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Commission Regulation (EC) No 2870/2000 of 19 December 2000 laying down Community reference methods for the analysis of spirits drinks
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This method is suitable for the determination of egg yolk concentration in the range of 40 to 250 g/l in egg liqueur and liqueur with egg.
ISO 3696:1897 Water for analytical laboratory use — Specifications and test methods.
The ethanol-soluble phosphorus compounds found in egg yolk are extracted and assayed photometrically as a phosphorus molybdate complex.
dissolve 20 g of ammonium molybdate (CAS 12054-85-2), (NH 4 ) 6 Mo 7 O 24 .4H 2 O in 400 ml water at 50 o C;
dissolve, in another vessel, 1 g of ammonium vanadate (CAS 7803-55-6), NH 4 VO 3 , in 300 ml hot water, allow to cool, then add 140 ml of concentrated nitric acid (CAS 7697-37-2). Combine the cooled solutions in a 1 000 ml volumetric flask and make up to the 1 000 ml mark.
Samples are stored at room temperature prior to analysis.
dihydrogen phosphate solution (ml) | 0 | 2 | 4 | 6 | 8 | 10 |
P 2 O 5 (mg) | 0 | 0,167 | 0,334 | 0,501 | 0,668 | 0,835 |
The egg yolk content in g/l is calculated from the following formula:
where:
conversion factor for total P 2 O 5 in g in 100 g of egg yolk
value established from the calibration curve
mass per unit volume (g/ml) of the egg-based liqueur at 20 o C
weight of the egg-based liqueur in g
dilution factor for a 5 ml aliquot of ash solution.
Statistical results of the interlaboratory test:
the following table gives the values for egg yolk.
The following data were obtained from an international method performance study carried out to internationally agreed procedures.
Year of interlaboratory test: | 1998 |
Number of laboratories: | 24 |
Number of samples: | 5 |
Analyte: | Egg yolk |
Samples | A | B | C | D | E |
---|---|---|---|---|---|
Number of laboratories retained after eliminating outliers | 19 | 20 | 22 | 20 | 22 |
Number of outliers (laboratories) | 3 | 4 | 2 | 4 | 2 |
Number of accepted results | 38 | 40 | 44 | 40 | 44 |
Mean value | 147,3 | 241,1 | 227,4 | 51,9 (*) 72,8 (*) | 191,1 |
Repeatability standard deviation (S r ) g/l | 2,44 | 4,24 | 3,93 | 1,83 | 3,25 |
Repeatability relative standard deviation (RSD r ) (%) | 1,7 | 1,8 | 1,8 | 2,9 | 1,7 |
Repeatability limit (r) g/l | 6,8 | 11,9 | 11,0 | 5,1 | 9,1 |
Reproducibility standard deviation (S R ) g/l | 5,01 | 6,06 | 6,66 | 3,42 | 6,87 |
Reproducibility relative standard deviation (RSD R ) (%) | 3,4 | 2,5 | 2,9 | 5,5 | 3,6 |
Reproducibility limit (R) g/l | 14,0 | 17,0 | 18,7 | 9,6 | 19,2 |
Sample types
Advocaat, blind duplicates
Advocaat, blind duplicates
Advocaat, blind duplicates
Advocaat (diluted), split levels (*)
Advocaat, blind duplicates]
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