feat Section 4 Malt Analytica-EBC ‘Method 4.1 41 Sampling of Malt Refer to Section 0 (Safety) for relevant waming and 2 Reference safety precautions. EBC Method 3.1 (Barley: Sampling of Barley). 1 Scope Proceed according to the instructions given in EBC ‘This document deals with methods for sampling malts. Method 3.1. ‘September 1997 Page 1 of 1Analytica-EBC Section 4 Malt Method 4.2 4.2 Moisture Content of Malt Refer to Section 0 (Safety) for relevant warning and safety precautions. 1 Scope L.1 The determination of the moisture content of all malts by loss in mass on drying under specified conditions. 1.2 The ISO Method for moisture content of grain (IS0712-1985)which is used for barley (EBC Method 3.2) must not be used for malt as the conditions of dying are such that chemical condensations occur in which water is formed as a product of reaction. 2 Field of Application The method can be applied to all malts. 3 References 3.1 EBC Method 1.1 (Care and Adjustment of Apparatus: Buhler MiagDisc Mill, DLFU). 3.2. EBC Method 3.2 (Barley: Moisture Content of Barley 3.3. EBC Method 4.1 (Malt: Sampling of Malt) 4 Principle 4.1 The sample is milled to form a fine grist. 4.2 The grist is dried in an oven that has been previously standardized. 4.3. The moisture content of the malt is calculated from the loss in mass during drying. 5 Reagent Desiccant of self indicating silica gel. 6 Apparatus 6.1 Mill, Bithler Universal Laboratory Disc Mill (ype DLFU) set to a gap of 0,2 mm to give a fine grind. Instructions for the use of the mill are given in EBC Method 1.1. 6.2 Oven, fitted with automatic control capable of holding temperature within + 0,5 °C and large enough to hold all samples on one shelf in such a manner that no sample is outside the area indicated by test to give comparable results in duplicate samples. Standardize by placing weighed duplicate samples in the oven at 105 to 106 °C and dry for 3 h+5 min. Allow to cool ina desiccator for at least 20 min to room temperature, weigh and redry 1 h longer. If oss of moisture is more than 0,10 2/100 g sample raise temperature 1° C and again test with new duplicate samples. Take as standard the lowest temperature below 107 °C to give a moisture content that after 3 h drying is within 0,10 g/100 g sample of the value obtainable at the same temperature within 4 h. Keep the oven venti- lation open and the oven door closed during the entire 3h drying period. 6.3 Moisture dishes, of metal construction (e.g. aluminium), about 50 mm diameter and not more than 20 mm depth and supplied with tightly fitting lids. 6.4 Desiccator, containing a thick perforated plate of metal or porcelain, 65 Balance, accuracy + 0,0005 g. 7 Preparation of Samples ‘See EBC Method 4.1. 8 Procedure 8.1 Using a DLFU mill setting of 0,2 mm finely grind about 20 g of malt. Mix thoroughly and im- mediately place about 5 g of ground sample in a clean, dry moisture dish, previously tared to 0,001 g. Close the dish and weigh immediately to 0,001 g. 8.2 Remove the cover from the dish and place in the preheated oven for 3 h +5 min at the standardized temperature, starting the timing from the point when the standardized temperature is regained. Replace the lid and remove from the oven. Allow to cool in a desiccator for at least 20 min to room temperature. 8.3 Reweigh the dish and contents to 0,001 g. Page 1 of 2Analytica-EBC 9 Expression of Results 9.1. Calculation 9.1.1 Calculate the moisture percentage (M) of the sample using the formula: where: ‘W, =mass in g of sample before drying 'W, = mass in g of sample after drying 9.1.2 Report the moisture percentage of the sample to one decimal place. 9.2 Precision ‘The precision values below % (nvm) were determined from the data of a collaborative trial carried out by the EBC Analysis Committee in 1992. Between 17 to 26 laboratories analysed malt samples at 6 levels. These precision values were obtained by the former method which stipulated the use of copper sulphate for standardizing the oven. Range s Rog 3.81073, 0,13 06 Section 4 Malt Method 4.2 10 Bil jography Bénard, M., Journal of the Institute of Brewing, 1992, 98,81 Page 2 of 2 October 2000Analytica-EBC Section 4 Malt Method 4.3.1 43.1 Total Nitrogen of Malt: Kjeldahl Method Refer to Section 0 (Safety) for relevant waming and safety precautions. 1 Scope ‘The determination of the total nitrogen content of malt by a Kjeldahl procedure. 2 Field of Application 2.1 ‘The method can be applied to all malts. 2.2 The results of the Kjeldahl method and the al- temative Dumas combustion method (EBC Method 4.3.2) differ, the latter giving somewhat higher results. It is of the utmost importance to specify the method in reporting (see 7.2) 3 Reference EBC Method 3.3.1 (Barley: Total Nitrogen of Barley, Kjeldahl Method). 4° Principle 4.1 Nitrogenous compounds in the malt are di- ‘gested with hot sulphuric acid in the presence of cata- lysts to give ammonium sulphate. 4.2 The digest is made alkaline with sodium hy- droxide solution and ammonia so released is distilled into an excess of boric acid solution. 4.3. The ammonia is titrated with standard acid so- lution. October 2004 5 Procedure Proceed according to instructions given in EBC Method 3.3.1 6 Precision ‘The precision values given below (% m/m dry mat- ter) were determined from the data of a collaborative trial, carried out by the EBC Analysis Committee in 1990, in which 12 to 16 laboratories analysed malt samples at 6 levels in the range 1,56 to 1,87 % m/m. Range (% mim) _r4,(Yemim) _R,, (Jo m/m) 1,56 to 1,87 0,05 0413 7 Bibliography 7.1 Bénard, M., Journal of The Institute of Brew- ing, 1992, 98, 81. 7.2 Buckee,G.K., Journal of The Institute of Brew- ing, 1994, 100, 57. Page | of |Analytica-EBC _ Section 4 Malt DEL ORENA EL Method 4.3.2 4.3.2 Total Nitrogen of Malt: Dumas Combustion Method Refer to Section 0 (Safety) for relevant warning and safety precautions. 1 Scope ‘The determination of the total nitrogen content of malt by a combustion method based on the Dumas princi- ple. 2 Field of Application 2.1 The method can be applied to all malts. 22 The results of the Dumas combustion method and the altemative Kjeldahl method (EBC Method 4.3.1) differ, the latter giving somewhat lower results. It is of the utmost importance to specify the method in reporting (see 7.2). 3 Reference EBC Method 3.3.2 (Barley: Total Nitrogen of Barley, Dumas Combustion Method). 4 Principle 4.1 The sample is combusted in the presence of oxygen at about 1000 °C to give oxides of nitrogen which are then reduced catalytically to nitrogen, Other products of combustion are removed by selective ad- sorption, or separated from elemental nitrogen on a chromatographic column, 4.2. The nitrogen gas is measured with a thermal conductivity detector. October 2004 4.3 Thenitrogen content is calculated from the de~ tector response. The detector is calibrated by measur- ing the response given by an organic compound of known nitrogen content. 4.4 Automated combustion analysers for nitrogen are available which rely on either helium or carbon dioxide as the carrier gas. 5 Procedure Proceed according to the instructions given in EBC Method 3.3.2. 6 Precision The precision values given below (%e m/m dry mat- ter) were determined from the data of a collaborative trial, carried out by the EBC Analysis Committee in 1994, in which 16 to 17 laboratories analysed malt samples at 4 levels in the range 1,23 to 1,86 % m/m. Range (% m/m) 1,23 to 1,86 1,5 (% m/m) 0,063 R,, (4b mim) 0,116 7 Bibliography 7.1 Johansson, C.-G., Journal of The Institute of Brewing, 1996, 102, 249. 7.2 Buckee,G.K.,Joumal of The Institute of Brew- ing, 1994, 100, 57. Page 1 of 1Analytica-EBC Refer to Section 0 (Safety) for relevant warning and safety precautions. 1 Scope ‘The determination of average com weight as a measure of barley quality. 2. Field of Application ‘The method applies to all malts. 3 Reference EBC Method 3.4 (Barley: Thousand Com Weight of Barley). September 1997 Section 4 Malt Method 4.4 44 Thousand Corn We ht of Malt 4 Principle 4.1 Thenumber of coms in a sample of known mass is counted, 4.2 ‘The mass (g) of 1000 coms of malts calculated. 5 Procedure Proceed according to the instructions given in EBC Method 3.4. Page 1 of 1Analytica-EBC Section 4 Malt Method 4.5.1 45.1 Extract of Malt: Congress Mash Refer to Section 0 (Safety) for relevant warning and safety precautions. 1 Scope 1.1 The determination of the potential of malt for producing wort solubles by a standard mashing pro- ‘gramme. 1.2 This procedure is also used for the determina- jon of saccharification rate, odour, speed of filtra- tion, pH of wort, colour, viscosity of wort, soluble nitrogen content and free amino nitrogen content. 2 Field of Application ‘The method can be applied to all malts below 15 EBC colour units. 3 References 3.1 International Standard, Water for analytical laboratory use ~ Specification and test methods, ISO 3696:1987 E). 3.2 EBC Method 1.1 (Care and Adjustment of Ap- paratus: Care and Adjustment of Apparatus: Bihler Miag Disc Mill, DLFU). 3.3. EBCMethod 4.7.1 (Malt: Colourof Malt: Spec- trophotometric Method). 3.4 EBC Method 4.7.2 (Malt: Colour of Malt: Visual Method). 3.3 EBC Method 8.2.1 (Wort: Specific Gravity of, ‘Wort using a Pyknometer) or EBC Method 8.2.2 (Wort: Specific Gravity of Wort using a Density Meter). 3.6 EBC Method 8.3 (Wort: Extract of Wort). 4 Principle 4.1 The extract content of malt is determined after mashing and filtration, from the extract content of resulting wort, by the determination of the specific gravity of the wort using a pyknometer or a density meter. ‘October 2004 4.2 The extract content of the wort is obtained from the specific gravity by means of the sugar table (Plato table) for 20 °C. 5 Reagents 5.1 During the analysis, unless otherwise stated, use water of at least grade 3 as defined in ISO 3696:1987 ®. 5.2. Iodine solution, 0,01 molfitre. Dissolve 1,27 g of iodine crystals and 2,5 g of potassium iodide in water and dilute to 500 ml, Prepare a fresh iodine so- lution every month, Store in a brown bottle and in the dark. 6 Apparatus 6.1 Biihler Miag dise mill, DLFU (Bithler GmbH, Germany; see the List of Suppliers) as specified in EBC Method 1.1. The gap between the grinding discs is 0,20 mm. 6.2 Balance, accurate to 0,1 g under load of 750 g. 6.3 Mash beakers and stirrers of stainless steel, pure nickel or brass (but not copper). Brass beakers must be cleansed only by washing with water. 6.4 Mashing bath, a water bath with suitable heat- ing and temperature control. The speed of stirring must be between 80 to 100 rpm. 6.5. Glass rod, length 250 mm and 8 mm diameter. 6.6 Conical flasks, 500 ml with a mark at 100 ml 6.7 Funnels, 200 mm diameter with a stem which reaches to the bottom of the conical flask. 68 Fluted filter papers, 320 mm diameter. Schleicher and Schuell No. 597 1/2, Macherey-Nagel & Co. No. 614 1/4, RC. Binzer No. 12 and 53 or equivalent. 6.9 Pyknometer or density meter. See EBC Method 8.2.1 or 8.2.2. Page 1 of 3Analytica-EBC 6.10 Water bath at 20,00 + 0,05 °C, of a depth so that the pyknometers are immersed with the calibra- tion mark below water level. 6.11 Balance accurate to 1 mg, 6.12 Porcelain spot plate. 6.13 Glass rod, about 3 mm in diameter. 7 Preparation of Samples 7.1 Take duplicate quantities of approximately 55 g of malt and grind in the DLFU disc mill. Use the method specified in EBC Method 1.1. 7.2. Transfer each portion of ground malt to amash beaker and mix well with a spatula, Take portions for moisture determination and weigh a portion of 50,0 g in the mash beaker. 8 Procedure 8.1 Mashing 8.1.1 Attemperate the mashing bath to 45 °C. 8.1.2 Stir 200 ml of water at a temperature of about 46 °C into each beaker with a glass rod and avoid balling. Ensure that the temperature in the mash is exactly 45 °C. 8.1.3 Place the beaker immediately in the mashing bath and set the stirrers in motion. Maintain the tem- perature of 45 °C in the mash for exactly 30 min. 8.1.4 Raise the temperature of the mash 1 °Ca minute for 25 min. 8.1.5 When the temperature reaches 70°C add a fur- ther 100 ml of water at 70°C. Measure the saccharifi- cation rate from this point. Section 4 Malt Method 4.5.1 8.1.7 Maintain the temperature of 70 °C for 1 h, Cool the mash to room temperature in 10 to 15 min, 8.1.8 Wash the stirrer with a small amount of water, dry the outside of the beaker and adjust the contents of the beaker to 450,0 + 0,2 g by addition of water. 8.2 Filtration 8.2.1 Stir the contents of the beaker thoroughly with a glass rod and empty immediately and completely into a filter. Ensure that the filter paper does not project over the edge of the funnel. 8.2.2. Retum the first 100 ml of the filtrate to the fun- nel. Take a portion for colour measurement. Use the procedure specified in EBC Method 4.7.1 or 4.7. Retum the portion into the flask after colour meas- urement, 8.2.3. Stop filtration when the cake appears dry, or, if slow filtration occurs, after 2 h. 8.2.4 Note the speed of filtration of the mash during the filtration stage. Express the speed of filtration as “normal” ifthe filtration is complete within I hour. If it is longer than 1 hour, express it as “slow”, No other expressions must be used. 8.2.5 Note the odour of the mash organoleptically. Express the odour as “normal” when it corresponds to the type of malt analysed. When the normal aro- matic smell of a Munich malt is absent record it as “non aromatic”. In addition note any foreign odours. 8.3. Determination ofthe specific gravity of the wort See EBC Method 8.2.1 or 8.2.2. 9 Expression of Results 9.1 Calculation 8.1.6 Transfer a drop of the mash to a spot on the porcelain plate and add a drop of iodine solution 10 minutes after the addition of the water. Repeat this test at 5 minute intervals until saccharification is com- plete: that is when a clear yellow spot is obtained. If saccharification is not complete after 1 hour, stop the test. Express the result in minutes and report in peri- ods of five minutes, e.g. under 10 minutes, 10 to 15 ‘minutes and so on. October 2004 9.1.1 Calculate the extract content of wort. See EBC Method 8.3. 9.1.2 Calculate the extract content of malt according to the formulae: P(M+800) 2) E,%om)- BE E, - 100 b) E, [% (wm) = 99 -H Page 2 of 3Analytica-EBC Section 4 Malt Method 4.5.1 where E, = the extract content of sample, in % (m/m) E, = the extract content of dry malt, in % (m/m) the extract content in wort, in % Plato M = the moisture content of the malt, in % (m/m) 800 = the amount of distilled water added into the ‘mash to 100 g of malt, in ml 9.1.3. Express the result in % (m/m) to one decimal place and then calculate as percent dry matter (% d.m.), 9.2 Precision ‘The precision values given below (% d.m.) were d termined from the data of a collaborative trial carried out by the EBC Analysis Committee in 1992. Partici- pating laboratories analysed malt samples at 3 levels in the range 79,3 to 81,4 % dam. No. of Range 1, Laboratories (% Fine grind 171027 79,3t081.4 058 12 October 2004 Page 3 of 3Analytica-EBC Section 4 Malt Method 4.6 46 Hot Water Extract of Malt: Constant Temperature Mash Refer to Section 0 (Safety) for relevant warning and safety precautions. 0 Introduction For certain parts of the procedure alternative techniques may be followed which relate to the use of specialised mashing baths where the mash is stirred continuously. The rate of stirring must be such as to Just maintain the mash in suspension and excessive speeds must be avoided. Under excessive stirring conditions higher values for extract, colour and viscosity may be obtained for some malts. 1 Scope 1.1 The determination of Hot Water Extract of ale, lager and distilling malts using a constant temperature infusion mashing procedure of a coarsely ground sample (0,7 mm). 1.2 The wort produced by this mashing procedure isused for ancillary analyses, such as the determination of saccharification rate, colour, viscosity of wort, soluble nitrogen content, free amino nitrogen content, fermentability, and pH. 13. Fine/coarse difference may be derived by simultaneously determining the Hot Water Extract of ‘a more finely ground grist (0,2 mm) from a second test portion of the malt sample. 2 Field of Application The method can be applied to all ale, lager and distilling malts, below 15 EBC colour units. 3 References 3.1 EBC Method 1.1 (Care and Adjustment of Apparatus: Bilhler Miag Disc Mill, DLFU). 3.2 EBC Method 4.1 (Malt: Sampling of Malt), 3.3. International Standard, Water for Analytical Laboratory Use, Specification and Test Methods, ISO 3696, 1987 (E). 4 Principle 4.1 Maltis milled to produce a grist. 4.2 Soluble material within the grist is extracted with hot water during mashing. 4.3 At the end of mashing, insoluble material is removed by filtration leaving a clear wort. 4.4. The specific gravity of the clear wort is determined at 20°C and from this value the Hot Water Extract is calculated. 5. Reagents S.1 Unless otherwise stated, use only reagents of recognised analytical grade and water of atleast grade 3 as defined in ISO 3696: 1987. 5.2 Iodine solution, 0,02 moVlitre iodine in water. 6 Apparatus 6.1 Mill. A Bithler Universal Laboratory Disc Mill (type DLFU) must be used for the determination. Feeler gauges, one of 0,2 mm and one of 0,7 mm, are required for adjusting the disc gaps. Instructions for the use of the mill are given in EBC Method 1.1. 6.2 Water bath. A bath sufficiently sensitive to ‘maintain the mash temperature at 65 +0,5°C and fitted with a mechanical stirring device and false bottom to censure an even temperature distribution in the loaded bath. The water level must correspond with or be higher than the level of the mash. Magnetic followers for use in this bath must be bar shaped and 45 mm in length. 63 Balances. For grist an accuracy of + 0,05 g, and for specific gravity measurement an accuracy of £0,001 g is required. 64 Mashing beakers, 600 ml, stainless steel. 6.5 Hot water dispenser, glass, aluminium or stainless steel construction, 360 + 10 ml. Page 1 of 3