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Seguimiento en línea de la vinificación usando un
sistema de inyección en flujo
P. Pérez Juan 2; J. González-Rodríguez1; and M.D. Luque de Castro 3
(1) R & D Department, Pérez Barquero S.A., Avda. de Andalucía 27, E-14550 Montilla (Córdoba) Spain
Phone: 34-957650500, Fax: 34-957650208, e-mail: [email protected]
(2) LIEC, Laboratory and Enological Research of Castilla, Polígono industrial. Calle XV, parcela R-113, E-13200
Manzanares (Ciudad Real), Spain. Phone: 34-926647115, e-mail: [email protected]
(3) Analytical Chemistry Department, Annex C-3, Campus of Rabanales, University of Córdoba, E-14071 Córdoba, Spain
Phone: 34-957218615; e-mail: [email protected]
Introduction
An approach for on-line monitoring of the alcoholic fermentation (alcohol degree, volatile acidity, total phenols and anthocyans index, catechins, readily
assimilable nitrogen, urea and ammonium) is proposed. These are the main parameters monitored in fermentation processes in order to both obtain a quality
product and avoid any problem during the fermentation stage or subsequent stages, for red and white wines and must. The methods have been characterised in
terms of dynamic linear ranges (0-12% for alcoholic degree, 0.02-1 g of tartaric acid/l for volatile acidity, 20-70 units for total phenols and 20-500 mg/l for
anthocyan index, 10-250 mg of gallic acid/l for catechins, 15-400 mg/l for readily assimilable nitrogen and 0-25 mg/l for both urea and ammonium), repetitivity,
reproducibility and limits of detection and quantification. The full automation of the methods can be achieved by a computer provided with the appropriate
software and active interfaces for controlling both pumps and valves and passive interfaces for collecting the data from the detectors. The on-line monitoring of
the target parameters is thus performed at the required frequency.
Readily Assimilable Nitrogen
Abbreviations:
PP: Peristaltic Pump, R: Reactor, D: Detector, m: membrane
IV: Injection Valve, SV: Selection Valve, TB: Thermostatic Bath
W: Waste
Total Phenols and
Anthocyans
Urea and Ammonium
FLOW
Grape
PROCESS
Reception of Raw material
Pre-fermentation
New wine
Urea
Readily Assimilable Nitrogen
Fermentation process
Red wines: Anthocyans, Catechins
Total Phenols
New wine maduration
Ethanol, Urea, Volatile Acidity,
Ammonium. Red wines: Catechins,
Anthocyans, Total Phenols
Vintage wine
Catechins
CONTROL
Ageing
Ageing wine
Final processes
Market
Ethanol, Urea, Volatile Acidity,
Readily Assimilable Nitrogen
Red wines: Total Phenols, Anthocyans,
Catechins
Ethanol
Volatile Acidity
Analytical features
Methods
Parameter
Ethanol
Volatile
Acidity
Total Phenols
Anthocyans
Catechins
Assimilable
Nitrogen
Urea
Ammonium
Ref.
FI
Ref.
FI
Ref.
FI
Ref.
FI
Ref.
FI
Ref.
FI
Ref.
FI
Ref.
FI
Repeatability
0,13
0,26
0,033
0,038
1,021
2,122
4,232
6,233
3.10
2.57
4.10
1.35
0.185
0.523
0.123
0.432
Sr (g/l)
0,05
0,15
0,012
0,013
0,032
0,043
0,061
0,081
0.56
0.45
0.67
0.472
0.066
0.098
0.041
0.065
Reproducibility
0,29
0,31
0,042
0,046
2,312
3,012
9,232
12,21
5.30
3.56
6.30
3.94
0.214
1.345
-
1.212
SR (g/l)
0,09
0,19
0,015
0,016
0,091
0,123
0,802
1,083
1.02
0.95
1.98
1.23
0.076
0.132
-
0.12
r
-
1,66
-
1,32
-
1,81
-
1,76
-
0.646
-
0.497
-
2.205
-
2.489
FobsR
-
1,49
-
1,18
-
1,83
-
1,82
-
0.867
-
0.386
-
3.017
-
-
F1-α
-
1,69
-
1,84
-
1,84
-
1,84
-
1.69
-
1.69
-
4.24
-
4.24
LOD
0,02
0,01
0,041
0,032
0,231
0,229
0,953
0,543
2.2
4.5
8
10
0.15
0.9
0.08
0.6
LOQ
0,07
0,03
0,084
0,086
0,455
0,530
1,380
1,110
6.1
5.85
9.4
11.6
-
1.02
-
0.67
Samples h-1
3
7
5
10
40
50
3
25
3
23
2
20
9
15-16
9
15-16
Fobs
Units
Ethanol: % (v/v); Volatile Acidity: g tartaric/l; Total Phenols: Abs units; Catechins: mg gallic/l; Anthocyans, Assimilable Nitrogen, Urea and Ammonium: mg/l
Conclusions
FI methods are simple, unexpensive and easy to implement
Pervaporation allows on-line
shortcomings of gas diffusion
monitoring
without
High sampling rates and no pretreatments are needed
Good correlation with the reference methods
the
Seguimiento en línea de la vinificación usando un
sistema de inyección en flujo
P. Pérez Juan 2; J. González-Rodríguez1; and M.D. Luque de Castro 3
(1) R & D Department, Pérez Barquero S.A., Avda. de Andalucía 27, E-14550 Montilla (Córdoba) Spain
Phone: 34-957650500, Fax: 34-957650208, e-mail: [email protected]
(2) LIEC, Laboratory and Enological Research of Castilla, Polígono industrial. Calle XV, parcela R-113, E-13200
Manzanares (Ciudad Real), Spain. Phone: 34-926647115, e-mail: [email protected]
(3) Analytical Chemistry Department, Annex C-3, Campus of Rabanales, University of Córdoba, E-14071 Córdoba, Spain
Phone: 34-957218615; e-mail: [email protected]
Introduction
An approach for on-line monitoring of the alcoholic fermentation (alcohol degree, volatile acidity, total phenols and anthocyans index, catechins, readily
assimilable nitrogen, urea and ammonium) is proposed. These are the main parameters monitored in fermentation processes in order to both obtain a quality
product and avoid any problem during the fermentation stage or subsequent stages, for red and white wines and must. The methods have been characterised in
terms of dynamic linear ranges (0-12% for alcoholic degree, 0.02-1 g of tartaric acid/l for volatile acidity, 20-70 units for total phenols and 20-500 mg/l for
anthocyan index, 10-250 mg of gallic acid/l for catechins, 15-400 mg/l for readily assimilable nitrogen and 0-25 mg/l for both urea and ammonium), repetitivity,
reproducibility and limits of detection and quantification. The full automation of the methods can be achieved by a computer provided with the appropriate
software and active interfaces for controlling both pumps and valves and passive interfaces for collecting the data from the detectors. The on-line monitoring of
the target parameters is thus performed at the required frequency.
Readily Assimilable Nitrogen
Abbreviations:
PP: Peristaltic Pump, R: Reactor, D: Detector, m: membrane
IV: Injection Valve, SV: Selection Valve, TB: Thermostatic Bath
W: Waste
Total Phenols and
Anthocyans
Urea and Ammonium
FLOW
Grape
PROCESS
Reception of Raw material
Pre-fermentation
New wine
Urea
Readily Assimilable Nitrogen
Fermentation process
Red wines: Anthocyans, Catechins
Total Phenols
New wine maduration
Ethanol, Urea, Volatile Acidity,
Ammonium. Red wines: Catechins,
Anthocyans, Total Phenols
Vintage wine
Catechins
CONTROL
Ageing
Ageing wine
Final processes
Market
Ethanol, Urea, Volatile Acidity,
Readily Assimilable Nitrogen
Red wines: Total Phenols, Anthocyans,
Catechins
Ethanol
Volatile Acidity
Analytical features
Methods
Parameter
Ethanol
Volatile
Acidity
Total Phenols
Anthocyans
Catechins
Assimilable
Nitrogen
Urea
Ammonium
Ref.
FI
Ref.
FI
Ref.
FI
Ref.
FI
Ref.
FI
Ref.
FI
Ref.
FI
Ref.
FI
Repeatability
0,13
0,26
0,033
0,038
1,021
2,122
4,232
6,233
3.10
2.57
4.10
1.35
0.185
0.523
0.123
0.432
Sr (g/l)
0,05
0,15
0,012
0,013
0,032
0,043
0,061
0,081
0.56
0.45
0.67
0.472
0.066
0.098
0.041
0.065
Reproducibility
0,29
0,31
0,042
0,046
2,312
3,012
9,232
12,21
5.30
3.56
6.30
3.94
0.214
1.345
-
1.212
SR (g/l)
0,09
0,19
0,015
0,016
0,091
0,123
0,802
1,083
1.02
0.95
1.98
1.23
0.076
0.132
-
0.12
r
-
1,66
-
1,32
-
1,81
-
1,76
-
0.646
-
0.497
-
2.205
-
2.489
FobsR
-
1,49
-
1,18
-
1,83
-
1,82
-
0.867
-
0.386
-
3.017
-
-
F1-α
-
1,69
-
1,84
-
1,84
-
1,84
-
1.69
-
1.69
-
4.24
-
4.24
LOD
0,02
0,01
0,041
0,032
0,231
0,229
0,953
0,543
2.2
4.5
8
10
0.15
0.9
0.08
0.6
LOQ
0,07
0,03
0,084
0,086
0,455
0,530
1,380
1,110
6.1
5.85
9.4
11.6
-
1.02
-
0.67
Samples h-1
3
7
5
10
40
50
3
25
3
23
2
20
9
15-16
9
15-16
Fobs
Units
Ethanol: % (v/v); Volatile Acidity: g tartaric/l; Total Phenols: Abs units; Catechins: mg gallic/l; Anthocyans, Assimilable Nitrogen, Urea and Ammonium: mg/l
Conclusions
FI methods are simple, unexpensive and easy to implement
Pervaporation allows on-line
shortcomings of gas diffusion
monitoring
without
High sampling rates and no pretreatments are needed
Good correlation with the reference methods
the