Determination of the carbon isotope ratio 13C/12C of CO2 in sparkling wines: Method using isotope ratio mass spectrometry (IRMS)- Modification
RESOLUTION OIV-OENO 512-2014
DETERMINATION OF THE CARBON ISOTOPE RATIO 13C/12C OF 
IN SPARKLING WINES: METHOD USING ISOTOPE RATIO MASS SPECTROMETRY (IRMS) - MODIFICATION
THE GENERAL ASSEMBLY,
IN VIEW of Article 2 paragraph iv of the Agreement of 3 April 2001 establishing the International Organisation of Vine and Wine,
ON THE PROPOSAL of the "Methods of Analysis" Sub-Commission,
CONSIDERING the resolution Oeno 7/2005 (Method OIV-MA-AS314-03) "DETERMINATION OF THE CARBON ISOTOPE RATIO 13C/12C OF 
IN SPARKLING WINES: METHOD USING ISOTOPE RATIO MASS SPECTROMETRY (IRMS)" appearing in the Compendium of International Methods of Wine and Must Analysis,
DECIDES to modify the method OIV-MA-AS314-03 by changing paragraph 6: Apparatus, and sub-paragraph 7.1: sampling procedures, as follows:
To paragraph 6: Apparatus, at the end of the sub-paragraph "Continuous-flow systems (CF-IRMS)", the following will be added:
-
Gas Sampler-IRMS. A peripheral system may be used for the on-line gas preparation, isolation of and introduction of into the isotope ratio mass spectrometer.
To sub-paragraph 7.1: CO2 sampling procedures, points "d" and "e" will be added as follows:
-
d. Refrigerate the sample at 4-5 °C, before quickly transferring the liquid into a vial and sealing it with a Teflon-silicone septum cap. Then 50
L of liquid is then transferred into a 10 mL vial and analysed. If necessary, the vial should be filled with helium in order to remove the atmospheric .
- e. After refrigerating the sample, the bottle is opened at room temperature and a sample of 200 µL of liquid is taken using a pipette and placed in suitable vials. The vials are immediately resealed then placed in an ultrasonic bath for 10 min prior to analysis.
The statistical results of the inter-laboratory test for sampling procedures 7.1.d and 7.1.e are given in ANNEX E.
To sub-paragraph 9 (Precision) some modifications are added:
9. Precision
Details on the inter-laboratory test on precision of the method are given in Annexes D and E.
To sub-paragraph 9.1 (Repeatability):
9.1. Repeatability
9.1.1 Characteristics of sampling procedures 7.1.a-c
= 0.21 ‰
r = 0.58 ‰
9.1.2. Characteristics of sampling procedures 7.1.d and 7.1.e
= 0.21 ‰
r = 0.56 ‰
To sub-paragraph 9.2 (Reproducibility):
9.2. Reproducibility
9.2.1 Characteristics of sampling procedures 7.1.d and 7.1.e
= 0.68‰
R= 1.91‰
Annexes (A,B,C,D,E)
Annex E was added to the method:
ANNEX E
Statistical results of the inter-laboratory test on sparkling and gasified wines
Sampling procedures 7.1.d and 7.1.e
In accordance with method OIV-MA-AS1-09: R2000, the following parameters were defined as part of an inter-laboratory test conducted with 16 laboratories.
Year of the inter-laboratory test: 2013-2014
Number of laboratories:16
Type of samples: Sparkling and gasified wines
Number of samples: 3, as blind duplicates
Parameter measured: 13C
|
INDICATORS |
WINE NO. 1 |
WINE NO. 2 |
WINE NO. 3 |
|
Number of laboratories |
16 |
14 |
16 |
|
Number of repetitions |
2 |
2 |
2 |
|
Minimum |
-32.90 |
-33.10 |
-23.64 |
|
Maximum |
-29.83 |
-30.97 |
-20.57 |
|
Repeatability variance sr2 |
0.0467 |
0.0118 |
0.0648 |
|
Inter-group variance sL2 |
0.43853 |
0,29762 |
0.51616 |
|
Reproducibility variance sR2 |
0.4852 |
0.3094 |
0.5810 |
|
Overall average |
-31.42 |
-31.83 |
-22.15 |
|
Repeatability standard deviation |
0.22 |
0.11 |
0.25 |
|
r limit |
0.612 |
0.307 |
0.720 |
|
Reproducibility standard deviation |
0.70 |
0.56 |
0.76 |
|
R limit |
1.971 |
1.574 |
2.157 |
|
Wine No. 1 |
Wine No. 2 |
Wine No. 3 |
Z-score |
Z-score |
Z-score |
||||
|
Laboratory Code |
A |
B |
A |
B |
A |
B |
Wine No. 1 |
Wine No. 2 |
Wine No. 3 |
|
Lab 1 |
-31.40 |
-31.69 |
-31.56 |
-31.88 |
-21.93 |
-22.12 |
-0.18 |
-0.19 |
0.16 |
|
Lab 2 |
-31.23 |
-31.29 |
-31.43 |
-31.41 |
-21.46 |
-22.04 |
0.23 |
-0.73 |
0.52 |
|
Lab 3 |
-32.65 |
-32.12 |
-32.15 |
-32.13 |
-23.41 |
-23.64 |
-1.39 |
-0.56 |
-1.81 |
|
Lab 4 |
-31.55 |
-31.50 |
-31.46 |
-31.66 |
-22.40 |
-22.54 |
-0.15 |
0.48 |
-0.42 |
|
Lab 5 |
-31.50 |
-31.30 |
-31.80 |
-31.90 |
-22.00 |
-22.30 |
0.03 |
-0.04 |
0.00 |
|
Lab 6 |
-31.46 |
-31.75 |
-31.96 |
-31.75 |
-22.39 |
-22.10 |
-0.27 |
-0.05 |
-0.13 |
|
Lab 7 |
-31.48 |
-30.66 |
-31.29 |
-29.35 |
-21.47 |
-20.57 |
0.50 |
2.71 |
1.48 |
|
Lab 8 |
-29.83 |
-30.17 |
-29.73 |
-31.35 |
-21.50 |
-21.96 |
2.04 |
2.31 |
0.55 |
|
Lab 9 |
-30.96 |
-30.90 |
-31.34 |
-31.21 |
-22.22 |
-22.27 |
0.70 |
0.99 |
-0.13 |
|
Lab 10 |
-32.34 |
-32.29 |
-32.68 |
-32.75 |
-23.25 |
-23.14 |
-1.29 |
-1.60 |
-1.37 |
|
Lab 11 |
-32.90 |
-32.70 |
-33.10 |
-33.10 |
-23.00 |
-23.50 |
-1.98 |
-2.29 |
-1.45 |
|
Lab 12 |
-31.91 |
-31.68 |
-32.22 |
-32.14 |
-22.58 |
-22.66 |
-0.54 |
-0.63 |
-0.62 |
|
Lab 13 |
-31.03 |
-31.10 |
-31.61 |
-31.68 |
-21.78 |
-21.74 |
0.51 |
0.33 |
0.51 |
|
Lab 14 |
-31.25 |
-30.93 |
-31.43 |
-31.54 |
-22.01 |
-22.02 |
0.57 |
0.62 |
0.17 |
|
Lab 15 |
-30.89 |
-30.88 |
-31.59 |
-31.47 |
-21.08 |
-21.07 |
0.76 |
0.53 |
1.41 |
|
Lab 16 |
-31.05 |
-30.98 |
-31.24 |
-30.97 |
-21.090 |
-21.490 |
0.58 |
1.30 |
1.13 |
 |
Bibliography
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- Laetitia Gaillard, Francois Guyon ⁄, Marie-Hélène Salagoïty, Bernard Médina, Authenticity of carbon dioxide bubbles in French ciders through multiflow-isotope ratio mass spectrometry measurements. Food Chemistry. 2013, 141: 2103–2107