Abstract
Accurate determination of the gas content in coalbeds is important for safe mining. Currently, gas desorption by drilling underground boreholes is the most commonly used gas determination method. However, this method is not very accurate and needs to be improved. In this study, we established a laboratory protocol based on coal adsorption studies to analyse factors affecting the measurement accuracy. The results showed that exposure time, sampling method, sample weight, particle size and gas loss estimate significantly affected the gas content measurement using gas desorption by drilling underground boreholes. Longer exposure time and increased particle size resulted in higher relative errors. Sampling by coring is more accurate than sampling by drilling. The higher the sample weight is for samples weighing less than 240 g, the larger the error of the in situ measurements of desorbed gas, residual gas and lost gas is. The error tends to stabilize for heavier samples. The gas losses at different exposure times calculated using the commonly used Barrer model, power function method and negative exponent method were compared. The gas loss error within 0–12 min, computed with the Barrer model, and after 12 min, computed with the power function method, is minimal. The modified formula of gas loss was obtained using the combination of a fitting analysis and the relationship between gas loss and exposure time. Subsequently, the optimal procedure for in situ gas content measurements using gas desorption by drilling underground boreholes was determined. The gas content errors for anthracite, gas coal, lean coal and long flame coal, which were measured using gas desorption by drilling underground boreholes and corrected using the gas loss formula, decreased significantly to less than 10%, thus, meeting the engineering accuracy norm.
Keywords
Introduction
Energy released by coal and gas outbursts can not only destroy underground roadway, ventilation facilities and production equipment, resulting in huge economic losses to the mine and great difficulties in resuming production, but is also a serious safety threat for underground workers (Díaz Aguado and González Nicieza, 2007; Yang et al., 2014). Therefore, timely forecasts and coal and gas outburst prevention are very important. Gas content is one of the major parameters used to study coalbed gas. It reveals the internal energy or the risk of gas and coal outbursts of the coalbed and therefore is an important forecast indicator and one of two key parameters for assessing outburst prevention (Cao et al., 2001; Wold et al., 2008; Zhang and Lowndes, 2010). The measurement of gas pressure is infeasible in the majority of coal mines in China. Thus, the gas content is frequently used as an evaluation index for outburst prevention. The test accuracy therefore directly affects mine safety. The gas content determines the reliability of outburst risk prediction and the effectiveness and economy of gas control measures, thus, it plays an important role (Wang et al., 2013).
Comparison of different methods for determination of gas content.
GDDUB: gas desorption by drilling underground boreholes.
However, field results showed that these methods need much data and are affected by several uncertainty factors in practice. Moreover, each step of the determination process might introduce errors to the final result (Creedy, 1986). According to statistics, the error of gas content, determined using GDDUB, reaches values as high as 50% (Chen et al., 2010). Therefore, it is necessary to systematically study factors causing errors in the application of GDDUB and to propose reasonable measures to reduce errors to improve the accuracy and reliability of forecasting coalbed gas emission and outburst accidents and ensure safe coal mining (Liang et al., 2012).
Errors of the gas content measured using GDDUB are mainly due to estimates of in situ gas desorption and gas loss. Therefore, we focused on these two parts in this paper. First, we conducted laboratory experiments to determine the effects of exposure time, sampling methods, particle size and sample weight on the gas content determination. Then, we calculated the gas losses at different exposure times using three different gas desorption models (i.e. Barrer mathematical model (Barrer, 1951), power function method and negative exponent function method) and analysed their calculation errors. Lastly, we conducted a fitting analysis on the experimental results, obtained the correction formula, taking the theoretical relationship of gas loss and exposure time into consideration, and optimized the process for in situ gas content measurements using GDDUB. The research results provide a reliable basis to reduce errors in gas content measurement and prevention of coal and gas outbursts.
Sample preparation and methods
Samples
Industrial analysis and adsorption values.
A = ash; a = Langmuir's volume; ad = air dried; b = Langmuir's pressure; M = moisture; Ro, max = maximum reflectance of vitrinite; V = volatile matter.
Experimental scheme
The experimental equipment mainly included a high-pressure tank, sealing piston, vacuum pump, gas cylinders, press machine and computers. The high-pressure tank was self-designed and developed. At a height of 40 mm from the inner bottom of the tank, four small holes need drilled with a diameter of 16 mm were drilled and distributed uniformly along the perimeter with an internal tapping of 16 mm×1.5 mm. At the centre of the bottom disk of the tank, two small holes with a diameter of 8 mm were drilled along its radial direction to the centre of the bottom disk, where a small hole with diameter of 12 mm and internal tapping of size 12 mm × 1.5 mm was drilled. This hole was designed to install both the gas injection and exhaust pipes of the simulation borehole. The sealing piston was connected to the press machine using eight screws, two Y-type gaskets and one O-ring. The device withstood seal gas pressures greater than 10 MPa. Figure 1 shows the device design.
Schematic of coal sample adsorption experimental setup. 1 – press pump; 2 – press; 3 – PC; 4 – data collector; 5 – sealing piston; 6 – Y-type gasket; 7 – O-type seal; 8 – high pressure tank; 9 – pressure transmitter; 10 – coal samples; 11 – gas injection and exhaust pipes; 12 – precision pressure gauge; 13 – gas cylinders. The experimental coring procedure is as follows. Steps 1–3 are the same as those of the drilling method; (4) use the coring pipe for sampling at an exposure time of 3 min, rapidly place the intact coal sample into the sample tank, tightly close the tank, make sure no gas is leaking and measure the amounts of gas desorption and residual gas; and (5) repeat all steps nine times to test the coal samples exposed for 5, 7, 10, 12, 15, 20, 30, 50 and 70 min, and record the results.

Determination of actual gas content
To calculate the error in gas content measured using the direct method, it is necessary to first determine the actual gas content, i.e. to determine the gas adsorption constants a and b in the laboratory (Table 1). The actual gas content was calculated indirectly as the sum of free gas content and adsorbed gas content (Xu andWang, 2011), that is
The adsorbed gas content of coal X
a
can be calculated using the Langmuir's equation considering the impact of moisture, ash, temperature and combustible material percentage, that is
The free gas content of coal X
f
can be calculated using the equation of state of gas
Bringing the actual pressure and temperature of the gas and the experimentally derived adsorption constants a and b in equations (1)–(3), the actual gas contents of the five coal samples at different pressures were calculated. The gas contents were used for comparison with data from other methods.
Experimental results
The exposure time, sampling methods, sample weight, sample particle size and other factors directly affected the measured gas content. The experimental results were analysed to study the characteristics of these effects on the measured gas content and to find a method for error reduction.
Effect of exposure time on the measured gas content
The main error of the gas content measurement using GDDUB is introduced by the calculation of gas loss, which is closely related to the exposure time. The longer the exposure time is, the greater the error of estimated gas loss. Thus, the relationships of desorbed, lost and residual gas contents of coal at different exposure times and the exposure time were measured. Figures 2 and 3 show the experimental results from drilling and coring methods, respectively.
Relationships of desorbed, residual and lost gas contents measured using the drilling method to the exposure time. Relationships of desorbed, residual and lost gas contents measured using the coring method to the exposure time.

There is no significant difference in the time curves of the two sampling methods (Figures 2 and 3). In other words, the relationships of desorbed, residual and lost gas contents and the exposure time are similar for different sampling methods.
Within 0–20 min of exposure time, the measured lost gas content increased significantly with increasing exposure time. Within 20–70 min, the lost gas content increased with increasing exposure time at a slower rate and eventually reached a stable state. The change in the slope of the fitted curve declined, indicating that the rate of gas desorption also decreased over time.
Within 1 h of on-site desorption, the desorbed gas content decreased with increasing exposure time. The decline rate was significantly greater at exposure times less than 30 min. The change in the slope of the fitted curve declined, indicating that the rate of gas desorption also decreased over time.
The amount of residual gas decreased gradually with increasing exposure time and eventually reached equilibrium.
Effect of sampling methods on the measured gas content
The heat produced from friction-induced collision could result in changes in temperature at the time of sampling. The temperature difference due to different sampling processes affects the determination of desorption gas content and gas content loss. The desorption rate is accelerated, and the loss of gas content increases when the temperature rises (Yue et al., 2015). In order to avoid the effects of temperature change on experimental results, we placed the coal tank in a water bath at a constant temperature (20 ℃) to determine the gas content of samples collected using different methods.
Figure 4 shows the relationship between the relative error of gas content and the exposure time measured using drilling and coring methods.
Relationships of the relative error of gas content measured using the drilling and coring methods to the exposure time.
The relative error of gas content measurements using both drilling and coring methods increases with increasing exposure time. The results determined using both methods differed little within 15 min, while the difference in the results of both methods increased as the exposure time increased, with the coring method being more accurate. The gas contents determined using the coring method were more reliable in practical underground applications with longer sampling times (Yang et al., 2010).
The error rate increased slower within 15 min and then increased quickly within 15–70 min using the drilling method. Therefore, the linear fittings of errors before and after 15 min have the following fitting equations using 15 min as the demarcation point
Bringing equations (4) and (5) into equation (7), one obtains
The linear fitting of the error curve measured using the coring method has the following equation
Once the gas content is measured, the more accurate actual gas content can be derived from the corresponding relative error formula at the selected exposure time.
Effect of sampling weight on the measured gas content
The weight of the samples from the field has an effect on the measured gas content. Samples with different weights were experimentally tested at an exposure time of 1 h in order to study the effects of sample weight; gas content; and desorbed, lost and residual gas contents (Figure 5).
Relationship of desorbed, residual and lost gas contents to the sample weight.
The desorbed, residual and lost gas contents measured using GDDUB increased with increasing sample weight. The rate of increase notably reduced and eventually stabilized once the sample weight reached 240 g. Figure 6 shows the relationship between gas content (and error) and the sample weight determined using GDDUB.
Relationships of gas content and error determined using GDDUB to the sample weight. GDDUB: gas desorption by drilling underground boreholes.
The coalbed gas content determined using GDDUB increased with increasing sample weight. The rise in gas content with increasing sample weight was greater for samples weighing 0–240 g and became smaller and stabilized for samples weighing 240–500 g. Similarly, the relative error of the measured gas content decreased with increasing sample weight and eventually stabilized.
Linear fitting of errors for samples weighing 0–240 g has the following equation
The correlation coefficient was 0.992, suggesting a high degree of fit. By bringing equation (12) into equation (7), the resulting equation is
The analysis shows that a sample weight of 240 g was most suitable for the underground determination of the coalbed gas content. If the sample weight was less than 240 g, equation (13) could be used for correction of the gas content.
Effect of sample size on measured gas content
The microporous structure of coal is one of the main factors affecting the gas content. The micropores have a significant internal surface area, which adsorbs free gas. When coal is broken, the micropore structure is destroyed and exposed to the local atmosphere. The residual gas content depends on the degree of breakage (Jiang et al., 2013; Wei et al., 1997). For large sample particle sizes the centre is far away from the coal surface, thus, gas emitted from the micropores also passes a longer distance. When only considering coal particle size, the coal sample with a larger particle size has therefore a slower adsorption process, smaller gas desorption rate and greater residual gas content (Wu et al., 2011; Zhou et al., 2012).
In order to study the effect of coal particle size on the measured gas content, the desorbed, lost and residual gas contents of coals with different particle sizes were experimentally measured at an exposure time of 3 min and an on-site desorption of 1 h (Figure 7).
Relationship of desorbed, lost and residual gas contents to the coal particle size.
The on-site desorbed gas content and the lost gas content of the Linhuan No. 9 coal sample measured using GDDUB declined with increasing coal particle size, while the residual gas content increased with increasing particle size (Figure 7).
The relative error of the gas content reduced with increasing coal particle size (Figure 8). For samples with sizes smaller than 1 mm, the rate of increase in error increased with decreasing particle size. However, for samples with particle sizes larger than 1 mm, the rate of increase in error decreased with decreasing particle size and was significantly smaller (Xu et al., 2015).
Relationship of the relative error of gas content determined using GDDUB to the coal particle size. GDDUB: gas desorption by drilling underground boreholes.
Based on our analysis, the smaller the particle size of coal samples, the larger the initial desorption rate, lost gas content, residual gas content and the relative error and vice versa. Using the drilling method for measurement of the coalbed gas content, samples with particle sizes should be larger than 1 mm because of severe coal breakage.
Selection and verification of models for calculating gas content under multiple factors
The above-mentioned experiments showed that the rate of gas desorption from coal samples was very high in the initial exposure period, while in situ sampling by drilling requires a longer time. In other words, the collected coal sample will inevitably be exposed to air for a period of time before it is sealed into the tank. Gas is rapidly desorbed and escapes into the air during this period, making it difficult to be collected (Li and Yang, 2012). Therefore, the accurate and effective determination of the gas loss is critical for the accurate determination of the original gas content of the target coalbed (Diamond and Schatzel, 1998).
Comparison of lost gas content estimated using different calculation models
It is difficult to directly measure the gas using current technologies. Thus, it is often estimated or indirectly obtained. Because the estimation will introduce various errors (Yan, 2010), it is necessary to compare the gas loss deduced from different calculation methods and use these methods to reduce the errors.
In order to obtain a more accurate estimation formula, under the same sampling method (the drilling method), sample weight (240 g), sample particle size (1–2 mm) and different exposure time (3, 5, 10, 15, 30 and 60 min), we compared and analysed the gas losses estimated using the three most common methods, namely the Barrer method (√t method), the power function method and the negative exponential function method.
Experimental data of adsorbed gas amount determined at different exposure times.

Adsorption curve of coal samples at different exposure times.
Figure 9 shows that within 0–12 min, the error of gas loss estimated using the Barrer model is the smallest. After 12 min, the error of gas loss estimated using the power function is the smallest. The fitting curve of the gas loss with time finds the following:
The error formula of the Barrer model is
The error formula of the negative exponential function is
The error formula of the power function is
By bringing equations (14) to (16) into equation (7) as well as the three equations in Table 3, one can obtain the following formula:
The correction formula for the Barrer model is
The correction formula for the negative exponential function is
The correction formula for the power function is
When calculating gas loss, the Barrer model combining equation (17) should be used for samples with exposure times less than 12 min, and the power function method combining equation (19) should be used for samples with exposure times greater than 12 min.
Verification
Gas content of different coal samples.

The relative error in measuring gas content error of different Ro,max.
Coals with a higher degree of metamorphism have higher maximum vitrinite reflectances (Ro, max; %) (GB/T23249-2009, 2009). Meanwhile, the relative errors before and after correction are reduced with increasing Ro, max, which suggests that a higher degree of metamorphism has less impact on the measured coal gas content. Table 4 shows that the error of the gas content determined using GDDUB alone was as large as 40%, while the error of the gas content obtained using the proposed method was smaller than 10%, indicating that the proposed method was more accurate and could meet the actual accuracy requirements. Overall, GDDUB along with the correction formula is very reliable for measurements of the coalbed gas content.
Conclusions
In this work, we established a laboratory protocol, which was used to study the effects of exposure time, sampling method, sample weight, sample particle size and gas loss estimation on the coalbed gas content measured using GDDUB. The following main conclusions are made:
With increasing exposure time, (a) the lost gas content increased, while its rate decreased and stabilized after a certain period of time; (b) the desorbed gas content decreased, and the residual gas content slowly reduced and eventually stabilized; and (c) the relative error of the gas content increased. The measured gas content can be corrected in practice using the fitting equations (8), (9) and (11). When the exposure time is within 15 min, the gas contents measured using the drilling method and the coring method differ slightly. With increasing exposure time, the gas content measured using the coring method was more accurate than that using the drilling method. The coring method is more reliable for underground in situ measurements of gas content with longer sampling times. The measured gas content increased with increasing sample weight. The gas content of the samples weighing 0–240 g increases with increasing sample weight, while the gas content of samples weighing 240–500 g tends to be stable. Samples with weights of 240 g are more appropriate for underground in situ measurements. If the sample weight is below 240 g due to practical field constraints, equation (13) can be applied to improve the accuracy of the gas content measurement. The relative error of the gas content declined with increasing sample particle size. Using the drilling method for measurement of the coalbed gas content, samples with particle sizes should be larger than 1 mm. When estimating the gas loss, the Barrer model along with its correction formula should be used to determine the gas loss of samples exposed for less than 12 min, while the power function along with its correction formula should be used to compute the gas loss of samples exposed for more than 12 min.
Footnotes
Acknowledgements
We acknowledge the editors for insightful suggestions on this work. And our deepest gratitude goes to the reviewer Dr Tim A Moore and the anonymous reviewers for their careful work and thoughtful suggestions that have helped improve this paper substantially.
Declaration of Conflicting Interests
The author(s) declared no potential conflicts of interest with respect to the research, authorship, and/or publication of this article.
Funding
The author(s) disclosed receipt of the following financial support for the research, authorship, and/or publication of this article: This research was supported by the National Natural Science Foundation of China (No. 51304189), the Program for Innovative Research Team in University of Ministry of Education of China (IRT13098). This work is also funded by the Priority Academic Program Development of Jiangsu Higher Education Institutions.
