THE INSTITUTE OF BREWING ANALYSIS COMMITTEE REVISED METHODS OF EXTRACT DETERMINATION

Following a Brewer's Society request to consider a change from a standard Miag Disc Mill setting of 0·5 mm to one of 0·7 mm the Analysis Committee has re-evaluated the determination of hot water extract. It is recommended that from 1st December 1979–1. A Miag Disc Mill setting of 0·7 mm be adopted for grinding malt for the determination of hot water extract. 2. Where an estimate of the fine/coarse grind hot water extract difference is required, mill settings of 0·2 mm and 0·7 mm respectively should be used. The reproducibility of this procedure is adequate to separate malts into classes with high and low values but analytical tolerances cannot be recommended for commercial transactions. Revised methods for setting the Miag Disc Mill and for determining the hot water extract of fine and coarse ground malts are given in Appendix I. It is proposed that all mashes should be made in stainless steel beakers, the use of the standard brewers' mash flask being limited to making the mash to the correct volume at the end of the determination. It is recommended that, from 1st December 1979, the 0·7 mm Miag Disc Mill setting should replace also the 0·5 mm setting in all Recommended Methods for coloured malts, dark malts, roasted barley and unmalted grain. It is further recommended that from 1st December 1979 all specific gravity determinations for laboratory extracts of malt, coloured malt, dark malt, roasted barley, unmalted grain, sugars, syrup, caramel and spent grains should be made at 20°C.     

DETERMINATION OF THE MOISTURE CONTENT OF BARLEY

The method of the International Organization for Standardization, (ISO 712–1985) for the determination of moisture in cereals and cereal products, has been tested by members of the Analysis Committee of the European Brewery Convention on samples of barley. The method, which relies on loss in mass on drying at 130–133°C for 2 h, is recommended for use as a replacement for the current method, based on loss in mass on drying at 105–107°C for 3 h. It was judged that precision values were independent of concentration over the range 11 to 13% m/m. Repeatability (r₉₅) and Reproducibility R₉₅) values of 0.13 and 0.55 respectively were obtained over this range. At a mean level of 21.7% m/m, the r₉₅ and R₉₅ values were 0.27 and 2.6 respectively. This was probably due to errors associated with the double drying technique which is necessary for samples at this moisture content.     

DETERMINATION OF NITRATE IN BEER BY ION CHROMATOGRAPHY

¹A method, relying on ion chromatography, for the determination of nitrate in beer, has been collaboratively tested by members of the European Brewery Convention (EBC) and the Brewery Convention of Japan (BCOJ). Precision values were judged to be acceptable. Repeatability (r₉₅) and reproducibility (R₉₅) values were 1.5, 0.96, 5.1, and 9.3, 10.4, 13.5 respectively for corresponding mean levels of 6.5, 26.2 and 52.8 mg/litre. However, r₉₅ and R₉₅ values of 1.5 and 2.3 respectively were obtained for an aqueous solution of nitrate ions at a mean level of 20.7 mg/litre. The determination of nitrate is recommended for use and inclusion in Analytica-EBC, as an additional analyte in the International Method which relies on ion chromatography for estimating chloride, sulphate and phosphate.     

EXTRACT AND COLOUR DETERMINATION OF TORREFIED PRODUCTS (WHEAT,BARLEY AND RYE)—COLLABORATIVE TRIAL

A procedure for preparing torrefied products for analysis has been examined and the effects of this procedure on the determination of laboratory extract and colour have been collaboratively tested by the Analysis Committee of the Institute of Brewing. White malts of DP levels 50° and 100° IOB were used as the sources of enzymes in the mixed mash procedure. With these malts r₉₅ and R₉₅ values for extract of the torrefied products ranged from 1.7 to 10.2 and 12.4 to 21.9 resp. on mean extracts ranging from 244 to 270 litre °/kg. The r₉₅ and R₉₅ values for colour ranged from 1.6 to 2.3 and 2.2 to 3.8 resp. on mean colours ranging from 2.7 to 3.5 EBC units.     

DETERMINATION OF ANIONS IN BEER BY ION CHROMATOGRAPHY

A method relying on ion chromatography, with suppressed ion detection, for the determination of anions in beer, has been collaboratively tested by members of the American Society of Brewing Chemists, the European Brewery Convention and the Brewery Convention of Japan. Precision values obtained for the determination of chloride, sulphate and phosphate in beer were judged to be acceptable. Repeatability (r₉₈) and reproducibility (R₉₈) values for chloride were 5.7, 12.6, 12.5 and 15.0, 38.4, 36.8 respectively at corresponding mean levels of 68.7, 218.6 and 322.5 mg/litre. r₉₈ and R₉₈ values for sulphate were 7.5, 6.2, 7.6 and 44.8, 54.0, 46.5 respectively at corresponding mean levels of 101.4, 205.1 and 122.6 mg/litre. r₉₈ and R₉₉ values for phosphate were 14.1, 11.9, 24.9 and 78.7, 53.8, 84.0 at corresponding mean levels of 411.5, 224.1 and 397.5 mg/litre. Whilst the r₉₈ value for nitrate was acceptable, the value for R₉₈ was unsatisfactory. The ion chromatographic method for determining chloride, sulphate and phosphate in beer is recommended for use and inclusion in Analytica -EBC as an International Method.     

DETERMINATION OF TOTAL NITROGEN IN BARLEY AND MALT BY COMBUSTION METHOD—COLLABORATIVE TRIAL

A combustion method, relying on the Dumas principle, for the determination of total nitrogen in barley and malt, has been collaboratively tested by the Analysis Committee of the European Brewery Convention. Repeatability, r₉₅, and reproducibility, R₉₅, values were 0.063 and 0.116% of dry matter, respectively, for samples with nitrogen contents in the range 1.23 to 1.86% N of dry matter. There was no significant difference between these values for barley and malt. The Analysis Committee approved the adoption of the combustion method for inclusion in Analytica EBC as an alternative method.     

THE DETERMINATION OF ALCOHOL IN BEER USING THE SCABA AUTOMATED METHOD (COLLABORATIVE TRIAL)

The Institute of Brewing Analysis Committee has organised two collaborative trials for the analysis of alcohol using the ServoChem Automatic Beer Analyser (SCABA). The mean repeatability (r₉₅) values for the two trials were 0.051% and 0.034% V/V respectively. The value for the second trial could however be judged to be dependent on concentration (m) at 0.008m% V/V. The Reproducibility (R₉₅) values of both trials were judged to be dependent on concentration at 0.027m% V/V and 0.025m% V/V respectively. The combined data for the two trials gave r₉₅ = 0.044% V/V and R₉₅ = 0.026m% V/V.     

ESTIMATION OF FERMENTABLE CARBOHYDRATES — COLLABORATIVE TRIAL

A procedure relying on high performance liquid chromatography, for the estimation of fermentable carbohydrates in wort, has been tested collaboratively and adopted by the Institute of Brewing Analysis Committee as a Recommended Method. A radially compressed cartridge containing silica modified with tetraethylenepentamine is used with an eluting solvent of acetonitrile/water. The results of a preliminary trial indicated that better precision is achieved using manual measurements of peak height and omitting an internal standard. In the main trial where 5 laboratories analysed 5 sample pairs the repeatability (r₉₅) and reproducibility (R₉₅) values found with their mean concentration levels (m) to which they are applicable were: fructose (0.0256 + 0.0660m) and (0.0711 + 0.0691m) for 0.17–1.01 g/100 ml; glucose 0.090m and 0.139m for 0.80–2.07 g/100 ml; sucrose 0.095 and (0.0746 + 0.1663m) for 0.12–3.88 g/100 ml; maltose 0.219 and 0.917 for 4.17–6.09 g/100 ml; maltotriose 0.122 and 0.236 for 0.97–1.19 g/100 ml. The precision values for the sums of the total fermentable sugars were 0.578 and 1.040 for 6.71–14.24 g/100 ml.     

DETERMINATION OF THE SOLUBLE IRON CONTENT OF FILTER AIDS: A COLLABORATIVE TRIAL

The international method for the determination of the soluble iron content of filter aids has been collaboratively tested by members of the Analysis Committee of the European Brewery Convention to obtain repeatability (r₉₈) and reproducibility (R₉₈) values. It was Judged that precision values were dependent on the quantity of the soluble iron content of the filter aids over the range 32 to 220 mg/kg. Repeatability (r₉₈) value of 0.050 m and reproducibility value (R₉₈) of 0.255 m were obtained over this range.     

DETERMINATION OF MOISTURE,TOTAL AVAILABLE EXTRACT AND SOLUBLE EXTRACT IN SPENT GRAINS

The methods for the determination of moisture⁴, total available^3,4 and soluble extracts⁴ in spent grains have been collaboratively tested by members of the Analysis Committee of the European Brewery Convention to obtain repeatability (r₉₅) and reproducibility (R₉₅) values . Repeatability and reproducibility values of 0.1 and 0.67 respectively were obtained for spent grain moisture's ranging between 4 and 8% m/m in pre-dried and pro-milled samples. In a pro-dried and unmilled sample containing 3.4% m/m moisture the values obtained were 0.3 and 1.5 respectively . For total available extract (MEBAK) these values were 0.5 and (2.2+0.045 m) respectively, with total available extract ranging from 9 to 42% m/m dry matter, where m refers to the actual value. The values for the pre-dried and unmilled sample containing an extract of 41.2% m/m were 0.5 and 4.6 respectively . The precision values for soluble extract were dependent on the extract level of the sample over the range 6 to 40% m/m dry matter. A repeatability value of 0.13+0.007 m and a reproducibility value of 0.2+0.06 m were obtained over this range. Values for the same pre-dried and unmilled sample with a soluble extract of 38.7% m/m were 1.3 and 3.8% m/m respectively .     

COLLABORATIVE DETERMINATION OF THE PH OF BEER AND WORT

A method for the determination of pH in wort and beer has been tested for precision by the Analysis Committee of the Institute of Brewing . Over the pH range 3.94 to 5.04 it was judged that precision values were independent of the pH value of the sample. Values for r₉₅ and R₉₅ were 0.025 and 0.129 respectively .     

Determination of the N‐Nitrosodimethylamine Content of Beer and Malt — A Collaborative Trial

After about fifteen years a study was carried out to determine the variation in results of the N‐nitrosodimethylamine (NDMA) determination in beer and malt carried out in different laboratories, in order to obtain an overall view of the precision of the various methods used. Two collaborative trials were carried out by the EBC Analysis Committee during 1998. Repeatability values (r₉₅) for beer in the range of 0.09 ÷ 0.13 and for malt 0.33 ÷ 0.42 were found. Reproducibility values (R₉₅) for beer in the range of 0.45 ÷ 0.54 and for malt 0.65 ÷ 4.08 were obtained.     

INSTITUTE OF BREWING: ANALYSIS COMMITTEE RECOMMENDED MILL FOR MALT ANALYSIS

The Miag Disc Mill is now the standard mill for malt analysis. A method of setting the gap between the grinding discs by mean of a feeler gauge has been adopted. Using the recommended setting 5.0 for the measurement of Hot Water Extract the replication error is 0.8 litre °/kg. The error due to the mills is negligible compared with the errors arising from the remaining parts of the measurement.     

DETERMINATION OF VICINAL DIKETONES IN BEER BY GAS CHROMATOGRAPHY (HEADSPACE TECHNIQUE)—COLLABORATIVE TRIAL

Two methods for the determination of vicinal diketones in beer have been collaboratively tested by the Analysis Committee of the Institute of Brewing and are recommended for use. Both methods employ gas chromatography and are essentially the same, except that one relies on the use of a packed column and the other on a capillary column. For diacetyl it was judged that repeatability (r₉₅) values were independent of concentration over the range 0.04 to 0.19 mg/litre. Over this range, r₉₅ values for diacetyl of 0.028, 0.020 and 0.026 mg/litre were obtained for capillary, packed columns and combined results respectively. Values for reproducibility (R₉₅) were judged to be dependent on the mean level (m). R₉₅ values were 0.032 + 0.68 m, 0.01 + 0.47 m and 0.005 + 0.67 m were obtained for capillary, packed columns and combined results respectively. For both methods the r₉₅ and R₉₅ values for 2,3-pentanedione were judged to be independent of concentration over the range 0.02 to 0.07 mg/litre. For capillary columns, packed columns and combined results respectively, r₉₅ values were 0.009, 0.009, 0.010 mg/litre and R₉₅ values were 0.037, 0.042 and 0.038 mg/litre.     

Determination of Boiled Wort Colour

A method for the determination of boiled wort colour has been collaboratively tested by the Analysis Committee of the European Brewery Convention. In this trial the 14th EBC Standard Malt and two commercial malts were tested by 21 laboratories. Repeatability (r₉₅) and reproducibility (R₉₅) values of 0.33 ? 0.42 and 1.12 ? 1.44 EBC units were obtained respectively at a mean level of 4.7 ? 5.2 EBC units. At a mean level of 8.9 EBC units these respective values were 0.44 and 2.25 EBC units. The data sets could be split into two sub?sets for laboratories using either the included heating plate boiling procedure or the glycerol/oil bath boiling procedure. Statistical analysis of both sub?sets revealed that reproducibility is unambiguously better for the glycerol/oil bath procedure at all levels. For repeatability the situation is less clear. The evaluated method is recommended for inclusion in Analytical?EBC.     

DETERMINATION OF ETHANOL IN BEER BY GAS CHROMATOGRAPHY (DIRECT INJECTION)—COLLABORATIVE TRIAL

A method employing gas chromatography for the determination of ethanol in beer has been collaboratively tested by the Analysis Committee of the Institute of Brewing. It was judged that precision values were independent of concentration over the range 0.93 to 6.05% V/V ethanol. Repeatability (r₉₅) and reproducibility (R₉₅) values of 0.061 and 0.136 respectively, were obtained over this range. At a mean level of 9.17% V/V, the r₉₅ and R₉₅ values were 0.154 and 0.284 respectively. This was probably due to dilution errors as the sample had to be diluted to bring it within the linear range of the method. A comparison of the precision values given by the gas chromatographic method, with those obtained in 1991/1992 by 8 laboratories in a major brewing company using 12 sample pairs, for the IOB Recommended Distillation Method, revealed that there is no significant difference between the precision data for the two methods.     

SPECTROPHOTOMETRIC DETERMINATION OF MALT COLOUR

The International Method for the determination of the colour of beer has been tested by members of the Analysis Committee of the European Brewery Convention on samples of wort produced from a laboratory extract of malt using methods EBC 4.4 and EBC 4.4.5. The method, which relies on the spectrophotometric determination of colour at 430 nm, on clarified worts, is recommended as the designated reference method in place of the current visual method using EBC colour discs. The change will take effect from 1st January 1996. It was judged that precision values were dependent on the intensity of the colour of the sample over the range 3.6 to 25.3 EBC units. Repeatability (r₉₈) and Reproducibility (R₉₈) values of r₉₈ 0.18Mean ? 0.28 and R₉₈ = 0.13Mean + 0.46 were obtained over this range.     

Determination of the Total Soluble Nitrogen Content of Malt and Beer by the Dumas Combustion Method: Collaborative Trial

The determination of the total soluble nitrogen content of malt and beer, by the Dumas procedure, has jointly been collaboratively tested by the Analysis Committee of the Institute of Brewing (IOB) and the European Brewery Convention (EBC). Five samples of beer (range 362 to 1159 mg/l) and five samples of malt (range EBC 0.598 to 0.798 %m/m (dry basis) and IOB 0.534 to 0.706 %m/m (dry basis)) were distributed to eighteen participating laboratories for analysis. Precision values were judged to be independent of the mean soluble nitrogen content for malt by both IOB and EBC methodologies. Values for r₉₅ and R₉₅ were 0.047 and 0.136%m/m for EBC laboratory wort and 0.039 and 0.144 %m/m for IOB laboratory wort respectively. Precision values for beer were judged to be dependent upon the mean nitrogen content (m) in the case of r₉₅ and independent of the mean nitrogen content in the case of R₉₅. Values for r₉₅ and R₉₅ were 0.074m and 120 mg/l respectively.     

DETERMINATION OF THE VOLATILE COMPONENTS OF BEER

A method relying on headspace sampling and gas chromatography for the determination of the lower boiling point volatile compounds (fusel oils) in beer, has been approved by the Analysis Committee of the Institute of Brewing (IOB), for inclusion in Recommended Methods of Analysis. In view of the large values obtained for precision in terms of repeatability (r₉₅) and reproducibility (R₉₅) and the differences in gas chromatographic equipment used by individual brewing laboratories, the method is considered not to be ideal, but is given as a guideline only. The IOB Analysis Committee has recommended a method relying on gas chromatography and flame photometric detection for the determination of dimethyl sulphide in beer. Repeatability (r₉₅) and reproducibility (R₉₅) values of 3.3 μg/litre and 3.66+0.168 m μg/litre (where m is concentration), respectively, were obtained over the range 20–50 μg/litre. Methods currently used in brewing laboratories, for the measurement of vicinal diketones, are being surveyed with a view to obtaining a suitable method for collaborative testing by the Analysis Committee.     

COLLABORATIVE DETERMINATION OF SPECIFIC GRAVITY BY DENSITY METER

A method employing a density meter for the determination of specific gravity (SG) has been tested for the determination of the gravity (G) of beer, aqueous sugar solutions and aqueous ethanol solutions by the Analysis Committee of the Institute of Brewing. The term “gravity”, used throughout this report is defined by the equation G = SG × 1000. Repeatability (r₉₅) and reproducibility (R₉₅) values were calculated over the range 994.6 to 1124.2 gravity. For beer, it was judged that precision values were independent of the gravity of the sample. Values for r₉₅ and R₉₅ were 0.1 and 0.9, respectively, for instruments with a 5 figure display and 0.08 and 0.32, respectively, for instruments with a 6 figure display, over the range 999.1 to 1017.0 gravity. For solutions of ethanol in water, precision was also independent of the gravity of the sample. Values for r₉₅ and R₉₅ were 0.1 and 0.3, respectively, for instruments with a 5 figure display and 0.05 and 0.19, respectively, for instruments with a 6 figure display, over the range 994.6 to 999.1 gravity. For aqueous sugar solutions the values of r₉₅ and R₉₅ increased with increasing gravity. At 1049.3 gravity, values for r₉₅ and R₉₅ were 0.1 and 0.8, respectively, for instruments with a 5 figure display and 0.07 and 0.35, respectively, for instruments with a 6 figure display. At 1124.2 gravity values for r₉₅ and R₉₅ were 0.2 and 1.4, respectively, for instruments with a 5 figure display and 0.16 and 1.35, respectively, for instruments with a 6 figure display.