CHARACTERIZATION AND ANALYSIS OF INDIVIDUAL

FLY-ASH PARnCLES FROM COAL-FIRED POWER

STATIONS BY A ~OMBINA~ON OF OPTICAL
MrCROSCOPY, ELECTRON MICROSCOPY AND
QUANTITATIVE ELECTRON MICROPROBE. ANALYSIS
A. R. RAMSDENand M. SHIBAOKA
CSIRO Institute of Energyand Earth Resources,PO Box 136,North Ryde,NSW,Australia2113

(First recei& 7 July 1981and injirrclifwm 4 December 1981)

Ahtract-Quaatitative elsctroa microprobeanalysi!Sbss been used to determk tbc iaorgaaic cbemiai

compositionof iadividuai!ly-asbpartick previousiyCategorizAon the basis of propertiesEcognkabk by
~~ta~~~~.
Smn&egoriesnUybetW@ZUk
(1) lmfimeddct&ai mine&s (prki@ly quartz),
(2) irr&ar-spong,y part&s derivedfrom partly-fusedclay minera&
(3) vesicularcolourkss glass (in the form of irregutr partkki aad ccnospbefes)derivedfrom vi8cous
m&S,
(4) solid gks (mostly in tbe form of spberkal particks and sometimes pigmental) derivedfrom fluid
mehs

INTRODUCIION particles. Knowledge of the bulk composition of the

In the present paper a method is described in which
light microscopy, xanning ekctron microscopy and
electron microprobe analysis are combined in order to
obtain precise quantitative data on the chemical
compositions of indict particles of fly-ash from
which the range and trends in composition of the
various types of particle motphology can be de-
termined. Advantages of the method include the use of:
(1) coloured epoxy resin as an embedding medium
in order to enhance contrast between fly-ash particles
and background when preparing polished sections for
light microscopy,
(2) a special Robinson back-scattered electron de-
tector with a scanning electron microscope @EM) in
order to obtain ~~q~lity images of the inorganic
constituents of the fly-ash in the polished sections and
(3) a computerized energy-dispersive X-ray system
in conjunction with an electron microprobe in order to
obtain rapid quantitative analyses of many individual
fly-ash particles in the polished sections, su5cient to
characterize the range and trends in composition
within the particle population.
Precise quantitative characterization of fly-ash by
other means is diicult because the ash is composed of
a heterogeneous population of microscopically small
2191
ash is not generally sufficient because the inorganic
material in coal is not uniformly distributed either
within a lump or within individual particles of puIver-
ixed coal ConsequentIy its behaviour di&rs from one
coal partick to~ot~~~y~~~ly~mp~
even within single particles.
Sever-a1f~ors~nt~~~ to thiscomplexity, includ-
ing those inherent in the coal itselfsuch as the mode of
occurrence of the mineral matter (whether finely
disseminated or present as relatively large inclusions)
and the thermal behaviour of the coal in the furnace,
e.g. interaction between the inorganic and organic
constituents of the burning coal particles and the
chemical and physical environments through which
these particles pass within the furnace. All these
factors, together with the wide range of meRingpoints
and/or damnation temperatures likely to be ex-
hibited by a heterogeneous assemblage of mineral
matter, contribute towards the ultimate characteristics
of the fly-ash.
Characterization of fly-ash is important, however,
whoa attempting to understand how the material has
formed and to what extent this process determines its
behaviour in the installation with regard to problems
of slagging, corrosion and precipitation, In addition,
the characterization of fly-ash should improve under-
2192 A. R. RAMSDENand
standing and prediction of the consequences (both
short and long term) of ash dumping and utilization,
and the associated problems related to atmospheric
dispersal of the fine particles.
PREVIOUS WORK
Despite the fact that fly-ash consists of micro-
scopiallly-fine particks, the use of microscopic
methods for the routine study of such material has
only recently found general acceptance, primarily as a
consequence of the development of the SEM.
Light microscopy has been used to character&
particulate matter such as fly-ash in terms of partick
morphologies and their opticoll appearance (Hamilton
and Jarvis, 1%3)and, more recently, Fisher et al. (1978)
have recognized 11 categories of partick on the basis of
such observations.
Transmission electron microscopy (coupled with
light microscopy) has also been used to study details of
the formation of fly-ash during tk combustion of
pulverizd coal (Ramsden, 1968; Shibaoka and
Ramsden, 1977) and its sign&ance to electrostatic
precipitation (Paulson and Barn&n, 1970). In combi-
nation with X-ray microanalysis it has also been used
to obtain information on the chemical composition of
such part&s (Yakowitz et al., 1972).
It is tk SEM, however, that has found tk greatest
application in recent years. Several workers have used
it for morphokgical studies (Bonafede and Kiss, 1973;
Baker et al., 1975; Jan de Zeeuw and Abresch, 1976;
Chiu, 1978; Gibbon, 1979; Carpenter et al., 1980), and
the importance of this instrument for accurate sizing of
particks has baen demonstrated by Bagaini and
Ondov (1976). Where the instrument is equipped for
energy diaper&e X-ray analysis, it has proved possible
to determine semiquantitatively the elements present
in individual particles (Mid&man and Geller, 1976;
Small and Zolkr, 1977; Fisher et al., 1978; Parungo et
al., 1978; Capron et al., 1979; Hayes et al., 1978).
Scanning cketron microscopes, however, are generally
less satisfactory than electron microprobes when ac-
curate quantitative analyses are required.
Several workera have used the SEM as a supplement
to other analytical methods such as neutron activation
and photoekctron spectroscopy in order to study trace
ekmenta at the sur&ce of fly-ash partkIm (Huktt et al.,
1974,1975,1976; Rothenberg and De Nee, 1979). Such
Table 1. Maccral analyses of the pukkcd
Power station
ash source Vitrinite
Lindddl 45
Munmornh No. 3 52
unit boikr
Vales Point No. 1 55
unit boikr
Wallerawang No. 6 56
unit boiler
M. SHIBAOKA
information has also been obtained by other micros-
copic methods such as Auger electron spectroscopy
(Powell and Spicer, 1978) and laser microprobe analy-
sis (Blaha et al., 1979).
SAMPLES AND METHODS
Samples
Four fly-ash sampka and four original coal samples
from four of the main power stations in New South
Wales, Australia, have been analysed (Tabk 1). Liddell,
Munmorah and Vales Point are located in the Hunter
Valley and Newcastk areas on the northern margin of
the Sydney Baain, whereas Wailerawang is located near
Lithgow on the western margin of the Sydney Basin.
Because the coals supplied to the individual stations
come from a variety of coal mines it is not possible to
indicate precisely which coal was in use at the time the
fly-ash samples were collected. In general, however, the
Liddell power station uses tk Rayswater seam, the
Munmorah and Vales Point stations use the Great
Northern and otkr seams from the top of the
Newcastk coal measures, and tk Walkrawang Rower
station uses coal from tk Lithgow seam.
Maceral analyses of tk pulverixed coals (Table I)
indicate that all tk coals in use at the time of sampling
were bituminous co& rich in inertinite. Qualitative
electron microprobe analyses on the same samples
show that tk mineral matter consists predominantly
of clay and q- with minor carbonates and pyrite.
Quantitative microprok analyses (Table 2) suggest
that kaohnite is the principal clay mineral together
with minor illite, and that siderite is the principal
carbonate mineral.
Sample preparation and light microscopy
Most 5y-aah particles are colourkss and have a low
refractive index that makes them very difficult to see
under the light microscope when embedded in or-
dinary epoxy resin. Epoxy resin, however, is rciatiwly
stabk when subjected to electron bombardment, an
important consideration when material is pAacedin the
high vacuum environment of a SEM or electron
microprobe where contamination must k kept to a
minimum The addition of a blue pigment to tk epoxy
resin has been found to enhance the contrast of many
of the partides when vkwed under the light micro-
coals (vol %)
Exinitc 1nertinite Miaeral
4 47 4
3 42 3
2 39 4
4 40 trace
Characterization and analysis of individual fly-ash particles from coal-fired power stations 2193

scope. A blue background was chosen since pre-

liminary examination indicated that no blue particles
were present in the fly-ash samples.
To prepare the polished sections, a small quantity
(approximately O.Sg) of fly-ash was added to about
2ml of epoxy resin to which a few drops of blue
pigment (CIBAGEIGY pigment dye) had been
added. The mixture was stirred thoroughly and then
poured into a 2Scm cubic mould constructed of
aluminium foil to form a layer approximately 3 mm
thick. After hardening overnight the mould was
topped up with clear epoxy resin and left to set. The
block was then removed from the mould, and an
oblique cut was made diagonally from top to bottom
of the pigmented ash-bearing surface layer to ensure
that a representative population of particles was
exposed despite the unavoidable segregation that
occurred during hardening of the resin. This diagonal
surface was then ground and polished for microscopic
examination using standard petrographic procedures.
Incident light microscopy using strain-free oii im-
mersion objectives was employed in order to categor-
ize the various types of particles present in the ash
in terms of their morphologies and optical properties.
The samples were then lightlyrepolished to remove the
oily surface layer and coated with carbon in a vacuum
evaporator for examination in the SEM and analysis in
the electron microprobe.

Analysis by scanning electron microscopy and electron

microprobe
A Cambridge S600 SEM was used to supplement the
information obtained by light microscopy. Back-
scattered electrons (collected by a special Robinson
detector) were used for imaging rather than the
secondary electrons more usually employed with this
tw of instrument. In this mode, imaging arises
primarily from differences in atomic number, resulting
in excellent discrimination between the inorganic fly-
ash particles and the organic embedding medium
whilst at the same time suppressing distracting ar-
tifacts such as polishing scratches that are highlighted
in the secondary electron mode where relief is an
important factor in the image. Char is the only
constituent of the ash that cannot be distinguished
~~~to~y by this method of observation.
A Cambridge Microm V electron microprobe
fitted with a LINK System 860 energy dispersive X-ray
analyser was used to obtain quantitative chemical
compositions of individual fly-ash particles. This in-
strument, with a probe diameter of about 1 hrn, enables
analysis for all inorganic elements present in the
particle to be carried out in about 60 s. Because of the
rapidity and comprehensive nature of the analysis,
many particles can be investigated in a relatively short
time and compositional trends may be identified
within the particle types previously categorized by
microscopic examination Experience suggests that a
total of at least 30 particles representative of the types
present in the population shot&l be analysed in order
2194 A. R. RAMSDEN
and M. SHIBAO~~A
to determine the essential characteristics of these
trends.
Bulk chemical analysis
The bulk composition of each fly-ash was de-
termined on approximately 1 g samples following the
X-ray fluorescence method of Norrish and Hutton
(f949). Sodium was determined separateiy by atomic
absorption spectrometry.
RESULTS
Particle types
Despite a seemingly bewildering array of particle
shape, size and internal structure, mkroscopic exam-
ination (both iigbt and ckctron) suggests that the
part&s can be assigned to one of the seven categories,
althougb not all the types are neoessarily present in
each ash and their relative proportions vary con-
siderably between samples. In addition, transitional
varieties occur that cannot be t&gned to any one type
and in some instances two or more partick types are
found embedded together to form agglonaemtes. The
seven types of particle observed are outlined below:
(1) Unfused mineral particles were mostly quartz
and were readily meogn&d in m&ted light by their
low r&ctance and polishing relief (they are harder
than most other constituents of fly-ash). They were
relatively large particles, occupying the silt-size range
(4-150 pm), and many displayed the sub-angular to
sub-rounded morphologies typical of sedimentary
quartz Particles of this type were also readily recog-
nixed in the SEM (Fig 1).
(2} Irregular-spongy perticles (Figs 2{a) and 3)
occurred in the Liddell and Wallerawang a&es, They
ranged up to about 0.1 mm in size and most had a platy
II Si
Fig. 1. Jktrital quartz particle (SEM image) and analyscd composition.
morphology reflecting the original sedimentary tex-
ture oft he coal particles from which they were released
during combustion. Particles of this type were atso
commonly visible as cavity fillings within large frag-
ments of unburnt fusinite char where they were
protected from complete fusion by the unburned
fusinite cell walls. In some cases the ash particles
retained a well-developed cleavage typical of kaolinite.
Many particles had a bright opalescent white appear-
ance in reflected light caused by multiple internal
reflections within the fine spongy texture. Investigation
with the SEM at magnifications of 20,000 revealed the
presence of numerous pm-sized bubbles and cavities
dispersed throughout the material. As both mor-
phology and chemical ~m~sition (see later) indicate
that such particles are derived from original clay
minerals, these fine bubbles probably contain struc-
tural water liberated during decomposition and partial
fusion of these hydrous minerals. With increasing
fusion these particles become kss white and lose their
sub-microscopic spongy texture; instead, fine vesicles
appear that are visible under the light microscope. In
rare instances particles were dark in colour, pre-
sumably due to retention of unburned carbonaceous
matter.
(3) Vesicular glass particles (Figs 2(b) and 4) were
common in all the sampIes studied. There was, how-
ever, a wide diversity within this group. Many particles,
especially in the Liddell fly-ash, were rounded to
spherical shapes or were clearly the broken fragments
of such particles. Other particles, especially in the
Wallerawang fly-ash, were mostIy irregular. The in-
tensity of vesiculation and size of the vesicles also
varied ~nsiderably, some particles being relatively
solid, others being thin-walled and extremely in-
substantial. Although readily visible in the SEM, some
particles were very difficult to see in reflected light
wt %
sio* too*04
Al2O3 0.1 4
NtO 0.00
Fe0 * 0.18
K20 @OO
t&p @OO
CaO 0.00
TiO, 0.01
L MnO DO0
R205 0.43
503 O-03
ci,o 0.00
Total loo*85
*Total iron
expressed as Fe0
Fig- 2. Photkromphs of: (a) km?ular-spongy pertick, (b) vesicular gim oGI1QIchtrc,(c) solid ghss puti&, (d) dmdritic iron oxide particle. (c) crystalline iron oxide particle containing
magnetite (brown) and bamatitc (white) and (f) fuskite char particle.
 Characterization and analysis of individual fly-ash particles from coal-fired power stations 2197

,;::;, S.D. N

SiO2 49.88 1.31 3

Al,03 42.10 1.05 3
WO 0.21 0.10 3
Fe0 * 0.22 0.10 3
K20 0.09 0.03 3
Na20 0.02 0.03 3
CaO o-02 0.02 3
Ti02 o-15 0.13 3
bin0 o-01 0.01 3
p2°5 0.17 O-04 3
93 O;i6 O-07 3
Cl,0 I*10 0.54 3
Total 93.98

* Total iron
exwessed as Fe0

Fig. 3. Irregular-spongy particle (SEMimage)and analysed composition.

without the aid of the pigmented embedding medium.
Most particles were colourless or showed light brown
coloration. The appearance and ~rn~sition of a
typical cenospheric variety are shown in Figs 2(b) and
4. The markedly different appearance of this particle
under the light microscope, Fig. 2(b), arises from its
high transparency.
(4) Solid glass particles (Figs 2(c) and 5) were
generally completely free of vesicles or, when the
particles were large, contained a small number of
relatively large cavities. In reflected light they ranged
from colourless to shades of very deep translucent
brown depending upon the concentration of iron oxide
and probably other pigments (such as manganese
oxide). Solid glass particles were also readily recog-
nized in the SEM because of their relatively high
average atomic number. Some particles (mostly light
brown in colour) showed incipient dendritic crystalliz-
ation of iron oxides. The appearance and composition
of a light-grey solid glass particle are shown in Figs 2(c)
and 5.
(5) Dendritic iron oxide particles (Figs 2(d) and 6)
were relatively rare and may have been entirely absent
from the Wallerawang fly-ash; they were most
common in the iron-rich Liddell fly-ash Most den-
dritic iron particles were spherical and similar in size
to the solid glass particles, however, they were readily
distinguished from the latter by being much brighter

Mean
(Wt O/o) S*“* N
SiO2 66.66 0.65 3
A1203 20.28 O-23 3
M90 0.07 0.10 3
Fe0 * 0.15 o*os 3
o-53 0407 3
6.62 0.29 3
CaO 1.60 0.22 3
fiOz 0.04 o-07 3
MnO 0.01 0.01 3
p2°5 o.ti 0.25 3
503 0.07 o-04 3
Cl20 0.04 0.02 3
Total 96.25

K c,o + Total iron _ _

Fig. 4. Spherical v&c&ted glass particle @EM image) and analyscd ~rn~~tion.
2198 A. R. RAMSDEN and M. SHIBAOKA

37.63 0.31 3
22.64 0.23 3
0.27 0.03 3
12.37 0.15 3
0.31 0.02 3
0.01 0.11 3
12.46 0.07 3
2.88 0.15 3
Ca MnO 0.18 0.01 3
‘2’5 0.23 0.12 3
503 0.01 0.02 3
Cl,0 0.04 0.03 3
Fe
Total 91*09
w

Y K Ca T' *Total irqn

expressed as Fe0
I

Fig. 5. Solid glass particle (SEM image) and analysed composition (elliptical distortion in the SEM image is due to the
inclined viewing angk).

both in reflected light and ia the SEM due to the
presence of abundant dendritic iron oxide crystallites
in a generally subordinate gfass matrix. Two oxides
could be distinguished in reelected light, a darker
variety resembling magnetite (Fe,O,) and a brighter
oae resembling haematite (Fe,03). These two oxides
were intimately iatergrowa and indicate that the
dendrites initially formed in the reducing part of the
furaace as Fe30,. followed by partial conversion to
Fe,O, under cooler and/or oxidizing conditions.
(6) Crystalline iron oxide particles (Figs 2(e) and 7)
were also relatively rare and may have been entirely
absent from the Vales Point and Wallerawang fly-
ashes; they were most common in the iron-rich Liddell
tly-ash. Most crystailiae iron oxide part&s contained
large cavitic$ were spherical and of similar size to the
dendritic particles, however they differed from the
latter in consisting almost entirely of non-deadritic
ironoxidecryst&withonlytmcesofinterstMghtss.
As with the dendritic varktk, both magnetite and
haematite could be mcogked in reflected light al-
though this distinction could not he made ia the SEM.
The appearance and composition of a typical particle
are shown ia Figs 2(e) and 7.
Transitional varieties between solid glass, dendritic
and wholly crystalline oxide particles also existed,

e
(“wf:;)S.D. N
SiO;! 15.1f O-69 3
Ai2o3 7.80 0.36 3
M90 2.18 0,23 3
Fe203* 69.51 0.23 3
‘(20 0.13 0.05 3
Na$ 0.14 0.25 3
Co0 2.76 0.09 3
Ti02 0.33 0.03 3
MnO 2.13 0.08 3
p2°5 0.23 O-20 3
503 0.06 0.03 3
Cl,0 0.05 0.01 3
Total 100.43

Fig. 6. Dendritic iron oxide particle (SEM image) and analysed composition (elliptical distortion in the SEM image is due to
the inclined viewing angle).
 Characterization and analysis of individual By-ash particles from coal-fired power stations 2199

Fe
,;;:;o, S.D. N

SiO2 2.19 0.94 3

AI2o3 2.96 0.57 3
M90 2.92 0.31 3
Fe203* 87.00 0.24 3
K20 0.02 0.02 3
Na20 0.36 0.20 3
Co0 1.60 0.40 3
TiO2 0.03 0.03 3
MnO 2.72 0.21 3
p2°5 ori1 0.02 3
SO3 0.03 0.06 3

Fig. 7. Crystalline iron oxide particle (SEM image) and analysed composition.

reflecting variations in initial composition of individ-
ual particles and their thermal and impact histories.
Unambiguous identification could not always be made
in retlected light, particularly with the dry immersion
optics of the electron microprobe, but identification
could readily be achieved with oil immersion or with
the superior resolving power and magnification range
of the SEM.
(7) Unburnt char particles, Fig. 2(f), were most
common in the Liddell fly-ash (where it is suspected
that an over-run of feed coal may have occurred at the
time the furnace was sampled) but were rare in the
other samples. Highly irregular skeletal particles of
unburnt inertinite were most common, but complex
cenospheres typical of those known to be derived from
vitrinite during combustion of pulverized coal also
occurred. Some char particles were quite large (up to
0.5 mm). Unlike the glassy material the char particles
were opaque and thus appeared relatively bright in
reflected light, Fig. 2(f). Being composed largely of
carbon they were much darker than the atomically
heavier inorganic ash particles in the SEM and were
very difficult to distinguish from the embedding
medium in the back-scattered electron mode.
Particle composition
Chemical compositions of individual fly-ash par-
ticles in the Liddell, Munmorah, Vales Point and
Wallerawang ashes are shown in Tables 3 to 6,
respectively. In general, the analytical totals are ac-
ceptable considering the finely particulate nature of the
material. Water is probably present in some of the
particles and it is omitted from the analyses. Some of
the particles, however, proved to be so insubstantial
that unacceptably low totals (< !I0 %) were obtained
due to the presence of large amounts of (unanalysed)
epoxy resin under the electron beam. Fortunately, the
energy dispersive method of analysis ensures that all
the significant inorganic elements are detected so that
it is permissible to normalize the analyses to take
account of the diluting effect of the organic matter.
Whilst not recommended as a routine procedure, this
method does enable maximum information to be
obtained from expensive electron microprobe time.
Where such normalization has been carried out this is
indicated in the tables.
For convenience, the analyses in each table have
been grouped according to particle type and then
arranged in order of increasing SiO, content. Several
general facts emerge from the data:
(1) identity of the detrital quartz particles is con-
firmed,
(2) identity of the iron oxide particles is confirmed,
(3) vesicular glass and solid glass particles are all
essentially alumino-silicate glasses, but they contain a
wide range of other constituents (principally FeO,
CaO, MgO, TiO, and MnO) and
(4) the irregular-spongy particles have simple com-
positions consisting almost entirely of SiOr and
A1,O1. Several particles approximate to the com-
position of theclay mineral kaolinite. In the Liddell fly-
ash, where they are most common, several of the
particles contain unusually high amounts of chlorine.
This, however, can be attributed to contamination
from the embedding resin, as the chlorine was ab-
sorbed by these highly porous particles during harden-
ing of the epoxy resin.
Bulk compositions
Bulk compositions of the four ash samples ex-
pressed conventionally as individual elemental oxides
are given in Table 7.
SiOr, ranges from 47.88 wt “/, in the Liddell fly-ash
to 66.41 wt “/, in the Wallerawang ash.
 Table3. Chemical
composition of individud parti& in Liddeti5y-ash (wt “/

Partick type Remarks

SiO, Al*03 Mg<) FcO* K,O Na20$ CaO TiOa MnO P*05 SOS c&w Total

Crystalheoxide 4.16 1.95 4.83 79.92 na 4.25 0.21 1.56 0.33 na 97.24
6.22 3.82 5.01 74.03 :g na 3.82 0.15 1.62 0.13 na 94.80
1.10 4.83 1.65 72.75 0.00 M 243 0.13 1.28 0.13 na 92.39
Dcndritic
oxide 1.76 3.18 54.98 0.01 ml 8.53 a20 2.03 0.96 0.04 98243
ii%! 8.70 16.67 34.57 1.43 na 9.80 0.40 1.47 103.55
27.91 17.17 2.91 46.57 0.21 na 2.21 SE 1.11 0.28 OT3 99.07
28.25 7.92 15.42 30.33 1.55 na 10.38 3.73 0.47 1.73 0.14 99.91
soiii glass 11.48 5.82 212 6S.5.53 na 4.85 0.18 1.48 0.68 0.00 92.31
17.93 7.31 3.61 60.00 zz na 4.18 a14 1.90 0.37 95.59
7.91 55.02 0.30 119 3.68 0.48 1.03 0.0s 071 9266
z: 9.77 :z 50.213 0.80 0s 201 0.43 0.39 95.58
1.8.% 7.55 7.60 0.18 119 2582 w3 E 0-0s ZII 99.12
z 25.04 s.13 15s 0.83 na 15.13 a71 Q29 0.17 10226
4247 22.61 249 24.32 0.70 84 9.16 0.65 0.57 0.40 :z 103.45
vtsicukr glass 38.55 3.65 27.86 0s na 1.64 4.07 0.51 0.19 99.26
39.85 z 1.76 2s.u) 0.78 M 1.68 1.25 0.57 0*;1 99.95
41.70 l&B 3.73 25.86 0.23 08 4.50 1.14 z 98.14
43.S3 3Sm a47 1.68 0.17 na 17.76 0.12 0.12 :: 99.16
45.70 3.34 21.14 a44 M 3.82 0.47 o&E 98.66
47.33 3.55 24.84 QS2 na E 1.41 0.12 a12 104.82
51.71 &74 4% 1.51) na 17.65 0.78 0.27 100.46
1.11 6.97 a79 Ck32 4.SS 0.28 E
2: am 0.44 0.53 S-Till 2.87 0.00 3.67 0.09 z-g
74h 1.31 4.65 238 111 1.23 at-n 0.18 im? 99123
Irregular-spongy 41.68 a46 0.26 0.21 111 0.05 7.71
47.10 0.29 0.18 M E-z! E Q24 0.42 ZE
47.84 EZ a40 O.S8 na a15 0.27 3.51 wi.72
4800 z MS 0.33 0.41 1111 0.07 E 0.18 0.31 9a58
48.fa 38.83 0.35 M OX?8 0.11 1.79 90.75
49.81 41.20 :g g M 0.21 z 0.38 0.73 93.60
11986 45.75 :: a26 O-31 na 0.05 0.19 2.62 99.70
51.19 43.79 0.23 0.00 Om tm 0.01 :z 0.25 97.28
53.12 44.11 a41 O-48 M 0.10 0.43 0.09 E 99.33
62.20 36.39 E 0.31 0.43 M MI8 0.16 0.21 0.38 lOa
97.71 1.89 O.Ql 0.00 0.77 na 0.00 a00 0.19 M Nn.64 Dctritalqmutz
102.11 0.91 0.80 0.12 0.00 M a04 0.04 0.26 Da 103.64 Dwital quartz
 Tabk 4. Chemicalcomposition of individualparticks in Munmorah fly-ash (wt%)

Partkk type SiOl A&O, MgO FcO* KZO Na,O COO TiO, MnO P,Ol so, Cl,ot Total Remarks

crystallius oxide 1.27 1.90 5.76 71.26 a00 a41 1.58 0.03 8.16 0.00 0.00 0.04 90.41
2.76 248 248 65.37 0.01 a00 3.44 a04 a06 ai 0.10 0.00 92%
Dcnclriticoxide 15.57 8.30 4.57 55.99 al5 0.00 1.03 0.08 7.20 a00 O-00 0.03 9292
2256 5.43 9.14 46.96 aol 0.47 9.28 a39 2.00 0.00 a04 0.01 95.29 Angular slag frag
!Midgkss 35.% 21.55 1.83 31.71 0.36 0.27 0.45 a24 1.04 a05 0.00 0.04 93.49
46.m 19.88 15.10 11.82 3.04 0.16 a06 5.56 a03 al3 0.09 0.01 101.89
47.16 24.69 0.35 0.81 3.31 0.10 a24 14.02 a08 0.35 0.02 0.40 91.55
47.41 2267 0.72 2.69 233 1.20 2.10 22.96 a04 0.16 0.00 0.02 101.59
47.97 29.80 1.11 3.32 1.18 0.86 Q87 8.17 a04 a63 0.05 0.10 94.12
49.53 30.94 299 13.98 1.01 a46 0.79 0.84 a00 0.05 0.00 0.03 100.63
53.30 13.26 5.10 23.14 1.77 0.50 1.44 0.47 1.02 0.03 a02 0.00 100.08
55.15 37.47 2.38 5.43 1.50 0.51 0.12 1.61 0.12 0.10 0.00 0.10 104.40
56.24 33.79 0.22 0.61 6.98 aol 0.18 0.32 0.17 aos 0.10 1.35 100.00 Normalized
72.26 16.49 0.65 3.66 1.46 0.50 0.56 6.85 O.fM 0.42 0.07 0.08 103.05
17.84 11.03 0.27 0.71 4.26 0.32 a75 5.24 0.05 0.50 0.00 0.01 100.99
Vesicularglass 41.64 26.54 2.22 22.66 0.83 0.49 0.60 1.83 0.44 0.00 0.00 0.00 97.24
47.88 43.80 0.47 0.74 0.56 0.75 1.11 2.00 0.00 0.06 0.21 0.20 97.73
49.59 4232 0.62 0.81 0.99 0.26 0.00 a65 0.03 0.0 0.00 0.03 95.30
so.30 47.24 0.17 0.22 0.20 0.29 0.00 0.00 0.00 0.16 0.08 0.12 98.87
50.56 4251 0.27 0.10 0.22 0.10 0.00 0.13 0.02 0.13 0.06 0.00 94.10
53.23 41.65 0.39 O.% 0.73 0.12 0.20 0.12 a00 0.25 0.12 0.01 97.76
53.25 34.22 1.69 4.09 1.18 0.72 0.67 294 a00 0.15 0.02 0.07 99.00
6282 24.88 1.98 5.71 1.57 1.32 0.49 1.58 0.02 0.04 0.03 0.06 100.52
6290 25.42 0.81 1.62 286 5.59 as5 0.02 0.16 0.08 0.W 0.00 99.99 Normalized
63.01 2a60 al6 0.53 4.97 0.53 0.07 0.54 0.00 0.15 0.07 0.14 90178
70.77 23.58 0.36 226 1.21 0.46 0.19 1.15 a04 0.00 0.14 0.06 lOO.01
8231 10.87 0.75 1.29 3.00 a43 0.15 0.33 0.06 0.13 0.14 0.55 100.00 Normalized
83.23 11.00 0.W 0.38 3.99 0.97 0.08 0.13 0.00 0.14 0.02 0.05 100*06
92.53 5.72 0.55 0.90 1.24 0.23 0.11 0.33 0.00 0.37 0.05 0.01 10204
Mined loo.73 0.23 0.00 0.14 0.00 a00 0.00 0.70 0.02 a36 0.00 0.00 101.55 Dctritat quartz

* Total iron expressalas FeO.

 Table 5. Chemicalcompositionof individualpart&s in Vaks Point fly-ash(wt %)

Partick type SiOl AlA h4gO FcO* K,O Na,O CaO TiO, MnO P,O, SO3 c40t Total RCIMkS

Dcndriticoxide (7) 11.45 8.26 56.17 0.02 0.00 1.37 0.52 0.63 0.00 0.12 0.05 94.46
solidgkss 1297 2.08 44.43 0.40 0.26 1.16 1.84 1.77 0.15 0.02 2.22 loa Normalixu-l
15.79 0.43 1.31 3.75 0.72 0.51 38.10 a01 0.11 0.00 O.tXl 101.29
18.74 12.56 17.00 1.83 al2 o.o5 5.20 0.25 al7 0.14 ao2 98.01
19.75 4.43 26.85 0.89 0.21 0.78 1.12 al7 0.12 0.01 98.79
33.33 8.10 0.62 0.57 al0 11.13 a22 a14 a20 a07 E lals7
51.01 3214 6.17 5.62 1.76 0.50 a05 265 aoo 00~ 1W.W
5212 33.86 o.sl 10.53 0.92 a20 a43 a39 Z a00 dos :I 99.45
23.73 0.69 4.68 276 a41 1.04 959 ali 0.21 0.00 aoo 97.7s
z 19.49 0.57 1.42 4.72 a48 o.35 17.64 o.a9 a24 0.06 aos
57.49 23.& 5.52 222 0.53 O.29 8.91 1.55 a09 a30 a00 o.00 :I
6S.87 l&A6 O.o4 0.10 1205 2.30 ox2 a34 0.02 aoo a03 0 99.52
6470 13M a54 16.37 a81 al0 ass a36 1.01 a31 0.~ 0.14 99.99 Normalixed
71.4s 2a93 a47 a90 7.67 a57 0.24 am a07 a20 ao7 a01 RX.79
VUkUklglMS 47.46 41.62 a66 0.74 a71 0.38 a20 al2 a25 9241
53.17 44.25 as8 1.0s a89 0.26 a21 a00 :E 0.09
0 14 0.16
0.11 a03 Ma73
S4.72 39.88 a43 1.36 1.72 a24 0.87 a4o a00 a00 0.10 a28 lOa Nor~~lizd
31.99 1.82 5.65 0.71 a01 ao7 0.00 aoo 99.27
SW2 E 0.37
o.so 144
1:o3 aos a01 0.05 O.Qs 91.03
6S.2s 21.53 a48
a72 1.05
1.43 ;: :z a87
afi 14.33
0.87 al7 al4 0.15 022 laQO0 No-
6S36 15.65 a30 1.51 1.22 aal a01 o.s4 99.99 Normalked
6s.53 21.25 a44 1.00 1.46 a33 a74 0.60 0.01 E 0.14 al4 91.81
65.63 24.46 al7 o.~8 281 0.05 0.29 0.12 0.07 98.90
67.26 2Q82 :: 1.32
1.94 219
7.11 o-22 au7 al2 0.00 0.11 0.W 0.07 97.88
67.68 24.91 0.73 1.61 2.80 0.48 o.31 o.84 a00 0.18 0.08 0.37 lOO.fB Norma&d
7a45 18.59 0.91 1.20 4.70 0.04 0.08 O.fH 0.12 0.05 0.00 3.05 100.00 Nommlized
Mineral loo.41 0.32 0.00 0.00 0.00 0.00 o.o4 o.oo ao2 0.43 0.00 0.03 101.25 Dctritalquartz

l Total iron expsscd as FcO.

t Cootamioatioafrom theembeddingresin.
 Tabk 6. Chcmicai composition of individualpnrtkla in Wdkrawan8 fly-ash (wt “/

P8ftkktypc =h 403 k&O FcO* KzO NazO CaO TiO, MnO PlOS so, Cl,Ot Total Remarks

wlhrm 38.o7 27.76 0.47 0.24 247 0.11 a34 24.81 a05 a21 0.00 0.12 94.66
67.82 17.39 a32 a34 2.42 0.21 0.22 10.69 o.oo 0.63 0.0 0.08 loo.12
VUkUhr#Sl8 36.11 14.31 0.30 0.47 2% O.o4 a17 46.82 a00 aoo 0.12 aoo l#AO
u.33 47.02 a26 0.17 1.99 o.10 am 1.16 O.ol o.o2 o.o6 a07 95.30
47.02 37.15 a32 0.10 1.44 ao2 a11 4.70 o&I 0.06 0.15 91.21
47.32 0.21 0.28 235 0.24 0.45 24.46 a00 aoo sot 99.92
49.84 Et 0.28 0.24 2.45 0.10 a02 t: 0.15 94.25
53.61 37.93 0.83 0.30 4.23 0.1; E 0.35 0.14 0.00 E 1.31 lOO.fMJ Noixuxlkd
37.53 0.70 0.78 5.95 0.17 0.09 0.00 0.00 io8 O.OO lo233
ES 32.31 OSO 0.23 3.96 0.30 2; 0.15 o.00 0.20 a11 0-M %.07
58.9o 30.95 0.78 0.55 3.82 0.55 0.18 0.39 at@ 0.00 0.20 3.68 lOO.OO Normal&d
6232 28.75 0.31 0.10 273 0.12 0.38 0.43 a00 0.0s 0.17 ai 95.51
64.20 21.83 0.17 0.33 3.09 0.19 0.23 9.01 0.08 0.52 O.o2 0.32 lOaMI Notmabd
68.37 27.22 0.43 0.37 4.08 0.57 0.13 o.oo 0.12 ao2 0.01 101.33
7200 12.51 0.19 0.12 1.32 09; a28 4.o7 0.00 0.30 0.o4 a01 91.08
72.01 9.21 0.24 0.39 2.09 0.00 12% o.oo 0.24 0.06 O.OO 97.34
73.45 14.81 0.35 0.32 2.62 0.18 t: 0.14 0.00 0.20 0.10 all 9232
76.62 18.98 0.36 0.37 2.96 0.06 0.16 0.20 0.03 0.03 0.00 0.18 lOO.OO Norm&cd
78.17 14.20 1.61 2.06 4.97 0.22 0.05 a05 0.05 0.11 o.o7 101.56
78.91 11.84 0.28 a19 268 0.16 a19 3.57 0.00 0.36 0.09 1.72 lOO.fXI Normalkcd
81.54 13.35 0.19 0.18 25O 0.14 1.51 0.05 0.20 0.04 0.29 loO.OO Normxlized
83.58 9.95 0.33 o.o9 3.05 oa: 0.28 0.12 0.42 0.00 1.57 lOO.00 Normakd
84.67 12.u) 0:08 $E 0.11 0.00 0.29 0.08 100.29
88.53 10.76 E 0.16
0.05 233
200 0.12 1.32 0.00 a37 o.oo E 103.85
9o.o2 4.99 0.02 0.23 1.22 0.19 E 0.12 0.00 0.38 0.08 0.12 97.39
94.19 5.84 0.01 a10 0.68 0.21 0.03 0.46 0.02 0.28 0.17 0.09 10208
frreeuhr-tpongy 43.73 4a49 0.35 a23 1.31 0.19 0.2O 4.14 0.00 0.14 0.10 0.51 91.40
U.78 0.19 0.13 1.10 aoo 0.21 o.o9 0.01 0.12 0.24 0.14 93.60
z 46.87 0.16 ao8 1.58 0.19 0.05 0.00 a02 0.12 0.13 97.61
51.45 44.60 0.17 aoo a69 2: 0.03 0.03 a02 a03 aoo 97.09
51.82 45.44 0.00 a26 1.24 O.O2 0.15 0.13 0.00 0.03 0.25 lOO.OO
69.98 25.68 a53 0.08 1.91 a22 a22 0.38 O.o8 0.29 0.08 100.00 Normdid
MifJd 101.76 0.48 aoo 0.03 0.06 0.19 0.w O&2 0.01 a36 0.00 lo292 Dctritd qusrtz

* Totd iron exprcned u FcO.

t Coltwtion from WlbCddiU8resin.
2204 A. R. RAMSDENand M. SHIBAOKA

AI,O,, relatively constant in the Liddell (24.63

wt ?,), Vales Point (25.01 wt 7;) and Wallerawang
(24.49 wt “,,)ashes, but slightly higher (7.38 wt 7;) in the
Munmorah fly-ash.
Fe0 (total iron), ranges from 0.68 wt “, in the
Wallerawang ash to 12.00 wt 9, in the Liddell ash.
Although expressed as Fe0 it is clear from microscopic
observations that part (if not most) of the iron is
present as Fe,OA.
MgO, significantly lower (0.5 wt “/,) in the
Wallerawang fly-ash than in the other samples where it
ranges from 0.95 wt y; in the Vales Point sample to
1.65 wt % in the Liddell ash.
CaO, significantly lower (0.29 wt s;) in the
Wallerawang fly-ash in the other samples where it
ranges from 1.07 wt y0 in the Vales Point sample to
2.12 wt % in the Liddell ash.
K20, low in the Walkrawang (0.28 wt 7;) and
Liddell (0.64 wt %) ashes and significantly higher in the
Munmorah (1.66 wt %) and Vales Point (1.68 wt %)
ashes.
Na,O, sign&antly lower (0.08 wt 7;) in the
Wallerawang fly-ash than in the other sampks where it
ranges from 0.23 wt y0 in the Liddell ash to 0.74 wt %
in the Munmorah ash.
TiOs, relatively constant minor constituent in all the
ashes, ranging from 1.06 wt y0 in the Walterawang
sample to 1.28 wt y0 in the Munmorah sample.
MnO, only signi&mt in the Liddell fly-ash
(0.23 wt %), in all the other samples it is kss than
0.1 wt %.
P,O,, only significant in the Liddell sample
(0.23 wt %), in all the other samples it is less than
0.1 wt %.
SOJ, only significant in the Liddell sample
(0.17 wt %), in all the other samples it is less than
0.1 wt %.

DISCUSSION

Whilst it is possibk to use the combination of

optical m&mcopy, scaonirtg ebaron mkroacopy and
electron microprobe aualyris specif%ly to obtain
information relating the optical and morphological
properties of individual ey-osh partick to their com-
positions (Figs l-7), such an analysis does not ad-
equately cbotlrcterizc the ash as a whole. A more useful
approach is to plot the results of many analyses in
terms of the pseudo-ternary system silica-alumina-
“other oxides”, where “other oxides” comprises highly
variable amounts of CaO. MgO, KsO, NosO, FeO,
MnO and TiOs that may he expected to influence the
viscosity and/or cobur of the gkaa Wbem this is done
(Fig. 8) ready comparisons are pouibk between the
different ashes and several observations can be mpdt:
(1) The range of particle compositions observed in
each ash can be attributed to variable proportion of
quartz, clay and other minerals (principally the
FeMgCa-carbonates) in the original coals. The trends
 Cbaracteriziuion and anaIysis of individualfly-a& putides from coal-tired power stations 2205

SILICA SILICA

ALUMINA OTHER OXIDES ALUMINA SILICA OTHER OXIDES

SILICA

bllNERAL5
~~6UL~ -smN6Y
YESICULATED MASS
SOLID GLASS
OENDRlllC
CRYSTALLl#E
BULK CQMPOSllfON

/ f -.
ALUMNA OTHER OXIDES ALUMl~A OTHER OXIDES

Fig. 8. Compositional trends shown by gy-ash portides in the plaudotnnruy systetn

sihca-allu oxidesand their rcktionshipto bulkcompositioa.

are most clearly seen in the Liddell ash, but they also
apply to the other samples.
(2) Each type of particle occupies a zone in the
ternary diagranx unaltered minerals close to the silica
apex; crystalline iron oxide particles close to the “other
oxidt” apex; irregular-spongy particles close to the
kaolioite composition; glass particles within a tri-
angular zone bounded by silica, kaolinite and a com-
position near the aotre of the diagram but offset
towards the oxide apex.
(3) Depending on the particular asb in question,
varying amounts of overlap occur between the particle
types. With the exception of the deodritic iron oxide
tp, the least amount of overlap occurs in the Liddell
fly-ash. IO the Vaks Point and Munmorab ashes there
is considerabk overlap between vcsicuhtted and solid
glass particles, and in the Wallerawang fly-ash there is
considerable overlap bctwceo vesicular glass and
irregular-spongy particles.
(4) The deodritic iron oxide particles in the Liddell
ash appear to have formed at a constant SiOz.content
of 27.4f0.8 wt %, suggesting that composition (as
well as rate of cooling) may intluence the formation of
this texturc. On the other hand, dendritic particles of
lower and variabk SiOs content are present in the
Vales Point and Munmorab ashes, so that the signifi-
cance of the SiOs content on the formation of these
particles in the Liddell ash may be more apparent than
real.
(5) Dark-colourcd glass particlea,particularly in the
iron-rich Liddell fly-ash, include transitional varieties
in which various stagca of dcveIopment of dcndritk
texture can be seen. Some particles only show incipient
development of dcndritic iron oxide, others consist
predominantly of dcndritic iron oxide. Nondendtitic
iron oxide particles only appear close to the other
oxides apex, and contain significantly higher concen-
trations of Fe0 than do the dendritic types.
It is concluded that partick composition of a given
ash depends not only on the composition of the
original mineral matter (which determines the bulk
composition), but also on the history ofcach individual
part& within the furnace, such as its residence time,
maximum temperature, rate of cooling and to what
extent it is recycled through reducing and/or oxidizing
environments.
APPLICATlONS
Methods described hiGncnabie fly-ash to bc charac-
terixed in terms of the composition of its constituent
mkroscopic particles, it is therefore suggested that
they could usefully be applied to:
(1) determming, with incmascd precision, to what
extent the ash produced by experimental-scale com-
bustion rigs resembles that actually formed under
industrial conditions,
2206 A. R. RAMSDEN
(2) monitoring the changes that occur within
particle population as the ash is formed and passed
through the furnace to the precipitators, and correlat-
ing such changes with problems of slagging or corro-
sion or precipitation efficiency and
(3) understanding the relative behaviours of dif-
ferent pulverized coals during combustion in pul-
verized-fuel-fired boiler units.
Acknowle&ements-The ash and coal samples used in this
study were su~~liat to Dr D. J. Swaiue bv Mr Frank Walker
of tdt Ekctkiiy Commisaioa of New sokh Wales in March
1976. Preparation of the polished aampks for miaorcopic
study was the result of much patient and skilful work
performed by Mr E. Murray. Miss Judy Lcdsam carried out
maccral analyses on the pulverized coals, bulk cbamkal
compositionsoftIleaabeawcrede&&Ded by Magi
and Mr A. Mart&x using X-ray &to-,
was determined a+ratcly by Miss M. Ducbeau using
atomic absorption spectroscopy. The authors arc grateful to
Dr D. J. Swains for making the sampks avaiiabk for this
investigation.
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