This method describes the determination of dimethyl sulfide and its precursors in malt.
Malt intended for use in beer brewing or elsewhere in the food industry
DMS and the precursors of DMS (DMSP) are obtained from a finely ground malt sample by means of cold extraction. This aqueous extract is then boiled under alkaline conditions which converts the DMS precursors (DMSP) to free DMS. The DMS is determined using gas chromatography by means of the headspace technique.
Determination of free dimethyl sulfide (DMS) and its precursors in wort and beer
wort and beer
Free DMS is determined in wort and beer with a gas chromatograph using the headspace method. Calibration is performed at various concentrations within the relevant range. The relative peaks corresponding to the concentrations are evaluated.
Malt intended for use in beer brewing or elsewhere in the food industry
A (modified) Congress wort is produced from malt samples prior to analysis. NDMA present in the Congress wort is extracted using dichloromethane followed by concentration of the eluate. The determination is performed with a gas chromatograph using a packed Carbowax 20M column with a specific TEA detector (thermal energy analyzer); nitrosodipropylamine (NDPA) serves as an internal standard.
This detector analyzes nitrosamine according to the following procedure:
After exiting the GC column, the separated substances are heated to 500 °C in a pyrolyzer. At this temperature, the N-NO bond of the nitrosamine is broken, thus forming an NO radical (NO۰):
The gas mixture then flows through a special filter (CTRTM gas stream filter), which only allows the carrier gas and the NO radicals to pass. After exiting the filter, the NO radicals flow into a reaction chamber along with ozone, which is created by a special generator. The following chemical reactions take place in the chamber:
NO• + O3 |
→ |
NO2• |
NO2• |
→ |
NO2 + h•ν |
These NO radicals react with ozone, forming nitrogen dioxide in an excited state (NO2•). The NO2• molecules decompose spontaneously to form nitrogen dioxide in its common form (NO2), emitting radiation (h•ν) with a wavelength of approx. 600 nm.
Determination of free dimethyl sulfide (DMS) and its precursors in beer
wort
Dimethyl sulfide precursors (DMSP) in the wort are converted to dimethyl sulfide (DMS) by heating under aqueous, alkaline conditions. The DMS is determined using gas chromatography by means of the headspace technique.
The method describes how to determine the nitrate content of water photometrically with a cuvette test.
In an acidic sulfurous solution containing phosphorus, nitrate ions react with 2,6-dimethylphenol to produce 4-nitro-2,6-dimethylphenol.
The method is suitable for determining approx. 0.5–25 mg/l NO3-. If the ratio of chloride to nitrate ions is larger than 10, this may interfere with the reaction (if this is the case, according to DEV D 9-3, follow DIN 38405); likewise, nitrite ions exceeding approx. 0.2 mg/l may also interfere with the reaction. For their removal, refer to Remarks below.