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1、INTERNATIONAL STANDARD IS0 10753 First edition 1994-02-01 Coal preparation plant - Assessment of the liability to breakdown in water of materials associated with coal seams Ateliers de prkparation du charbon - Evaluation de la fiabilit4 de la fragmentation dans Ieau de mat an outlet (HI allows the s
2、ample to be run off. The Andreasen sedimentation apparatus is modified by reducing the length of stem of the pipette, so that the sample is withdrawn at the 100 mm mark. The apparatus shall be protected from all sources of vi- bration during the test. 5.10 Suction device, capable of applying a stead
3、y, controlled suction to the sedimentation pipette (5.9). NOTE 3 An aspirator is preferred for this purpose. 5.11 Evaporating dish, of nickel or stainless steel, having a diameter of 50 mm. 5.12 Flask, of capacity at least 2 litres. 5.13 Thermostatically-controlled bath, capable of being maintained
4、at approximately ambient tempera- ture, to within f 0,2 “C, and of suitable dimensions to contain the sedimentation apparatus (5.91, a measuring cylinder (5.8) and the flask (5.12). The bath shall operate without causing significant vi- bration or disturbance of the measuring cylinder and its conten
5、ts, when placed in the bath. NOTE 4 If a thermostatically controlled bath is not avail- able, a large container filled with water that has been al- lowed to attain room temperature may be used instead. 2 Copyright International Organization for Standardization Provided by IHS under license with ISO
6、Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 22:06:55 MDTNo reproduction or networking permitted without license from IHS -,-,- Q IS0 IS0 10753:1994(E) E F 200 mm A 1 B 100 mm KW A Graduated cylindrical flask B Pipette C 10 ml Reservoir D Three-way stopcock E Groundglass
7、 stopper F Small opening in stopper (to allow air to enter) G Suction application point H Outlet Figure 2 - Modified Andreasen sedimentation apparatus 5.14 Drying oven, well ventilated and capable of being maintained in the temperature range 105 “C to 110 “C. 5.15 Stop clock. 5.16 Analytical balance
8、(s), capable of weighing up to 20 g to the nearest 0,000 1 g and up to 200 Q to the nearest 0,Ol g. 5.17 Wash bottle, of capacity at least 400 ml, fitted with a fine spray-jet outlet. 5.18 Desiccator. 5.19 Vibration-free bench. 6 Sampling and preparation of test sample If sufficient material is avai
9、lable, take a representative sample containing a minimum of 1 kg in the 5,6 mm to 2,8 mm size fraction. If there is insufficient material to provide the required amount in this size fraction, crush all the larger shale and add the 5,6 mm to 2,8 mm size fraction of the crushed product to that size fr
10、action in the original material. If neither of these measures provides sufficient material, a size fraction of 5,6 mm to 1.0 mm shall be used instead. Full de- tails of the sample taken shall be included in the test report (see clause 10). NOTES 5 It may be useful to prepare and test separate repres
11、en- tative samples from the floor, roof and dirt bands for each seam. 6 If the test sample is obtained from raw coal by means of float and sink separation, this may affect the results of the test. Remove the dust from the test sample by gentle blowing with air and store the test sample, until re- qu
12、ired for testing, in a secure, sealed container. 7 Procedure 7.1 Determination of initial moisture content Determine the moisture content of the shale “as re- ceived” by weighing a IO Q portion, to an accuracy of f 0,000 1 g, drying in the oven (5.14) for 2 h at 105 “C to 110 “C and then reweighing.
13、 7.2 Preparation of test portion Dry for 2 h in the oven (5.14), at 105 “C to 110 “C, enough of the test sample to provide a mass of 120 Q, when dried, and place it in a sealed container. 7.3 Determination of residual moisture content Determine the residual moisture in the test portion by taking 10
14、g of the dried test sample (see 7.2), 3 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 22:06:55 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 107
15、53:1994(E) Q IS0 weighed to an accuracy of f 0,000 1 g, drying in the oven (5.14) to constant mass at 105 “C to 110 “C and then reweighing. 7.4 Agitation of test portion Weigh, to an accuracy of f 0,Ol g, 100 g of the dried test sample (7.2), place in the cylindrical jar (5.1) and add 500 ml of wate
16、r (clause 4). Seal the jar securely, place it in the rotation machine (5.2) and rotate it about a transverse axis (i.e. “end over end”) at a ro- tational frequency of 40 min- f 1 min- (speed of 40 r/min f 1 r/min) for 30 min. 7.5 Sieving of suspension Locate the funnel (5.4) in the neck of one of th
17、e measuring cylinders (5.8) and mount the 500 pm test sieve (5.3) in the funnel. Sieve the suspension result- ing from the agitation (7.4) through the test sieve, taking care to ensure that the solids are distributed evenly over the surface of the sieve. Use 250 ml of water (clause 4) to rinse out t
18、he jar and wash the residue on the sieve, applying the water by means of the wash bottle (5.17). Remove the sieve from the funnel, place it on the tray (5.5) and dry in the oven (5.14) at 105 “C to 110 “C for 1 h. Remove the tray containing the sieve from the oven. Brush off the dried material into
19、the tared con- tainer (5.6) and dry in the oven to constant mass (see note 7). Cool in the desiccator (5.18), to prevent ab- sorption of moisture, and weigh to an accuracy of f 01 g. NOTE 7 If the operation of drying to constant mass is likely to take more than 30 min, the mass measured at that time
20、 should be recorded and used to calculate the concen- tration of solids in the suspension passing through the sieve (see 7.8). This procedure is used in order that the proportion of material that is below a nominal particle size of 10 pm may be determined with the minimum of delay. 7.6 Treatment of
21、fines While the material retained on the sieve is being dried, rinse any fine particles adhering to the funnel into the measuring cylinder containing the suspension that has passed through the sieve, using 100 ml of water (clause 4). Dilute to 1 litre and place the measuring cylinder in the thermost
22、atically-controlled bath (5.13). 7.7 Preparation of water and apparatus for sedimentation Fill the flask (5.12) with water (clause 4) and place it, together with the sedimentation apparatus (5.9), in the thermostatically-controlled bath (5.13), main- tained, to within f 0.2 “C, at a temperature clos
23、e to ambient temperature. Allow at least 1 h to reach temperature equilibrium before proceeding with the procedure described in 7.8. Use this water whenever water is required for subsequent steps in the pro- cedure. 7.8 Adjustment of concentration of suspension Calculate the percentage of material p
24、assing through the 500 pm test sieve in accordance with 8.1, using the approximate mass of material retained on the sieve if necessary (see note 7). From this percentage, and the mass of the test portion (see 7.4), determine the concentration of solids in the suspension obtained as described in 7.6.
25、 If this concentration does not ex- ceed 20 g/l, use the suspension directly for the sedimentation (see 7.10). Otherwise, invert the cylin- der six times to mix its contents, transfer an appro- priate volume to the second measuring cylinder (5.8) and dilute to volume with water maintained as de- scr
26、ibed in 7.7. Keep the measuring cylinder, contain- ing the suspension to be used for the next step, in the thermostatically-controlled bath (5.13). NOTE 8 The concentration of the solids in the suspen- sion is adjusted to a level at which the particles may be as- sumed to be in free settlement, with
27、out mutual hindrance. The actual volume taken from the first measuring cylinder for dilution to 1 litre is not critical, provided that it is meas- ured accurately. If the suspension in the first measuring cylinder contains m g of solids, a measured volume of not more than 2.0 x lo4 ml should be tran
28、sferred to the sec- ond measuring Cylinder. 7.9 Determination of settling time Calculate the time r, in seconds, taken for particles of 10 pm nominal diameter to fall 100 mm, from the following equation: t = 1,223 x 1 06q . (1) where t is the dynamic viscosity of water, in Pascal seconds, at the tem
29、perature of the test). 1) The dynamic viscosity of water at different temperatures can be obtained from reference tables, e.g. Tables of physical and chemical constants, G.W.C. Kaye and T.H. Laby. 4 Copyright International Organization for Standardization Provided by IHS under license with ISO Licen
30、see=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 22:06:55 MDTNo reproduction or networking permitted without license from IHS -,-,- Q IS0 IS0 10753:1994(E) NOTE 9 The derivation of equation (1) is given in NOTE 12 This withdrawal should take between 25 s and annex A. 30 s. Altern
31、atively, the settling time may be determined from table 1, by interpolation if necessary. Turn stopcock D so that the 10 ml portion is dis- charged through outlet H into the tared evaporating dish (5.11). Wash out reservoir C with a few millilitres of water and add the washings to the contents of th
32、e evaporating dish. Determine the mass of the solids by evaporating to dryness and then drying to constant mass in the oven (5.14) at 105 “C to 110 “C. Cool in the desiccator (5.18) and weigh to an accuracy of f 0,000 1 g. Table 1 - Settling time for 10 km particles Temperature Settling time “C min
33、S 10 26 35 15 23 10 20 20 25 25 18 10 30 16 15 7.10 Determination of particles below 10 pm nominal size (slimes) by sedimentation NOTE 10 An alternative sedimentation technique may be used, provided that it can be demonstrated that it will produce results comparable with those obtained using the tec
34、hnique described below. Carry out this part of the procedure on a vibration-free bench (5.19). Fit the suction device (5.10) to the sedimentation ap- paratus (5.9). NOTE 11 It is important to fit the suction device before the settling is commenced, so that the withdrawal of a portion of the suspensi
35、on can take place smoothly and the apparatus is not disturbed while settling is in progress. Mix the suspension in the measuring cylinder, diluted if necessan/ as described in 7.8, by inverting it six times. Pour the suspension into the sedimentation apparatus, up to the 200 mm mark. Fit the pipette
36、 and replace the apparatus in the thermostatically- controlled bath. After allowing a few minutes for the apparatus to return to the temperature of the bath, remove it from the bath, place a finger over hole F (see figure2) and, while holding the pipette in place, agitate the suspension by inverting
37、 the apparatus six times. Immediately replace the apparatus in the bath and start the stop clock (5.15). After the time interval calculated in accordance with 7.9 has elapsed, withdraw a 10 ml portion of the suspension by connecting the pipette stem to the reservoir C via the stopcock D and applying
38、 steady suction at point G. NOTE 13 A check on the results of the determination of slimes may be carried out by shaking the suspension re maining in the sedimentation apparatus immediately after the withdrawal of the 10 ml portion, and then starting the stop clock and repeating the settling as descr
39、ibed above. In this case, the settling time will have to be calculated from equation tA.lj, making an appropriate correction to the value of h to allow for the portion of suspension removed. 7.11 Number of tests Carry out the entire procedure in duplicate. 8 Expression of results 8.1 Material passin
40、g through the 500 pm test sieve The proportion (ale) of material passing through the test sieve, expressed as a percentage by mass on a dry basis, is given by the following equation: lv(J = 100 i 1 1 OOm, - mJlO0 -M) 1 . . where (2) ml is the mass, in grams, retained on the 500 urn test sieve; MO is
41、 the mass, in grams, of the test portion; M is the residual moisture in the test portion, expressed as a percentage by mass. 8.2 Particles below 10 km nominal size (slimes) 8.2.1 No further dilution If the suspension obtained as described in 7.6 did not require further dilution (see 7.81, the propor
42、tion (w,J of solid material below 10 km nominal size in the test sample, expressed as a percentage by mass on a dry basis, is given by the following equation: 5 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545
43、001 Not for Resale, 04/22/2007 22:06:55 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 10753:1994(E) Q IS0 1 06?f12 +?O= ? “lo is the mass, in grams, of the test portion; M is the residual moisture in the test portion, expressed as a percentage by mass. 8.2.2 Further d
44、ilution If the suspension did require further dilution in ac- cordance with 7.8, the proportion (wIo) of solid mate- rial below 10 pm nominal size, expressed as a percentage by mass on a dry basis, is given by the following equation: 1 osm2 ?O= V?r+)(lOO -M) . * . where (4) m, is the mass, in grams,
45、 of solids in the 10 ml portion withdrawn from the sedimentation apparatus after the settling period; V is the volume, in millilitres, taken from the first measuring cylinder and diluted to 1 li- tre in the second measuring cylinder; “lo is the mass, in grams, of the test portion; M is the residual
46、moisture in the test portion, expressed as a percentage by mass. 8.3 Breakdown ratio The breakdown ratio B, expressed as a percentage by mass, is given by the following equation: The difference between two single results found on test portions, taken from the same test sample, by one operator using
47、the same apparatus within the shortest feasible time interval will exceed 5 %, rela- tive, on average not more that once in 20 cases during the normal and correct operation of the method. 9.2 Reproducibility limit The difference between two single results found on identical test material by two diff
48、erent operators using different apparatus at different times will exceed 10 %, relative, on average not more than once in 20 cases during the normal and correct operation of the method. 10 Test method The test report shall include the following information: a) the identification and history of the s
49、ample under test; b) whether the test sample contained material other than that naturally occurring in the 5,6 mm to 2,8 mm size fraction; c) the initial moisture content of the shale “as re- ceived” and the residual moisture content in the test portions after drying; d) the sedimentation technique used, if different from that described; e) the sedimentation test conditions, i.e. the volume of suspension diluted,