WO2012106749A1 - Structured gas desorption at constant temperature - Google Patents

Structured gas desorption at constant temperature Download PDF

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Publication number
WO2012106749A1
WO2012106749A1 PCT/AU2011/000128 AU2011000128W WO2012106749A1 WO 2012106749 A1 WO2012106749 A1 WO 2012106749A1 AU 2011000128 W AU2011000128 W AU 2011000128W WO 2012106749 A1 WO2012106749 A1 WO 2012106749A1
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Prior art keywords
gas
volume
canister
pressure
temperature
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Application number
PCT/AU2011/000128
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French (fr)
Inventor
Laxmi CHIKATAMARLA
Original Assignee
Runge Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Runge Ltd filed Critical Runge Ltd
Priority to PCT/AU2011/000128 priority Critical patent/WO2012106749A1/en
Publication of WO2012106749A1 publication Critical patent/WO2012106749A1/en

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/14—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
    • G01N7/16—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference by heating the material

Definitions

  • the present invention relates generally to the field of mining. More particularly, the invention relates to an apparatus and method for measuring the volume of gas in a coal sample. The invention finds particular application for measuring the volume of methane in a coal seam core sample.
  • Coalbed methane is gas that has been adsorbed onto the surface of micropore network of solid matrix of the coal. It is generally high quality gas with few impurities.
  • Gas content can be measured either by a) 'Slow Desorption' at reservoir or ambient temperature or b) 'Fast Desorption' at ambient temperature.
  • the former, at reservoir temperature, is practiced in the CBM industry, but the process is time consuming and delays the estimation of GIP resources. The latter is preferred by the coal mining industry for faster results to predict the outburst proneness of coal seams.
  • USBM United States Bureau of Mines
  • the total measured gas content (Qm) of a coal relates to the sum of the gas contents defined as Q1 , Q2 and Q3.
  • Q1 is the quantity of gas lost during the core retrieval process, subsequent to it being removed from its in-situ position and prior to its containment in the gas canister and expressed as the quantity per unit mass of coal.
  • Q2 is the quantity of measurable gas desorbed at atmospheric pressure from the intact coal core sample and expressed as the quantity per unit mass of coal. The lost gas is estimated from the initial field Q2 measurements by extrapolating the plot of cumulative desorbed gas content versus square root of time.
  • Q3 is the quantity of gas still contained in coal at one atmosphere of seam gas and expressed as the quantity per unit mass of coal.
  • Q3 is measured by the quantity of gas released after crushing the sample to fine powder in a closed container.
  • the Q2 measurements are done for significant time (several weeks to months) until the gas measurements are less than 10 cc day until a week. This procedure is adopted mainly to ensure that minimum gas is lost during Q3 measurement process, hence, the level of accuracy.
  • Q2 measurements are done for about an hour in the field and then a few hours in the laboratory to capture the trend of gas desorption for estimating lost gas (Q1). The sample is then taken out of canister for quick crush for Q3 measurements.
  • Q3 in the slow desorption equation represents a true residual gas content which ranges between 0.7 and 1.0 m 3 /t (CH 4 ) and 1.5-1.9 m 3 A (C0 2 ).
  • the invention resides in a method of gas content estimation including the steps of:
  • the invention resides in an apparatus for gas content estimation comprising:
  • a sealed canister for containing a core sample
  • a pressure differential assembly operating at a reduced pressure for measuring a second volume of gas from the sealed canister, the pressure differential assembly including a vacuum pump to produce the reduced pressure.
  • FIG 1 is a diagram of an apparatus for measurement of gas content by structured desorption
  • FIG 2 is a typical gas desorption curve.
  • Embodiments of the present invention reside primarily in method of structured gas desorption and an apparatus for working the method. Accordingly, the elements of the invention have been illustrated in concise schematic form in the drawings, showing only those specific details that are necessary for understanding the embodiments of the present invention, but so as not to obscure the disclosure with excessive detail that will be readily apparent to those of ordinary skill in the. art having the benefit of the present description.
  • adjectives such as first and second, left and right, and the like may be used solely to distinguish one element or action from another element or action without necessarily requiring or implying any actual such relationship or order.
  • Words such as “comprises” or “includes” are intended to define a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed, including elements that are inherent to such a process, method, article, or apparatus.
  • the apparatus comprises a sealed canister 10 that contains a coal core sample 11.
  • the core sample is obtained by conventional core drilling. It is important that the core sample be transferred from the drill to the canister 10 as quickly as possible to minimize the lost Q1 component of the desorbed gas.
  • the core canister 10 is placed in a temperature controlled chamber
  • the sealed canister 10 is fitted with a pressure gauge 13 so that the pressure in the canister can be monitored throughout the desorption process.
  • a canister valve 1 controls flow of gas from the canister into a manifold 15.
  • the manifold 15 has a number of other valves that operate to direct the desorbed gas to different measurement systems at different stages of the measurement technique, such as first stage valve 16 and second stage valve 17, which are described further below.
  • the manifold 1 also includes a GC valve 18 for taking a small gas sample 19 for a gas chromatograph (not shown).
  • the canister 10 is placed in the temperature controlled chamber 12.
  • the temperature controlled chamber 12 is a simple water bath. It will be appreciated that the invention is not limited to the use of a water bath and other temperature control methodologies, such as an oven, could be employed.
  • Second stage valve 17 is closed and first stage valve 16 is opened.
  • the gas expands into a graduated measurement chamber 20.
  • the gas content measurement is captured by pressure differential flushing and water displacement. Basically, as gas desorbs from the core sample the pressure increases in the canister, manifold and chamber to displace water into the reservoir 21. This process is allowed to continue for a few days to produce the part of the curve labelled as 'A' in FIG 2.
  • the actual time required to produce part ⁇ ' of the curve will vary with the specific coal seam conditions, but is typically 5 to 10 days.
  • the pressure differential assembly 30 comprises at least one chamber 31 that is evacuated by vacuum pump 32.
  • the three chambers 31 are connected by an inlet manifold 33 and an exhaust manifold 34. The benefit of this arrangement will become clearer below.
  • the chamber 31 Before opening second stage valve 17 the chamber 31 is evacuated by opening valve 35 to connect the chamber to vacuum pump 32.
  • the vacuum pump 32 may be a multi-stage rotary pump that reduces the pressure in the chamber to a few milliTorr.
  • valve 35 Once the chamber is evacuated (together with the inlet manifold 33) valve 35 is closed. To commence measurement of part 'B' of the curve in FIG 2 the second stage valve 17 is opened and gas flows into the chamber 31.
  • Each chamber 31 has a known volume, in the preferred embodiment it is two litres.
  • the pressure in each chamber 31 is monitored by a pressure gauge 36.
  • the pressure stabilises the chamber 31 is known to be full and the valve 37 is closed.
  • the chamber could be evacuated by opening valve 35 and then refilled by repeating the procedure. It is preferable to have a manifold of chambers 31 so that captured gas can be kept for further analysis. It is also quicker to switch to another chamber 31 then to wait for the chamber to be evacuated by the vacuum pump 32.
  • the total volume of gas desorbed during the second stage is measured by flow meter 38.
  • the number of filled two litre chambers provides a verification of the data.
  • the invention can be operated with one or more chambers.
  • two chambers 31 may be considered appropriate with one chamber being evacuated while the other is filling.
  • the actual time required to produce part 'B' of the curve will vary with the specific coal seam conditions, but is typically a few hours.
  • the data from the graduated measurement chamber 20 and the pressure differential assembly 30 is collated to produce the curve shown in FIG 2.
  • the arrow 40 indicates the point where valve 16 was closed and valve 17 was opened. Part TV of the curve is extrapolated towards zero time to obtain the Q1 data.
  • the data from the flow meter 38 may be transmitted directly to a personal computer or other processing device.
  • the part ⁇ ' measurement is conveniently input manually but could be automated using known level sensing technology. For instance, a magnetic float in the graduated measurement chamber would produce a signal in an adjacent coil.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
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Abstract

The invention provides a method and apparatus for estimating methane gas content of a coal bed core sample by structured desorption. A first portion of gas desorbed from the core sample is measured using fluid displacement and a second portion is measured by a flow meter. The volume of desorbed gas is used to estimate the total volume of methane gas in the coal bed.

Description

TITLE
STRUCTURED GAS DESORPTION AT CONSTANT TEMPERATURE
FIELD OF THE INVENTION
The present invention relates generally to the field of mining. More particularly, the invention relates to an apparatus and method for measuring the volume of gas in a coal sample. The invention finds particular application for measuring the volume of methane in a coal seam core sample.
BACKGROUND TO THE INVENTION
The ever increasing demand for energy sources has led to renewed interest in coalbed methane (CBM) gas, sometimes referred to as coal seam gas (CSG). Coalbed methane is gas that has been adsorbed onto the surface of micropore network of solid matrix of the coal. It is generally high quality gas with few impurities.
The presence of CBM is well known and is a serious safety risk in underground coal mines due to the potential for explosions and gas outbursts.
In recent decades CBM has become a viable economic resource to extract from the coal seams. As with most mining industries it is necessary to evaluate the coal seam reservoir before commencing mining. Measured gas content, gas saturation and permeability are fundamental to the evaluation of CBM reservoirs and their producibility. Direct measurement of gas content is critical to the determination of Gas in Place (GIP).
The direct measurement of gas content involves coring and capturing the coal seam into canisters for gas desorption measurements. Gas content can be measured either by a) 'Slow Desorption' at reservoir or ambient temperature or b) 'Fast Desorption' at ambient temperature. The former, at reservoir temperature, is practiced in the CBM industry, but the process is time consuming and delays the estimation of GIP resources. The latter is preferred by the coal mining industry for faster results to predict the outburst proneness of coal seams.
Worldwide, the CBM industry follows a traditional United States Bureau of Mines (USBM) method (Slow Desorption) for gas desorption measurements with some refinements. The USBM method involves constant temperature water baths and canisters with measurements carried out in the field and laboratory over several weeks, with very few changes to the process over the last 35 years. However, this process is painfully slow and ties up significant resources, such as capital and drill rigs, while waiting for the final results to make a decision to move forward with a drilling program.
Gas desorption is quantifiable as follows. The total measured gas content (Qm) of a coal relates to the sum of the gas contents defined as Q1 , Q2 and Q3.
Q1 is the quantity of gas lost during the core retrieval process, subsequent to it being removed from its in-situ position and prior to its containment in the gas canister and expressed as the quantity per unit mass of coal. Q2 is the quantity of measurable gas desorbed at atmospheric pressure from the intact coal core sample and expressed as the quantity per unit mass of coal. The lost gas is estimated from the initial field Q2 measurements by extrapolating the plot of cumulative desorbed gas content versus square root of time.
Q3 is the quantity of gas still contained in coal at one atmosphere of seam gas and expressed as the quantity per unit mass of coal. Q3 is measured by the quantity of gas released after crushing the sample to fine powder in a closed container. In the standard slow desorption technique, the Q2 measurements are done for significant time (several weeks to months) until the gas measurements are less than 10 cc day until a week. This procedure is adopted mainly to ensure that minimum gas is lost during Q3 measurement process, hence, the level of accuracy. For fast desorption techniques, Q2 measurements are done for about an hour in the field and then a few hours in the laboratory to capture the trend of gas desorption for estimating lost gas (Q1). The sample is then taken out of canister for quick crush for Q3 measurements.
There is a significant difference in the relative percentage of the Q1 ,
Q2 and Q3 components of the total gas content of a particular coal sample. Testing and analysis undertaken on a number of Bulli seam coal samples have shown the component percentages for fast desorption (Equation 1) and slow desorption (Equation 2).
Total Gas Content (Fast Desorption Method) = (5 - 10%) Q1 + (12 - 17%) Q2 + (73 - 83%) Q3 (Equation 1)
Total Gas Content (Slow Desorption Method) = (5 - 10%) Q1 + (75 - 90%) Q2 + (5 - 15%) Q3 (Equation 2)
Q3 in the slow desorption equation represents a true residual gas content which ranges between 0.7 and 1.0 m3/t (CH4) and 1.5-1.9 m3A (C02).
Recently there have been developments to measure the gas contents using downhole techniques such as RAMAN spectroscopy, the measurement of bubblepoint pressure of formation water equating to 'critical desorption pressure' and inference of gas content in the coal via use of conventional well logs. These techniques have met with varied acceptance in the industry, for want of field calibrations.
CBM exploration companies have expressed a desire to reduce the time and improve the efficiency of slow desorption without sacrificing accuracy or preference for slow desorption and reservoir temperature. OBJECTS OF THE INVENTION
It is an object of the present invention to overcome or at least alleviate one or more of the above limitations.
It is a further object to provide accurate coalbed gas content estimation in a reduced time compared to some known techniques.
SUMMARY OF THE INVENTION
In one form, although it need not be the only or indeed the broadest form, the invention resides in a method of gas content estimation including the steps of:
placing a core sample in a sealed canister;
controlling the temperature of the canister;
measuring a first volume of gas desorbing from the core sample at ambient pressure for a first time period;
measuring a second volume of gas desorbing from the core sample at reduced pressure for a second time period; and
calculating an estimate of the total gas desorbed from the core sample from the first volume and the second volume.
In another form the invention resides in an apparatus for gas content estimation comprising:
a sealed canister for containing a core sample;
a temperature controlling chamber surrounding the sealed canister;
a gas capture reservoir at ambient pressure for measuring a first volume of gas from the sealed canister; and
a pressure differential assembly operating at a reduced pressure for measuring a second volume of gas from the sealed canister, the pressure differential assembly including a vacuum pump to produce the reduced pressure.
Further features and advantages of the present invention will become apparent from the following detailed description. BRIEF DESCRIPTION OF THE DRAWINGS
To assist in understanding the invention and to enable a person skilled in the art to put the invention into practical effect, preferred embodiments of the invention will be described by way of example only with reference to the accompanying drawings, in which:
FIG 1 is a diagram of an apparatus for measurement of gas content by structured desorption; and
FIG 2 is a typical gas desorption curve.
DETAILED DESCRIPTION OF THE INVENTION
Embodiments of the present invention reside primarily in method of structured gas desorption and an apparatus for working the method. Accordingly, the elements of the invention have been illustrated in concise schematic form in the drawings, showing only those specific details that are necessary for understanding the embodiments of the present invention, but so as not to obscure the disclosure with excessive detail that will be readily apparent to those of ordinary skill in the. art having the benefit of the present description.
In this specification, adjectives such as first and second, left and right, and the like may be used solely to distinguish one element or action from another element or action without necessarily requiring or implying any actual such relationship or order. Words such as "comprises" or "includes" are intended to define a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed, including elements that are inherent to such a process, method, article, or apparatus.
Referring to FIG 1 there is a shown an apparatus for measurement of gas content by structured desorption. The apparatus comprises a sealed canister 10 that contains a coal core sample 11. The core sample is obtained by conventional core drilling. It is important that the core sample be transferred from the drill to the canister 10 as quickly as possible to minimize the lost Q1 component of the desorbed gas.
The core canister 10 is placed in a temperature controlled chamber
12 to maintain the coal at a coal seam temperature for accurate measurement of the gas desorption curve. The importance of this requirement depends strongly on the temperature differential between the coal seam temperature and the ambient temperature at the location of the measurement apparatus.
The sealed canister 10 is fitted with a pressure gauge 13 so that the pressure in the canister can be monitored throughout the desorption process. A canister valve 1 controls flow of gas from the canister into a manifold 15. The manifold 15 has a number of other valves that operate to direct the desorbed gas to different measurement systems at different stages of the measurement technique, such as first stage valve 16 and second stage valve 17, which are described further below. The manifold 1 also includes a GC valve 18 for taking a small gas sample 19 for a gas chromatograph (not shown).
After the core sample 11 is placed in the canister 10 the canister 10 is placed in the temperature controlled chamber 12. In the preferred embodiment the temperature controlled chamber 12 is a simple water bath. It will be appreciated that the invention is not limited to the use of a water bath and other temperature control methodologies, such as an oven, could be employed.
Once the temperature has stabilized the canister valve 14 is opened and gas seeps into the manifold 15. Second stage valve 17 is closed and first stage valve 16 is opened. The gas expands into a graduated measurement chamber 20. The gas content measurement is captured by pressure differential flushing and water displacement. Basically, as gas desorbs from the core sample the pressure increases in the canister, manifold and chamber to displace water into the reservoir 21. This process is allowed to continue for a few days to produce the part of the curve labelled as 'A' in FIG 2. The actual time required to produce part Ά' of the curve will vary with the specific coal seam conditions, but is typically 5 to 10 days.
When the part 'Α' curve starts to flatten the first stage valve 16 is closed and the second stage valve 17 is opened to allow gas to flow into a pressure differential assembly 30. The pressure differential assembly 30 comprises at least one chamber 31 that is evacuated by vacuum pump 32. In the preferred embodiment there are three chambers 31 for rapid switching between chambers as each fills. The three chambers 31 are connected by an inlet manifold 33 and an exhaust manifold 34. The benefit of this arrangement will become clearer below.
Before opening second stage valve 17 the chamber 31 is evacuated by opening valve 35 to connect the chamber to vacuum pump 32. The vacuum pump 32 may be a multi-stage rotary pump that reduces the pressure in the chamber to a few milliTorr. Once the chamber is evacuated (together with the inlet manifold 33) valve 35 is closed. To commence measurement of part 'B' of the curve in FIG 2 the second stage valve 17 is opened and gas flows into the chamber 31.
Each chamber 31 has a known volume, in the preferred embodiment it is two litres. The pressure in each chamber 31 is monitored by a pressure gauge 36. When the pressure stabilises the chamber 31 is known to be full and the valve 37 is closed. At this stage the chamber could be evacuated by opening valve 35 and then refilled by repeating the procedure. It is preferable to have a manifold of chambers 31 so that captured gas can be kept for further analysis. It is also quicker to switch to another chamber 31 then to wait for the chamber to be evacuated by the vacuum pump 32. By opening and closing each valve 35 and 37 in sequence the chambers are sequentially filled. The total volume of gas desorbed during the second stage is measured by flow meter 38. The number of filled two litre chambers provides a verification of the data.
As mentioned, there need not be three chambers 31. The invention can be operated with one or more chambers. For instance, two chambers 31 may be considered appropriate with one chamber being evacuated while the other is filling. The actual time required to produce part 'B' of the curve will vary with the specific coal seam conditions, but is typically a few hours.
The data from the graduated measurement chamber 20 and the pressure differential assembly 30 is collated to produce the curve shown in FIG 2. The arrow 40 indicates the point where valve 16 was closed and valve 17 was opened. Part TV of the curve is extrapolated towards zero time to obtain the Q1 data.
The inventor envisages that much of the process could be automated, in particular the rapid part 'B' desorption measurement. To this end the data from the flow meter 38 may be transmitted directly to a personal computer or other processing device. The part Ά' measurement is conveniently input manually but could be automated using known level sensing technology. For instance, a magnetic float in the graduated measurement chamber would produce a signal in an adjacent coil.
The above description of various embodiments of the present invention is provided for purposes of description to one of ordinary skill in the related art. It is not intended to be exhaustive or to limit the invention to a single disclosed embodiment. As mentioned above, numerous alternatives and variations to the present invention will be apparent to those skilled in the art of the above teaching. Accordingly, while some alternative embodiments have been discussed specifically, other embodiments will be apparent or relatively easily developed by those of ordinary skill in the art. Accordingly, this invention is intended to embrace all alternatives, modifications and variations of the present invention that have been discussed herein, and other embodiments that fall within the spirit and scope of the above described invention.

Claims

1. A method of gas content estimation including the steps of:
placing a core sample in a sealed canister;
controlling the temperature of the canister;
measuring a first volume of gas desorbing from the core sample at ambient pressure for a first time period;
measuring a second volume of gas desorbing from the core sample at reduced pressure for a second time period; and
calculating an estimate of the total gas desorbed from the core sample from the first volume and the second volume.
2. The method of claim 1 wherein the temperature of the canister is controlled so that the temperature of the core sample in the canister is approximately coal seam temperature. 3. The method of claim 1 wherein the step of controlling the
temperature of the canister includes placing the canister in a temperature controlled water bath.
4. The method of claim 1 wherein the first volume is measured by fluid displacement. 5. The method of claim 1 wherein the first volume of gas is measured over a period of days.
6. The method of claim 1 wherein the second volume is measured by pressure differential chamber filling.
7. The method of claim 1 further including the step of sequentially filling known volume chambers to determine the second volume.
8. The method of claim 7 wherein a known volume chamber is known to be full when a pressure gauge stabilises.
9. The method of claim 1 wherein the step of calculating an estimate of total gas desorbed is determined by extrapolating the first volume to zero time and adding the second volume.
10. An apparatus for gas content estimation comprising:
a sealed canister for containing a core sample;
a temperature controlling chamber surrounding the sealed canister;
a gas capture reservoir at ambient pressure for measuring a first volume of gas from the sealed canister; and
a pressure differential assembly operating at a reduced pressure for measuring a second volume of gas from the sealed canister, the pressure differential assembly including a vacuum pump to produce the reduced pressure.
11. The apparatus of claim 10 wherein the temperature controlling chamber is a set temperature water bath. 12. The apparatus of claim 10 further comprising a pressure gauge that monitors pressure in the sealed canister.
13. The apparatus of claim 10 further comprising a manifold of tubes and valves to sequentially direct gas from the sealed canister to the gas capture reservoir and the pressure differential assembly. 14. The apparatus of claim 10 wherein the gas capture reservoir comprises a graduated measurement chamber. 5. The apparatus of claim 10 further comprising a gas sample port for gas chromatography measurements.
16. The apparatus of claim 10 further comprising a flow meter that monitors gas volume flow to the pressure differential assembly.
17. The apparatus of claim 10 wherein the pressure differential assembly comprises a plurality of chambers fillable with gas from the sealed canister.
18. The apparatus of claim 17 wherein the vacuum pump produces a reduced pressure in the chambers.
19. The apparatus of claim 17 wherein the chambers are able to be sealed and removed.
20. The apparatus of claim 17 further comprising a pressure gauge on each chamber wherein the chamber is considered to be full when the pressure gauge reaches ambient pressure.
PCT/AU2011/000128 2011-02-07 2011-02-07 Structured gas desorption at constant temperature WO2012106749A1 (en)

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CN112504936A (en) * 2020-11-30 2021-03-16 中国地质大学（北京） Testing device and testing method for simulating and researching permeability of deep coal bed methane
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