Experimental Procedure for

3.0L reactor
Gasfilling (10s) - Formation (20s) –Depressurization (10s) – Thermal stimulation (10s)

This run was done after new volume probe which shows that

a. Reactor volume = 3270 mL

b. Pore volume in reactor = 1438.8 mL
c. Porosity of reactor = 43.0%
d. Criteria for injection: 10kPa/hr drop in gas pressure
e. The plan is to form 40% hydrate, 58% water and 2% gas. As in planning file in H5,
the input will be:
a. Control final reactor pressure at 6600 kPag
b. Vw = mL
c. Conversion is assumed at 95.00%
Assuming 99.0 % of gas can be converted into hydrate, and 40% hydrate saturation is
targeted

Gas Filling:

1. Check all venting closed after venting! (one for reactor one for gas storage vessel)
2. Chiller Temperature is set at 15 degrees
3. According to calculation (volume probe), a total of 4939.8 g of sand is required to fill
up 3270 ml reactor. (1603.2+1786.7+1550.9= 4940.8 g) Sand need to be reduced.
4. Reactor dismantling and washing – refilling of gas.
5. Connecting reactor to lines (Torque = 35 ft-lb or 56 N.m)
6. Gas filling data file started at 10s interval. The reactor is first purged (Check valves
from bottom-up) to ~1 MPa (10bar) thrice methane gas to remove any residual air.
(V2 to fill, V7 to purge)
7. Reactor is pressurized to 6700 kPag (corresponding to X.XXX mol) and allowed to
stabilize at 15.01 deg C. V6 was closed to maintain consistency in experimental
procedures.
8. Perform leak check on the top & bottom fittings (4 key places). Check if external
cylinder is closed
9. Control PCR at 6720.00 kPa gauge by opening V12 slowly once T stabilized. (+/- 5
kPa)
Water Injection:
10. In Formation file t = 5000 s, 1st Injection at 50 ml/min at 15 deg C from V8 was done:
(Deionized water at 7.0 MPa) to 9.5 MPa for 8 min 56 s around 450 mL.
Abrupt Leakage was found. It was deduced that the leakage was from inside of the reactor, where
the top was not well sealed. Next time, do not fill sand up to top and make sure that the reactor can
be sealed off without issue. Otherwise, there will be leakage.

MH Formation reaction will be continued to test the functionality of the rest of the equipment.
Do take note that the reactor lid need to be fully closed before sealing. Otherwise, maximum
pressure will be reduced, cannot target 9.6 MPa. Maximum pressure may be only 8.8 MP
Initial Pressure of the reactor is P = 9062 KPa Water injected is 450 mL.

Temperature was reduced to 2C from 15 C directly to induce MH formation at 12:54PM. To monitor P

and T during the weekend.

11. ONCE PRESSURE STABILIZED AT 9.5 MPA (AROUND 2.0 HR), COOLING BY ADJUSTING
THE CHILLER TEMPERATURE TO 13.0 DEG C.
12. TO ADJUST TO 12 DEG C AT 9:30 PM. AND ADJUST 1 DEGC DOWN EVERY 12 HOURS.

19/10/2018 4:22PM CHANGE FROM 10 DEG C TO 9 DEG C

13. AT T= 66169S, PRESSURE WAS 3240KPA, 2ND INJECTION AT 50 ML/MIN: (TOTAL =

153.35 ML). (TIME = 3 MIN 04S 153.33 ML) TOTAL: 153.3+114.17 = 267.47 ML.

14. INCREASE T STEP WISE FROM 0.8 DEGC TO 2 DEGC TO 4 DEGC TO 6 DEGC.
The final pressure is at 54.9 bar at top and 59.2 bar at bottom

Depressurization

1. Vtop and Vbot valve was closed, Start DAQ at 10s interval – CHECK WATER PRODUCTION is
recorded IN COM4!
2. 0 – 50s: Open control valve 100% to evacuate Vcv (CHG DIRECTION OF CONTROL – press
“Menu” to CHANNEL 4 -> PRESS “FUNC” to find direct/reverse action)-> nothing come out
3. 220 – 380 s: Slowly fully open V9 to obtain gas and water from top tubes for 300s. ->
 Water: 0.4 g
 Gas: - 33kPa (INITIAL GAS PRESSURE IN SV IS -108 KPA)
4. 380 – 600s: Slowly fully open V13 to obtain gas and water from bottom tubes. At t = 650 s, if
water and gas in GR stabilizes, control valve set to desired set point and direction, close V13
a. Water: 1.0 g
b. Gas: 72.0 kPa
5. (check VBot, V13 closed) T = 400s, open Vtop to begin dissociation slowly at 430s
6. To have pressure pick up to “4.0MPa”, regulate pressure surge by opening instrument air
valve and manually change the set point ABOVE 4.5 MPa.
a. Time of SP Change: (next time record time whereby SP is changed) -> not changed
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1. In the end of dissociation, Psv = 2212 kPa, Pcr = 60.0 kPa, and the Mass of H20 in GLS = 164.6g
DAQ is stopped and use 10s interval for “Venting”.
2. Venting of SV (V11) before opening of GLS to remove the water produced.
Purge Step:

1.

Injection Steps
1. Purge Twice, Refill, Purge 100mL.
2. Connect loosely (Hold onto valve properly!)
3. Pressurize to 2000kPa until few drops come out & tighten. (Make sure to press “enter” & hear the
sound!!)
4. Pressurize to 8000kPa (Record Initial Vol & Time)
5. SLOWLY OPEN V8 UNTIL YOU SEE PRESSURE DROP  PRESS RUN!
6. When desired pressure/volume achieved, close V8 & stop syringe pump.
7. Record volume remaining & check leakage.
8. Before disconnecting, DEPRESSURIZE from 8000kPa  2000kPa  500kPa