CN108254528B - Black shale water rock chemical reaction leaching test device and test method thereof - Google Patents

Black shale water rock chemical reaction leaching test device and test method thereof Download PDF

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CN108254528B
CN108254528B CN201810003654.8A CN201810003654A CN108254528B CN 108254528 B CN108254528 B CN 108254528B CN 201810003654 A CN201810003654 A CN 201810003654A CN 108254528 B CN108254528 B CN 108254528B
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valve
reaction
storage tank
water storage
conduit
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CN108254528A (en
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孙春卫
巫锡勇
孙靖杰
彭嘉骏
王森
凌斯祥
廖昕
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Southwest Jiaotong University
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Abstract

The invention provides a black shale water rock chemical reaction leaching test device and a test method thereof, wherein the black shale water rock chemical reaction leaching test device comprises a reaction container with a built-in reaction sample; the upper end of the reaction vessel is connected with a nitrogen tank and an oxygen tank, and the lower end of the reaction vessel is connected with a closed second water storage tank; a spray head is arranged at the upper part of a reaction sample in the reaction container and is connected with a closed first water storage tank; the spray head is also connected with a closed reaction solution detection box, and the reaction solution detection box is also connected with a second water storage tank; a sampling tube, a pH meter, a conductivity meter, a first dissolved oxygen meter and an oxidation-reduction potentiometer are arranged in the reaction solution detection box; the spray head is connected with the first water storage tank through a first peristaltic pump, and the spray head is connected with the reaction solution detection box through a second peristaltic pump; the nitrogen tank and the oxygen tank are also connected with a first water storage tank; the first water storage tank is provided with a first exhaust pipe, and the reaction solution detection box is provided with a second exhaust pipe; the method can detect the chemical components of minerals dissolved in the black shale solution leached by water under different dissolved oxygen contents and different acidic conditions.

Description

Black shale water rock chemical reaction leaching test device and test method thereof
Technical Field
The invention relates to a leaching test device, in particular to a black shale water rock chemical reaction leaching test device and a test method thereof.
Background
The black shale is rich in organic matters, disperses pyrite and siderite to be black, rarely fossils, has extremely thin layer structure, looks like carbonaceous shale, but does not pollute hands; when the thickness is large, a good crude oil rock system can be obtained. Generally, the environment is formed in the reducing environment of lakes and marshes in warm and humid climates; metal deposits such as uranium, copper, molybdenum, vanadium, nickel and the like are found in the black shale; black shale may serve as an indicator formation for oil; therefore, the research on the accumulation conditions of ions and elements of underground water in the evolution process of the black shale has important significance; however, the existing test device is difficult to detect the change of chemical property parameters under different conditions, and is difficult to simulate the change of chemical components of minerals dissolved in water-percolating black shale under different dissolved oxygen contents and different acidic conditions under field conditions.
Disclosure of Invention
The invention provides a black shale water rock chemical reaction leaching test device capable of detecting chemical components of minerals dissolved in water leaching black shale solution under different dissolved oxygen contents and different acidic conditions.
The technical scheme adopted by the invention is as follows: a black shale water rock chemical reaction leaching test device comprises a reaction container with a reaction sample arranged inside; the upper end of the reaction vessel is connected with a nitrogen tank and an oxygen tank, and the lower end of the reaction vessel is connected with a closed second water storage tank; a spray head is arranged at the upper part of a reaction sample in the reaction container and is connected with a closed first water storage tank; the spray head is also connected with a closed reaction solution detection box, and the reaction solution detection box is also connected with a second water storage tank; a sampling tube, a pH meter, a conductivity meter, a first dissolved oxygen meter and an oxidation-reduction potentiometer are arranged in the reaction solution detection box; the spray head is connected with the first water storage tank through a first peristaltic pump, and the spray head is connected with the reaction solution detection box through a second peristaltic pump; the nitrogen tank and the oxygen tank are also connected with a first water storage tank; the first water storage tank is provided with a first exhaust pipe, and the reaction solution detection box is provided with a second exhaust pipe.
Further, the first water storage tank is connected with a closed third water storage tank through a first exhaust pipe, a second dissolved oxygen instrument is arranged in the third water storage tank, and the third water storage tank is provided with a third exhaust pipe; the reaction solution detection box is connected with a fourth airtight water storage tank through a second exhaust pipe, a third dissolved oxygen instrument is arranged in the fourth water storage tank, and a fourth exhaust pipe is arranged on the fourth water storage tank.
Furthermore, a first permeable layer is arranged between the spray head and the reaction sample, and a second permeable layer is arranged below the reaction sample.
Further, the reaction vessel is arranged on the support platform.
Furthermore, the device also comprises a first four-way interface; the first four-way interface is respectively connected with a nitrogen tank through a first air duct, an oxygen tank through a second air duct, a first three-way interface through a first conduit and a second four-way interface through a second conduit; the first three-way interface and the second four-way interface are connected through a third conduit; the second four-way connector is also connected with the spray head and one end of a fourth conduit, and the other end of the fourth conduit is connected with the second three-way connector; the second three-way connector is also connected with a second water storage tank through a fifth conduit and connected with a reaction solution detection box through a sixth conduit; the first three-way connector is also connected with the first water storage tank through a seventh conduit; the first air duct is provided with a first valve; a second valve is arranged on the second row of gas guide pipes; a third valve is arranged on the first conduit; a fourth valve is arranged on the second conduit; a fifth valve is arranged on the third conduit, and the first peristaltic pump is arranged on the third conduit; a sixth valve is arranged on the fourth conduit; a seventh valve is arranged on the fifth conduit; the second peristaltic pump is arranged on the sixth conduit; an eighth valve is arranged on the first exhaust pipe; a ninth valve is arranged on the second exhaust pipe; a tenth valve is arranged on the third exhaust pipe; an eleventh valve is arranged on the fourth exhaust pipe.
A test method of a black shale water rock chemical reaction leaching test device comprises the following steps:
step 1: placing a reaction sample in a reaction container, filling deionized water in a first water storage tank and a third water storage tank, and closing all valves;
step 2: removing oxygen in the device, and opening a first valve, a fifth valve, a fourth valve, an eighth valve, a tenth valve, a seventh valve, a ninth valve and an eleventh valve; opening the nitrogen tank, and closing the nitrogen tank and the valve after the values of the second dissolved oxygen meter and the third dissolved oxygen meter are stable;
and step 3: opening the fifth valve and the seventh valve, starting the first peristaltic pump, and pumping the solution in the first water storage tank into the reaction container for reaction; simultaneously, sampling through a sampling tube, measuring the pH value of the solution through a pH meter, measuring the conductivity value of the solution through a conductivity meter, measuring the oxygen dissolution amount in the solution through a first dissolved oxygen meter, and measuring the oxidation-reduction potential of the solution through an oxidation-reduction potentiometer; after the parameters are stable, closing the valve;
and 4, step 4: opening a sixth valve, starting a second peristaltic pump to pump the solution in the reaction solution detection box into the reaction container for cyclic reaction; after the reaction is finished, closing the sixth valve, opening the seventh valve, starting the second peristaltic pump to pump the solution in the second water storage tank into the reaction solution detection tank, sampling through the sampling tube, and recording the readings of the pH meter, the conductivity meter, the first dissolved oxygen meter and the oxidation-reduction potentiometer; closing all valves;
and 5: opening the second valve, the third valve, the tenth valve and the eighth valve, and opening the oxygen tank to introduce oxygen; when the second dissolved oxygen meter reaches the test set value, closing the oxygen tank, the second valve, the third valve, the tenth valve and the eighth valve; opening the fifth valve, the seventh valve and the ninth valve, starting the first peristaltic pump to pump the aqueous solution in the first water storage tank into the reaction container for reaction, sampling simultaneously, and recording the readings of the pH meter, the conductivity meter, the first dissolved oxygen meter and the oxidation-reduction potentiometer; closing all valves;
step 6: and (5) repeating the step 4 and the step 5 to perform leaching test on the reaction sample under the condition of different dissolved oxygen concentrations.
The invention has the beneficial effects that:
(1) the invention can simulate the water percolation black shale under different dissolved oxygen contents and different acidic conditions under the field condition, and the chemical composition change of the mineral dissolved in the solution;
(2) the invention can accurately measure the parameters of the corresponding chemical properties through the instrument in the reaction solution detection box;
(3) the method can simulate the accumulation condition of ions and elements of underground water in the long-time black shale evolution process.
Drawings
FIG. 1 is a schematic structural diagram of a testing apparatus according to the present invention.
In the figure: 1-nitrogen tank, 2-oxygen tank, 3-first valve, 4-second valve, 5-first four-way joint, 6-third valve, 7-fifth valve, 8-fourth valve, 9-second four-way joint, 10-first peristaltic pump, 11-first three-way joint, 12-first water storage tank, 13-eighth valve, 14-third water storage tank, 15-second dissolved oxygen instrument, 16-tenth valve, 17-support table, 18-reaction vessel, 19-spray head, 20-first permeable layer, 21-reaction sample, 22-second permeable layer, 23-second water storage tank, 24-seventh valve, 25-second three-way joint, 26-sixth valve, 27-second peristaltic pump, 28-reaction solution detection tank, 29-sampling tube, 30-pH meter, 31-conductivity meter, 32-oxidation-reduction potentiometer, 33-first dissolved oxygen meter, 34-ninth valve, 35-fourth water storage tank, 36-third dissolved oxygen meter, 37-eleventh valve, 38-first air duct, 39-second air duct, 40-first conduit, 41-second conduit, 42-third conduit, 43-fourth conduit, 44-fifth conduit, 45-seventh conduit, 46-sixth conduit, 47-first exhaust pipe, 48-third exhaust pipe, 49-second exhaust pipe and 50-fourth exhaust pipe.
Detailed Description
The invention is further described with reference to the following figures and specific embodiments.
As shown in fig. 1, a black shale water rock chemical reaction leaching test device comprises a reaction container 18 with a reaction sample 21 inside; the upper end of the reaction vessel 18 is connected with the nitrogen tank 1 and the oxygen tank 2, and the lower end is connected with the closed second water storage tank 23; a spray head 19 is arranged at the upper part of a reaction sample 21 in the reaction container 18, and the spray head 19 is connected with a closed first water storage tank 12; the spray head 19 is also connected with a closed reaction solution detection box 28, and the reaction solution detection box 28 is also connected with a second water storage tank 23; a sampling tube 29, a pH meter 30, a conductivity meter 31, a first dissolved oxygen meter 33 and an oxidation-reduction potentiometer 32 are arranged in the reaction solution detection box 28; the spray head 19 is connected with the first water storage tank 12 through a first peristaltic pump 10, and the spray head 19 is connected with the reaction solution detection tank 28 through a second peristaltic pump 27; the nitrogen tank 1 and the oxygen tank 2 are also connected with a first water storage tank 12; the first water storage tank 12 is provided with a first exhaust pipe 47, and the reaction solution detection tank 28 is provided with a second exhaust pipe 49.
Further, the first water storage tank 12 is connected with a closed third water storage tank 14 through a first exhaust pipe 47, a second dissolved oxygen meter 15 is arranged in the third water storage tank 14, and a third exhaust pipe 48 is arranged in the third water storage tank 14; the reaction solution detection tank 28 is connected to a fourth sealed water storage tank 35 through a second exhaust pipe 49, a third dissolved oxygen meter 36 is provided in the fourth water storage tank 35, and a fourth exhaust pipe 50 is provided on the fourth water storage tank 35.
Further, a first water permeable layer 20 is arranged between the spray head 19 and the reaction sample 21, and a second water permeable layer 22 is arranged below the reaction sample 21.
Further, the reaction vessel 18 is disposed on the support table 17.
Further, the device also comprises a first four-way interface 5; the first four-way interface is respectively connected with a nitrogen tank 1 through a first air duct 38, an oxygen tank 2 through a second air duct 39, a first three-way interface 11 through a first conduit 40 and a second four-way interface 9 through a second conduit 41; the first three-way connector 11 and the second four-way connector 9 are connected through a third conduit 42; the second four-way connector 9 is also connected with the spray head 19 and one end of a fourth conduit 43, and the other end of the fourth conduit 43 is connected with a second three-way connector 25; the second three-way connector 25 is also connected with the second water storage tank 23 through a fifth conduit 44 and connected with the reaction solution detection tank 28 through a sixth conduit 46; the first three-way connector 11 is also connected with the first water storage tank 12 through a seventh conduit 45; the first air duct 38 is provided with a first valve 3; the second air duct 39 is provided with a second valve 4; the first conduit 40 is provided with a third valve 6; the second conduit 41 is provided with a fourth valve 8; the third conduit 42 is provided with a fifth valve 7, while the first peristaltic pump 10 is provided on the third conduit 42; the fourth conduit 43 is provided with a sixth valve 26; the fifth conduit 44 is provided with a seventh valve 24; the second peristaltic pump 27 is arranged on the sixth conduit 46; the first exhaust pipe 47 is provided with an eighth valve 13; the second exhaust pipe 49 is provided with a ninth valve 34; the tenth valve 16 is arranged on the third exhaust pipe 48; an eleventh valve 37 is provided in the fourth exhaust duct 50.
A test method of a black shale water rock chemical reaction leaching test device comprises the following steps:
step 1: placing a reaction sample 21 in a reaction container 18, filling deionized water in the first water storage tank 12 and the third water storage tank 14, and closing all valves;
step 2: removing oxygen in the device, and opening a first valve 3, a fifth valve 7, a fourth valve 8, an eighth valve 13, a tenth valve 16, a seventh valve 24, a ninth valve 34 and an eleventh valve 37; opening the nitrogen tank 1, and closing the nitrogen tank 1 and the valves after the values of the second dissolved oxygen meter 15 and the third dissolved oxygen meter 36 are stable;
and step 3: opening the fifth valve 7 and the seventh valve 24, starting the first peristaltic pump 10, and pumping the solution in the first water storage tank 12 into the reaction vessel 18 for reaction; simultaneously, sampling is carried out through a sampling pipe 29, the pH value of the solution is measured through a pH meter 30, the conductivity value of the solution is measured through a conductivity meter 31, the oxygen dissolving amount in the solution is measured through a first dissolved oxygen meter 33, and the oxidation-reduction potential of the solution is measured through an oxidation-reduction potentiometer 32; after the parameters are stable, closing the valve;
and 4, step 4: opening a sixth valve 26, starting a second peristaltic pump 27 to pump the solution in the reaction solution detection box 28 into the reaction vessel 18 for cyclic reaction; after the reaction is finished, the sixth valve 26 is closed, the seventh valve 24 is opened, the second peristaltic pump 27 is started to pump the solution in the second water storage tank 23 into the reaction solution detection tank 28, meanwhile, the sampling is carried out through the sampling pipe 29, and the readings of the pH meter 30, the conductivity meter 31, the first dissolved oxygen meter 33 and the oxidation-reduction potentiometer 32 are recorded; closing all valves;
and 5: opening the second valve 4, the third valve 6, the tenth valve 16 and the eighth valve 13, and opening the oxygen tank 2 to introduce oxygen; when the second dissolved oxygen meter 15 reaches the test set value, closing the oxygen tank 2, the second valve 4, the third valve 6, the tenth valve 16 and the eighth valve 13; opening the fifth valve 7, the seventh valve 24 and the ninth valve 34, starting the first peristaltic pump 10 to pump the aqueous solution in the first water storage tank 12 into the reaction vessel 18 for reaction, sampling simultaneously, and recording the readings of the pH meter 30, the conductivity meter 31, the first dissolved oxygen meter 33 and the oxidation-reduction potentiometer 32; closing all valves;
step 6: and repeating the step 4 and the step 5 to perform leaching test on the reaction sample 21 under the condition of different dissolved oxygen concentrations.
When in use, the nitrogen tank 1 is used for removing oxygen in the test device, and the oxygen tank 2 is used for providing oxygen with different contents for the reaction environment; the spray head 19 is arranged to provide a uniform and dispersed water flow; the reaction solution detection box 28 is in a sealed state except for corresponding detection instruments and conduits which are designed; the sampling tube 29 is used for collecting samples so as to provide corresponding samples for subsequent analysis of ions and elements in the solution; the pH meter 30 measures the pH value of the solution and the pH value of the reaction solution in real time; the conductivity meter 31 measures the conductivity value of the solution in real time to reflect the dielectric property of the reaction solution; the oxidation-reduction potentiometer 32 measures the oxidation-reduction property of the reaction solution in real time, the higher the oxidation-reduction potential is, the stronger the oxidation property is, and the lower the oxidation-reduction potential is, the lower the oxidation property is; the dissolved oxygen meter 33 detects the concentration of dissolved oxygen in water in real time; the dissolved oxygen meters in the third water storage tank 14 and the fourth water storage tank 35 can detect whether the concentration of dissolved oxygen in the solution meets the concentration required in the test or not, so that the accuracy of the test result is ensured; the first peristaltic pump 10 provides aqueous solutions with different dissolved oxygen concentrations for the reaction through the first water storage tank 12, so that the comparative analysis of results is facilitated; the aqueous solution in the reaction solution detection box 28 is a solution after a reaction, and the second peristaltic pump 27 is used to enable a cyclic reaction, and the solution in the reaction solution detection box 28 is pumped back into the reaction vessel 18 to perform the cyclic reaction, so that the oxidation reaction of the black shale under different acidic conditions can be simulated.
The dissolved oxygen concentration in the oxygen-containing aqueous solution, i.e., the dissolved oxygen concentration of the aqueous solution in the first water storage tank 12, is changed by the oxygen tank 2 to simulate different reaction conditions.
Providing data support for the change of the chemical property of the aqueous solution of the black shale in the oxidation reaction through the pH value, the conductivity value, the oxidation-reduction potential and the dissolved oxygen content recorded in the test process, and analyzing through measured data to obtain the accumulation condition of underground water ions and elements in the black shale evolution process; the sample is taken out through the sampling tube 29 to provide a material basis for subsequent chemical element and ion analysis tests; the invention provides a test device which can simulate the chemical composition change of minerals dissolved in black shale and solution of water percolation black shale under different dissolved oxygen contents and different acidic conditions under field conditions, and can measure the instrument parameters of corresponding chemical properties; the device can detect the change of chemical property parameters under different conditions, so that the accumulation condition of ions and elements of underground water in the evolution process of the black shale can be simulated for a long time.

Claims (5)

1. The black shale water rock chemical reaction leaching test device is characterized by comprising a reaction container (18) internally provided with a reaction sample (21); the upper end of the reaction vessel (18) is connected with the nitrogen tank (1) and the oxygen tank (2), and the lower end is connected with the closed second water storage tank (23); a spray head (19) is arranged at the upper part of a reaction sample (21) in the reaction container (18), and the spray head (19) is connected with a closed first water storage tank (12); the spray head (19) is also connected with a closed reaction solution detection box (28), and the reaction solution detection box (28) is also connected with a second water storage tank (23); a sampling tube (29), a pH meter (30), a conductivity meter (31), a first dissolved oxygen meter (33) and an oxidation-reduction potentiometer (32) are arranged in the reaction solution detection box (28); the spray head (19) is connected with the first water storage tank (12) through a first peristaltic pump (10), and the spray head (19) is connected with the reaction solution detection box (28) through a second peristaltic pump (27); the nitrogen tank (1) and the oxygen tank (2) are also connected with a first water storage tank (12); the first water storage tank (12) is provided with a first exhaust pipe (47), and the reaction solution detection box (28) is provided with a second exhaust pipe (49); the first water storage tank (12) is connected with a closed third water storage tank (14) through a first exhaust pipe (47), a second dissolved oxygen instrument (15) is arranged in the third water storage tank (14), and a third exhaust pipe (48) is arranged in the third water storage tank (14); the reaction solution detection box (28) is connected with a sealed fourth water storage tank (35) through a second exhaust pipe (49), a third dissolved oxygen meter (36) is arranged in the fourth water storage tank (35), and a fourth exhaust pipe (50) is arranged on the fourth water storage tank (35).
2. The black shale water rock chemical reaction leaching test device according to claim 1, wherein a first water permeable layer (20) is arranged between the spray head (19) and the reaction sample (21), and a second water permeable layer (22) is arranged below the reaction sample (21).
3. A black shale water rock chemical reaction leaching test apparatus according to claim 1, wherein the reaction vessel (18) is disposed on a support stand (17).
4. The black shale water rock chemical reaction leaching test device of claim 1, further comprising a first four-way interface (5); the first four-way interface is respectively connected with the nitrogen tank (1) through a first air duct (38), the oxygen tank (2) through a second air duct (39), the first three-way interface (11) through a first conduit (40) and the second four-way interface (9) through a second conduit (41); the first three-way connector (11) is connected with the second four-way connector (9) through a third conduit (42); the second four-way connector (9) is also connected with the spray head (19) and one end of a fourth conduit (43), and the other end of the fourth conduit (43) is connected with a second three-way connector (25); the second three-way connector (25) is also connected with a second water storage tank (23) through a fifth conduit (44) and connected with a reaction solution detection box (28) through a sixth conduit (46); the first three-way connector (11) is also connected with the first water storage tank (12) through a seventh conduit (45); a first valve (3) is arranged on the first air duct (38); a second valve (4) is arranged on the second air duct (39); a third valve (6) is arranged on the first conduit (40); a fourth valve (8) is arranged on the second conduit (41); a fifth valve (7) is arranged on the third conduit (42), and the first peristaltic pump (10) is arranged on the third conduit (42); a sixth valve (26) is arranged on the fourth conduit (43); a seventh valve (24) is arranged on the fifth conduit (44); a second peristaltic pump (27) is arranged on the sixth conduit (46); an eighth valve (13) is arranged on the first exhaust pipe (47); a ninth valve (34) is arranged on the second exhaust pipe (49); a tenth valve (16) is arranged on the third exhaust pipe (48); an eleventh valve (37) is arranged on the fourth exhaust pipe (50).
5. The method of testing a black shale water rock chemical reaction leaching test apparatus of claim 4, comprising the steps of:
step 1: placing a reaction sample (21) in a reaction container (18), filling deionized water in a first water storage tank (12) and a third water storage tank (14), and closing all valves;
step 2: removing oxygen in the device, and opening a first valve (3), a fifth valve (7), a fourth valve (8), an eighth valve (13), a tenth valve (16), a seventh valve (24), a ninth valve (34) and an eleventh valve (37); opening the nitrogen tank (1), and closing the nitrogen tank (1) and the valve after the values of the second dissolved oxygen meter (15) and the third dissolved oxygen meter (36) are stable;
and step 3: opening a fifth valve (7) and a seventh valve (24), starting a first peristaltic pump (10), and pumping the solution in a first water storage tank (12) into a reaction vessel (18) for reaction; simultaneously sampling through a sampling tube (29), measuring the pH value of the solution through a pH meter (30), measuring the conductivity value of the solution through a conductivity meter (31), measuring the oxygen dissolving amount in the solution through a first dissolved oxygen meter (33), and measuring the oxidation-reduction potential of the solution through an oxidation-reduction potentiometer (32); after the parameters are stable, closing the valve;
and 4, step 4: opening a sixth valve (26), and starting a second peristaltic pump (27) to pump the solution in the reaction solution detection box (28) into the reaction container (18) for cyclic reaction; after the reaction is finished, the sixth valve (26) is closed, the seventh valve (24) is opened, the second peristaltic pump (27) is started to pump the solution in the second water storage tank (23) into the reaction solution detection box (28), and simultaneously, the sampling is carried out through the sampling pipe (29), and the following records are respectively carried out: readings of a pH meter (30), a conductivity meter (31), a first dissolved oxygen meter (33), and an oxidation-reduction potentiometer (32); closing all valves;
and 5: opening a second valve (4), a third valve (6), a tenth valve (16) and an eighth valve (13), and opening the oxygen tank (2) to introduce oxygen; when the second dissolved oxygen meter (15) reaches the test set value, closing the oxygen tank (2), the second valve (4), the third valve (6), the tenth valve (16) and the eighth valve (13); opening a fifth valve (7), a seventh valve (24) and a ninth valve (34), starting a first peristaltic pump (10) to pump the aqueous solution in the first water storage tank (12) into a reaction vessel (18) for reaction, and simultaneously sampling, and respectively recording: readings of a pH meter (30), a conductivity meter (31), a first dissolved oxygen meter (33), and an oxidation-reduction potentiometer (32); closing all valves;
step 6: and (5) repeating the step 4 and the step 5 to perform leaching test on the reaction sample (21) under the condition of different dissolved oxygen concentrations.
CN201810003654.8A 2018-01-03 2018-01-03 Black shale water rock chemical reaction leaching test device and test method thereof Expired - Fee Related CN108254528B (en)

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