ISRM Codes
ISRM Codes
ISRM Codes
143
Suggested Methods for Determining Water Content, Porosity, Density, Absorption and Related Properties and Swelling and Slake-Durability Index Properties
PART 1: SUGGESTED METHODS FOR DETERMINING WATER CONTENT, POROSITY, DENSITY, ABSORPTION AND RELATED PROPERTIES
NOTES The sample should if possible be large, to minimise the influence of experimental error. Alternative test methods are available calling for samples in different form; selection from among these should be based on the nature of rock to be tested.
The presence of pores in the fabric of a rock material decreases its strength, and increases its deformability. A small volume fraction of pores can produce an appre(iiO Rock constituents ciable mechanical effect. The following terms and symbols will be used to Information on the porous nature of rock materials is frequently omitted from petrological descriptions, but denote the masses and volumes of rock constituents is required if these descriptions are to be used as a when calculating physical properties such as porosity guide to mechanical performance. Sandstones and car- or density. bonate rocks in particular occur with a wide range of Grains (the solid component of the sample), mass Ms, porosities and hence of mechanical character; igneous volume Vs rocks that have been weakened by weathering processes Pore water, mass Mw and volume Vw also have typically high porosities. Pore air, zero mass and volume Va Most rocks have similar grain densities and therefore Pores (voids), with volume Vv = Vw + Va have porosity and dry density values that are highly Bulk sample mass M --- Ms + M~ correlated (see note (v) equation 4). A low density rock Bulk sample volume V -- V~ + Vv is usually highly porous. It is often sufficient, therefore, Density of water p~ -- mass of water per unit volume to quote values for porosity alone, but a complete description requires values for both porosity and (iv) Definitions, terminology and preferred S.I. units density. Those physical properties pertinent to the methods " Microscopic techniques used to determine volumetric of test about to be described may be defined in terms content of mineral grains, do not provide a sufficiently of the rock sample constituents listed above. accurate estimate of volumetric pore content, and exMW perimental techniques are required. However, micro- Water content w x 100 (~) scopy and also techniques such as mercury injection Me and permeability testing, can provide useful supplemenVW tary information on the shape and size of pores. Degree of saturation S, loo (%)
x
V~
= - - x 100 V = V---~ _ M _ Ms + My V V
VV
Vo
144
Relative density d (specific gravity) Dry density pa Dry relative density (dry) da (specific gravity)
l-)
The sample should not take up water in the interval between drying and mass determination. Where necessary the sample container should be covered with an airtight lid and stored in a dessicator during cooling.
(vii) Determination of the bulk volume I/ (-) Caliper method. The bulk volume of specimens in the form of regularly shaped prisms or cylinders may be (kg) calculated from vernier or micrometer caliper measure_ Ms + VvPw Saturated density Psat ments. An average of several readings for each dimenV (m3) sion, each accurate to 0.1 mm, should be used in the calculation of bulk volume. Saturated relative density dsat = Ps (-) Buoyancy method. The bulk volume of regular or ir(saturated specific gravity) Pw regular specimens may be calculated using Archimedes (kg) principle, from the difference between saturated-surface_ Ms Grain density Ps (m 3) dry and saturated-submerged sample weights. The (density of solids) V~ method is not suited to friable, swelling or slaking rocks. P8 Grain relative density d~ (-) The sample is then transferred underwater to a Ps (grain specific gravity) basket in an immersion bath. Its saturated-submerged (N) least one hour, with periodic agitation to remove Unit weight 7 = Pg (m 3) trapped air. The sample is then transferred underwater to a basket in an immersion bath. Its saturated-submerged (v) Interdependence equations mass M~ub is determined to an accuracy of 0.1 g from The physical properties defined above are interrethe difference between the saturated-submerged mass lated, so that any one property may be calculated if of the basket plus sample and that of the basket alone. others are known. The sample is then removed from the immersion For simplicity only three properties will be referred bath and surface dried with a moist cloth, care being to in the text, namely, water content, porosity and dry taken to remove only surface water and to ensure that density of rock. The equations listed below may be used no rock fragments are lost. Its saturated-surface-dry to calculate any of the remaining properties from these mass M~a, is determined to an accuracy of 0.1 g. three. The sample bulk volume is calculated as Whereas water content, degree of saturation and porosity are usually expressed as percentages, the void V - M s a t - M~,b ratio is usually expressed as a dimensionless ratio. The Pw following interdependence equations have been given Mercury displacement method. High surface tension to conform to the above. prevents mercury penetrating all but the largest pores 100wpa in rock. The specimen is forced under mercury and S, (?/o) its volume determined from the displaced fluid volume. npw A calibrated tube may be incorporated in the apparatus n (-) for this purpose, or the displacement may be measured el00 - n by a micrometer screw gauge--electric contact tech(kg) nique. Alternatively a technique may be employed p = 1+ Pa (m 3) where the displaced mercury volume is obtained by mass determination. The apparatus should give results lOOpe (kg) accurate to 0.5~o of the specimen bulk volume, and Ps 100 - n (m 3) should be periodically calibrated using a standard sphere or cylinder. Water displacement method. The bulk volume of a (vi) Determination of the grain mass M~ saturated-surface-dry sample may be determined by The grain mass Ms of the sample is defined as the water displacement using a technique similar to that equilibrium mass of the sample after oven drying at for mercury displacement. Alternatively the dry or partially dry sample may be coated in wax or plastic and a temperature of 105C. A thermostatically controlled, ventilated drying oven its bulk volume determined from the water volume discapable of maintaining a temperature of 105C accurate placed by the coated sample, corrected for the volume to 3C for a period of at least 24 h is required. of coating material. The method requires accurate The sample is regarded as 'oven dry' when successive determination of coating volume and is best applied mass determinations at intervals of 4 hr yield values to large bulk samples where other techniques are imdiffering by less than 0.1~o of the sample mass. practical. Pd Pw
145
(b) A sample container of non-corrodible material, including an airtight lid. (c) A dessicator to hold sample containers during cooling. (d) A balance of adequate capacity, capable of weighing to an accuracy of 0.01% of the sample weight.
3. P R O C E D U R E
vo=
Msat
Ms
Pw
The Washburn-Bunting method (Washburn & Bunting, 1922). A rock specimen is oven-dried and immersed
in mercury. The pressure on the mercury is reduced that the pore air expands, leaves the rock and is trapped above the mercury column. The volume of pore air Va is measured directly in a calibrated tube, after pressure has been equalised with that of the atmosphere. The method is rapid but is best suited to rocks with high porosity.
(ix) Determination of grain volume V~ Boyle's law method. The pressure-volume relationship
for a container filled with gas only is obtained, then for the same container filled with specimen plus gas. The difference in compressibility is due to the volume Vs of incompressible grains, and this volume may be calculated from the results. One type of Boyle's law single-cell porosimeter employs a graduated mercury pump to measure volume displacement, together with a Bourdon gauge to measure pressure change. Boyle's law double cell techniques employ pressure equalization between two containers at different initial pressures. Pulverization method. After determination of bulk volume and grain mass, the oven-dry sample is pulverized and its grain volume Go determined by displacement of an equivalent volume of liquid (e.g. toluene) in a volumetric flask. Porosity calculated from bulk volume and grain volume using the pulverization method is termed total porosity, since the pore volume obtained includes that of 'closed' pores. Other techniques give effective porosity values since they measure the volume of interconnected pores only.
(a) The container with its lid is cleaned and dried, and its mass A determined. (b) A representative sample comprised at least 10 lumps each having either a mass of at least 50 g or a minimum dimension of ten times the maximum grain size, whichever is the greater, is selected. For in situ water content determination sampling, storage and handling precautions should be such that water content remains within 1% of the in situ value. (c) The sample is placed in the container, the lid replaced and the mass B of sample plus container determined. (d) The lid is removed and the sample dried to constant mass at a temperature of 105C. (e) The lid is replaced and the sample allowed to cool in the dessicator for 30 min. The mass C of sample plus container is determined. 4. CALCULATION Water content w = pore water Mass Mo grain Mass Ms B-C C-A
x 100%.
x
100%
5. REPORTING OF RESULTS
The water content should be reported to the nearest 0.1% stating whether this corresponds to in situ water content, in which case precautions taken to retain water during sampling and storage should be specified.
146
International Society for Rock Mechanics 2. APPARATUS (b) Density values should be given to the nearest 10kg/m 3 and porosity values to the nearest 0.11;/o. (c) The report should specify that bulk volume was obtained by caliper measurement and that pore volume was obtained by water saturation.
(a) An oven capable of maintaining a temperature of 105C to within 3C for a period of at least 24 hr. (b) A dessicator to hold specimens during cooling. (c) A measuring instrument such as vernier or micrometer caliper, capable of reading specimen dimensions to an accuracy of 0.1 ram. (d) Vacuum saturation equipment such that the specimens can be immersed in water under a vacuum of less than 800 Pa (6 torr) for a period of at least one hour. (e) A balance of adequate capacity, capable of determining the mass of a specimen to an accuracy of 0.01%. 3. PROCEDURE (a) At least three specimens from a representative sample of a material are machined to conform closely to the geometry of a right cylinder or prism. The minimum size of each specimen should either be such that its mass is at least 50 g (for an average density rock a cube with sides of 27 mm will have sufficient mass) or such that its minimum dimension is at least ten times the maximum grain size, whichever is the greater. (b) The specimen bulk volume V is calculated from an average of several caliper readings for each dimension. Each caliper reading should be accurate to 0.1 mm. (c) The specimen is saturated by water immersion in a vacuum of less than 800Pa (6 tort) for a period of at least 1 hr, with periodic agitation to remove trapped air. (d) The specimen is removed and surface dried using a moist cloth, care being taken to remove only surface water and to ensure that no fragments are lost. Its saturated-surface-dry mass M~,, is determined. (e) The specimen is dried to constant mass at a temperature Of 105C, allowed to cool for 30 min in a dessicator, and its mass is determined to give grain mass Ms. Specimens in this test are generally of sufficient coherence not to require containers, but these should be used if the rock is at all friable or fissile. 4. CALCULATIONS
V~, --
Msa,
Ms
100Vv n = ---V-~% Pd = - - . V
MS
5. REPORTING OF RESULTS (a) Individual results for at least three specimens per rock sample should be reported, together with average results for the sample.
(a) A representative sample comprising at least 10 lumps of regular or irregular geometry, each having either a mass of at least 50g or a minimum dimension of at least 10 times the maximum grain size, whichever is the greater, is selected. The sample is washed in water to remove dust. (b) The sample is saturated by water immersion in a vacuum of less than 800 Pa (6 torr) for a period of at least one hour, with periodic agitation to remove trapped air. (c) The sample is then transferred under water to the basket in the immersion bath. Its saturated-submerged mass Ms,b is determined to an accuracy of 0.1 g from the difference between the saturated-submerged
Suggested Methods for Determining Water Content mass of the basket plus sample and that of the basket alone. (d) The sample container with its lid is cleaned and dried, and its mass A is determined. (e) The sample is removed from the immersion bath and surface-dried with a moist cloth, care being taken to remove only surface water and to ensure that no rock fragments are lost. The sample is transferred to the sample container, the lid replaced, and the mass B of saturated-surface-dry sample plus container is determined. (f) The lid is removed and the sample dried to constant mass at a temperature of 105C, the lid replaced and the sample allowed to cool for 30 min in a dessicator. The mass C of oven-dry sample plus container is measured. 4. C A L C U L A T I O N S 4. Saturated-surface-dry mass Grain weight Bulk volume Pore volume Porosity Dry density of rock
Msa, = B - A 2. A P P A R A T U S
147
(a) An oven capable of maintaining a temperature of 105C to within 3C for a period of at least 24 hr. It should have forced ventilation exhausting to outside atmosphere. (b) Specimen containers of non-corrodible material, including airtight lids. (c) A dessicator to hold specimen containers during cooling. (d) A balance of adequate capacity, capable of mass determination to 0.001 g. (e) A mercury-displacement volume measuring apparatus capable of measuring specimen volume to
0.5%.
(f) Grinding equipment to reduce the sample to a pulverized powder less than 150 #m in grain size. (g) A calibrated volumetric flask and stopper (conveniently 50 cm3). (h) A constant temperature water bath. (i) A vacuum apparatus capable of maintaining a vacuum with a pressure of less than 800 Pa (6 torr). (j) A soft brush of camel hair or of a similar softness.
Ms=C-A
V = MSat Msab
Pw
vv=
Msat - -
Ms
3. P R O C E D U R E
Pw
lOOVv
V
Ms
Pd= V
5. R E P O R T I N G O F R E S U L T S
(a) The report should include porosity and dry density values for the sample, and should specify that bulk volume was obtained by a buoyancy technique and that pore volume was obtained by water saturation. (b) Density values should be given to the nearest 10 kg/m 3 and porosity values to the nearest 0.1~o.
4. S U G G E S T E D M E T H O D FOR POROSITY/DENSITY DETERMINATION USING MERCURY DISPLACEMENT AND GRAIN SPECIFIC GRAVITY TECHNIQUES
1. S C O P E (a) The test is intended to measure the porosity, the dry density and related properties of a rock sample in the form of lumps or aggregate of irregular geometry. It is particularly suitable if the rock material is liable to swell or disintegrate if immersed in water. The test may also be applied to regularly shaped rock specimens or to coherent rock materials, but other techniques are usually found more convenient in these cases.
(a) A representative sample is selected comprising at least ten rock lumps, the shape and size of lumps suiting the capabilities of the volume measuring apparatus. The minimum size of each lump should preferably be either such that its mass exceeds 50 g or such that its minimum dimension is at least ten times the maximum grain size, whichever is the greater. Specimens of swelling or fissile rock should be sampled and stored to retain water content to within 19/o of its in situ value prior to testing. (b) Each specimen is brushed to remove loose material and its volume V is measured by mercury displacement. Mercury adhering to the specimen is carefully removed, ensuring that no rock fragments are lost. (c) The specimen container with its lid is cleaned, dried and its mass A is determined. (d) The specimen is placed in the container, the lid replaced and mass B of container plus specimen at initial water content is determined. (e) The lid is removed and the specimen oven dried to constant mass at a temperature of 105C and allowed to cool for 30 min in a dessicator. The mass C of container plus oven-dry specimen is determined. (f) Steps (b)-(e) are repeated for each specimen in the sample. (g) Together the specimen was crushed and ground to a grain size no exceeding 150 #m. A number of representative sub samples of about 15g of the pulverized material are selected and oven-dried. (h) The mass D of a clean, dry volumetric flask plus stopper is determined to 0.001 g. (i) The flask is filled with a fluid such as toluene that is non-reactive with the rock, is brought to equilibrium temperature in the constant temperature bath, and the
148
International Society for Rock Mechanics 5. S U G G E S T E D METHOD POROSITY/DENSITY DETERMINATION MERCURY AND BOYLE'S LAW FOR
liquid level is adjusted accurately to the 50 cm 3 graduation. The flask is removed, stoppered and its mass E determined to 0.001 g. (j) The flask is emptied and dried, and the 15 g subsample of dry, pulverized rock added with the aid of a funnel. The mass F of flask, sample and stopper is measured to 0.001 g. (k) The flask and subsample are evacuated for about 20 min and sufficient fluid added to thoroughly wet the sample. Further fluid is then added and the flask carefully evacuated to remove air. The flask is replaced in the constant temperature water bath and the liquid level adjusted accurately to the 50 c m 3 graduation. (1) The stoppered flask with its contents is allowed to cool and its mass G is determined to 0.001 g. (m) Steps 0)-(1) are repeated for each subsample of pulverized material.
USING TECHNIQUES
DISPLACEMENT
1. SCOPE (a) This test is intended to measure the porosity, the dry density and related properties of a rock sample. A sample in the form of specimens of a specific size and shape to suit the apparatus is usually required to ensure accurate results. (b) The method should only be used for rocks that do not shrink appreciably during oven-drying.
2. A P P A R A T U S
x 100%
The procedure given below relates to a test using the Kobe type of single cell Boyle's Law porosimeter (Fig. 1). Any similar apparatus of equivalent accuracy may however be used. The apparatus consists essentially of the following: Oven drying equipment: (a) An oven capable of maintaining a temperature of 105C to within 3C for a period of at least 24 hr. (b) A specimen container of non-corridible material including an airtight lid. (c) A dessicator to hold specimen containers during cooling. (d) A balance of adequate capacity, capable of determining the mass of a specimen to an accuracy of 0.01%. A Boyle's law porosimeter such as a Kobe porosimeter having the following features: (e) A mercury screw-piston pump with micrometer graduated to measure the volume of displaced mercury to an accuracy of 0.01 c m 3. Conveniently one turn of the screw pump changes the volume of the specimen chamber by 1 c m 3. (f) A specimen chamber with removable cap to allow insertion of the specimen. (g) A sight glass inscribed with a reference line, an electric indicator-contact or other means of registering a mercury datum level in the cap. (h) A gas inlet and outlet, each with a shutoff valve, also a source of inert gas such as helium. Air may be used with some loss of accuracy, but must be adequately dried. (i) A precision pressure gauge or pressure transducer with a range from 100 kPa to about 400 kPa, connected to measure the gas pressure in the specimen chamber.
3. P R O C E D U R E
Ps =
v+
F-D
where V I = calibrated volume of flask, usually 50 cm 3 (c) Grain mass (d) Dry density of rock M~ = C - A
MS --
Pd ~
(e) Porosity
n -
lO0(ps -
p,~) % .
Ps
5. R E P O R T I N G
O F RESULTS
(a) Individual dry density values for each specimen in the sample should be reported, together with average values for the sample. Porosity values for each subsample should also be reported together with the average value. (b) The report should sPecify that the bulk volume was obtained using a mercury displacement technique, and that the porosity was calculated from grain volume measurements using a pulverization technique. (c) The grain density or grain specific gravity for the sample should be reported. The water content at which bulk volume measurement took place should be specified, stating whether this corresponds to in s i t u water content. (d) Density values should be given to the nearest 10 kg/m 3 and porosity values to the nearest 0.1 percent.
(a) At least three specimens are selected from a representative sample of material and each specimen is tested separately to obtain an average result for the sample. The size and shape of a specimen should allow only a small clearance with the specimen chamber to
149
/2
PRESSURE GAUGE
GAS OUTLET
[Z:GAS
INLET
MERCUI:~Y
~\\"1.
i,'~//,tP\\\]
NCORE
SPECIMEN
r\-,~///-//'~,
", - ~]
MICROMETER S C A L E [
, ,
N \.
711
ensure accurate results. The chamber is usually cylindrical and accepts a standard size of rock core. The size of each specimen should preferably be either such that its mass is a minimum of 50 g or that its minimum dimensions are at least ten times the maximum grain size, whichever is the greater. (b) The specimen container with its lid is cleaned, dried and its mass A is determined. (c) The specimen is placed in the container, dried to constant mass at a temperature of 105C and the lid is replaced. It is allowed to cool for 30 min in a dessicator, and the mass B of oven-dry specimen plus container is determined. (d) Use of the porosimeter: the mercury pump reading at the start of each compression or displacement cycle is termed the 'start point'. Inlet and outlet valves are closed at the start of a compression cycle so that the initial pressure P1 is atmospheric. The start point and also the pressure P2 at the end of a compression cycle are usually selected as standard for the apparatus, to ensure that the specimen still floats on mercury at the end of the cycle, hence avoiding imbibition that might occur if specimens became deeply immersed. (e) To flush the specimen chamber with gas; inlet valve is closed, the outlet opened and the pump advanced until mercury reached the datum. The outlet is then half shut, the inlet opened and the pump
retracted to beyond the start point. The inlet, then the outlet valve is closed. (f) To determine the compression factor Cf for the cell: the specimen chamber is first flushed with gas, the outlet valve opened and the pump advanced to the start point. The outlet valve is shut with the specimen chamber at atmospheric pressure P1. The pump is advanced and a micrometer reading Co taken when the pressure reaches P2. The chamber is again flushed with gas, and with the outlet valve open the pump is advanced to a new start point 10cm 3 beyond the original one. The outlet is closed with the chamber at atmospheric pressure P1 and the pump advanced, a micrometer reading C1 being taken when the pressure again reaches P2. The compression factor is computed from the formula: 10 CI = 10 - (Co - C1)"
This factor is dependent on ambient pressure and should be periodically checked. (g) Each test comprises a displacement stroke followed by a compression stroke with the specimen chamber empty (a blank run), then a displacement
150
International Society for Rock Mechanics however, the porosity and density of the rock material should be determined directly using techniques such as those proposed earlier (methods 2-5). (c) The test should only be used for rocks that do not appreciably disintegrate when immersed in water. 2. APPARATUS (a) A sample container of non-corrodible material, water tight and of sufficient capacity to contain the sample packed in dehydrated silica gel. (b) A quantity of dehydrated silica gel. (c) A balance of adequate capacity, accurate to 0.5 g. 3. PROCEDURE (a) A representative sample is selected comprising at least ten rock lumps. The size of each lump should be such that its mass exceeds 50 g or such that its minimum dimension is at least ten times the maximum grain size, whichever is the greater. (b) The sample in an air-dry condition is packed into the container, each lump separated from the next and surrounded by crystals of dehydrated silica gel. The container is left to stand for a period of 24 hr. (c) The container is emptied, the sample removed, brushed clean of loose rock and silica gel crystals and its mass A determined to 0.5 g. (d) The sample is replaced in the container and water is added until the sample is fully immersed. The container is agitated to remove bubbles of air and is left to stand for a period of one hour. (e) The sample is removed and surface-dried using a moist cloth, care being taken to remove only surface water and to ensure that no fragments are lost. The mass B of the surface-dried sample is determined to 0.5g. 4. CALCULATION Void index It, B-A A x 100%.
stroke followed by a compression stroke with the specimen in the chamber. The procedure is as follows: (h) With the inlet valve shut and the outlet open, the pump is advanced until the mercury reaches the datum. The micrometer reading R1 is recorded. (i) The chamber is flushed with gas, the pump advanced to the start point and the valves closed with the chamber at atmospheric pressure P1. The pump is advanced and a micrometer reading R2 recorded when the pressure reaches Pz(j) The specimen is removed from the dessicator and inserted in the chamber. The chamber is flushed with gas and step (h) repeated, recording the displacement stroke micrometer reading R3 at which mercury reaches the datum. (k) Step (i) is repeated, recording the compression stroke micrometer reading R4 when the pressure again reaches P2. 4. CALCULATIONS Bulk volume Grain volume Grain weight Porosity Dry density of rock By
= R3 --
R1
5. REPORTING OF RESULTS (a) Individual dry density and porosity values for each specimen in the sample should be recorded, together with average values for the sample. (b) The report should specify that the bulk volume was obtained using a mercury displacement technique, and that the porosity was calculated from grain volume measurements using a Boyle's law technique. (c) Density values should be given to the nearest kg/m 3 and porosity values to the nearest 0.1 porosity percent.
5. REPORTING OF RESULTS
(a) The void index for the sample should be reported to the nearest 1%. (b) The report should specify that the void index is defined as the water content after dessicator drying followed by a one-hour period of immersion. REFERENCES
1. American Petroleum Institute. API recommended practice for core-analysis procedure. Am. Petrol. Inst. Recommended Practice RP 40 (1960). 2. British Standards Institution. Methods for sampling and testing mineral aggregates, sands and fillers. British Standard 812 (1967). 3. British Standards Institution. Methods of testing soils for civil engineering purposes. British Standard 1377 (1967). 4. Buell A, W. Porosity and permeability analysis. In Subsur/?lce Geologic Methods. Colorado Sch. Mines. pp. 168 179 11949).
151
Meeting, Soc. Professional Well Log Analysts, Tulsa, Oklahoma. 15 pp (1960). Manger G. E. Method dependent values of bulk, grain and pore volume as related to observed porosity. U.S. Geol. Survey Bul. N 1203, 20 pp (1966). Morgenstern N. R. & Phukan A. L. T. Non linear deformation of a sandstone. Proc. 1st Int. Congress Rock Mech. Lisbon 1, 543-548 (1966). Obert L., Windes S. L., Duvall W. I. Standardised tests for determining the physical properties of mine rock. U.S. Bur. Mines Report of Investigations 3891 (1946). Washburn E. W. & Bunting E. N. Determination of porosity by the method of gas expansion, American Ceramic Soc. 5, No. 48, 112 (1922).
PART 2" SUGGESTED METHODS FOR DETERMINING SWELLING A N D SLAKE-DURABILITY INDEX PROPERTIES
NOTES
as determination of the liquid and plastic limits, the grain size distribution, or the content and type of clay minerals present.
1. SUGGESTED M E T H O D
DETERMINATION UNDER ZERO OF
FOR THE OF