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APPENDICES

APPENDIX A: Palynological and Kerogen Analyses A2

APPENDIX B: ASTM International Coal Quality A27


Protocols

APPENDIX C: Table of Vitrinite Reflectance A35

APPENDIX D: Table of Maceral Composition A36

APPENDIX E: Raw Data for Core Logs*

APPENDIX F: Raw Data for Vitrinite Reflectance*

APPENDIX G: Raw Data for Maceral Analysis*

APPENDIX H: Coal Etching Microphotographs*

*
These appendices are in digital form
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 palynological analysis shows barren of palynomorph. This sample consists of


dominant liptinite (10 %), vitrinite (60 %), inertinite (30 %) and like amorphous gel (AOM)
(10 %).

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

The palynological analysis shows barren of palynomorph. This sample composes of


liptinite (5 %), vitrinite (60 %), inertinite (30 %) and like amorphous gel / AOM (5 %).

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)

23. SBA 09A LC

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

24. SBA 09B LC

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)

APPENDIX B: ASTM INTERNATIONAL COAL QUALITY


PROTOCOLS

Determination of Moisture (ASTM D 3173-03, 2012f)


The gross coal samples were distributed on tared pans and were weighed. The pans

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

measured. The percent total moisture was calculated as follows:

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
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B = weight of empty capsule and cover in grams
C = weight of analysis sample used in grams

Determination of Volatile Matter (ASTM D 3175-02, 2012g)

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

Determination of Total Sulfur (ASTM D3177-02, 2012h)

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

total sulphur in the samples was calculated as follows:

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

measurements, the bomb and the calorimeter were prepared.

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

from the holder.

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

seconds was required.

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

Determination of the Heat Capacity of the Calorimeter

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

estimated to the nearest 0.0001°C.

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

the calorimeter (E in J/°C) was calculated as follows:

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

Determination of the Heat Capacity of Coal

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

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