roran—mean random reflectance measured in oil.
measured in oil of polished surfaces of vitrinite and other 3.2.2.1 Discussion—Other organizations may use other ab-
macerals present in coals ranging in rank from lignite to breviations for mean maximum and mean random reflectance.
anthracite. This test method can be used to determine the
reflectance of other macerals. 4. Summary of Test Method
1.2 The values stated in SI units are to be regarded as 4.1 The reflectance of the maceral vitrinite or other macerals
standard. No other units of measurement are included in this is determined in this test method by illuminating a polished
standard. surface of a section of coal in immersion oil using a micro-
scopic system that photometrically measures the amount of
1.3 This standard does not purport to address all of the light reflected from the surface. The reflected light is recorded
safety concerns, if any, associated with its use. It is the in percent reflectance after calibration of photometric equip-
responsibility of the user of this standard to establish appro- ment by measuring the reflected light from standards of
priate safety, health, and environmental practices and deter- reflectance as calculated from their refractive indices.
mine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accor- 5. Significance and Use
dance with internationally recognized principles on standard-
5.1 The mean maximum reflectance of the vitrinite compo-
ization established in the Decision on Principles for the
nent in coal as determined by this test method is often used as
Development of International Standards, Guides and Recom-
an indicator of rank as presented in Classification D388,
mendations issued by the World Trade Organization Technical
independent of petrographic composition, and in the charac-
Barriers to Trade (TBT) Committee.
terization of coal as feedstock for carbonization, gasification,
2. Referenced Documents liquefaction, and combustion processes.
2.1 ASTM Standards:2 5.2 This test method is for use in scientific and industrial
D121 Terminology of Coal and Coke research.
D388 Classification of Coals by Rank
6. Apparatus
D2797 Practice for Preparing Coal Samples for Microscopi-
cal Analysis by Reflected Light 6.1 Microscope—Any microscope equipped for reflected
light microscopy (such as a metallurgical or opaque-ore mi-
3. Terminology croscope) can be used, provided the lens combination of
3.1 Definitions—For definitions of terms, refer to Terminol- objective and eyepieces permits examination of the specimen
ogy D121. at a magnification between 400 and × 750, such that particles
of 1 µm can be resolved. The objectives shall be constructed so
that samples can be examined in oil with plane-polarized light
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal and have the highest quality of antireflection coatings. The
and Coke and is the direct responsibility of Subcommittee D05.28 on Petrographic microscope shall be able to project an image at similar
Analysis of Coal and Coke.
Current edition approved Nov. 1, 2019. Published November 2019. Originally magnification to a photomultiplier tube and to support the
approved in 1969. Last previous edition approved in 2011 as D2798 – 11a. DOI: photomultiplier tube housing. Means shall be provided to
10.1520/D2798-11AR19.
2
position the tube housing laterally to obtain maximum re-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
sponse. The microscope shall have a circular stage that is
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on capable of rotating a specimen through 360°. The mechanical
the ASTM website. stage attached to the microscope stage shall enable the analyst

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 D2798 − 11a (2019)
to move the specimen accurately (within 0.1 mm) to a given 6.9 Calibration Standards—Prisms constructed of high-
field location. A combination of objective and circular stage index glasses or synthetic minerals shall be used as standards
shall permit centering. The viewing eyepiece shall be supplied to calibrate the photometer for reflectance measurement. These
with a crosshair or grid to be used as a reference to locate standards must be durable, isotropic, resistant to corrosion, free
precisely the area sampled by the phototube. During from internal flaws or fractures, and have negligible light
measurement, no light shall be permitted to enter the observ- absorption. A prism with sides that form a 30-60-90° triangle is
er’s end of the viewing eyepiece. the most effective shape, with the side between the 30 and 90°
angles highly polished and used as the reflectance-measuring
6.2 Polarizer and Illuminator—The light incident on the surface. The prisms shall be enclosed, except for the polished
vertical illuminator of the microscope shall be plane-polarized surface, in a durable, lightabsorbent, water- and oil-resistant
by a prism or sheet polarizer. The vertical illuminator can mount; polyester or epoxy resin, made light absorbent with a
contain a Berek prism, a Smith illuminator, or high-quality dye or filler, serves adequately. It is desirable to have a number
glass plate. The polarizer shall be oriented at 45° when using a of different standards with reflectances near those of the
Berek prism or at 0° when using a Smith illuminator or glass vitrinite studied; these also serve to check the linear response
plate. of the photometer. The reflectance of each standard shall be
6.3 Photomultiplier Tube—In combination with the micro- calculated to the nearest 0.001 % by means of the following
scope optical system, light source, and filter used, the photo- equation:
multiplier photometer shall be capable of detecting the mini- R s 5 100~ n g 2 1.5180! 2 / ~ n g 11.5180! 2 (1)
mum light reflected from the limited portion of the coal sample
(see 6.8). The high voltage supplied to the photomultiplier tube where:
must be within the prescribed range to obtain linearity of Rs = standard reflectance in oil of the glass, % and
response. This is usually from 300 to 1100 V for side-window ng = refractive index of the glass at 546-nm wavelength, to
tubes and from 1000 to 1500 V for end-window tubes. the nearest 0.0001 index value.
Photodiode arrays, channeltrons, or other light-measuring de- NOTE 1—Most coal laboratories in North America use the following
Bausch and Lomb Co. or Schott Co. optical glasses (the reported
vices are acceptable alternatives providing that sufficient gray refractive index at 546 nm and the calculated standard reflectance in oil
levels obtainable will enable reliable differentiation of signal are given in parentheses):
equivalent to 0.01 % reflectance and that the system is linear in Bausch and Lomb Schott
the range of the reflectance measured.
689 309 (1.6935; 0.299 %) SF8-689-312 (1.6945; 0.303 %)
6.4 Photometer Amplifier—The signal from the photomulti- 751 278 (1.7566; 0.532 %) SF13-714-276 (1.7477; 0.496 %)
plier tube shall be amplified and displayed by a galvanometer, 827 250 (1.8351; 0.895 %) LaF12-836-423 (1.8400; 0.921 %)
850 324 (1.8543; 0.996 %) LaSF9-850-322 (1.8567; 1.009 %)
digital meter, or recorder. When adjusted for operation, the 915 213 (1.9235; 1.390 %) LaSF18-913-325 (1.9273; 1.413 %)
amplifier and meter shall be capable of reliably distinguishing 980 222 (1.9907; 1.817 %) LaSF6-961-249 (1.9670; 1.662 %)
differences in signal equivalent to 0.01 % reflectance and shall Other standards available that can be used include the following:
be linear in the range of reflectance measured. Leucosapphire (1.77; 0.59 %)
Yttrium aluminum garnet, YAG (1.84; 0.92 %)
6.5 Recorder or Meter—The recorder or meter used shall Gadolinium gallium garnet, 3G (1.98; 1.73 %)
have a response time at full scale of no more than 1 s to detect Silicon carbide (2.663; 7.52 %)

the maximum reflectance level during rotation of the micro- 6.10 Immersion Oil—The oil shall be a nondrying, noncor-
scope stage. rosive type that will not react with coal, does not contain
carcinogens, and has a refractive index within the range from
6.6 Light Source—The light source shall have a regulated
1.515 to 1.519 at 546 nm and 25 °C. Within the specified range,
power supply to provide for stable output. Some photometers
the refractive index of the oil is not critical provided the
and recorders require supplemental voltage-stabilizing trans-
specified value of 1.5180 is used in calculating reflectance of
formers if the line voltage fluctuates.
standards as specified in 6.9. Periodic checking of the refrac-
6.7 Filters—The light shall be made approximately mono- tive index of the oil is discretionary.
chromatic green by passage through an interference filter or
6.11 Sample-Leveling Press—A conventional manual level-
combination of filters with peak transmittance of 546 6 5 nm
ing device can be used to level sample briquettes and glass
and a half-peak transmittance bandwidth of less than 20 nm.
standards when they are mounted on microscope slides with
Insert the filter into the light path after the sample and before
modeling clay.
the photomultiplier tube.
6.8 Limiting Aperture—A limiting aperture made of nonre- 7. Test Specimen
flecting and opaque material shall be placed approximately in
7.1 Prepare the sample briquette in accordance with Practice
the focal plane of the eyepiece at its central axis to restrict light
D2797.
to the photomultiplier tube window so that only a small area of
the reflectance standard or sample is sensed. The diameter of
8. Setting Up and Calibrating the Apparatus
the aperture shall be selected to provide an effective field of
measurement (sensed spot) of about 5 µm diameter or about 8.1 Turn on the photometer and light source and allow
20-µm2 area. equipment to warm up for at least 1⁄2 h.

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 D2798 − 11a (2019)
8.2 Mount the glass standards and a polished briquette glass reflectance standard. If values change during rotation
containing the sample on slides using modeling clay and a more than 0.03 %, then the system alignment shall be checked.
leveling press or use a leveling briquette holder. 8.12 Measure the same areas of the glass reflectance stan-
8.3 Place the mounted briquette on the stage, apply immer- dards each time the calibration is made.
sion oil, and verify leveling of the mount and stage by checking 8.13 Glass standards should be cleaned at least once a
that there is no systematic focus change when the briquette is month to avoid oxidation and changes in reflectances.
moved laterally on the stage. Use Köhler illumination. To
minimize glare, restrict the illuminated field by means of the 9. Procedure for Measuring Maximum Reflectance of a
field diaphragm so that the diameter is about one third or less Sample
than the size of the full field. Adjust any other provisions of the
9.1 Immediately after calibrating the system, place a pol-
illuminator to reduce scattered light in the system.
ished briquette of the sample on the microscope stage and
8.4 Verify the position of the limiting aperture of the apply immersion oil.
photometer with respect to the field of view. This can be done
9.2 Adopt a systematic scheme of transection of the bri-
by moving a small bright object of the sample across the
quette for selection of areas to be measured. Transect intervals
position of the crosshair or reticle that marks the photometer-
shall be such that the entire surface of the briquette or
sensed spot, ascertaining that readings are highest when the
briquettes will be sampled for the component being measured.
bright object is within the sensed area or by using back-lit
The transect spacing shall be suitable for a total of 100
illumination of the measuring aperture if so equipped.
measurements.
8.5 Using a small, distinctive feature of the sample as a 9.3 Using the procedure specified in 9.2, select the location
guide, adjust the microscope so that the axis of rotation of the to be measured. Slight adjustments to the maceral position may
stage is coincident with the photometer-sensed spot. This is be made to obtain a scratch-free area of uniform appearance.
accomplished by adjusting the centering screws of the objec- Rotate the circular stage slowly (approximately 4 r/min)
tive or stage. The purpose is to eliminate movement of the through 360°. Reflectance will vary progressively from a
object grain or area from the sensed spot when the stage is maximum value to a minimum value as the stage is rotated.
rotated. Observe and record the maximum value. If the effective field of
8.6 Adjust the polarizer to a 45° position when using a measurement does not remain on the component being mea-
Berek prism or 0° when using a Smith illuminator or glass sured when the stage is rotated, then recenter the objective or
plate. Place a glass standard covered with clean immersion oil stage as described in 8.5. Avoid taking measurements of areas
on the microscope stage and focus on the polished surface. that are near highly reflecting grains such as pyrite. Because
some relief and nonplanarity may develop during polishing,
8.7 With no light reflected from the standard to the
avoid edges of particles and particles near the edge of the
phototube, adjust the photometer zero setting or dark current.
briquette.
8.8 Place on the microscope stage a briquette of opaque
9.4 Move the stage to the next area to be measured and
resin that has a hole 5 mm in diameter and 5 mm deep which
repeat 9.3. Continue the location selecting and measuring
is filled with immersion oil. Measure the reflectance of the hole
procedure. After approximately 1⁄2 h of operation, remove the
to ensure that a reflectance of 0.00 6 0.03 % is obtained
briquette and recheck the calibration of the glass standards. If
thereby ensuring that parasitic reflectances of the objective are
this value indicates a drift equivalent to more than 0.01 %
minimal. If the reflectance of the hole exceeds the stated limits,
reflectance of the initial standard reflectance value, discard the
then another objective having a higher quality anti-reflection
set of readings on the coal sample and rerun the measurements
coating shall be used.
after recalibrating the system in accordance with 8.7.
8.9 Then allow the reflected light to impinge on the tube. 9.5 When determining the reflectance of vitrinite, continue
Adjust the photometer amplifier or the illumination to obtain a the procedure until at least 100 measurements have been
meter or recorder scale setting that conveniently represents the obtained. The number of measurements for any other maceral
calculated reflectance of the glass standard (see Appendix X1). will vary according to the application of the data.
8.10 Without changing the settings, measure the reflectance 9.6 For blends that contain coals of different rank, 150
of one or more additional standards to check that the photom- measurements are necessary to determine the mean maximum
eter system measures correctly in the range to be studied. reflectance.3
8.10.1 Because the photometric system cannot give a linear
response to a wide range of light flux, standards with reflec- NOTE 2—Although the term “maximum reflectance” is used, the actual
value obtained in this method may not represent the true maximum
tance values close to that of the coal being measured should be reflectance axis of the reflectance indicatrix, an imaginary surface that
used. At least two standards having reflectances that span the
range of the coal being measured should be used.
8.11 Make all standardization measurements under the same
conditions used in measuring vitrinite reflectance. When mea-
suring mean maximum reflectance of vitrinite, rotate the stage 3
Supporting data have been filed at ASTM International Headquarters and may
through 360° and note the maximum reflectance value of the be obtained by requesting Research Report RR:D05-1021.

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 D2798 − 11a (2019)
defines a coal’s three-dimensional distribution of reflectances.4,5 The gram generated by automatic systems. If a correction to mean-maximum
reflectance indicatrices of most coals approximate those of uniaxial reflectance is made, results obtained by using an automated microscope
negative optical materials. All particles of such coals, regardless of system should be statistically equivalent to manually derived vitrinite
orientation, will display a true maximum reflectance in at least one reflectance results as determined in Section 9.
direction in polarized light. However, some higher rank coals, especially
anthracites, can have biaxial optical properties. In these cases, the mean 11. Report
value obtained by this ASTM method is a mean apparent maximum rather
than a mean true maximum reflectance. The apparent maximum reflec- 11.1 Report the following information:
tance is intermediate between the true maximum and the true intermediate 11.1.1 Mean and standard deviation of the readings of
reflectance. Determination of the true maximum reflectances of biaxial
coals can be obtained by (1) measurements on three different oriented maximum or random reflectance of vitrinite, as percent reflec-
surfaces of a polished coal block4 or (2) a graphical method applied to tance in immersion oil, shall be noted. Compute the mean as
measurements from particulate samples.5 the sum of the individual measurements divided by the total
number of measurements; the standard deviation is the square
10. Measuring Random Reflectance of a Sample root of the computed variance. It is suggested that the spread of
10.1 Assure that there is neither a polarizer nor an analyzer individual reflectance values be indicated either as a table of
in the light path between the lamp and the photomultiplier tube. the individual maximum reflectance values or as a frequency
distribution in the form of a histogram or a table of percents
10.2 Immediately after calibrating the system, place a pol-
within reflectance classes.
ished briquette on the microscope stage and apply immersion
oil. NOTE 4—Classes commonly span 0.1 % reflectance intervals, for
example 0.60 through 0.69 %.
10.3 Adopt a systematic scheme of transection of the NOTE 5—For informational purposes, the relationship between mean
briquette for selection of areas to be measured. Transect maximum and mean random reflectance has been determined through
intervals shall be such that the entire surface of the briquette or regression analysis from the 1991 to 1995 interlaboratory round-robin
briquettes will be sampled for the component being measured. exercise. The equation developed was found to be as follows for single
The transect spacing shall be suitable for a total of 100 seam coals between 0.7 and 1.7 mean maximum reflectance:
measurements. Mean Maximum Reflectance 5 20.034
10.4 Using the procedure specified in 10.3, select the 11.09 ~ Mean Random Reflectance! (2)
location to be measured. Slight adjustments to the maceral
position may be made to obtain a scratch-free area of uniform 11.1.2 Sample preparations and measuring equipment, or
appearance. Observe and record the reflectance value. Avoid indication of compliance with Test Method D2798 and Practice
taking measurements of areas that are near highly reflecting D2797 shall be noted.
grains such as pyrite. Because some relief and nonplanarity can 11.1.3 Any provisions made to check polish quality, such as
develop during polishing, avoid edges of particles and particles a check of measurements after repolish or comparison of
near the edge of the briquette. measurements from two mounts of the same sample shall be
noted.
10.5 Move the stage to the next area to be measured and
repeat 10.4. Continue the location selecting and measuring 12. Precision and Bias
procedure. After approximately 1⁄2 h of operation, remove the
briquette and recheck the calibration of the glass standards. If 12.1 Precision—The following criteria should be used for
this value indicates a drift equivalent to more than 0.01 % judging the acceptability of results on representative minus
reflectance of the initial standard reflectance value, discard the 850-µm (No. 20) subsamples within the mean maximum
set of readings on the coal sample and rerun the measurements reflectance range of 0.7 and 1.7 %.
after recalibrating the system in accordance with 8.7. 12.1.1 Repeatability—Duplicate results by the same
laboratory, using the same operator and equipment, should not
10.6 When determining the reflectance of vitrinite, continue
be considered suspect unless the results differ by more than
the procedure until at least 100 measurements have been
0.02 % actual reflectance.
obtained. The number of measurements for any other maceral
will vary according to the application of the data. 12.1.1.1 This test method does not require duplicate deter-
minations to be made. The repeatability value was developed
10.7 More than 100 measurements are necessary to test because most laboratories occasionally monitor and check
blends that contain coals of different rank. within laboratory precision as part of internal quality control
NOTE 3—Automated microscopy systems are used to measure random practices.
reflectance and estimate mean maximum vitrinite reflectance and coal 12.1.2 Reproducibility—The results submitted by two or
blend percentages. Users should be aware that the particle size consist, more laboratories, using different equipment, operators, date of
briquette polishing quality, surface leveling procedure, binder/coal ratio
used, and maceral composition will significantly affect the final reflecto-
test, and different representative subsamples of the same
sample, should not be considered suspect unless the results
differ by more than 0.06 % actual reflectance.
4
Levine, J. R. and Davis, A., “Reflectance Anisotropy of Upper Carboniferous 12.2 Bias—Because there is no accepted reference material
Coals in the Appalachian Foreland Basin, Pennsylvania, U.S.A.,” International
for obtaining the bias for the procedure in this test method for
Journal of Coal Geology, Vol 13, 1989, p. 341.
5
Kilby, W. E., “ Recognition of Vitrinite with Non-Uniaxial Negative Reflec- measuring reflectance of vitrinite, no specific statement is
tance Characteristics ,” International Journal of Coal Geology, Vol 9, 1988, p. 267. being made. All aspects of sample preparation (as specified in

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 D2798 − 11a (2019)
Practice D2797) and the condition of the glass reflectance made and polished by the twelve paticipating individual laboratories and
standards can impact reflectance measurement. (2) relectance measurements determined on a common set of glass
standards were found to closely parallel measurements determined on
NOTE 6—Based on the results from the interlaboratory round-robin glass standards used by the twelve participating laboratories.
study conducted by the twelve participating laboratories to establish the
precision values during 1991 to 1994, it was found that; (1) the difference 13. Keywords
between laboratories for reflectance was not significant when comparing
briquettes prepared and polished by a common laboratory to briquettes 13.1 coal; maceral; microscopy; rank; reflectance; vitrinite

APPENDIX

(Nonmandatory Information)

X1. CARE AND CALIBRATION OF GLASS STANDARDS

X1.1 Care of Glass Standards X1.2.5 Record the calculated value of the first glass stan-
X1.1.1 Keep immersion oil on glass standard and store dard in a table as shown in Table X1.1.
standard in a container with a lid to minimize dust accumula- X1.2.6 Read and record the stage position and the maxi-
tion on the surface of the standard. mum reflectance of the centers of all other glass standards
X1.1.2 Periodically remove the oil and carefully clean the without adjusting the photometer system.
surface of the polished glasses with a mild detergent such as X1.2.7 Place the second glass standard under the micro-
used for cleaning optical glass. Apply fresh immersion oil to scope objective and move to the recorded coordinates for that
the surfaces and store in the appropriate container. glass surface. Repeat X1.2.3 through X1.2.6.
X1.2 Preparation of a Matrix of Determined Reflectance X1.2.8 Repeat X1.2.7 for each remaining glass standard.
Values for the Glass Set
X1.2.9 Using the recorded values in the table, disregard
X1.2.1 Set up the microscope system in accordance with 8.1
those values associated with highly inconsistent readings
through 8.7.
(greater than 0.2 % reflectance difference) such as shown for
X1.2.2 Place the first glass standard under the microscope glass No. 5 in Table X1.1.
objective and move to the center area of the glass surface.
X1.2.10 Average all other readings except the adjusted
X1.2.3 Record the position of the mechanical stage. value that corresponded to the calculated reflectance and record
X1.2.4 Adjust voltage on the photometer to the calculated the determined average value. This value is the one for the
reflectance value of the glass standard as the maximum value specified area of the glass that is to be used for instrument
obtainable as the stage is rotated 360°. calibration as given in 8.7.

TABLE X1.1 Example of Calibration Matrix for Glass Standards

Glass Number 1 2 3 4 5 6
Calibration on No. 1 0.303A 0.508 0.914 1.014 1.351 1.649
Calibration on No. 2 0.302 0.496A 0.906 1.002 1.360 1.654
Calibration on No. 3 0.304 0.504 0.921A 1.007 1.363 1.650
Calibration on No. 4 0.307 0.508 0.924 1.008A 1.386 1.670
Calibration on No. 5 0.324 0.554 0.928 1.049 1.413A 1.703
Calibration on No. 6 0.307 0.509 0.914 1.014 1.361 1.662A
Determined average 0.305 0.507 0.915 1.009 n.u.B 1.656
Stage coordinates 3 × 118 3 × 110 3 × 103 12 × 118 12 × 110 12 × 103
A
Adjusted photometric reading from calculated reflectance values of glass standards.
B
n.u. = values not used for calculation of other reflectances or calibration of equipment because readings were inconsistent with others during construction of matrix.

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