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122   PETROPHYSICAL EVALUATION OF GAS SHALE RESERVOIRS

                               15
                                                   Mesopore                  Macropore

                             Incremental PV (%pu)    10 5  Micropore          Gas adsorption


                                                                                     MICP








                                0
                                 1                   10                  100                 1,000
                                                          Pore width (nm)
            FIGURE 6.6  A comparison between pore size distribution defined by incremental pore volume using mercury porosimetry and gas
            adsorption data (the arrows show the difference between peak positions in the mesopore area) for a gas shale sample from the Perth
            Basin, WA.


            diameters around 3 nm is about 60 kpsi. This high pressure,     • Measuring  the  gas  filled  porosity  using  helium
            as suggested by Giesche (2006), could compress the sample   pycnometry
            and subsequently decrease the measured pore throat size     • Heating the samples continuously up to succession of
            especially at smaller sizes.                             three characteristic retort temperatures (T  = 250°F, T  =
                                                                                                     1
                                                                                                              2
                                                                     600°F, and T  = 1300°F)
                                                                               3
            6.3.2  Fluid Saturation Measurement                       • Measuring the volumes of pore water and oil after having
                                                                     recovered fluid volumes from a retort experiment
            There are two common methods for fluid extraction used     • Measuring the gas volume by subtracting the recov­
            by commercial labs in conventional reservoirs: Dean Stark   ered fluids volume (water + oil) from measured pore
            and the retort method. Both methods are documented in    volume
            the recommended practice 40 (API, 1998). These methods
            can be used for gas shale; however, they are performed on     • Calculating total pore volume by summation of
            the crushed shale samples. The technique used by the Gas   extracted pore fluids and gas filled porosity
            Research Institute (GRI) to measure water and hydro­      • Calculating appropriate  saturation by dividing fluid
            carbon saturation is by performing Dean Stark method     volume by total pore volume
            with toluene (Luffel and Guidry, 1992). There are some
            limitations with this technique; although crushing the   It is worth mentioning that any water released before T  is
                                                                                                              1
            shale samples facilitates removing the pore fluid with   free water. A significant quantity of water that is released up
            the use of toluene, it still presents some difficulties in the   to T  can be capillary‐bound/clay‐bound water and finally
                                                                    2
            extraction  of  fluid  from  nanopores  (Handwerger  et  al.,   water extracted by T  is the indicator of structural water. The
                                                                                 3
            2011). Besides, this technique cannot differentiate  between   retort method also provides a measure of the free oil (mea­
            free water  and  bound  water,  and  typically only a   sured at T ) and the bound oil at T .
                                                                                            3
                                                                        2
            combination of these two volumes is reported (Sondergeld   Apart from these two methodologies, it is possible to
            et al., 2010).                                       extract the water content of the gas shale samples using
              The retort distillation method is a fluid extraction tech­  the thermogravimetric analyzer (TGA), based on the
            nique that involves sequential heating of the sample under   simple assumption that two fluid phases are present in the
            atmospheric pressure. During the heating process water and   shale sample: gas and water. During thermogravimetric
            oil are vaporized, collected, and measured by condensing the   analysis, crushed samples are heated in an inert atmosphere
            fluids into a graduated cylinder. The commercial procedure   and the mass loss due to pore fluid vaporization is
            available for performing the retort method on tight shales is   recorded in real time.  Then, water saturation can be
            as follows (Handwerger et al.; 2011):                  measured by relating the mass loss in the sample to
                                                                 the water evaporation only (Handwerger et al., 2012). The
                 • Measuring the bulk density by mercury immersion  temperature steps used for TGA are similar to those used
                 • Crushing the samples and weighing             in the retort method.
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