Analysis of Micronutrients in Fruit Juice Using the Avio 200 ICP-OES
QUANTITATIVE ANALYSIS OF ELEMENTS IN WINE · 2018-11-01 · ICP- Spectrometry coupled to Mass...
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QUANTITATIVE ANALYSIS OF ELEMENTS IN WINE
USING “STATE OF THE ART” SPECTROSCOPY
U. Oppermann & J. KnoopShimadzu Europa GmbH, Duisburg
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Wine Analysis - Overview
Introduction
European Norms EN/DIN
Analysis of Wine
AAS: sequential
ICP-OES: simultaneous
ICP-MS: ultra trace
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Wine Production
1. Vintage2. Mashing3. Wine pressing4. Fermentation5. Tapping6. Aging7. Storage
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Regulations
European Union wine regulation
Latest update from 9th March 2012
Testing physical parameters
Density
Turbidity
Color
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Control Limits
Aluminium 8.00 mg/l
Arsenic 0.10 mg/l
Lead 0.25 mg/l
Boron 80 mg/l
Cadmium 0.01 mg/l
Copper 2.00 mg/l
Zinc 5.00 mg/l
Tin 1.00 mg/l
Trichloromethane 0.10 mg/l
Trichloroethene 0.10 mg/l
Tetrachloroethene 0.10 mg/l
Trichloromethane, Trichloroethene & Tetrachlorethene(total)
0.20 mg/l
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Copper/ Zinc
Concentration
• Metallic bitter taste > 1.0 mg/L
• Generate turbidity > 0.5 mg/L
• Copper oxidation > 0.5 mg/L
• Reducing the flavour >0.5 mg/L
• Influence on fermentation > 20 mg/L
Table 1: Influence of copper concentrations in wine
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Boron
Fertilizer
5 – 500 g/ha
Accumulated in the ground
B consumption during growth 200 g/ha
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Sulfur
Conservation, to prevent Oxidization
European Limits:
Dry Wine: 160 – 260 mg/L
Medium Wine: 300 – 350 mg/L
Sweet Wine: 400 mg/L
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Antimony?
Wine in PET- Bottles – Prof. Dr. Rainer Jung, University Rhein/Main
Languedoc Producer SKALLI in 2010: 2,5 Mio. PET bottles
http://blog.campus-geisenheim.de/index.php/2010/12/wein-aus-pet-flaschen-und-bechern-prof-dr-rainer-jung-im-interview-mit-dem-wiesbadener-kurier/
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Quantitative Analysis (1)
Sequential…..…in Flame and furnace atomization using AA-7000Determination of Cu, Zn, Al, Cd, Pb, und P
Important: BGC SR/D2
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Quantitation of Heavy Metals(2)
….using simultaneous ICP-OES: ICPE-9820
http://www.shimadzu.eu/sites/default/files/AN_SCA_115_023_Wine_0.pdf
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Dual View: Axial & Radial
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Vacuum Spectrometer
CCD Detector
ICP
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Echelle Spectrum
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P 213.62nmCu 213.60nm
105order
104order
106order
1 picture element (pixel)
Echelle Spectrum
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Sample Preparation
• Dilution with H2O 1:1• Alcohol concentration approx. 5 %• HNO3 concentration 0.1 %• Calibration range: 0.005 to 50 mg/L.
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Argon Plasma with Minitorch
Parameters for element concentrations acc. to European wine directive:
RF Power 1.2 kW
PL Gas 10 L/min
AX Gas 0.6 L/min
CA Gas 0.7 L/min
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Multielement Calibration
Selected Calibration range from: 0 - 1000 µg/L
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Boron Calibration 5 to 1000 µg/L
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Boron Peak Profile
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Antimony Calibration 5 to 1000 µg/L
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Antimony Peak Profile
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Quantitation of Heavy Metals(3)
….using high sensitivity ICPMS-2030
http://www.shimadzu.eu/sites/default/files/AN_SCA_115_023_Wine_0.pdf
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ICP- Spectrometry coupled to Mass
Analysis Technique: Multi-element analysis : simultaneous as in ICP-OES
Extremely sensitive => analysis of ultra-traces (< ppb => ppt).
Mini Torch
TechnologyMass detector
Detection, identification
and quantification of
ions
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Welcome in the World of Traces
1a 2a 3b 4b 5b 6b 7b 1b 2b 3a 4a 5a 6a 7a 0
Na Mg Al Si P S Cl Ar
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
Cs Ba *L Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
Fr Ra **A
*L La Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
**A Ac Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
He<1ppt
O F Ne10~100pptOther
1~10ppt
N
8
Li Be B C
H
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Multielement Analysis
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Analytical Results
Element concentrations are below MAC´s
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Outlook
• Bordeauxmixture: CaCO3 + CuSO4
• Fungicide• Accumulation in soil• Ban from 2016?• Until 2018 tolerated in EU
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Conclusion
AAS, ICP-OES and ICP- MS are ideal tools for
quantification of wine.
The systems are able to accept a wide variety
of samples and offering the flexibility for a
perfect match allowing easy operation and
high sample throughput.
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Thank You….
…and please enjoy your wine!