Validation of the analysis of volatile compounds of wines by gas chromatography
RESOLUTION OIV-OENO 606-2018
VALIDATION OF THE ANALYSIS OF VOLATILE COMPOUNDS OF WINES BY GAS CHROMATOGRAPHY (OIV-OENO553-2016)
|
WARNING: this resolution amends the following resolution: - OIV-OENO 553-2016 |
THE GENERAL ASSEMBLY,
IN VIEW with Article 2, paragraph 2 iv of the Agreement of 3 April 2001 establishing the International Organisation of Vine and Wine,
At the proposal of the “Methods of Analysis” Sub-Commission,
CONSIDERING Resolution OIV-OENO 553-2016 adopted by the General Assembly in 2016 concerning analysis of volatile compounds of wines by gaseous phase chromatography
DECIDES to complete the method for the analysis of volatile compounds of wines by gas chromatography (OIV-MA-AS315-27: 2016) with the following text:
Footnote:
Type II for ethyl acetate, propan-1-ol, 2-methylpropan-1-ol, butan-1-ol, 2-methyl-butan-1-ol, 3-methylbutan-1-ol, acetoïn, ethyl lactate, hexan-1-ol, 3-ethoxypropanol, ethyl octanoate, butyrolactone, diethyl succinate and 2-phenyl ethanol.
Type III for methanol.
Type IV for other products (ethanal, butan-2-ol, butane-2,3-diol (levo + meso), propane-1,2-diol, diethyl malate).
C1 – Organisation of the study - Samples
This study was carried out by the Comité Interprofessionnel du Vin de Champagne in Epernay. A prevalidation occurred during October/December 2015 and actual interlaboratory during March/April 2016.
The trial involved 11 samples: two white wines identified B and E, two red wines identified C and F and one rosé wine identified A (blindly replicated) + one of the samples spiked with butan-2-ol, butan-1-ol, acetoin, hexan-1-ol and diethyl malate (identified D).
C2 - Fidelity
13 laboratories participated in the interlaboratory study:
- Autoridade de Segurança Alimentar e Económica, Lisbon, Portugal;
- Bundesinstitut für Risikobewertung, Berlin, Germany;
- Bureau National Interprofessionnel du Cognac, Cognac, France;
- Comité Interprofessionnel du vin de Champagne, Epernay, France;
- Czech Agriculture and Food Inspection Authority, Brno, Czech Republic;
- Instituto dos Vinhos do Douro e do Porto, Porto, Portugal;
- Laboratoire DUBERNET, Montredon Corbières, France;
- Laboratorio Arbitral Agroalimentario, Madrid, Spain;
- Landesuntersuchungsamt, Mainz, Germany;
- Miguel Torres S.A.- Finca, Barcelona, Spain;
- Service Commun des Laboratoires Bordeaux-Pessac (SCL MINEFI), Pessac, France;
- Service Commun des Laboratoires Montpellier (SCL MINEFI), Montpellier, France;
- Union Nationale de Groupements des Distillateurs d'alcool (UNGDA), Malakoff, France.
The results were evaluated according to the OIV protocol (Collaborative study OIV MA-AS1-07:R2000).
ISO 5725-2 §7.5 recommends to look for any functional relationship between the fidelity values and the content, which is expressed by the graphs below the data tables for each product.
C3 - Results tables
compound |
r |
R |
ethyl acetate |
0.18x – 1.8 |
0.33x – 1.7 |
methanol |
0.22x – 4.3 |
0.28x – 3.2 |
propan-1-ol |
4 mg/l |
7 mg/L |
2-methylpropan-1-ol |
0.20x – 1.4 |
0.36x – 0.7 |
butan-1-ol |
0.07x + 0.2 |
0.14x + 0.3 |
2-methylbutan-1-ol |
0.23x – 2.7 |
0.40x – 5.0 |
3-methylbutan-1-ol |
0.35x – 35.7 |
0.45x – 41.8 |
acetoïn |
0.14x + 1.2 |
0.33x + 2.1 |
ethyl lactate |
0.23x – 1.6 |
0.29x + 4.2 |
hexanol |
0.07x + 0.3 |
0.10x + 0.8 |
3-ethoxypropanol |
0.59x – 0.4 |
0.46x + 0.4 |
ethyl octanoate |
0.5 mg/l |
0.7 mg/l |
butyrolactone |
0.25x + 0.8 |
0.20x + 4.1 |
diethyl succinate |
0.31x + 0.8 |
0.55x + 0.4 |
2-phenylethanol |
0.24x + 0.3 |
0.50x – 2.6 |
where x is the measured concentration
|
Ethyl acetate - Fidelity |
|
|||||
repeatability and reproducibility |
|
|||||
wine A |
wine B |
wine C |
wine D |
wine E |
wine F |
|
Method |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
No. of laboratories that submitted results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories that submitted compliant results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories after elimination of outliners |
12 |
12 |
12 |
13 |
12 |
13 |
Number of measurement values without outliners |
42 |
42 |
42 |
23 |
42 |
46 |
Mean (mg/L) |
26.4 |
60.5 |
55.5 |
60.6 |
25.5 |
68.4 |
Repeatability s.d. Sr |
1.6 |
2.6 |
2.4 |
1.4 |
1.1 |
6.0 |
RSDr % |
5.9 |
4.2 |
4.3 |
2.4 |
4.3 |
8.8 |
Limit of repeatability r |
4.5 |
7.4 |
6.9 |
4.5 |
3.2 |
17.3 |
Relative limit of repeatability r% |
16.9% |
12.2% |
12.3% |
7.4% |
12.5% |
25.3% |
Reproducibility s.d. SR |
2.8 |
4.7 |
4.4 |
8.8 |
2.2 |
7.3 |
RSDR % |
10.7 |
7.7 |
8.0 |
14.5 |
8.5 |
10.6 |
Limit of reproducibility R |
8.1 |
13.4 |
12.6 |
25.8 |
6.2 |
20.7 |
Relative limit of reproducibility R% |
30.5% |
22.1% |
22.7% |
42.6% |
24.2% |
30.3% |
HORRAT R |
1.1 |
0.9 |
0.9 |
1.7 |
0.9 |
1.2 |
 |
Methanol - Fidelity |
|
|||||
repeatability and reproducibility |
|
|||||
wine A |
wine B |
wine C |
wine D |
wine E |
wine F |
|
Method |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
No. of laboratories that submitted results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories that submitted compliant results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories after elimination of outliners |
13 |
13 |
13 |
13 |
13 |
13 |
Number of measurement values without outliners |
46 |
46 |
46 |
23 |
46 |
46 |
Mean (mg/L) |
66.8 |
57.2 |
129.8 |
57.8 |
59.4 |
165.6 |
Repeatability s.d. Sr |
3.8 |
2.6 |
7.4 |
3.0 |
3.3 |
11.9 |
RSDr % |
5.6 |
4.5 |
5.7 |
5.2 |
5.5 |
7.2 |
Limit of repeatability r |
10.8 |
7.4 |
21.2 |
9.5 |
9.4 |
34.1 |
Relative limit of repeatability r% |
16.2% |
12.9% |
16.3% |
16.3% |
15.8% |
20.6% |
Reproducibility s.d. SR |
5.1 |
4.6 |
11.4 |
4.2 |
5.4 |
15.4 |
RSDR % |
7.6 |
8.1 |
8.8 |
7.3 |
9.0 |
9.3 |
Limit of reproducibility R |
14.5 |
13.2 |
32.5 |
12.3 |
15.3 |
43.9 |
Relative limit of reproducibility R% |
21.7% |
23.1% |
25.0% |
21.3% |
25.7% |
26.5% |
HORRAT R |
0.9 |
0.9 |
1.1 |
0.8 |
1.0 |
1.3 |
 |
Propan-1-ol - Fidelity |
|
|||||
repeatability and reproducibility |
|
|||||
wine A |
wine B |
wine C |
wine D |
wine E |
wine F |
|
Method |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
No. of laboratories that submitted results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories that submitted compliant results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories after elimination of outliners |
13 |
13 |
13 |
13 |
13 |
13 |
Number of measurement values without outliners |
46 |
46 |
46 |
23 |
46 |
46 |
Mean (mg/L) |
31.1 |
36.1 |
39.5 |
36.7 |
32.9 |
22.7 |
Repeatability s.d. Sr |
1.5 |
1.4 |
1.8 |
0.8 |
1.4 |
1.5 |
RSDr % |
4.7 |
3.8 |
4.6 |
2.4 |
4.1 |
6.8 |
Limit of repeatability r |
4.2 |
4.0 |
5.3 |
2.7 |
3.9 |
4.4 |
Relative limit of repeatability r% |
13.4% |
11.0% |
13.4% |
7.4% |
11.8% |
19.4% |
Reproducibility s.d. SR |
2.0 |
2.1 |
3.0 |
1.5 |
2.1 |
1.9 |
RSDR % |
6.3 |
5.9 |
7.5 |
4.1 |
6.4 |
8.3 |
Limit of reproducibility R |
6.7 |
7.3 |
10.2 |
4.4 |
7.2 |
6.4 |
Relative limit of reproducibility R% |
21.6% |
20.1% |
25.7% |
11.9% |
22.0% |
28.3% |
HORRAT R |
0.7 |
0.6 |
0.8 |
0.4 |
0.7 |
0.8 |
 |
2-methylpropan-1-ol - Fidelity |
|
|||||
repeatability and reproducibility |
|
|||||
wine A |
wine B |
wine C |
wine D |
wine E |
wine F |
|
Method |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
No. of laboratories that submitted results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories that submitted compliant results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories after elimination of outliners |
13 |
13 |
13 |
12 |
13 |
13 |
Number of measurement values without outliners |
46 |
46 |
46 |
21 |
46 |
46 |
Mean (mg/L) |
21.2 |
22.2 |
40.0 |
30.8 |
17.7 |
49.9 |
Repeatability s.d. Sr |
0.9 |
1.4 |
1.6 |
3.0 |
0.7 |
3.3 |
RSDr % |
4.0 |
6.4 |
4.1 |
9.6 |
3.7 |
6.5 |
Limit of repeatability r |
2.5 |
4.1 |
4.7 |
9.5 |
1.9 |
9.4 |
Relative limit of repeatability r% |
11.6% |
18.3% |
11.8% |
30.8% |
10.8% |
18.9% |
Reproducibility s.d. SR |
2.4 |
2.7 |
4.6 |
7.5 |
1.9 |
6.1 |
RSDR % |
11.5 |
12.2 |
11.5 |
24.2 |
10.8 |
12.3 |
Limit of reproducibility R |
6.9 |
7.7 |
13.2 |
22.0 |
5.5 |
17.5 |
Relative limit of reproducibility R% |
32.8% |
34.7% |
33.0% |
71.5% |
30.8% |
35.1% |
HORRAT R |
1.1 |
1.2 |
1.3 |
2.5* |
1.0 |
1.4 |
*presumed outlier, not considered for computation of fidelity.
 |
|
Butan-1-ol – Fidelity repeatability et reproducibility |
|
|||||
|
|
|||||
vin A |
vin B |
vin C |
vin D |
vin E |
vin F |
|
Method |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
No. of laboratories that submitted results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories that submitted compliant results |
9 |
8 |
10 |
13 |
9 |
10 |
No. of laboratories after elimination of outliners |
9 |
8 |
10 |
13 |
9 |
10 |
Number of measurement values without outliners |
28 |
26 |
34 |
23 |
28 |
32 |
Mean (mg/L) |
0.87 |
0.87 |
1.77 |
11.36 |
0.81 |
1.36 |
Repeatability s.d. Sr |
0.05 |
0.07 |
0.14 |
0.29 |
0.07 |
0.15 |
RSDr % |
5.5 |
7.8 |
8.2 |
2.6 |
8.4 |
11.0 |
Limit of repeatability r |
0.14 |
0.20 |
0.42 |
0.92 |
0.20 |
0.44 |
Relative limit of repeatability r% |
16.2% |
23.1% |
23.9% |
8.1% |
24.8% |
32.1% |
Reproducibility s.d. SR |
0.14 |
0.13 |
0.20 |
0.67 |
0.14 |
0.26 |
RSDR % |
15.6 |
15.0 |
11.3 |
5.9 |
17.5 |
19.3 |
Limit of reproducibility R |
0.39 |
0.38 |
0.58 |
1.96 |
0.41 |
0.76 |
Relative limit of reproducibility R% |
45.2% |
43.9% |
32.5% |
17.3% |
50.9% |
55.7% |
HORRAT R |
1.0 |
0.9 |
0.8 |
0.5 |
1.1 |
1.3 |
 |
2-methylbutan-1-ol - Fidelity
repeatability and reproducibility
wine A |
wine B |
wine C |
wine D |
wine E |
wine F |
|
Method |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
No. of laboratories that submitted results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories that submitted compliant results |
9 |
9 |
9 |
9 |
9 |
9 |
No. of laboratories after elimination of outliners |
9 |
9 |
9 |
9 |
9 |
9 |
Number of measurement values without outliners |
32 |
32 |
32 |
16 |
32 |
32 |
Mean (mg/L) |
24.3 |
22.4 |
47.6 |
22.6 |
20.4 |
52.0 |
Repeatability s.d. Sr |
1.4 |
1.1 |
2.2 |
0.3 |
0.7 |
3.8 |
RSDr % |
5.7 |
4.7 |
4.6 |
1.3 |
3.6 |
7.3 |
Limit of repeatability r |
4.0 |
3.1 |
6.4 |
1.0 |
2.2 |
11.0 |
Relative limit of repeatability r% |
16.6% |
13.7% |
13.3% |
4.3% |
10.6% |
21.2% |
Reproducibility s.d. SR |
1.7 |
1.5 |
4.7 |
0.8 |
1.5 |
5.7 |
RSDR % |
6.9 |
6.8 |
9.9 |
3.5 |
7.3 |
10.9 |
Limit of reproducibility R |
4.8 |
4.4 |
13.7 |
2.4 |
4.3 |
16.3 |
Relative limit of reproducibility R% |
19.9% |
19.6% |
28.6% |
10.6% |
21.2% |
31.4% |
HORRAT R |
0.7 |
0.7 |
1.1 |
0.4 |
0.7 |
1.2 |
The laboratories that summed the peaks of 2-methylbutan-1-ol and 3-methylbutan-1-ol are excluded.
 |
|
3-methylbutan-1-ol - Fidelity |
|
|||||
repeatability and reproducibility |
|
|||||
wine A |
wine B |
wine C |
wine D |
wine E |
wine F |
|
Method |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
No. of laboratories that submitted results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories that submitted compliant results |
9 |
9 |
9 |
9 |
9 |
9 |
No. of laboratories after elimination of outliners |
9 |
9 |
9 |
9 |
9 |
9 |
Number of measurement values without outliners |
32 |
32 |
32 |
16 |
32 |
32 |
Mean (mg/L) |
142.2 |
147.8 |
200.5 |
150.2 |
134.4 |
201.7 |
Repeatability s.d. Sr |
7.1 |
6.1 |
9.4 |
0.9 |
5.1 |
15.0 |
RSDr % |
5.0 |
4.1 |
4.7 |
0.6 |
3.8 |
7.5 |
Limit of repeatability r |
20.8 |
17.8 |
27.5 |
2.9 |
14.9 |
44.0 |
Relative limit of repeatability r% |
14.6% |
12.1% |
13.7% |
1.9% |
11.1% |
21.8% |
Reproducibility s.d. SR |
8.2 |
9.3 |
15.7 |
3.6 |
8.5 |
18.2 |
RSDR % |
5.8 |
6.3 |
7.8 |
2.4 |
6.3 |
9.0 |
Limit of reproducibility R |
23.7 |
26.9 |
45.2 |
10.9 |
24.6 |
52.6 |
Relative limit of reproducibility R% |
16.6% |
18.2% |
22.5% |
7.3% |
18.3% |
26.1% |
HORRAT R |
0.8 |
0.8 |
1.1 |
0.3 |
0.8 |
1.3 |
The laboratories that summed the peaks of 2-methylbutan-1-ol and 3-methylbutan-1-ol are excluded.
 |
Acetoin - Fidelity |
|
|||||
repeatability and reproducibility |
|
|||||
wine A |
wine B |
wine C |
wine D |
wine E |
wine F |
|
Method |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
No. of laboratories that submitted results |
13 |
12 |
13 |
13 |
12 |
13 |
No. of laboratories that submitted compliant results |
12 |
9 |
13 |
13 |
10 |
13 |
No. of laboratories after elimination of outliners |
11 |
7 |
13 |
13 |
9 |
13 |
Number of measurement values without outliners |
38 |
24 |
46 |
23 |
30 |
46 |
Mean (mg/L) |
5.6 |
2.1 |
19.8 |
53.4 |
2.4 |
21.4 |
Repeatability s.d. Sr |
0.7 |
0.2 |
1.7 |
2.6 |
0.5 |
1.8 |
RSDr % |
11.5 |
8.3 |
8.8 |
4.9 |
19.7 |
8.5 |
Limit of repeatability r |
1.9 |
0.5 |
5.0 |
8.3 |
1.4 |
5.2 |
Relative limit of repeatability r% |
33.4% |
24.7% |
25.2% |
15.5% |
58.0% |
24.3% |
Reproducibility s.d. SR |
1.3 |
0.6 |
3.4 |
6.5 |
0.7 |
3.5 |
RSDR % |
23.1 |
28.3 |
17.2 |
12.2 |
30.2 |
16.6 |
Limit of reproducibility R |
3.7 |
1.7 |
9.7 |
19.2 |
2.1 |
10.1 |
Relative limit of reproducibility R% |
66.2% |
82.8% |
48.9% |
36.0% |
87.3% |
47.3% |
HORRAT R |
1.9 |
2.0 |
1.7 |
1.4 |
2.2* |
1.6 |
*presumed outlier, not considered for computation of fidelity
 |
|
Ethyl lactate - Fidelity |
|
|||||
repeatability and reproducibility |
|
|||||
wine A |
wine B |
wine C |
wine D |
wine E |
wine F |
|
Method |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
No. of laboratories that submitted results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories that submitted compliant results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories after elimination of outliners |
13 |
13 |
13 |
13 |
13 |
13 |
Number of measurement values without outliners |
46 |
46 |
46 |
23 |
46 |
46 |
Mean (mg/L) |
81.5 |
21.4 |
149.2 |
21.8 |
34.3 |
118.2 |
Repeatability s.d. Sr |
5.4 |
1.3 |
11.9 |
1.0 |
2.7 |
9.1 |
RSDr % |
6.6 |
6.3 |
8.0 |
4.6 |
7.7 |
7.7 |
Limit of repeatability r |
15.5 |
3.9 |
34.2 |
3.1 |
7.6 |
26.1 |
Relative limit of repeatability r% |
19.0% |
18.0% |
22.9% |
14.2% |
22.2% |
22.1% |
Reproducibility s.d. SR |
8.9 |
4.0 |
17.7 |
3.8 |
5.0 |
13.0 |
RSDR % |
11.0 |
18.9 |
11.8 |
17.4 |
14.7 |
11.0 |
Limit of reproducibility R |
25.5 |
11.5 |
50.3 |
11.1 |
14.3 |
37.0 |
Relative limit of reproducibility R% |
31.3% |
53.8% |
33.7% |
51.0% |
41.7% |
31.3% |
HORRAT R |
1.3 |
1.9 |
1.6 |
1.7 |
1.5 |
1.4 |
 |
|
Hexan-1-ol - Fidelity |
|
|||||
repeatability and reproducibility |
|
|||||
wine A |
wine B |
wine C |
wine D |
wine E |
wine F |
|
Method |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
No. of laboratories that submitted results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories that submitted compliant results |
11 |
12 |
11 |
13 |
11 |
10 |
No. of laboratories after elimination of outliners |
11 |
12 |
11 |
13 |
10 |
10 |
Number of measurement values without outliners |
36 |
38 |
38 |
23 |
34 |
34 |
Mean (mg/L) |
1.81 |
1.53 |
1.99 |
13.68 |
1.60 |
1.22 |
Repeatability s.d. Sr |
0.12 |
0.16 |
0.20 |
0.39 |
0.10 |
0.32 |
RSDr % |
6.6 |
10.6 |
10.2 |
2.9 |
6.6 |
26.1 |
Limit of repeatability r |
0.35 |
0.47 |
0.59 |
1.23 |
0.31 |
0.93 |
Relative limit of repeatability r% |
19.2% |
30.7% |
29.7% |
9.0% |
19.2% |
76.2% |
Reproducibility s.d. SR |
0.29 |
0.30 |
0.50 |
0.70 |
0.21 |
0.65 |
RSDR % |
15.8 |
19.8 |
25.1 |
5.1 |
13.1 |
53.2 |
Limit of reproducibility R |
0.82 |
0.87 |
1.43 |
2.05 |
0.60 |
1.87 |
Relative limit of reproducibility R% |
45.4% |
56.7% |
71.9% |
15.0% |
37.7% |
152.9% |
HORRAT R |
1.1 |
1.3 |
1.7 |
0.5 |
0.9 |
3.4* |
*presumed outlier, not considered for computation of fidelity.
 |
|
3-ethoxypropanol - Fidelity |
|
|||||
repeatability and reproducibility |
|
|||||
wine A |
wine B |
wine C |
wine D |
wine E |
wine F |
|
Method |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
No. of laboratories that submitted results |
12 |
12 |
12 |
12 |
12 |
11 |
No. of laboratories that submitted compliant results |
7 |
11 |
8 |
11 |
11 |
6 |
No. of laboratories after elimination of outliners |
7 |
11 |
8 |
10 |
11 |
6 |
Number of measurement values without outliners |
21 |
37 |
23 |
17 |
30 |
17 |
Mean (mg/L) |
1.7 |
3.6 |
1.4 |
3.7 |
3.0 |
1.1 |
Repeatability s.d. Sr |
1.0 |
0.4 |
0.1 |
0.4 |
0.4 |
0.1 |
RSDr % |
62.4 |
10.9 |
7.5 |
11.3 |
14.4 |
6.5 |
Limit of repeatability r |
3.2 |
1.4 |
0.3 |
2.1 |
1.3 |
0.2 |
Relative limit of repeatability r% |
189.2% |
39.3% |
22.7% |
55.9% |
42.7% |
20.2% |
Reproducibility s.d. SR |
1.4 |
0.6 |
0.5 |
0.7 |
0.8 |
0.2 |
RSDR % |
81.3 |
16.5 |
33.3 |
17.6 |
27.7 |
22.6 |
Limit of reproducibility R |
4.0 |
1.7 |
1.4 |
1.9 |
2.4 |
0.7 |
Relative limit of reproducibility R% |
239.8% |
47.5% |
97.7% |
52.6% |
80.1% |
67.7% |
HORRAT R |
5.5* |
1.3 |
2.2* |
1.3 |
2.0 |
1.4 |
*presumed outlier, not considered for computation of fidelity.
 |
|
Ethyl octanoate - Fidelity |
|
|||||
repeatability and reproducibility |
|
|||||
wine A |
wine B |
wine C |
wine D |
wine E |
wine F |
|
Method |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
No. of laboratories that submitted results |
12 |
12 |
12 |
12 |
12 |
12 |
No. of laboratories that submitted compliant results |
7 |
9 |
5 |
9 |
9 |
4 |
No. of laboratories after elimination of outliners |
7 |
9 |
5 |
8 |
9 |
4 |
Number of measurement values without outliners |
19 |
30 |
10 |
13 |
30 |
10 |
Mean (mg/L) |
0.8 |
1.1 |
0.7 |
1.0 |
1.0 |
0.8 |
Repeatability s.d. Sr |
0.03 |
0.2 |
0.3 |
0.1 |
0.2 |
0.4 |
RSDr % |
4.1 |
20.6 |
47.0 |
10.3 |
24.0 |
49.5 |
Limit of repeatability r |
0.1 |
0.7 |
1.2 |
0.3 |
0.7 |
1.4 |
Relative limit of repeatability r% |
12.5% |
60.7% |
171.1% |
34.4% |
70.6% |
171.3% |
Reproducibility s.d. SR |
0.2 |
0.3 |
0.6 |
0.1 |
0.3 |
0.8 |
RSDR % |
29.9 |
23.5 |
91.4 |
8.2 |
31.8 |
90.3 |
Limit of reproducibility R |
0.7 |
0.8 |
2.0 |
0.3 |
0.9 |
2.4 |
Relative limit of reproducibility R% |
88.8% |
67.9% |
292.8% |
25.3% |
92.0% |
288.8% |
HORRAT R |
1.8 |
1.5 |
5.4* |
0.5 |
2.0 |
5.5* |
*presumed outlier, not considered for computation of fidelity.
 |
|
Butyrolactone - Fidelity |
|
|||||
repeatability and reproducibility |
|
|||||
wine A |
wine B |
wine C |
wine D |
wine E |
wine F |
|
Method |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
No. of laboratories that submitted results |
10 |
10 |
10 |
10 |
10 |
10 |
No. of laboratories that submitted compliant results |
10 |
10 |
10 |
10 |
10 |
10 |
No. of laboratories after elimination of outliners |
8 |
8 |
7 |
10 |
9 |
8 |
Number of measurement values without outliners |
26 |
28 |
24 |
17 |
30 |
28 |
Mean (mg/L) |
12.8 |
10.9 |
18.8 |
11.3 |
8.2 |
19.1 |
Repeatability s.d. Sr |
1.4 |
1.2 |
1.6 |
1.2 |
2.9 |
2.1 |
RSDr % |
11.1 |
10.6 |
8.6 |
10.3 |
34.9 |
11.1 |
Limit of repeatability r |
4.2 |
3.4 |
4.8 |
3.9 |
8.5 |
6.3 |
Relative limit of repeatability r% |
33.1% |
31.2% |
25.5% |
34.3% |
102.7% |
32.8% |
Reproducibility s.d. SR |
2.6 |
2.0 |
2.6 |
3.9 |
2.9 |
2.8 |
RSDR % |
19.9 |
18.2 |
13.9 |
34.4 |
35.6 |
14.5 |
Limit of reproducibility R |
7.4 |
5.7 |
7.6 |
11.6 |
8.5 |
8.0 |
Relative limit of reproducibility R% |
57.9% |
52.7% |
40.7% |
103.1% |
102.9% |
42.1% |
HORRAT R |
1.8 |
1.6 |
1.4 |
3.1* |
3.1* |
1.4 |
*presumed outlier, not considered for computation of fidelity.
 |
|
Diethyl succinate - Fidelity |
|
|||||
repeatability and reproducibility |
|
|||||
wine A |
wine B |
wine C |
wine D |
wine E |
wine F |
|
Method |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
No. of laboratories that submitted results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories that submitted compliant results |
13 |
10 |
13 |
10 |
12 |
13 |
No. of laboratories after elimination of outliners |
11 |
10 |
13 |
10 |
12 |
12 |
Number of measurement values without outliners |
40 |
34 |
46 |
17 |
35 |
42 |
Mean (mg/L) |
6.5 |
3.3 |
15. 9 |
4.0 |
3.7 |
10.7 |
Repeatability s.d. Sr |
0.7 |
0.4 |
1.8 |
1.5 |
0.6 |
1.9 |
RSDr % |
11.0 |
11.2 |
11.2 |
37.8 |
16.1 |
17.4 |
Limit of repeatability r |
2.1 |
1.1 |
5.1 |
5.0 |
1.7 |
5.4 |
Relative limit of repeatability r% |
31.7% |
32.6% |
32.1% |
126.4% |
47.1% |
50.2% |
Reproducibility s.d. SR |
1.3 |
1.5 |
3.2 |
1.9 |
1.3 |
2.4 |
RSDR % |
20.5 |
44.9 |
20.0 |
48.6 |
35.4 |
22.0 |
Limit of reproducibility R |
3.8 |
4.3 |
9.0 |
5.8 |
3.7 |
6.7 |
Relative limit of reproducibility R% |
58.6% |
129.2% |
56.9% |
145.6% |
101.7% |
63.0% |
HORRAT R |
1.7 |
3.4* |
1.9 |
3.7* |
2.7* |
2.0 |
*presumed outlier, not considered for computation of fidelity.
 |
|
2-phenylethanol - Fidelity |
|
|||||
repeatability and reproducibility |
|
|||||
wine A |
wine B |
wine C |
wine D |
wine E |
wine F |
|
Method |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
ISO 5725-2 |
No. of laboratories that submitted results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories that submitted compliant results |
13 |
13 |
13 |
13 |
13 |
13 |
No. of laboratories after elimination of outliners |
12 |
12 |
12 |
12 |
12 |
13 |
Number of measurement values without outliners |
42 |
42 |
42 |
21 |
42 |
46 |
Mean (mg/L) |
19.4 |
18.8 |
47.0 |
18.7 |
15.6 |
53.1 |
Repeatability s.d. Sr |
1.4 |
2.4 |
4.5 |
1.0 |
1.4 |
4.2 |
RSDr % |
7.4 |
13.0 |
9.6 |
5.3 |
9.1 |
7.8 |
Limit of repeatability r |
4.2 |
7.0 |
13.0 |
3.2 |
4.1 |
11.9 |
Relative limit of repeatability r% |
21.5% |
37.4% |
27.7% |
17.1% |
26.3% |
22.5% |
Reproducibility s.d. SR |
2.9 |
3.0 |
6.8 |
1.4 |
1.7 |
8.8 |
RSDR % |
15.1 |
16.2 |
14.5 |
7.6 |
11.0 |
16.6 |
Limit of reproducibility R |
8.4 |
8.7 |
19.5 |
4.2 |
4.9 |
25.2 |
Relative limit of reproducibility R% |
43.1% |
46.2% |
41.4% |
22.4% |
31.5% |
47.4% |
HORRAT R |
1.5 |
1.6 |
1.6 |
0.7 |
1.0 |
1.9 |
 |