DIN EN 13040-2008 Soil improvers and growing media - Sample preparation for chemical and physical tests determination of dry matter content moisture content and laboratory compacte.pdf

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1、January 2008DEUTSCHE NORM English price group 11No part of this standard may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 65.080!$K 25 mm and /o

2、r flexible fibres 80 mm shall be physically reduced in equal parts and as few times as are necessary to be 25 mm and 80 mm for flexible fibres. Thoroughly mix the whole sub-sample with the broken particles that have been retained on the sieve taking care to minimize physical damage to the sample as

3、a whole. Any observed foreign material such as plastic, metal or glass shall be recorded. Include this observation in the test report (13). NOTE This test sample is suitable for physical methods of analyses. 8.5 Test sample passing through a 20 mm square aperture sieve Take about 5 l of test sample

4、(8.3) and using a scoop, pass the material through a 20 mm screen and agitate gently if required. If more than 10 % volume is retained on the screen then the procedure shall be inappropriate to the material under test. If less than 10 % is retained, this material shall be broken down in equal parts

5、and as few times as necessary to permit the entire sample to pass through the sieve. EN 13040:2007 (E) 7 9 Preparation of the dried ground (or otherwise size reduced) test sample 9.1 Apparatus 9.1.1 Grinding apparatus, able to grind the whole sub-sample without contamination, e.g. cutting mill, ultr

6、acentrifuge mill, pestle and mortar. 9.1.2 Screen or sieve, of diameter 2 mm round hole in accordance with ISO 565. 9.1.3 Ventilated oven, capable of maintaining a temperature of 75 C 5 C or other means of sample drying 9.2 Procedure Dry a portion of the test sample (8.1) until it crumbles to the to

7、uch, using one of the following methods: a) at 75 C 5 C in a ventilated oven; or b) where it is necessary to prevent losses by conventional oven drying methods, freeze drying or milling in the presence of dry ice. It shall be recorded with the results when a technique like the type presented in b) i

8、s used. The particle size shall be reduced so that the dried sample is able to pass through the 2 mm mesh sieve (9.1.2). It may be necessary to chop, cut or otherwise reduce large particles prior to milling. For samples that can be milled, ensure that during grinding no heat is generated and no inad

9、vertent sub-sampling occurs, in that some particle sizes are excluded from the milling process either as dust or as excessively hard particles. For samples that cannot be milled, e.g. expanded foam, other means for reducing the particulate size such as knives or scissors may be used. 10 Determinatio

10、n of dry matter content 10.1 Apparatus 10.1.1 Sample tray, capable of holding no less than 50 g of the sample and constructed of material thermally stable up to 150 C. 10.1.2 Drying oven, ventilated, fan assisted, capable of holding sample trays (10.1.1) and maintaining 103 C 2 C. 10.1.3 Analytical

11、balance, with a scale interval of 0,01 g and a capacity of weighing 500 g. 10.2 Procedure Determine the mass of the empty tray (mT), by heating it to 103 C in an oven and cool it in the desiccator. After cooling weigh the tray to get (mT). Transfer approximately 50 g of the mixed prepared sample (8.

12、1) in the tray (10.1.1), spread to an even depth not exceeding 2 cm. and without delay weigh to an accuracy of 0,01 g. (mW). Place the tray in the oven (10.1.2) and dry until the difference between two successive weighings does not exceed 0,1 g. Record the dry mass of the sample and tray (mD). NOTE

13、Loss of volatile matter Drying the sample at 75 C and 103 C may lead to losses of certain volatile components such as free ammonia. Therefore, where these components are to be determined the analyses shall be performed on the un-dried sample. EN 13040:2007 (E) 8 11 Calculation 11.1 Dry matter conten

14、t Calculate the dry matter content of the sample, as received, using the following equation: ()()100TWTDM=mmmmD (2) where DMis the dry matter content expressed as a percentage by mass; mWis the mass in grams of the wet sample plus tray; mD is the mass in grams of the dried sample plus tray; mT is th

15、e mass in grams of the empty dry tray. 11.2 Moisture content Calculate the moisture content of the sample as received using the following equation: ()()WDmWT100mmWmm=(3) where Wmis the moisture content expressed as a percentage by mass; mWis the mass in grams of the wet sample plus tray; mDis the ma

16、ss in grams of the dried sample plus tray; mTis the mass in grams of the empty dry tray. 12 Precision - Moisture content The precision of the moisture content measurement of three separately prepared samples should be in accordance with Table B.1. A summary of the results of an interlaboratory trial

17、 to determine the precision of the method in accordance with ISO 5725 1 to 6 is given in Annex B. NOTE The values derived from the interlaboratory trial may not be applicable to concentrations and matrices other than those given. 13 Test report The test report shall contain the following information

18、: a) reference to this European Standard (EN 13040:2007); EN 13040:2007 (E) 9 b) all information necessary for complete identification of the sample; c) percentage by mass of material that has been cut according to clause 8.2; d) method and temperature of drying; e) results of the determination to t

19、he nearest 0,1 % by mass; f) details of any operations not specified in the European Standard or regarded as optional, as well as any factor which may have affected the results. EN 13040:2007 (E) 10 Annex A (normative) Determination of laboratory compacted bulk density A.1 General A.1.1 This annex s

20、pecifies a method to estimate the laboratory compacted bulk density of a laboratory sample of a soil improver or growing media in its “as received state“ and enables a calculated sample weight to be taken, which will accurately represent the required (small) volume of sub-sample as required for anal

21、ysis. A.1.2 This method enables computation and expression of analytical results on a weight in volume basis when results are obtained from analysis of a known weight of sub-sample. NOTE This procedure may be inappropriate for use with wet, sticky or very coarse materials. A.2 Principle Fit a one li

22、tre cylinder with an extension collar, fixed screen/flow beaker and funnel, and fill it with the material. The fixed screen/flow breaker shall be omitted for materials that contain more than 10 % by weight greater than 20 mm in any dimension. Apply compaction, except for very compressible or springy

23、 materials, and weigh the final contents of the cylinder. A.3 Apparatus A.3.1 Test Cylinder A rigid test cylinder as shown in Figure A.1, having a nominal capacity of 1 000 ml 30 ml, and a diameter (d) of 99 mm - 105 mm in accordance with Table A.1. EN 13040:2007 (E) 11 Dimensions in millimetres 123

24、45170 50 mmhd1d60 60Key 1 plunger (for mass see Table A.1) 5 test cylinder 2 supported fall controller d diameter as per Table A.1 3 funnel h height as per Table A.1 4 removable collar d1diameter (d - 5mm) 1 mm Figure A.1 Laboratory compacted bulk density test cylinder, collar, fall controller and p

25、lunger EN 13040:2007 (E) 12 Table A.1 Dimensions of cylinder and corresponding plunger mass Diameter (d) Height (h) Volume Mass of Plunger (mm) (mm) (ml) (g) 99,0 130 1 000 634 100,0 127 997 650 101,0 125 1 001 664 102,0 122 997 678 103,0 120 1 000 692 104,0 118 1 002 706 105,0 116 1 004 720 Toleran

26、ce 1mm 30ml 5g The capacity should be checked by weighing to the nearest 1 g, the empty cylinder and a clear rigid striking plate which is larger than the surface of the cylinder. Fill the cylinder with tap water; apply the striking plate wiping all the exterior surfaces until dry and re-weigh. The

27、difference between the two weighings should equal 1 000 g 30 g. Repeat the test, the difference between the two tests should not exceed 5 g. A.3.2 Removable collar, 50 mm high and of the same internal diameter as the cylinder. A.3.3 Plunger, having a diameter (d1) 5 mm less than both the cylinder an

28、d the collar and having a mass as per Table A.1 to maintain a pressure of 9,17 g/cm2. A.3.4 Funnel with a slope at approximately 60 , with a lower diameter to fit the collar. A.3.5 Supported fall controller: Sieve with a perforated plate or woven wire screen with an approximate 200 mm diameter, 20 m

29、m square apertures or 20 mm mesh size, independently supported approximately 5 mm above the funnel and not connected to it or the cylinder. A.3.6 Analytical balance, with a scale interval of 1 g and a capacity of weighing 5 000 g. A.3.7 Straight edge. A.3.8 Scoop, 250 ml to 500 ml capacity. A.3.9 Tr

30、ipod, to support the fall controller (A.3.5). A.4 Procedure A.4.1 Manually, but carefully homogenize and gently open up any agglomerations or accretions that have resulted from handling or transportation of the sample. (8.1) NOTE Care should be taken to avoid reducing the inherent particle size, whi

31、ch would render the material finer than it was at the time of manufacture. A.4.2 Take about 5 l of the homogenized sample (A.4.1) and using the scoop (A.3.8), pass the material through the screen (A.3.5) gently agitating the material if required. If a more than 10 % volume is retained on the screen

32、then the procedure is inappropriate for the material under test. If a less than 10 % volume is retained, break the material down as described in 8.3. EN 13040:2007 (E) 13 A.4.3 Weigh the empty test cylinder (A.3.1) to the nearest 1 g using the balance (A.3.6). Place the collar (A.3.2) and the funnel

33、 (A.3.4) in position. Place the screen (A.3.5) in position approximately 5 mm above the funnel. A.4.4 Gently spread out approximately 5 l of the screened homogenized material (A.4.2) once again and, using the scoop (A.3.8), take equal amounts of the material throughout the mass, filling the apparatu

34、s by sprinkling the material on top of the screen/flow breaker (A.3.5). Material from each aliquot not immediately passing through the screen may be gently agitated with finger tips to assist the process. Material of each aliquot retained on the screen (but not exceeding 10 % of the total volume) sh

35、all be reduced in size (by halving for a minimum number of times), by hand or with the aid of any simple tool so that it just passes the screen before the next aliquot is applied. A.4.5 Once the apparatus has overfilled, remove the screen and strike off the excess material level with the top of the

36、collar using the straightedge (A.3.7). Gently place the plunger (A.3.3) on the material, leave for 180 s 10 s, then carefully remove the plunger and collar taking care not to vibrate the cylinder, then use the straight edge (A.3.7) to strike off the material level with the top of the cylinder avoidi

37、ng further compaction or disturbance. Weigh the material and cylinder to the nearest 1 g using the balance. Record the result (mX). If the material is very compressible and the top surface is found to be below the top of the cylinder when the plunger is removed after static compaction of 180 s 10 s,

38、 then compaction is inappropriate for the test material. In these circumstances repeat the procedure without applying the plunger to provide a measure of the un-compacted bulk density. Record if the plunger was not used and include that information in the test report (13). Striking off may be diffic

39、ult with very coarse, fibrous, woody or otherwise heterogeneous materials, and large pieces might have to be removed by hand, cut with a pair of scissors or broken off level with the top of the cylinder. Any resulting depressions on the surface of the cylinder should be filled from the remainder of

40、the sample. A.4.6 Repeat 3 times using fresh material each time to obtain a mean value. A.5 Expression of results Calculate the arithmetic mean of all the results obtained using the following equation: xLmmn=(A.1) where mL is the arithmetic mean mass in grams of sample and cylinder; mXis the mass in

41、 grams of the cylinder and sample; mX is the sum of the mass in grams of n replicates where n is the number of replicates. The laboratory bulk density is given by the following equation: L0DmmLV= (A.2) where LDis the laboratory bulk density in grams per litre; EN 13040:2007 (E) 14 mothe mass in gram

42、s of the empty test cylinder; mLis the arithmetic mean mass in grams of sample and cylinder; V is the volume in litres of the test cylinder. A.6 Use and storage of material A.6.1 Because of the physical characteristics of material subjected to this procedure will have been altered, the material used

43、 in this test should not be used subsequently for the determination of any physical properties such as moisture content, particle size analysis or water retention. However, it may be used for other analyses where a dried sample is appropriate. A.6.2 If not for immediate use the sample should be plac

44、ed into a moisture-proof bag or container and the container sealed and stored below 5 C but not frozen. A.7 Precision - Compacted laboratory bulk density The repeatability and reproducibility of the compacted laboratory bulk density content measurement in three separately prepared samples should be

45、in accordance with Table B.2. A summary of the results of an interlaboratory trial to determine the precision of the method in accordance with ISO 5725 1 to 6 is given in Annex B. NOTE The values derived from the interlaboratory trial may not be applicable to concentrations and matrices other than t

46、hose given. A.8 Test report The test report shall contain the following information: a) reference to this European Standard (EN 13040:2007); b) all information necessary for complete identification of the sample; c) results of the determination to the nearest 5 g per l; d) details of any operations

47、not specified in the European Standard or regarded as optional, as well as any factor which may have affected the results. EN 13040:2007 (E) 15 Annex B (informative) Results of an interlaboratory trial to determine moisture content and laboratory compacted bulk density An interlaboratory trial was o

48、rganized in 1995 under the auspices of the European Committee for Standardization, to test the procedures specified in this European Standard. In this trial the number of laboratories given in Table B.1 and Table B.2 determined the moisture content and the laboratory compacted bulk density in three

49、types of samples. Table B.1 Summary of the results of an interlaboratory trial for the determination of moisture content Sample Unfertilized peat perlite Coarse bark Composted straw and domestic sewage Number of laboratories retained after eliminating outliers 18 17 18 Number of outliers (laboratories) 1 2 1 Mean Value % m/m 61,34 60,03 53,31 Repeatability standard deviation, sr % m/m 0,43 0,95 0,69 Repeatability relative standard deviation % 1,99 4,41 3,62 Repeatability limit, r = 2,8sr % m/m 1,22 2,65 1,93 Reproduci