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APPENDIX A: PALYNOLOGICAL AND KEROGEN ANALYSES
RESEARCH AND DEVELOPMENT CENTRE FOR OIL AND GAS TECHNOLOGY (PUSAT
PENELITIAN DAN PENGEMBANGAN TEKNOLOGI MINYAK DAN GAS BUMI)
“LEMIGAS”
Jalan Ciledug Raya Kav. 109, Cipulir, Kebayoran Lama, Jakarta 12230
No palynomorph can be recovered from 25 samples were carried out standard palynological
preparation. This is likely due to the strong degree of metamorphism or coalification
1. SBA 04 LC
The maceral particle has small to medium size with poor to moderate sorting which
represent high energy condition. Because of high vitrinite, it is interpreted that the coal was
formed on the lower delta plain environment.
vitrinite
A2
2. SBA 08 LA
The sample SBA 08 LA has no palynomorphs (barren). This sample consists of dominant
liptinite (5 %), vitrinite (50 %), inertinite (25 %) and like amorphous gel / AOM (20 %).
AOM
A3 inertinite
vitrinite
3. LC 205 B
The palynological analysis shows barren of palynomorph (barren). This sample composed
of dominant liptinite (10 %), vitrinite (55 %), inertinite (30 %) and like amorphous gel /
AOM (5 %).
A4
inertinite
vitrinite
4. LA 470 M 16 deg
Based on palynological analysis the sample shows barren of palynomorph. This sample
consists of liptinite (10 %), vitrinite (40 %), inertinite (40 %) and like amorphous gel / AOM
(10 %).
A5
vitrinite
inertinite
5. LBT 07 LA
Barren palynomorph is resulted from sample LBT 07 LA. This sample consists of liptinite
(5 %), vitrinite (60 %), inertinite (25 %) and like amorphous gel / AOM (10 %).
A6
vitrinite
6. SBA 09 LA
A7
AOM
inertinite
vitrinite
7. SBA 11 LC
The sample SBA 11 LC has no playnomorph (barren). This sample consists of liptinite (5
%), vitrinite (60 %), inertinite (25 %) and like amorphous gel / AOM (10 %).
A8
vitrinite
AOM
inertinite
8. SBA 12 LA
The palynological analysis shows barren of palynomorph. This sample consists of liptinite
(5 %), vitrinite (45 %), inertinite (20 %) and like amorphous gel / AOM (30 %).
A9
AOM
liptinite
(resin)
vitrinite
inertinite
9. LC 205 C
The sample LC 205 C has no palynomorh (barren). This sample consists of liptinite (5 %),
vitrinite (55 %), inertinite (30 %) and like amorphous gel / AOM (10 %).
A10
inertinite
AOM
vitrinite
10. LC 205 A
The palynological analysis shows barren of palynomorph. This sample consists of liptinite
(5 %), vitrinite (55 %), inertinite (30 %) and like amorphous gel / AOM (10 %).
A11
AOM
inertinite
vitrinite
11. LBT 01 LC
The sample LBT 01 LC has no palynomorh (barren). It consists of inertinite (50 %) and
vitrinite (40 %) component, with poor sorting of medium to large size maceral particle.
A12
vitrinite
inertinite
12. LBT 04 LA
The palynological analysis shows barren of palynomorph (barren). This sample composes
of dominant liptinite (5 %), vitrinite (40 %), inertinite (50 %) and like amorphous gel /
AOM (5 %).
A13
vitrinite
13. LBT 04 LC
The sample LBT 04 LC has no palynomorh (barren). This sample consists of dominant of
liptinite (5 %), vitrinite (40 %), inertinite (50 %) and like amorphous gel / AOM (5 %).
A14
inertinite
vitrinite
14. LBT 06 LA
The palynological analysis shows barren of palynomorph (barren). This sample consists of
dominant liptinite (5 %), vitrinite (40 %), inertinite (50 %) and like amorphous gel / AOM
(5 %).
A15
inertinite
liptinite
vitrinite
15. LBT 09 LA
The sample LBT 09 LA has no palynomorh (barren). This sample consists of dominant
liptinite (20 %), vitrinite (15 %), inertinite (10 %) and like amorphous gel / AOM (55 %).
A16
AOM
vitrinite
inertinite
16. LBT 09 LC
The palynological analysis shows barren of palynomorph (barren). This sample consists of
dominant liptinite (10 %), vitrinite (50 %), inertinite (30 %) and like amorphous gel / AOM
(10 %).
A17
inertinite
AOM
vitrinite
17. LBT 10 LC
The sample LBT 10 LC has no palynomorh (barren). This sample consists of dominant
liptinite (5 %), vitrinite (40 %), inertinite (25 %) and like amorphous gel / AOM (30 %).
A18
inertinite vitrinite
AOM
18. LBT 11 LC
The palynological analysis shows barren of palynomorph (barren). This sample consists
dominant of liptinite (15 %), vitrinite (40 %), inertinite (15 %) and like amorphous gel /
AOM (30 %).
A19
Liptinite
(resin)
AOM inertinite
vitrinite
19. SBA 01 LA
The sample SBA 01 LA has no palynomorh (barren). This sample consists of dominant of
liptinite (5 %), vitrinite (50 %), inertinite (30 %) and like amorphous gel / AOM (15 %).
Poor sorting of small to large size of maceral particle represent of high energy condition.
According to high vitrinite in this sample, it is expected the coal was formed on the lower
delta plain environment.
A20
vitrinite
AOM
inertinite
20. SBA 02 LC
The palynological analysis shows barren of palynomorph (barren). This sample consists of
dominant liptinite (5 %), vitrinite (50 %), inertinite (40 %) and like amorphous gel / AOM
(5 %).
Poor sorting of medium to large size of maceral particle represent of high energy condition.
According to high vitrinite in this sample it is expected that coal was formed on the lower
delta plain environment.
A21
inertinite
vitrinite
21. SBA 05 LC
The sample SBA 05 LC has no palynomorh (barren). This sample consists of dominant
liptinite (5 %), vitrinite (55 %), inertinite (35 %) and like amorphous gel / AOM (5 %).
Poor sorting of medium to large size of maceral particle represent of high energy condition.
According to high vitrinite in this sample, it is expected that coal was formed on the lower
delta plain environment.
A22
inertinite
vitrinite
22. SBA 06 LC
The palynological analysis shows barren of palynomorph (barren). This sample consists of
dominant liptinite (10 %), vitrinite (50 %), inertinite (30 %) and like amorphous gel / AOM
(10 %).
Poor sorting of medium to large size of maceral particle represent of high energy condition.
According to high vitrinite in this sample it is expected that coal was formed on the lower
delta plain environment.
A23
vitrinite
inertinite
Liptinite
(resin)
The sample SBA 09 LC has no palynomorh (barren). This sample consists of dominant
liptinite (5 %), vitrinite (50 %), inertinite (25 %) and like amorphous gel / AOM (20 %).
Poor sorting of medium to large size of maceral particle represent of high energy condition.
According to high vitrinite in this sample, it is also interpreted that coal was formed on the
lower delta plain environment.
A24
inertinite
vitrinite
AOM
The palynological analysis shows barren of palynomorph (barren). This sample consists of
dominant of liptinite (5 %), vitrinite (45 %), inertinite (20 %) and like amorphous gel /
AOM (30 %).
Poor sorting of medium to large size of maceral particle represent of high energy condition.
According to high vitrinite in this sample, it is expected that coal was formed on the lower
delta plain environment with a high degree of decomposition (AOM component).
A25
inertinite
AOM
vitrinite
25. SBA 12 LA
The sample SBA 12 LA has no palynomorh (barren). This sample consists of dominant
liptinite (10 %), vitrinite (55 %), inertinite (30 %) and like amorphous gel / AOM (5 %).
Poor sorting of small to large size of maceral particle represent of high energy condition.
According to high vitrinite in this sample, it is expected that coal was formed on the lower
delta plain environment.
A26
inertinite
vitrinite
liptinite
(resin)
were placed in an air drying oven with a maintained temperature of no more than 40 °C. The
coal samples were gently stirred frequently until the surface of the coal appeared to be dry.
The weight of the pans with the coal samples was recorded. The percent weight loss after
drying was calculated. The drying and weighing of the coal samples were repeated until the
A27
calculated weight loss is less than 0.1%/hour. The coal samples were allowed to dry until it
reached equilibrium with the ambient temperature and humidity before the final weight was
where:
ADL = air dry loss in weight %
R = residual moisture in weight %
where:
L = loss in weight in air drying in grams
G = weight of gross sample in grams
where:
W = weight of sample used in grams
H = weight of sample after heating in grams
Determination of Ash (ASTM D3174-04, 2012c)
The coal samples were pulverized to pass a 250 mm sieve. One (1) gram (weighed
to the nearest 0.1 mg) of sample was weighed and transferred to a weighed capsule which
was covered immediately. The uncovered capsule was placed in a cold furnace. The capsule
was heated gradually until the temperature reaches 450 to 500°C in 1 hour. After the second
hour, the coal samples were heated to a temperature of 700 to 750 °C. The capsule was
heated continually for another 2 more hours. After heating, the capsule was removed from
the muffle, covered and cooled under conditions to minimize moisture pickup. The capsule
was then weighed. The ash percent in the sample was calculated as follows:
where:
A = weight of capsule, cover and ash residue in grams
A28
B = weight of empty capsule and cover in grams
C = weight of analysis sample used in grams
The coal samples were pulverized until it passed through the 250 µm sieve. One (1)
gram of the sample was weighed in a pre-weighed platinum crucible with cover. The
crucible was placed on platinum supports before inserted directly into the furnace chamber
with a maintained temperature of 950 ± 20°C. Regulation of the temperature within the
prescribed limit is critical. After the rapid discharge of volatile matter has subsided, the
crucible was inspected to make sure that the cover is still properly sealed. After heating the
crucible for 7 minutes, it was removed from the furnace. The crucible was allowed to cool
and was weighed after. The percent volatile matter was calculated as follows:
where:
A = weight of sample used in grams
B = weight of sample after heating in grams
One (1) gram of the coal sample (weighed to the nearest 0.1 mg) was mixed
thoroughly with 3 grams of Eschka mixture [2:1 by weight light calcined magnesium oxide
(MgO) and anhydrous sodium carbonate (Na2CO3)] on a glazed paper. The mixture was
transferred in a porcelain crucible and covered with 1 gram of Eschka mixture. The crucible
was heated over an electrically heated muffle with a rise in temperature of 800 ± 25 °C in an
hour. This maximum temperature was maintained until all black particles disappear upon
stirring. The crucible was removed and the content was transferred into a 200-mL beaker.
A29
The sample was digested with 100 mL of hot water for 30 to 45 minutes with occasional
stirring. The resulting solution was filtered through a filter paper while decanting the
insoluble material in the beaker. The insoluble material in the beaker was washed several
times with hot water before filtering. After filtering, the insoluble matter was washed again
for five times with hot water while keeping the mixture well agitated. The filtrate amounting
to ~250 mL was neutralized to methyl orange using sodium hydroxide (NaOH). One (1) ml
of hydrochloric acid (HCl) was added to the filtrate. The filtrate was boiled while slowly
adding 10 mL or more of barium chloride (BaCl 2) which must be in excess. The solution
was boiled for another 15 minutes then left for at least 2 hours at below boiling temperature.
The solution was filtered through a Whatman No. 42 filter and was washed with hot water.
One (1) drop of silver nitrate (AgNO 3) was added and it produced a slight opalescent
mixture upon addition. The wet filter with barium sulfate (BaSO 4) was collected and
transferred to a weighed porcelain crucible. The paper was smoked off in the muffle furnace
and allowed to burn. The temperature was increased to 800 ± 25 °C and heated until constant
weight was achieved. The remaining BaSO4 was weighed up to the nearest 0.1 mg.
Correction for the sulfur was applied. This was done by the analysis of a weighed portion of
a standard sulfate using the prescribed reagents and operations in full compliance with the
standard. For a series of solutions covering the approximate range of sulfur concentrations
in the samples, add to or subtract from the weight of BaSO 4 determined for the sample. The
where:
A = weight of BaSO4 precipitated in grams
B = weight of BaSO4, correction in grams
C = weight of sample used in grams
A30
Determination of Calorific Value (ASTM D 5865-04, 2012d)
The calorific value was determined using a bomb calorimeter. Before the actual
Preparation of Bomb
The bomb was rinsed to wet the internal seals and surface areas of the bomb. One
(1) mL of water was added to the bomb before the assembly. A measured fuse was
connected in accordance with the manufacturer’s guidelines. The bomb was assembled and
oxygen was admitted to a consistent pressure between 2 and 4 MPa (20 and 30 atm). The
same pressure was strictly maintained for all measurements of heat capacity. Otherwise, the
sample was discarded. The oxygen was controlled to prevent the sample from being blown
Preparation of calorimeter
The calorimeter vessel was filled with water at a maintained temperature of not
more than 2°C below room temperature. The assembled bomb was then placed in the
calorimeter. The bomb calorimeter was checked to assure that no oxygen bubbles leak from
the bomb. If there was any evidence of leak, the bomb was exhausted and the sample was
discarded. The mass of water used for the test was M ± 0.5g where M is a fixed mass of
water. Adjustments were made to compensate for change in the density of water with
temperature. The calorimeter vessel was positioned in the jacket and the stirrers were
started. Stabilization of the calorimeter vessel’s temperature at ±0.001 °C for more than 30
Acid correction
For coal samples, acid correction was done using the titration method. The interior
of the bomb containing the indicator was washed with distilled water until the washings are
free of acid. The washings were combined with the rinse of the capsule and were titrated
with the standard solution of sodium carbonate (Na2CO3). The acid correction (e1) was
calculated as follows:
A31
where:
Vt = volume of titrant in milliliters
NNa2CO3 = concentration of Na2CO3 in normality (equivalent per liter)
Fuse correction
The fuse correction was determined by weighing the combined pieces of unburned
fuse and subtracting from the original weight. The difference was the weight in milligrams
of the fuse consumed in firing (m). Any ball of oxidized metal was removed from the ends
before weighing. The fuse correction for the heat of combustion of the firing fuse (e2) was
calculated as follows:
where:
m = weight in milligrams of fuse consumed during combustion
Km = 5.9 J/mg (1.4 cal/mg) for No. 34 B&S gauge Chromel C
Km = 7.5 J/mg (1.8 cal/mg) for No. 34 B7S iron wire
Km = 0.00 J/mg for platinum or palladium wire provided the ignition energy is constant
After the preparation of the bomb calorimeter, the heat capacity of the calorimeter
was determined by burning one (1) gram of benzoic acid into a sample holder. Before
reading the temperature observations, the liquid-in-the glass thermometer was tapped to
avoid errors caused by liquid sticking to the walls of the capillary. All the readings were
The calorimeter vessel was allowed to stabilize for 5 minutes. The jacket
temperature was adjusted within 0.01°C and was maintained for 3 minutes. The charge was
fired and the time was recorded as (a) and the temperature as (t a). The jacket temperature
was adjusted to match that of the calorimeter vessel temperature as it rapidly increased. The
temperature of the jacket and the calorimeter vessel was kept equal as possible.
A32
Approaching the final stabilization temperature, the temperature was adjusted to within
0.01°C. The subsequent readings were recorded every minute until three successive readings
have intervals of ±0.001°C. After the rate of change has stabilized, the final temperature was
recorded as (tc) and the time of reading as (c). The corrected temperature rise was calculated
as follows:
where:
t = corrected temperature rise in °C
ta = initial temperature reading at time of firing in °C
tc = final temperature reading in °C
Ce = thermometer, emergent stem correction
Cr = radiation correction
Then, the calorimeter was opened and the bomb was removed. The pressure was
released at a uniform rate. The bomb interior was examined to make sure that there are no
unburned sample or sooty deposit. Otherwise, the test was discarded. The heat capacity of
where:
Hc = heat of combustion of benzoic acid in J/g
m = mass of benzoic acid in grams
e1 = acid correction
e2 = fuse correction in Joules
One (1) gram of coal sample was weighed and was placed into the sample holder.
The same amount of coal sample was burned under the same conditions in the calorimeter.
The acid and fuse corrections (e1 and e2) were determined using the same method as stated
A33
above. In addition to these, the sulfur corrections (e3) were calculated from the weight %
sulfur determined in the sulfur analysis. The sulfur corrections were calculated as follows:
where:
e3 = correction for the difference between the heat of formation of H 2SO4 from SO2 with
respect to the formation of HNO3 in Joules
S = sulfur in the sample in weight %
m = mass of sample in grams
A minimum of 0.4 grams of combustion aid such as benzoic acid, ethylene glycol,
mineral oil or a gelatin capsule was used. The correction for use of combustion aid was
calculated as follows:
where:
Ha = heat of combustion of the combustion aid in J/g (cal/g)
ma = mass of combustion aid in grams
The calorific value of the analysis sample was computed by multiplying the
corrected temperature rise, adjusted for extraneous heat effects by the heat capacity and
dividing by the mass of the sample. The calorific value was calculated as follows:
where:
Qvad(gross) = gross calorific value at constant volume as determined in J/g (cal/g)
Ee = heat capacity of the calorimeter in J/°C (cal/°C)
t = corrected temperature rise
e1 = acid correction
e2 = fuse correction
e3 = sulfur correction
e4 = combustion aid correction
A34
m = mass of the sample in grams
APPENDIX C: TABLE OF VITRINITE REFLECTANCE (%Ro)
A35
APPENDIX D: TABLE OF MACERAL COMPOSITION
A36
A37