BFR Annex 3 IRMS Part 1

GERMAN FEDERAL INSTITUTE
FOR RISK ASSESSMENT
IRMS – Stable Isotopes – Part 1

Dr. Melanie Gimpel
Overview
• What is an isotope?
• Isotopic fractionation
• Geographical origin
• Botanical origin
• Isotopic methods in the food area
• Delta notation
Melanie Gimpel, Stable Isotopes Analysis of Wine – IRMS Introduction page 2

What is an isotope?
Different atomic mass
12 Same atomic number 13

6 C 6 C
“light“ isotope
98.9 % “heavy“ isotope
1.1 %
Neutron
Proton
„Isotope“ (old greek) = ísos, „equal“ + topós, „place“: same place in the periodic table
Natural abundance of the heavy isotopes
• Precise Isotope Ratios
Element Minor Isotope Natural Abundance [%]
Hydrogen 2H (D) 0.01557
Carbon 13C
1,11140
Nitrogen 15N
0.36630
Oxygen 18O
0.20004
Sulfur 34S
4.21500

Information from stable isotopes
Stable Isotopes Information provided

Carbon Feed, plant type (photosynthetic pathway)
13C/12C
Hydrogen Geographical origin

2H/1H or D/H
Oxygen Geographical origin (sea level and distance

18O/16O from the shore)
Nitrogen Agricultural practice
15N/14N
Sulphur Geological origin, agricultural practice

34S/32S
Strontium Geological origin

87Sr/86Sr

13C abundance in the environment I

13C abundance in the environment II

Isotopic fractionation
• Isotopic fractionation is the shift in the abundance of the isotopes of an
element caused by physical or chemical processes.
• The fractionation is thermodynamic and thus temperature-dependent.
• Isotopic effects are primarily influenced by the relative mass difference of

the isotopes.
• Isotopic effects and the resulting isotope fractionations therefore lead to

particularly significant isotope shifts for elements with relatively low mass
(approx. 40 u).
• Examples of isotope fractionating processes:

• evaporation
• freezing
• precipitation
• chemical reactions

δ13C - Isotope fractionation by photosynthesis
C3 plant C4 plant CAM
CO2 fixation Calvin cycle Hatch-Slack cycle Crassulacean Acid

Metabolism
Primary product 3-Phosphoglyceric Oxaloacetic acid C4 pathway via
acid (C3) (C4) malate
13C depletion Relatively strong, Relatively low, Intermediate
„light“ plants „heavy“ plants position
δ13C values -24…-32 [‰] -10…-16 [‰] -12…-30 [‰]
Examples of food Wheat, rye, rice, Maize, sugar Pineapple, vanilla,

sugar beet, cane, millet succulent plants
grapes, potatoes

δ2H and δ18O - Geographical Origin –

δ2H and δ18O- Geographical Origin II - Rainout effect
Source: http://web.sahra.arizona.edu/programs/isotopes/oxygen.html

δ2H and δ18O- Geographical Origin II – Global Meteoric Water
Line
Source: http://web.sahra.arizona.edu/programs/isotopes/oxygen.html

Delta (δ) Notation
• Variations in the natural abundance of stable isotopes are expressed using delta
(δ) notation.
ℎ ℎ )*+
• Isotopic ratio R: ( )= ( = ),
ℎ ℎ +
)-.
0
( = )/ (=
. 1
• Delta (δ) in ‰: δ ‰ =[ !"#
- 1] *1000
$ %& '&
2)*34567 = -25,5 ‰
• Expression of isotopic ratios as
ppm, permil ‰ , at% (Atom Percent) and APE (Atom Percent Excess)

Primary Calibration Material
• Isotopic ratios are expressed versus these materials that define the δ-
scales
Element Ratio Isotope delta scale
Hydrogen VSMOW
2H/1H (Standard Mean Ocean Water)
Carbon VPDB
13C/12C (Pee Dee Belemnite)
Nitrogen Atmospheric Nitrogen
15N/14N
(Air N2)
Oxygen
18O/16O VSMOW
• Reference standard materials are available from the International Atomic Energy
Agency (IAEA) in Vienna, the NIST (National Institute of Standards and
Technology) and the USGS (United States Geological Survey)

International Methods
Year Method Product Fraction Techniques Isotope ratios
1987 OIV method OIV-MA-AS311-05 Wine Ethanol SNIF-NMR (D/H)I, (D/H)II, R
1991 AOAC method 998.12 Honey Honey, proteins IRMS 13C/12C
1993 CEN (TC174 N108, ENV 12140) Fruit juice Sugar IRMS 13C/12C
1995 AOAC method 995.17 Fruit juice Ethanol (from SNIF-NMR (D/H)I, (D/H)II, R
fermentation)
1996 OIV method OIV-MA-AS2-12 Wine Water IRMS 18O/16O
1997 CEN (TC174 N109, ENV 12141) Fruit Juice Water IRMS 18O/16O
2000 AOAC Official method 2000.19 Maple syrup Ethanol (from SNIF-NMR (D/H)I, (D/H)II, R
fermentation)
2001 OIV method OIV-MA-AS312-06 Wine Ethanol IRMS 13C/12C
2004 AOAC method 2004.01 Fruit juice & Ethanol (from IRMS 13C/12C
maple syrup fermentation)

2006 AOAC method 2006.05 Vanillin Vanillin SNIF-NMR (D/H)I
2010 OIV method OIV-AS312-07 Wine Glycerol GC-C-IRMS, 13C/12C
HPLC-IRMS
2014 OIV method OIV-MA-AS314-03 Sparkling CO2 IRMS 13C/12C
Wine
2017 OIV method Wine Glucose, HPLC-IRMS 13C/12C
RESOLUTION OIV-OENO 479- Fructose,

2017 Glycerol,
Ethanol
GERMAN FEDERAL INSTITUTE
FOR RISK ASSESSMENT
Thank you for your attention

Melanie Gimpel
German Federal Institute for Risk Assessment

Max-Dohrn-Str. 8-10  10589 Berlin, GERMANY
Phone +49 30 - 184 12 - 0  Fax +49 30 - 184 12 - 47 41
[email protected]  www.bfr.bund.de/en

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GERMAN FEDERAL INSTITUTE

FOR RISK ASSESSMENT

IRMS – Stable Isotopes – Part 1

• Isotopic methods in the food area

Melanie Gimpel, Stable Isotopes Analysis of Wine – IRMS Introduction page 2

12 Same atomic number 13

• Precise Isotope Ratios

Element Minor Isotope Natural Abundance [%]

Hydrogen 2H (D) 0.01557

Melanie Gimpel, Stable Isotopes Analysis of Wine – IRMS Introduction page 4

Stable Isotopes Information provided

Hydrogen Geographical origin

Oxygen Geographical origin (sea level and distance

Sulphur Geological origin, agricultural practice

Strontium Geological origin

Melanie Gimpel, Stable Isotopes Analysis of Wine – IRMS Introduction page 5

Melanie Gimpel, Stable Isotopes Analysis of Wine – IRMS Introduction page 6

Melanie Gimpel, Stable Isotopes Analysis of Wine – IRMS Introduction page 7

• The fractionation is thermodynamic and thus temperature-dependent.

• Isotopic effects are primarily influenced by the relative mass difference of

• Isotopic effects and the resulting isotope fractionations therefore lead to

• Examples of isotope fractionating processes:

Melanie Gimpel, Stable Isotopes Analysis of Wine – IRMS Introduction page 8

C3 plant C4 plant CAM

CO2 fixation Calvin cycle Hatch-Slack cycle Crassulacean Acid

δ13C values -24…-32 [‰] -10…-16 [‰] -12…-30 [‰]

Examples of food Wheat, rye, rice, Maize, sugar Pineapple, vanilla,

Melanie Gimpel, Stable Isotopes Analysis of Wine – IRMS Introduction page 9

Melanie Gimpel, Stable Isotopes Analysis of Wine – IRMS Introduction page 10

Melanie Gimpel, Stable Isotopes Analysis of Wine – IRMS Introduction page 11

Melanie Gimpel, Stable Isotopes Analysis of Wine – IRMS Introduction page 12

• Expression of isotopic ratios as

Melanie Gimpel, Stable Isotopes Analysis of Wine – IRMS Introduction page 13

Element Ratio Isotope delta scale

Melanie Gimpel, Stable Isotopes Analysis of Wine – IRMS Introduction page 14

maple syrup fermentation)

RESOLUTION OIV-OENO 479- Fructose,

Thank you for your attention

German Federal Institute for Risk Assessment

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