METHOD OF MANUAL SAMPLING OF COAL IS : 436 (PART-1 / SECTION -1) Page 1 0f 8 DKTypes of coal according to size Indian coals had originally been divided into five size groups, but for the purpose of sampling coal should be divided into the following three size groups. (1)Coal, Run-of-mine: - Unscreened coal is containing all sizes, mainly 23 to 0 cm. (2)Coal, Large: - Coal with nominal size 15 to 5 cm, the upper limit not exceeding 23 cm. (3)Coal, Small: - Coal with nominal size 5 to 0 cm. Terminolo; (1)Increment: - The quantity of coal taken by a single operation of the sampling implement. (2)Lot: - The quantity of coal offered for disposal at one time. (3)Sub-lot: - The quantity of coal in each of the groups into which is a lot is divided for the purpose of sampling. For the purpose of sampling, a lot shall be divided into a numbers of sub-lots of approximately in equal weights. (4)Composite sample (for a lot): - The quantity of coal obtained by mixing together equal quantities of coal from each of the laboratory samples representing the sub- lots into which the lot has been divided. (5)Gross sample: - Sample has collected from a sub-lot, that is, the quantity of coal obtained by aggregating together all the increments drawn from the same sub-lot. Note: - The division of a lot into a numbers of sub-lots depending upon the weights of the lot and then drawing a representative gross sample from each of the sub-los separately. The gross samples after suitable reduction are to be tested individually for determination of important characteristics of coal and compositely for others. A proper procedure for valid interpretation of the test results so as to evaluate the average level of quality as also the extent of variation in the average for a lot with 95 % confidence Page 2 of 8 DK(6) Moisture sample: - A sample to be used exclusively for the purpose of determining total moisture. (7) Laboratory sample: - The quantity of coal obtained by reducing a gross sample by following a specified procedure for laboratory testing. (8)Sample di remainder rejected. ion: - The process whereby a part of the sample is retained and the (9)Sample reduction: - The process of crushing or grinding the sample to reduce the particle size and of mixing and sample-dividing in successive stage. Coal sample taken from (1)Conveyers (2) Wagons during loading or unloading (3) Ships during loading or unloading (4)Stock pile (5) Loaded wagons (6) Loaded ships (7)Seam in situ Sampling scoop for collect coal sample Fo,2 Sauruno Scour (Cansorry Ske ano Th) Tense ae a= Page 3 of 8 DKNumber of sub-lots / gross samples Weight of the lot (MT) | No. of sub-lots / gross samples Up to 500 7 2 | 501 to 1000 3 1001 to 2000 4 2001 to 3000 5 Over 3000 6 Weight of gross sample | S.No. | Sample “| Coal, Run of mine | Coal, Large | Coal, Small Weight of gross sample, Min 350 kg 175 kg 75 kg 2 | Weight of increment, Approx 5 kg 5 kg 5 kg. eo Numbers of increments, Min 70 35. 15 Selection of wagons A minimum of 25% of the wagons shall be selected at random from the sub-lot and to ensure the randomness of selection the procedure may be followed. A set of random numbers are given in table. Having selected the set, any one numeral shall be chosen from it at random. Starting from the selected numeral and continuing on with the numerals in any direction, right of left, up or down, the succeeding numerals shall be copied out one y one till the numerals copied is equal to the numbers of wagons to be chosen. The numerals which are greater than the size of the sub-lot or which have already occurred shall be omitted. The numerals noted down in this manner shall then be arranged in the ascending order of magnitude. Page 4 of 8 DKRandom numbers table | 24 15 40 49 36 52 43 42 23 57 48 19 21 16 02 10 54 41 31 27 26 38 18 08 33 20 09 46 14 sa 47 55 39 37 03 45 07 11 13 51 01 44 28 a5 06 34 Be 59 32 29 56 | 30 60. 17 58 be} 04 22 50. 0s Exampl: Suppose there are 60 wagons in a lot of approximately 3600 tonnes. According to table, this would require the division of the into 6 sub-lots, each consisting of 10 wagons of approximately 600 tonnes. Considering any particular sub-lot, if 25 % of the wagons have to be select at random for drawing the gross sample, it shall imply that 3 wagons have to be selected out of 10 in the sub-lot. Suppose random numeral is 06. Proceeding further in any direction, say up, and omitting the numeral which is greater than 10, the numerals encountered are 06, 09 and 02. Arranging them in one order, the sequence 02, 06 and 09 obtained for first sub- lot. Thus select wagons for other 5 sub-lots. Reduction of gross sample :- The place set apart for the treatment of gross sample shall preferably be enclosed, roofed over, cool and free from draughts. Where this is not possible, precautions shall be taken against loss of fine wind-borne sample, contamination with moisture and contamination with foreign matter. Select a hard and clean surface free of cracks for sample mixing, quartering and other operations. Do not let cinders, sand, chippings from the floor or any other foreign matter get into the sample. Page Sof 8 DKRun —of-mine, Coal Large Coal Small Coal Original Original >5cm “Sem ‘Sem ‘Sem Preferably Preferably Mechanical Mechanical v * and 4rejected sawsreares a] \ : after carefully e L/ rmiing coning ane \J quartering, Y 7 land 3 rejected 2and 4 retained 1 7 after carefully I ring coingane J quartering Ts "12.5 mm by “12.5 mm by jaw ctsher jaw crusher jaw crusher + t ¥ -3.35 mm by -3.35 mm by “3.35 mm by Palmac type Palmactype Palmac type of mill of mill of mill 7 7 x 7 1 z Reduced repeatedly Reduced repeatedly 2kg sample 2 kg sample 2 kg sample v ¥ + Pass through Pass through Pass through: 212 micron 212 micron 212 mieron leve we sleve + + v | 1.5 kg sample 1.5 kg sample 1.5 kg sample Page 6 of 8 DKMoisture sample:- At first stage of reduction of the gross sample to 12.5 mm, collect 5 kg sample by not less than 10 approximately increments, while the coal is being discharged from the jaw crusher of after it has been collected in a heap. Reduce this sample to as near to 1 kg as possible and put the sample so reduced in an air-tight tin and seal it without delay. Laboratory sampl The sample ground to pass through 212 micron IS Sieve. From the ground material, 1.5 kg shall be taken which shall constitute the laboratory sample. Each laboratory sample shall be divided into three equal parts, one for the purchaser, and another for the supplier and the third for the reference. The sample shall be kept in glass or polyethylene containers and shall be sealed and marked properly. In grinding the sample to pass 212-micron IS Sieve, it has been found that unnecessarily fine grinding is harmful. The ground coal should have following approximate particle size distribution: 1. Passing 212-micron IS Sieve and retained on 125-micron IS Sieve 35% 2. Passing 125-micron IS Sieve and retained on 63-micron IS Sieve 30-35% 3. Passing 63-micron IS Sieve Remainder Reporting of test result: 1, When a composite sample has been tested, only one test result shall be available and that result shall be reported as the value of the characteristic for the lot. 2. When only two laboratory samples have been analyzed individually from a lot, the average of the two available test results shall be reported as the value of characteristic for the lot sampled. 3. When three or more laboratory samples have been tested individually, the average (X) and the range (R) of the test results shall be calculated as follows for assessing the average level and the extent of variation in the average: If for any characteristic, Xs, Xa, - Xnare the results of analysing n laboratory samples, than Page 7 of 8 DKX= Xa, Xo, Xa / R= The difference between the maximum and the minimum of the test results The average level of the characteristic in the lot shall be reported as equal to X. 4. The limits for variation of the average quality in the lot shall be reported as X + hR Where h is constant , the value of which depends upon the number of laboratory sample. Number of laboratory | Value of the constant samples analysed (n) (h) 3 1.30 4 0.72 5 0.51 6 0.40 Rejection of suspect test result: Arrange all the test results obtained by analysing n laboratory samples in the ascending order of magnitude and designated them as x1, x2, Xe, when xis the smallest and xy is the largest test results. If x is suspect, calculate the value of K; from Ki = (Xn ~ Xna) / (Xn ~ Xa) Ifx; is suspect, calculate the value of K2 from Ko= (x2 - x1) / (Xn ~ x1) If the calculated value of Ki or K2 exceeds the corresponding one given in table, the suspect result shall be rejected, otherwise not. Sample size (n) Value of Ki or Ke 3 0.941 4 0.765 5 0.642 6 0.560 Example :- Test results 28.9, 26.9, 26.8, 26.7,26.1 Suspected test result is 28.9 Test result in ascending order 26.1, 26.7, 26.8, 26.9, 28.9 K,=(28.9- 26.9) / (28.9-26.1) =2.0/2.8=0.714 Since the value of exceeds the corresponding tabulated value 0.642 for sample size 5, the test result shall be rejected. Page 8 of 8 DK- PROXIMATE ANALYSIS OF COAL IS : 1350 (PART-1) Page 1 of 8 DKDetermination of moisture Total moisture: - The coal which has been exposed to contact with water in the seam or in a washery, or coal and coke, wetted by rain, may carry free or visible water. This water plus the moisture within the material, is referred to as total moisture. Methods: - (a) Indirect method (1)Drying in air ( one stage) > Method-1(at 200 °C) for coke sample crushed to pass 16 mm IS sieve > Method-2 for coal(at 108 + 2°C) for laboratory sample of coal crushed to pass 212-micron IS sieve (2)Drying in air (two stage) (3) Drying in a minimum-free-space oven( for coke) (b)Direct method D ir (two stage) / Determination of total moisture Stage one (Air-Drying) (1)This method applies to a moisture sample of 1 kg coal crushed to pass a square mesh screen of 12.5 mm. (2)Use non-corrodible trays approximately 1000 cm? in are and large enough to hold the entire sample. (3)Weight empty tray and then tray plus sample to the nearest 0.5 g (4)Spread the material evenly on the tray. (5)Allow the material in the tray to air-dry at atmospheric temperature in a well ventilated place free from dust. (6)Take the drying to be complete when the change in mass during an hour is less than 0.1% of the sample. Record this mass. (7)Also follow this procedure for sample container or sample bag. (8)Calculate % moisture by loss in mass method for both sample and sample container or sample bag as example formulas. Page 2 of 8 DKM1 = Empty tray weight, M2 = Tray weight + sample weight before air drying M3 = Tray weight + sample weight after air drying (M2-M3) % Moisture= X = ————— * 100 (M2-M1) (9)Air drying moisture = Moisture of sample + Moisture of sample container. Stage two (Oven-Drying) (1)For this method use ventilated drying oven, weighing vessel (40 cm? in area) made of silica, glass or stainless steel with cover. (2)Crush the air-dried material to pass 2.90 mm IS sieve. (3)Heat the empty vessel at 108 + 2 °C and weigh after cooling for 20 minutes. (4)Spread uniformly in the weighing vessel about 10 g of the crushed material and weigh. (5)Heat the uncovered vessel in the drying oven at a temperature of 108 + 2 °C until there is no further loss in mass. (6) This normally takes 1.5 to 3 hours. (7)Replace the cover, cool in a desiccator for 20 minutes and weigh. (8) Calculate % moisture by loss in mass method. If Air-Drying moisture is X% and Oven-drying moisture is Y%, than %Total Moisture = X + Y*(100-X/100) Drying in air (one stage-method-2) / Determination of inherent moisture (1)This method applies to laboratory sample of coal crushed to pass 212-micron IS sieve. (2) Weighing vessel (approximately 10 cm? in area) made of silica, glass or stainless steel with cover. (3)Heat the empty vessel at 108 + 2 °C and weigh after cooling for 20 minutes. (4)Spread uniformly in the weighing vessel about 1.5 g of the crushed material and weigh. Page 3 of 8 DKIDetermination of volatile matter DK (5)In weighing vessel, so that there is not more than 0.15 g of the material per cm? area. (6)Heat the uncovered vessel in the drying oven at a temperature of 108 + 2 °C until there is no further loss in mass. (7)This normally takes 1.5 to 3 hours. (8)Replace the cover, cool in a desiccator for 20 minutes and weigh. (9) Calculate % moisture by loss in mass method. Moisture Precision percentage Reparability Reproducibility Up to 3.0 0.1 units 0.2 units Over 3.0 3.0% of the arithmetic | 6.0 % of the arithmetic mean of the duplicate_| mean of the duplicate values : values In this method used equipments and vessels should be as per IS 1350 (Part-1). For reference see images of crucible and stand as below. (1) Use air-dried material passing through 212-micron IS sieve. (2)Heat the covered vessel with stand in muffle furnace at a temperature of 900 + 10 °C for 7 minutes. (3)Remove crucibles wit stand from the furnace, cool the crucibles first on metal for 5 minutes and then in a desiccator for 10 minutes. (4)Weigh empty crucible with lid and weigh accurately into crucible 1.00 to 1.01 g of sample. (5)Replace the lid and tap the crucible on a clean hard surface until the sample forms a layer of even thickness. (6)Heat the covered vessel with stand in muffle furnace at a temperature of 900 + 10 °C for 7 minutes. (7)Remove crucibles wit stand from the furnace, cool the crucibles first on metal for 5 minutes and then in a desiccator for 10 minutes. (8) Weigh crucible with lid accurately. (9)Calculate the volatile matter of the sample on air-dried basis as follows: Page 4 of 8(“\ Y ey m4] | | | | N Ni N N N ) N is SUMEESEIN Lo ‘ All dimensions in millimetres, 6B Sultable for Making Several Determinations at @ Timo All dimensions ia millisetees, Fro. 5 Stuica Cavers avo Lip tet tomes ane Page 5 of 8 DK(m2-™3) % VM =—————._ *100- M0 (m2-™1) Where MO = % moisture in the sample on air dried basis; M1 = mass in g of empty crucible and lid; M2 = mass in g of crucible plus lid and sample before heating; M3 = mass in g of crucible plus lid and sample after heating. Volatile Matter Precision __percentage Reparability Reproducibility For coals 1.0 % of the arithmetic 1.0 % of the arithmetic mean of the duplicate | mean of the duplicate values determinations For coke 0.2 units 0.4 units Determination of ash (1)In this method used equipment's and vessels should be as per IS 1350 (Part-1). Muffle furnace up to 950 °C and dish of silica, porcelain or platinum, 10 to 15 mm deep, such a size that, with the amount of sample used, the spread does not exceed0.15 g/cm? Use air-dried material passing through 212-micron IS sieve. (2) Heat the covered vessel with 900 °C for 10 minutes. (3)Remove crucibles with from the furnace, cool the crucibles first on metal for 5 minutes and then in a desiccator for 10 minutes. (4) Weigh empty crucible without lid and weigh accurately into crucible 1.00 to 2.00 g of sample according to size of crucible. (5) Distribute the material so that the spread does not exceed 0.15 g/cm?. Page 6 of 8 DKI(6)Insert the uncovered dish into the muffle furnace at room temperature. (7)Raise the temperature to 500 °C in 30 minutes and to 815+10°C in further 30 to 60 minutes. (Cover the dish with its lid if the ash is light and fluffy.) (8)Maintain at this temperature for 60 minutes. (9)Remove the dish from the muffle furnace and allow to-cool, first on a cold metal slab for 10 minutes and finally in desiccator for 15 minutes. (10) Weight the dish and re-ignite at the same temperature until the change in mass of the ash is less than 0.001 g. (11) Calculate the ash of the sample follows: (m2-™ma) % Ash =. * 100 (m2-™4) Where M1 = mass in g of empty dish; M2 = mass in g of dish and sample; M3 = mass ing of dish and ash; M4 = mass in g of dish after brushing out the ash and on reweighing Ash Precision percentage Reparability Reproducibility Up to 10.0 0.2 units 4.0 units Over 10.0 2.0% of the arithmetic | 3.0 % of the arithmetic mean of the duplicate | mean of the duplicate values values Page 7 of 8 oKReporting of results Conversions [To obtain: [multiply [Air Dry Dry Basis [As Received [AR by: |(100 - tm38) /(460- Tm4)_|200 /(100 - Tn36) |- [AD by: | [200/ (200 = 1en%) [(200 = Trn96) /(400 - im86) DB by: _|{100- 1m) 700 - [(200 - Tm96) /100 DAF, multiply DB by 100/(100-A)] As Received (AR): includes Total moisture (Tm) Air Dried (AD): includes Inherent moisture (Im) only Dry Basis (DB): excludes all Moisture Dry Ash Free (DAF): excludes all Moisture & Ash. “The Proximate Analysis of any coal ie the % contents of Moisture, Ash (A), Volatile Matter (VM), Fixed Carbon (FC) - also Sulphur (5) and Calorific Value (CV) - ean be expressed on any of the above bases. Example: AR AD DB, DAF Tr 71.00 - = = in 2.00 2.20 = : eh (A) 22.00 23.21 73.50 S vM '30.00 33.03 33.70 33.0 FC. 56.00 ‘51.75 52.80 61.0 Sulfur (3) 1.00 1.10 2.12 = ecy "3000, ‘3809 5989) = ARB TO. : "AS RECEIVED BASIS | AIR DRY BASIS: DRY BASIS DRY ASH FREE Tm 6.56 a S = ma 0.80 035 = = Ash (A) 7.74 8.22 328 = VM 35.32 37.50 37.80, aa2a FC 36.14 59.60 60.08 65.51 ‘Sulfur (S) 1.39) 148 1.49 - ‘acy, 7035, 7467, 7527 = ADBTO ‘AS RECEIVED BASIS | AIR DRY BASIS: DRY BASIS. DRY ASH FREE. Tm 656 : 5 = en (0.80 O85 = S Ash (A) 774. 322 329 = VM 35.32 37.50, 27.80 aa22 FC. 56.14 59.60 60.08. 65.51 Sulfur (5) 1.39 1.48, 2.49 = cv 7033, 7486. 7526 = DBTO. ‘AS RECEIVED BASIS | AIR DRY BASIS DRY BASIS. DRY ASH FREE im 6.56 = = = en 0.80 0.85 = = “Ash (A 7.75, B22 229) = VM 35.32 37.50, 37.80 aa.22 FC 56.14 59.60 60.08. 65.51 Sulfur (S) 1.39 ag 1.49 = cv 7032, 7466 7526 = Page 8 of 8 DK