THE BRITISH BEEF ORIGIN PROJECT (BBOP)

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THE BRITISH BEEF ORIGIN PROJECT (BBOP)

Authors: Dr Simon Kelly

Food & Environment research Agency

Sand Hutton

York

YO41 1LZ

Key workers: Niusa Marigheto (IFR)

Malcolm Baxter, Nicola Brereton, Simon Kelly

& Martin Rose (Fera)

Dennis Homer & Kim Matthews (AHDB/EBLEX)

Stefan Hoelzl, Susanne Rummel & Christian Dekannt

(sub-contractors, BSPG)

Meat Promotion Agencies Agriculture & Horticulture Development Board - EBLEX

Hybu Cig Cymru – HCC, Meat Promotion Wales

Quality Meat Scotland

Start Date: 3rd December 2007

Date of report March 2010

Sponsor: UK Food Standards Agency

FSA Project Number: Q01123

The British Beef Origin Project (BBOP - Q01123) – Final Report

Contents

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Table of Contents 1 Executive Summary ................................. ........................................................................ 4

2 Background to project ............................. ........................................................................ 5

2.1 Social and economic context ............................................................................................................................. 5

2.2 Scope of project ................................................................................................................................................ 6

2.3 References ........................................................................................................................................................ 6

3 Background to stable isotope and multi-element anal ysis in food origin

determinations .................................... ............................................................................. 7

3.1 Natural abundance isotope ratios ...................................................................................................................... 7

3.2 Delta notation .................................................................................................................................................... 8

3.3 Strontium isotopic ratios .................................................................................................................................... 9

3.4 Multi-element (trace element) concentrations .................................................................................................. 10

3.5 References ...................................................................................................................................................... 10

4 Literature Review ................................. .......................................................................... 11

4.1 Beef meat ........................................................................................................................................................ 11

4.2 Lamb meat ...................................................................................................................................................... 13

4.3 Poultry meat .................................................................................................................................................... 13

4.4 Summary ......................................................................................................................................................... 14

4.5 References ...................................................................................................................................................... 15

5 Authentic beef sampling ........................... .................................................................... 17

5.1 English beef sampling ..................................................................................................................................... 17

5.2 Welsh beef sampling ....................................................................................................................................... 17

5.3 Scottish beef sampling .................................................................................................................................... 17

5.4 Sample logging and Storage ........................................................................................................................... 17

6 Experimental tasks ................................ ........................................................................ 19

6.1 Preparation of beef muscle defatted dry mass and measurement of the bio-element stable isotope composition

(δ2H‰, δ13C‰, δ15N‰ and δ34S‰) ........................................................................................................................... 19

6.2 Extraction of strontium from beef muscle tissue ............................................................................................... 19

6.3 Multi-element measurements by ICP-MS ........................................................................................................ 19

7 Results and discussion ............................ ..................................................................... 20

7.1 Evaluation of authentic British beef DDM hydrogen isotope (δ2H‰) measurements ........................................ 20

7.2 Evaluation of authentic British beef DDM carbon isotope (δ13C‰) measurements ........................................... 23

7.3 Evaluation of authentic British beef DDM nitrogen isotope (δ15N‰) measurements ......................................... 25

7.4 Evaluation of authentic British beef DDM sulphur isotope (δ34S‰) measurements .......................................... 26

7.5 Evaluation of authentic British beef DDM strontium isotope ratio (87Sr/86Sr) measurements ............................. 28

7.6 Multivariate analysis of authentic British beef elemental and stable isotope data ............................................. 31

7.7 References ...................................................................................................................................................... 36

8 Conclusions ....................................... ............................................................................ 37

9 Recommendations for further work .................. ........................................................... 37

10 Publications and other outputs .................... ................................................................ 38

10.1 Papers in preparation ................................................................................................................................. 38

10.2 Scientific presentations ............................................................................................................................... 38

11 Appendix I – Complete list of authentic beef sample s and data .............................. 39

12 Appendix II – Standard Operating Procedures of t he determination H, C, N, S stable

isotope ratios, 87Sr/86Sr isotope ratios and the multi-element composition of beef 91

Acknowledgements 122

The British Beef Origin Project (BBOP - Q01123) – F inal Report

Section 1: Executive Summary

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GLOSSARY

δ13C‰, δ13C‰PDB "Delta carbon-13 per mil''. The 13C/12C ratio expressed relative to the

international standard Pee Dee Belemnite. 13C/12C The ratio of the isotope of carbon with atomic mass 13 to the isotope of

carbon with atomic mass 12 PDB Pee Dee Belemnite - Calcium carbonate used as an international

standard for which the 13C/12C ratio is precisely known and is defined as 0 ‰ on the δ13C scale.

δ15N‰, δ15N‰AIR "Delta nitrogen -15 per mil''. The 15N/14N ratio expressed relative to the

international standard AIR. 15N/14N The ratio of the isotope of nitrogen with atomic mass 15 to the isotope of

nitrogen with atomic mass 14. AIR AIR - atmospheric air used as an international standard for which the

15N/14N ratio is precisely known and is defined as 0 ‰ on the δ15N scale. δ2H‰, δ2H‰VSMOW "Delta deuterium per mil''. The 2H/1H ratio expressed relative to the

international standard VSMOW. 2H/1H The ratio of the isotope of hydrogen with atomic mass 2 to the isotope of

hydrogen with atomic mass 1. VSMOW Vienna Standard Mean Ocean Water used as an international standard

for which the 2H/1H ratio is precisely known and is defined as 0 ‰ on the δ2H scale.

δ34S‰, δ34S‰CDT "Delta sulphur-34 per mil''. The 34S/32S ratio expressed relative to the

international standard CDT. 34S/32S The ratio of the isotope of sulphur with atomic mass 34 to the isotope of

sulphur with atomic mass 32. CDT Cañon Diablo Troilite used as an international standard for which the

34S/32S ratio is precisely known and is defined as 0 ‰ on the δ34S scale. EA Elemental Analyser SD The sample standard deviation of the mean, σ(n - 1) Abs diff The absolute difference between two measurements on separate

subsamples of the same test material. N Number of measurements IRMS Isotope Ratio Mass Spectrometry Discriminant analysis A supervised pattern recognition technique used to find a linear

combination of variables which characterize or separate two or more classes of objects or events.

Isotopologue The isotopologue of a chemical species has at least one atom with a

different number of neutrons than the parent.


Section 1: Executive Summary

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1 EXECUTIVE SUMMARY

• The main objective of this research was to apply isotopic and elemental analyses, in

combination with statistical processing, to distinguish the origin of beef meat from

cattle reared in England, Scotland and Wales. In this respect, the findings in this report

demonstrate that it is possible with a high degree of certainty to determine the origin of

British beef.

• The techniques described here are at their most useful when applied to specific origin

problems such as differentiating English beef from Scottish beef or Orkney (PDO) beef

from other Scottish beef. Consequently, the methodology in its current state can be

used to provide reliable origin information, but this is dependent upon the ‘intelligence’

supplied with the sample.

• The success of the multivariate statistical analysis of all the combined data, from

stable isotope ratio analysis and elemental concentrations, is summarised below:

Geographical origin of beef Correct classification rate (Cross-validated)

Wales or Scotland? 95 %

England or Scotland? 91%

England or Wales? 71%

Orkney or other Scotland? 95%

• Currently, stable isotope and elemental ‘finger-printing’ offers the only hypothesis

driven approach to establish the geographical origin of food. For example, our

understanding of how hydrogen isotopes in water vary over the British Isles (due to the

effects of the hydrological cycle) have been shown to be mirrored in bovine skeletal

muscle for cattle reared in Britain.

• Further research is required to validate the methodology for cooked and processed

beef. This would be extremely valuable for the assessment of beef origin in ready

meals and restaurant meals. Furthermore, the reference database currently lacks

samples from Northern Ireland and the Republic of Ireland.


Section 2: Background to project

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2 BACKGROUND TO PROJECT

2.1 Social and economic context

The European Union Protected Food Names Schemes came into force in 1993 and

offers an independent inspection and labelling system for the protection of food names on a

geographical basis or traditional recipe basis. A number of British beef products have been

protected under the scheme and there are also a number of others for which protection is

being sought. There are three designations:

• Protected Designation of Origin (PDO) - open to products which are produced and processed and prepared within a particular geographical area, and with features and characteristics which must be due to the geographical area e.g. Orkney beef.

• Protected Geographical Indication (PGI) - open to products which must be produced or processed or prepared within the geographical area and have a reputation, features or certain qualities attributable to that area e.g. Scotch beef and Welsh beef.

• Traditional Speciality Guaranteed (TSG) - open to products which are traditional or have customary names and have a set of features which distinguish them from other similar products. These features must not be due to the geographical area the product is produced in nor entirely based on technical advances in the method of production.

The original regulations (Council Regulation (EC) 2081/92 and 2082/92) were replaced in

March 2006 by Council Regulation (EC) 509/2006 for TSG products and Council Regulation

(EC) 510/2006 for PDO/PGI products. Manufacturers of protected foods usually charge a

premium for their produce due to increased production costs and consequently economic

incentives exist to replace genuine articles with inferior ones for financial gain.

As a result of concerns relating to BSE, Human variant CJD and the impact on the

internal market for beef, the EU introduced far-reaching legislation concerning labelling of

beef. An initial voluntary labelling system, introduced in 1997 (Council Regulation (EC) No

820/97 – now repealed), requires operators who label beef with claims about its origin,

production methods and characteristics to seek Government approval to make such claims.

This was enhanced by a compulsory system; the first of two stages of legislation was

introduced on 1st September 2000 (Regulation (EC) No 1760/2000 of the European

Parliament and of the Council) and initiated a system to provide correct, complete and

transparent information designed to enable consumers to make an informed choice about

retail beef in the marketplace and further designed to enable enforcement agencies to trace

back retail beef to where it originated. The second stage came into force on 1st January,

2002 and required the inclusion of additional precise information relating to where the source

animal of retail beef had been born and reared.


Section 2: Background to project

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Required labelling information includes:

(a) A traceability reference number or code;

(b) The name of the Member State or non-EC country in which the

animal or group of animals were born;

(c) The name of the Member State or non-EC country in which the

animal or group of animals were raised;

(d) ‘Slaughtered in: [name of Member State or non-EC country]’;

(e) Approval number of slaughterhouse;

(f) ‘Cutting/cut in: [name of Member State or non-EC country]’;

(g) Approval number(s) of cutting plant(s).

The introduction of compulsory beef labelling legislation means there is a growing

requirement for Enforcement Authorities, such as Customs and Trading Standards, to have

access to reliable analytical methods that can be used to verify origin labels on beef, whether

they are part of the Protected Food Names Scheme, subsidy claims or simply ‘suspect’

imported produce.

2.2 Scope of project

The methods for beef provenance determination used in this project were based on

measurements of stable isotopes of hydrogen (2H/1H), carbon (13C/12C), nitrogen (15N/14N),

sulphur (34S/32S) and strontium (87Sr/86Sr). Element profiling was also completed on the

authentic beef samples using inductively coupled plasma mass spectrometry (ICP-MS), which

permits a large range of macro (including Al, Ca, Mg, P, Na and K), micro (e.g. Mn, Fe, Co,

Ni, Cu and Zn) and trace (e.g. Sr, Mo, Cd, Pb and the lanthanides plus scandium and yttrium)

elements and their isotopes to be determined simultaneously. This strategy was implemented

following previous research that has shown the combination of multi-element data with

multivariate statistics to be a powerful technique for the source discrimination of a range of

food products.

2.3 References

EUROPEAN COMMISSION; Brussels, 6 May 1998; COM(98) 276 final, PROTECTION OF THE FINANCIAL INTERESTS OF THE COMMUNITIES, FIGHT AGAINST FRAUD, Annual Report 1997, 2.1.2.4. Infringement of the embargo on British beef


Section 3: Background to stable isotope and multi-e lement analysis

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3 BACKGROUND TO STABLE ISOTOPE AND MULTI -ELEMENT ANALYSIS IN FOOD

ORIGIN DETERMINATIONS

3.1 Natural abundance isotope ratios

Table 3-1 provides a broad overview of the way in which natural abundance isotope

ratios can be used for provenance determinations. Many natural phenomena, classed as

physico-chemical effects, can lead to isotope fractionation (measurable changes in the ratio of

the ‘heavy’ to ‘light’ isotope of a given element). Examples of such effects include

evaporation and condensation, crystallisation and melting, absorption and desorption, and

diffusion and thermodiffusion. As a first approximation, natural abundance measurements will

provide information on plant ‘type’ or diet (carbon and nitrogen isotope ratios), and

geographical origin (hydrogen, oxygen, sulphur and strontium isotope ratios).

Table 3-1 : Possible origin information available from different isotope ratios

Isotope ratio Fractionation Information

2H/1H

Hydrogen

evaporation, condensation,

precipitation

geographical

13C/12C

Carbon

C3 and C4 plants diet (geographical proxy)

15N/14N

Nitrogen

trophic level, marine and terrestrial

plants, agricultural practice

diet (geographical proxy)

18O/16O

Oxygen

evaporation, condensation,

precipitation

geographical

34S/32S

Sulphur

bacterial geographical (marine)

87Sr/86Sr Age of the rock and Rb/Sr ratio geological

The measurement of the stable isotope ratios of hydrogen and oxygen are applicable to

the characterisation of geographical origin because they are strongly latitude dependent.

Meteoric water that has passed through the meteorological cycle of evaporation,

condensation and precipitation finally constitutes groundwater and this exhibits a systematic

geographical isotope variation (Yuntseover and Gat, 1981). Decreasing temperatures cause a

progressive heavy-isotope depletion of the precipitation when the water vapour from oceans

in equatorial regions moves to higher latitudes and altitudes (Craig H, 1961). Evaporation of

water from the oceans is a fractionating process that decreases the concentration of the



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heavy isotopologues of water (1H2H16O, 1H1H18O) in the clouds compared to the sea. As the

clouds move inland and gain altitude, further evaporation, condensation and precipitation

events occur, decreasing the concentration of deuterium. Consequently, the ground water

reflects this isotopic gradient from the coast to inland areas (Dansgaard W, 1964). The

variation of oxygen-18 (18O) in the hydrosphere follows an analogous pattern to that of

deuterium (2H). Previous studies have clearly shown that the oxygen-18 and deuterium

content of water, consumed by animals, exhibits a strong correlation with the oxygen-18 and

deuterium content of organic compounds present in animal products such as milk, butter and

cheese (Manca G et al., 2001). This correlation is also found in animal tissues and has been

exploited by ecologists to determine the migratory patterns of birds (Wassenaar and Hobson,

2001) and insects (Hobson et al., 1999).

Local agricultural practices and animal diet affect 15N/14N and 13C/12C ratios respectively. C3

plants use the Calvin photosynthetic pathway to assimilate CO2. During this process the

plants discriminate against 13C and therefore possess relatively lower 13C/12C ratios than C4

plants that utilise the more energy efficient Hatch-Slack pathway. Since C3 plants

predominate at higher latitudes and C4 plants are more common in warmer climates at lower

latitudes (such as the tropics), there is a gradient of decreasing 13C/12C in plant material from

the equator to the poles, which can also be used as a proxy for geographical origin

determination. In addition to 15N signatures providing information about regional agricultural

practices, supplementary information may be obtained by measuring stable sulphur isotope

ratios (34S/32S). Sulphate reduction does not produce significant fractionation, such that

organic sulphur is clearly related to its source. Therefore, the soil or sea-spray, from which

sulphur in foods is derived, can provide useful geographical origin information.

3.2 Delta notation

Differences in isotope effects mentioned in the previous section are usually of the order

of a few percent. Consequently, changes in the isotopic ratio at natural abundance levels

often occur around the third or fourth significant figure. Isotope ratio analysis therefore

requires very precise measurement and this is achieved by measuring the ratio of the heavy

and light stable isotopes in the test material and comparing it to a reference compound of

nominal isotope ratio. The technique of differential analysis of sample and standard permits

very small differences in the isotopic composition of test samples to be reliably and accurately

determined. Thus, isotopic abundance of a sample relative to a reference is normally

expressed by the differential equation (1):

1000.R

RRδ

ref

refsampref

−= ……………………(1)



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Equation (1) can be simplified to (2)

1000.1R

Rδ

ref

sampref

−= ………………………….(2)

where δ ref is the isotope ratio of the sample expressed in delta units (‰, per mil) relative to

the reference material. Rsamp and Rref are the absolute isotope ratios of the sample and

reference material, respectively. Multiplying by 1000 converts the value to parts per thousand

(‰), or the more commonly used expression per mil (derived from the Latin mille meaning

one thousand and used in an analogous way to per centum or per cent). In essence the use

of equation (1) or (2) facilitates the comparison of isotope ratios, especially at the natural

abundance level when the differences being examined are relatively small.

3.3 Strontium isotopic ratios

Strontium is a group IIA element, an alkaline earth metal and has four naturally

occurring isotopes: 84Sr, 86Sr, 87Sr and 88Sr. Its ionic radius is similar to that of calcium and

strontium can substitute for calcium in a wide range of naturally occurring minerals. One

isotope, 87Sr, is formed through radiogenic decay of rubidium-87 (87Rb), with a decay half-life

of 49,000,000,000 years (Faure, 1986). Although biological processes, such as assimilation

and metabolism by plants and animals, may alter stable strontium isotope ratios in a similar

fashion as with the S, C, H, O and N isotopes, only the amount of excess radiogenic 87Sr is

evaluated in its use as a geological tracer. Any natural or instrumental mass dependent

fractionation of the 87Sr/86Sr ratio is normalized against an 86Sr/88Sr ratio of 0.1194 (Faure,

1986). In this manner the strontium isotopic ratios found in plants, and the animals that eat

them, are related to 87Sr/86Sr ratios of the bioavailable portion of the mineralised strontium

derived from the bedrock, which is the sum of the individual minerals therein, and their

geological ages: (87Sr/86Sr) = f(Rb/Sr, t), where t is the age of the rocks either that of primary

crystallization, metamorphosis and/or sedimentary deposition. As a first approximation, acidic

rocks (e.g. silica rich granites) have high 87Sr/86Sr values due to the high Rb/Sr ratios over

time, while basic rocks (e.g. basaltic and carbonate rocks) have relatively lower values.

Strontium isotope signatures can therefore be helpful in authenticity determinations, as they

have a different scope than the stable isotopes of the light elements. Thus, ideally, for

materials coming from different micro-regions within the same climate zone (and therefore

having similar δ2H‰ and δ18O‰ values) additional strontium isotope ratio analysis may

provide an additional level of geographical resolution provided that different lithologies exist

within that region. This rationale applies to all natural products including food crops and

animal tissues.



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3.4 Multi-element (trace element) concentrations

The multi-element composition of animal tissues reflects, to some extent, that of the

vegetation that they eat. The vegetation is the compositional reflection of the bioavailable and

mobilized nutrients present in the underlying soils from which they were cultivated. Alkaline

metals, especially rubidium (Rb) and cesium (Cs), are easily mobilised in the soil and easily

transported into plants and are therefore good indicators of geographical identity. Trace

element availability depends on several factors such as soil pH, humidity, porosity, clay and

humic complex, etc. (Kim and Thornton, 1993). Consequently, the range of soils present and

bioavailability mean that elemental composition may provide unique markers in food that

characterise geographical origin. It is important to note that the chemical composition of the

soil does not necessarily reflect that of the underlying lithology due to the deposition of glacial

till (or ‘drift’ geology) during the ‘ice-ages’. This is the case for most of Northern Europe,

which was covered by glacial till in lowland areas.

3.5 References

Craig, H. (1961). Isotopic variations in meteoric waters. Science, 133, 1702-1703.

Dansgaard, W. (1964). Stable isotopes in precipitation. Tellus, XVI(4), 436-468.

Faure, G. (1986). Principles of Isotope Geology (2nd Ed), pp 117-140, John Wiley &Sons, USA

Hobson, K. A., L. Atwell, et al. (1999). "Influence of drinking water and diet on the stable-hydrogen isotope ratios of

animal tissues." Proceedings of the National Academy of Sciences of the United States of America 96(14): 8003-

8006.

Kim, K. W., & Thornton, Y. (1993). Influence of Ordovician uraniferous black shales on the trace element composition

of soils and food crops, Korea. Applied Geochemistry Supplement, 2, 249-255

Manca, G., Camin, F., Coloru, G. C., Del Caro, A., Depentori, D., Franco, M. A., & Versini G. (2001). Characterization

of the geographical origin of Pecorino Sardo cheese by casein stable isotope (13C/12C and 15N/14N) ratios and free

amino acid ratios. Journal of Agricultural and Food Chemistry, 49(3), 1404-1409.

Wassenaar, L. I., & Hobson, K. A. (2001). A stable-isotope approach to delineate geographical catchment areas of

avian migration monitoring stations in North America. Environmental Science and Technology, 35(9), 1845-1850.

Yuntseover and Gat (1981) Atmospheric waters, IAEA Technical reports series 210 - Stable isotope hydrology,

(pp103-142).


Section 4: Literature Review

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4 LITERATURE REVIEW

Multi-element and isotopic analyses have previously been applied to a range of

foodstuffs to develop methods that will permit their geographical origins to be determined with

varying degrees of certainty.

A common theme of food authentication studies is the requirement for a database of

genuine samples to which the ‘suspect’ test sample can be compared to establish its

authenticity. Geographical origin determination is no exception, but the need to source

agricultural products from a wide range of countries is time consuming and costly.

Furthermore, in order to constrain an authenticity parameter such as geographical origin there

may be a requirement for a large number of independent variables to be measured and

statistically ‘screened’ in order to identify key tracers that differentiate the regions or countries

of interest. There have been a number of literature reviews that are dedicated entirely, or in

part, to the application of multi-element and isotope analysis to the determination of the

geographical origin. These include Horn et al., (1998), Anklam (1998), Rossmann (2001),

Kelly (2003, 2005) and Hölzl et al., (2004). In addition, the multivariate statistical techniques

used, in combination with a wide range of analytical methods including multi-element and

isotopic analysis, to classify food products according to their geographical and varietal origin

has been critically reviewed by Tzouros and Arvanitoyannis (2001).

Measuring elemental concentrations and isotopic variation in premium regional

products is arguably the best analytical strategy for accurately verifying geographical origin.

This approach is driven by the hypotheses outlined in Section 3 above describing the global

variation of isotope abundance of the ‘light’ bio-elements and ‘heavy’ geo-elements.

4.1 Beef meat

Some of the most recent research into the application of multi-element and multi-

isotopic measurements to determine geographical origin of meat has focused on beef and

lamb. Hegerding et al., (2002) investigated whether the oxygen-18 content of local ground

water, measured by isotope ratio mass spectrometry (IRMS), was preserved in the tissue

water of beef cattle originating from Germany, the United Kingdom and Argentina. Significant

differences were observed in the δ18O‰ value of tissue water from German cattle (n = 175)

and Argentian cattle (n = 42), permitting a reasonably secure classification of origin for these

specific countries, with a single isotopic parameter. However, the natural variation in δ18O‰

values did give rise to overlapping outliers in the German and Argentinean data sets and did

not provide sufficient resolution to discriminate the UK samples from either the German or

Argentinean cattle. Nor did it permit reliable discrimination of northern and southern

production regions within Germany.

Boner and Forstel (2004) characterised beef from Germany, Argentina and Chile by

measuring the δ18O‰ and δ2H‰ values of tissue water and δ13C‰, δ15N‰ and δ34S‰ values

of defatted protein, over a 2-year period. ‘Organically’ reared German beef cattle were



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chosen because these animals are generally reared on local pastures and fodder produced

on the same farm, which reduces the possibility of confounding factors produced by imported

feed materials. The authors suggested that a δ13C‰ value above -20‰ has been observed

as a limit for differentiating between conventionally and organically reared cattle in Germany,

based on the proportion of C4 maize in the diet. However, organic cattle feed may be

outsourced and consequently its composition changed if there is insufficient feed being

produced in the local area. The importance of the seasonal variation of δ2H‰ and δ18O‰ in

tissue water was emphasised for the correct interpretation of geographical origin. If the

production season was known, beef samples from Northern (n = 103) and Southern (n = 65)

Germany were correctly differentiated from Argentinian samples (n = 34) in 95% and 100% of

cases, respectively. Elevated δ34S‰ values (median +15.2‰) were shown to be extremely

useful in distinguishing the beef samples originating from Chile (n = 10).

A controlled cattle feeding experiment has been conducted by the Institut National de

la Recherche Agronomique at three distinct geographical sites in France (Renou et al.,

2004a). The study aimed to establish whether δ18O‰ of beef tissue water, measured by

IRMS, in combination with 1H, 2H and 13C spectrums of extracted beef lipid, measured by

NMR, could be used to distinguish the production sites and diet. Discriminant analysis, an

advanced statistical tool, was used to differentiate cattle fed on both the pasture and maize

diets at the three production sites. All pasture fed cattle were well classified, as were 94% of

the cattle fed on maize silage. However, the parameters chosen for the discriminant functions

were derived from the NMR spectroscopic analysis of the beef lipid fraction. In 2007 Heaton

et al., assessed beef samples originating from the major cattle producing regions of the world

(Europe, USA, South America, Australia and New Zealand) using IRMS and ICP-MS. C and

N isotope composition of the beef defatted dry mass and H and O isotope composition of the

corresponding lipid fractions were determined. It was observed that:

- intensive maize and/or C4 pasture feeding, during cattle production, gave rise to

significant differences in the 13C content of beef produced in Brazil and the USA

versus British beef fed predominantly on C3 pasture and fodder.

- the mean δ2H‰ and δ18O‰ values of beef lipid correlated well with the latitude of

production regions and the relationship between the H and O isotopic contents were

found to parallel the Meteoric Water Line.

These findings support the hypothesis that the systematic global variations in the 2H and 18O

content of precipitation are transferred through drinking water and feed into beef lipid. Multi-

element concentrations determined in the beef were combined with the stable isotope data

and submitted to multivariate analysis. Six key variables (δ13C‰ (defatted dry mass), Sr, Fe,

δ2H‰ (lipid), Rb and Se) were identified by canonical discriminant analysis as providing the

maximum discrimination between beef samples on the basis of the broad geographical areas

(Europe, South America and Australasia). Overall, 86.1% of cross-validated grouped cases

were correctly classified on the basis of region of origin. It was concluded that the

methodology in its current state can be used to provide reliable origin information, but this is

dependent upon the countries under investigation.



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4.2 Lamb meat

Piasentier et al., (2003) investigated the effectiveness of analysing δ13C‰ and δ15N‰

values of extracted lipid and residual protein fractions of lamb meat. Analyses were carried

out on 120 samples from 12 lamb types, produced in two distinct regions in each of the

following countries: Great Britain, Spain, France, Greece, Iceland and Italy. Canonical

discriminant analysis (CDA) was used to evaluate whether lamb meat from the different

production origins could be differentiated by its stable isotope ratios. 79.2% of the samples

were initially correctly classified and cross-validation of the discriminant model reduced this to

66.7% correct classification of geographical origin. In 2007, Camin et al. assessed the

suitability of multi-element (H, C, N, S) stable isotope ratio analysis as a means for

geographical provenance assignment of lamb meat from several European regions. The

defatted dry matter (crude protein fraction) from lamb meat was found to be a suitable probe

for ‘light’ element stable isotope ratio analysis. Significant differences were observed

between the multi-element isotope ratios of lamb samples from different regions. The mean

hydrogen isotopic ratios of the defatted dry matter from lamb were found to be significantly

correlated with the mean hydrogen isotopic ratios of precipitation and groundwater in the

production regions. Carbon and nitrogen isotopic ratios were influenced by feeding practices

and climate. Sulphur isotopic ratios were influenced by geographical location and surface

geology of the production region. The results permitted differentiation of lamb meat, from

most production regions, by inspection. However, more sophisticated evaluation of the data

using multivariate methods, such as linear discriminant analysis, achieved 78% correct

classification of the lamb meat..

4.3 Poultry meat

There have only been two very recent publications in peer-reviewed journals relating

specifically to the determination of the geographical origin of poultry on relatively small

sample sets. Franke et al., (2007a) measured the concentrations of a total of 72 different

elements in 25 poultry breast fillets originating from Switzerland (n = 7), France (n = 2),

Germany (n = 3), Hungary (n = 6), Brazil (n = 4) and Thailand (n = 3), by inductively coupled

plasma high resolution mass spectrometry (ICP-HRMS). Analysis of variance was used to

identify elements that were significantly different between the countries of origin examined.

Mean concentrations of four elements, arsenic, sodium, rubidium and thallium, were found to

be significantly different. However, the discrimination power among countries depends on the

numbers of samples, which are low. In the case of France there are only two samples. If you

assume that the populations of data for France are distributed normally there is only one

degree of freedom. Consequently, to generate normal distribution curves for the expected

entire populations for France to compensate for uncertainty in the estimates of the true

population (µ) and population variance (σ), the value of 63.66 (P=0.01) has to be used for the

t-distribution. If there were at least 11 observations for France then the value of t would drop

dramatically to 3.17 at the 99% confidence interval (10 degrees of freedom at P=0.01) making



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statistical significance discussions about natural variability more meaningful. The same

argument applies to the data presented for Germany and Thailand.

Franke et al., (2007b) also reports strontium isotope data for 22 poultry samples

and δ18O‰ data for water extracted from 78 poultry samples from Brazil, France, Germany,

Hungary, and Switzerland. The average values of 87Sr/86Sr were lowest for poultry meat

samples from Germany and highest for samples from Hungary. However, the pairwise

comparison among means did not specify any individual differentiation. Analysis of variance

of the poultry breast tissue water δ18O‰ showed significant differences between Brazil,

Germany, Hungary and Switzerland. However, the use of tissue water for δ18O‰ analysis

has been shown to be significantly affected by storage conditions. Increasing open storage

times, including post-mortem hanging or maturing, result in decreasing yield of tissue water,

increasing weight loss and increasing 18O/16O-ratio values in extracts. Higher rates of change

are associated with higher ambient storage temperatures, probably due to evaporation. The

technique therefore does not lend itself to the analysis of ‘off the shelf’ retail samples.

4.4 Summary

A number of the research articles reviewed above are described as ‘preliminary’ as the

authors acknowledge the relatively small numbers of authentic samples they have included in

their studies of geographical origin. This leads to the question of whether the number of

samples in the database is sufficient to be a true reflection of the commercial sample

population they will ultimately be compared against. Paradoxically, as databases are

expanded, and the number of samples analysed increases, the natural variation in elemental

composition and isotope ratios increases so that geographical origin interpretation actually

becomes more complex, due to natural variation and overlap in measured parameters from

the authentic sample populations. Authentication strategies involving the use of multi-isotopic

and multi-elemental parameters have been facilitated by increasingly rapid measurement

procedures. The use of ‘high productivity techniques’ such as multi-element continuous-flow

IRMS and multi-collector ICP-MS enable large quantities of data to be rapidly generated. In

principle, the most powerful methods are generally those that combine as many of the

elemental and isotopic signatures as possible, into a multi-dimensional authenticity matrix

where natural variation is more readily constrained and detection of mis-description is difficult

to subvert. Consequently, this analytical approach demands proper data pre-treatment.

Procedures such as normalization, transformation, weightings, prior probabilities etc., play an

important role in the interpretation of the data with multivariate software packages. It is then

critical that the robustness of the multivariate model is tested with techniques such as cross-

validation and ‘blind-testing’.

It is extremely important to quantify the repeatability and reproducibility of multi-element

and multi-isotopic measurements. In order to make meaningful origin assignments it is

necessary to know the measurement uncertainty so that differences in elemental



Page 15

concentrations, or isotope ratios, for commodities from different geographical origins can be

deemed as statistically significant or not. Control of long-term measurement repeatability with

matrix matched in-house reference material is essential if authentic databases are to be

established over a number years. Furthermore, if databases are to be developed on a

European scale for enforcement purposes, in the same way as the EU wine databank, then

long-term reproducibility is also of paramount importance (Commission Regulation (EC) No

2120/2004).

In the case of meat origin, there are many other confounding factors that must be

considered during the construction of authentic comparative databases. The protein turnover

times in muscle tissue means that isotopic signatures will have a ‘lag-time’ before they reflect

changes in feeding regime and changes in feed water as a result of livestock movement,

often prior to slaughter. The homogeneity of elemental and isotope signals between different

cuts of meat, or tissue types, from the same animal also needs to firmly be established and

characterised. As with food markets, the globalisation of feed markets and the desire to

obtain cheap sources of feed may mean that certain elemental and isotope signals will not

reflect the region of production. It is therefore important to recognize these restraints on

geographical interpretation until they have been characterised by appropriate controlled

feeding experiments. Similarly it is important not to use geographical models that are heavily

dependent on trace element markers from manufacturer’s processes, as this could lead to

uncontrollable variations. However, this does raise the alternative possibility of isotopic or

elemental labelling of premium food products, which could help to ensure that consumers do

not purchase food with a falsely declared origin.

In the longer-term it is hoped that a deeper understanding of how meteorological and

geochemical signatures are transferred into food systems may obviate the need for expensive

comparative databases of authentic foods. Ultimately this would allow the generation of

isotopic and multi-element maps for foods from different geographical locations, which could

be incorporated into traceability systems. For the moment though, there is a need for

comparative databases to be established for premium foods and for these to be used as

benchmarks in ongoing scientific developments in the near future. Completely overcoming

the need for comparative databases in food provenance determinations will be an extremely

challenging task.

4.5 References

Anklam E. (1998). A review of the analytical methods to determine the geographical and botanical origin of honey. Food Chemistry, 63 (4), 549-562.

Boner, M., & Forstel, H. (2004). Stable isotope variation as a tool to trace the authenticity of beef. Analytical and Bioanalytical Chemistry, 378(2), 301-310.

Camin, F., Bontempo, L., Heinrich, K., Thomas, F., Kelly S.D., et al., (2007). Multi-element (H,C,N,S) stable isotope characteristics of lamb meat from different European regions, Analytical and Bioanalytical Chemistry 389 (1), 309-320

Commission Regulation (EC) No 2120/2004 of 10 December 2004 amending Regulation (EC) No 2729/2000 laying down detailed implementing rules on controls in the wine sector



Page 16

Heaton, K., Kelly, S D., Hoogewerff, J., and Woolfe, M. (2007) “Verifying the geographical origin of beef: The application of Multi-element Isotope and Trace Element Analysis” Food Chemistry, 107, 506–515

Hegerding, L., Seidler, D., Danneel, H. J., Gessler, A., & Nowak, B. (2002) Oxygenisotope-ratio-analysis for the determination of the origin of beef. Fleischwirtschaft, 82(4), 95-100.

Hölzl, S., Horn, P., Rossmann, A., & Rummel, S. (2004). Isotope-abundance ratios of light (bio) and heavy (geo) elements in biogenic tissues: methods and applications. Analytical and Bioanalytical Chemistry, 378 (2), 270-272.

Horn, P., Hölzl. S., Todt, W., & Matthies, D. (1998). Isotope abundance ratios of Sr in wine provenance determinations, in a tree-root activity study, and of Pb in a pollution study on tree-rings. Isotopes in Environmental and Health Studies, 34(1-2), 31-42.

Kelly, S. D. (2003). Using stable isotope ratio mass spectrometry (IRMS) in food authentication and traceability. In M. Lees, Food Authenticity and traceability (pp 156-183). Cambridge: Woodhead Publishing Limited.

Kelly, S. D. Heaton, K. & Hoogewerff, J. (2005) Tracing the geographical origin of food: The application of multi-element and multi-isotope analysis. Trends in Food Science and Technology, 16, 555-567

Piasentier, E., Valusso, R., Camin, F., & Versini, G. (2003). Stable isotope ratio analysis for authentication of lamb meat. Meat Science, 64(3), 239-247.

Renou, J. P., Bielicki, G., Deponge, C., Gachon, P., Micol, D., & Ritz, P. (2004a). Characterization of animal products according to geographic origin and feeding diet using nuclear magnetic resonance and isotope ratio mass spectrometry. Part II: Beef meat. Food Chemistry, 86(2), 251-256.

Rossmann, A. (2001). Determination of stable isotope ratios in food analysis. Food reviews International, 17(3), 347-381.

Tzouros, N. E., & Arvanitoyannis, I. S. (2001). Agricultural produces: Synopsis of employed quality control methods for the authentication of foods and application of chemometrics for the classification of foods according to variety or geographical origin. Critical Reviews in Food Science and Nutrition, 41(4), 287-319.

Franke, B.M., Haldimann, M., Reimann, J., Baumer, B., Gremaud, G., Hadorn, R., Bosset, J-O and Kreuzer, M. (2007a). Indications for the applicability of element signature analysis for the determination of the geographic origin of dried beef and poultry meat. European Food Research and Technology, 225, (3-4), 501-509.

Franke, B.M., Koslitz, S., Micaux, F., Piantini, U., Maury, V., Pfammatter, E., Wunderli, S., Gremaud, G., Bosset, J-O., Hadorn, R. and Kreuzer, M. (published online in 2007b) Tracing the geographic origin of poultry meat and dried beef with oxygen and strontium isotope ratios, European Food Research and Technology, DOI 10.1007/s00217-007-0588-x


Section 5: Authentic beef sampling

Page 17

5 AUTHENTIC BEEF SAMPLING

5.1 English beef sampling

Five hundred authentic samples of English beef have been collected by Dennis Homer

directly from abattoirs located in: 1) Bamber Bridge (Lancashire); 2) Bridlington (Yorkshire); 3)

Shrewsbury (Shropshire); 4) Treburly (Cornwall); 5) Bridport (Dorset); 6) Chester (Cheshire);

7) Skegness (Lincolnshire). Meat from the neck, or from other less valuable parts of the

animal carcass, was collected with the corresponding Cattle Passport information. The

majority of this collection was previously financed by the English Beef and Lamb Executive

(EBLEX).

5.2 Welsh beef sampling

One hundred and eighteen samples of authentic Welsh beef have been collected by

Dennis Homer directly from abattoirs located in Powys, Conwy, Merthyr Tydfil and some

abattoirs located in England (Cheshire and Shropshire). Sampling was done with the

assistance of Hybu Cig Cymru - Meat Promotion Wales.

5.3 Scottish beef sampling

One hundred authentic Scottish beef samples were collected directly from abattoirs. The

sampling of authentic Scottish beef has been undertaken and financed in part by Quality Meat

Scotland (QMS). Dennis Homer (EBLEX) obtained authentic Scottish beef samples from the

border counties (Dumfriesshire, Roxburgshire and Berwickshire) where there was a greater

risk of misclassification of origin with English beef reared in Cumberland and Northumberland.

5.4 Sample logging and Storage

A summary of the sample collection, distribution and measurement is shown in Figure 1

below. Beef samples were stored at -20°C until they were processed for analysis. After

processing and measurement the samples are transferred to -40°C for long-term storage. The

passport information was recorded in an Excel database and the information was also

compiled in a Google Earth ‘KMZ’ file. Figure 2 shows the geographical location of the farms

where the cattle were reared prior to slaughter and collection of skeletal muscle tissue from

the abattoir. A complete list of beef samples collected, with corresponding farm location and

passport information, can be found in Appendix I.


Section 5: Authentic beef sampling

Page 18

Figure 5-1: A diagram showing the institutes involv ed in the collection, storage distribution and anal ysis of authentic beef samples and the flow of data.

Figure 5-2: Google Earth “KMZ” file showing the loc ations of the farms where British beef cattle were reared prior to slaughter and collection of skeletal muscl e tissue from the abattoir. Red markers = English b eef; green markers = Welsh beef and blue markers = Scott ish beef. The inset picture shows the locations of high throughput three species, or cattle only, abattoirs .


Section 6: Experimental tasks

Page 19

6 EXPERIMENTAL TASKS

6.1 Preparation of beef muscle defatted dry mass an d measurement of the bio-

element stable isotope composition ( δ2H‰, δ13131313C‰C‰C‰C‰, δ15N‰‰‰‰ and δ34S‰‰‰‰)

A detailed description of the preparation of defatted dry matter (DDM) from beef muscle

and measurement of δ2H‰, δ13C‰, δ15N‰ and δ34S‰ is provided in the Standard Operating Procedure at Appendix II of this report (page91).

6.2 Extraction of strontium from beef muscle tissue

A detailed description of the extraction of strontium from beef muscle tissue is given in

the Standard Operating Procedure at Appendix III of this report (page 114).

6.3 Multi-element measurements by ICP-MS

A detailed description of the acid digestion and ICP-MS measurement of beef muscle

tissue is given in the Standard Operating Procedure at Appendix IV of this report (page 122).


Section 7: Results and discussion

Page 20

7 RESULTS AND DISCUSSION

A complete list of beef samples collected from UK abattoirs, with corresponding results for

stable isotope and elemental composition, can be found in Appendix I. Bio-element stable

isotope composition (HCNS) and elemental concentrations in beef samples from different

British regions have been measured. The beef skeletal muscle defatted dried matter (DDM)

was used for this study and may be described as the ‘protein fraction’ of the beef sample.

This fraction of the meat is less sensitive to alteration processes and has already been used

in several previous studies (e.g. Camin et al., 2007, Nakashita et al., 2008, Boner and Förstel

2004, Heaton et al., 2008). The use of water from muscle tissue has been shown to be a

reliable and important tool for the determination and control of geographical origin, however,

only for samples taken in industrial slaughterhouses (Thiem et al., 2004, Horacek et al.,

2008). As the ultimate aim of the current research project is the testing of meat from retail

outlets, the water fraction of the samples has not been used. Generally, the isotope signature

of the beef meat is related to the isotope signature of the feed and water the animal ingests.

7.1 Evaluation of authentic British beef DDM hydrog en isotope ( δ2H‰)

measurements

The hydrogen isotopic composition of the water an animal drinks is a predominant

factor influencing the hydrogen isotopic composition of the animal’s tissues. As the isotopic

composition of water varies regionally (Boner and Förstel 2004) due to fractionation in the

global hydrological cycle, these variations are also ultimately incorporated into the meat

(Boner and Förstel 2004, Camin et al., 2007, Heaton et al., 2008). Lowlands close to the sea

and warm regions have water enriched in the heavy isotopes of hydrogen and oxygen (2H and 18O) whereas regions far away from the sea, at high altitudes and in cooler regions have

water with relatively depleted δ2H‰ values (Craig, 1961; Dansgaard, 1964).

Figure 7-1a: Annual average rainfall in the British Isles (mm)

Figure 7-1b: Mean annual δ2H‰V-SMOW values of precipitation for Western Europe.

www.waterisotopes.org



Page 21

If beef cattle feed on fresh pasture or fodder, a significant proportion of the animal’s

total water intake is from plant material. As the plant water is enriched in 2H with respect to

groundwater, due to evaporation from leaf stomata and the associated fractionation, the 2H

content of the animal is also relatively enriched. Moreover, hydrogen present in carbohydrate

and protein in food also contributes to the total metabolic pool of hydrogen present in the

animal.

In the British Isles the prevailing winds and precipitation patterns are dominated by the

Atlantic Ocean and this is reflected in the annual average rainfall pattern shown in Figure

7-1a. Furthermore, this pattern is reflected in the isotopic composition of the precipitation with

a South Westerly gradient of decreasing deuterium content from the western seaboard of the

British Isles through to the East coast.

A summary of authentic British beef defatted dry matter δ2H‰ values is shown in Table

7-1. The sample standard deviation (σn-1), minimum, maximum, range and number of

authentic beef samples measured are shown.

Table 7-1: Summary statistics for the δ

2H‰ measurement of authentic British beef defatted d ry mass samples

δδδδ2H [‰]V-SMOW ENGLAND WALES SCOTLAND

Mean -96.7 -96.3 -98.0

SD 4.1 3.4 3.4

Min -105.9 -105.0 -107.0

Max -86.2 -88.9 -90.7

Range 19.6 16.1 16.3

N 101 101 100

Table 7-1 clearly shows that examination of the mean δ2H‰ values for English, Welsh

and Scottish beef δ2H‰ does not provide a straightforward basis for the discrimination of

country of origin. The mean values range from -96.3‰ for Wales to -98.0 ‰ for Scotland.

This difference is less than the measurement uncertainty typically quoted for organic δ2H‰

measurements of ± 3‰. However, previous studies have shown that the isotopic signatures

of plant material and water are both transferred into animal tissues (Bowen et al., 2005,

Hobson et al., 1999, Rubenstein & Hobson., 2004). Furthermore, deuterium labelling has

been used to link hydrogen in dietary carbohydrate and water with hydrogen stable isotopes

in fatty acids produced by chickens (Zhang et al., 2005). Consequently, if the hydrogen

isotope composition of precipitation and ground water is known to exhibit an isotopic gradient

with latitude, distance from the sea and altitude, then beef skeletal muscle in equilibrium with

an animal’s diet should exhibit a gradient of high to low deuterium contents, as demonstrated

from the West to East coast of the British Isles respectively (Figures 7-2 and 7-3).

The hydrogen isotope values of the authentic British beef DDM, at each of the farm

locations, were plotted onto a Google Earth map of the British Isles as polygons that varied in

height and colour according to the magnitude of the measured δ2H‰ values (Figure 7-2).



Page 22

The red polygons show the farms that reared beef cattle with the highest δ2H‰ values

~ -96‰ in their skeletal muscle and the yellow polygons show the lowest δ2H‰ values

~ -107‰. This aids the visualisation of the hydrogen isotopic gradient, from the South West to

North East, across the British Isles. Figure 7-3 shows the same polygons for English beef

only. This also clearly shows the isotopic gradient and the effect of the ‘rain shadow’ of

Wales (Figure 7-1a) on the group of English farms in the orange cylinder (mainly Shropshire),

which have relatively depleted δ2H‰ values (lower polygon height) compared to the other

most westerly English farms directly exposed to the prevailing wind’s coastal precipitation

events.

Figure 7-2: The hydrogen isotope values of the auth entic British beef DDM, at each of the farm locatio ns. The polygons vary in height and colour according to the magnitude of the measured δ

2H‰ value. Figure 7-3: The hydrogen isotope values of the auth entic British beef DDM, at each of the farm locatio ns. The polygons vary in height and colour according to the magnitude of the measured δ

2H‰ value. English farms in the orange cylinder have relatively depleted δ

2H‰ values compared to the other most westerly farms directly on the coastline.



Page 23

7.2 Evaluation of authentic British beef DDM carbon isotope ( δ13C‰) measurements

The carbon isotope composition of beef is directly linked to the carbon isotope

composition of the pasture and/or fodder eaten by cattle. The proportion of C3 versus C4

photosynthetic plant material in the cattle’s diet determines whether the beef has an isotope

signature of around -27 to -24‰ (Camin et al., 2008) or of around -16 to -9‰, respectively, if

the cattle is almost exclusively fed on C4 plants (Schmidt et al., 2005). In the United Kingdom

and Europe ‘C4 signatures’ are derived from maize, as this is the only C4 fodder plant growing

on the European continent.

A summary of authentic British beef defatted dry mass δ13C‰ values is shown in Table



Table 7-2: Summary statistics for the δ13C‰ measurement of authentic British beef defatted d ry mass

samples

δδδδ13C [‰]PDB ENGLAND WALES SCOTLAND

mean -25.52 -25.91 -26.49

SD 1.51 1.48 0.64

min -27.60 -28.03 -27.58

max -19.64 -19.64 -24.54

range 8 8.39 3.04

N 101 101 100

There are no significant differences between the mean δ13C‰ values of beef DDM

observed in English, Scottish and Welsh beef. However, none of the Scottish beef samples

possessed δ13C‰ values indicating the feeding of maize fodder in the diet, which means that

Scottish samples possess a very narrow range of δ13C‰ values (~3‰). On the basis of

these data it can be concluded that Scottish beef samples are unlikely to contain any C4

signal, which is present in a proportion of the English and Welsh samples (Figure 7-4).

A controlled cattle feeding study has previously demonstrated that it takes up to 30

months for the δ13C‰ value of skeletal bovine muscle to reach complete equilibrium after a C3

to C4 diet switch (Bahar et al., 2006). The kinetics of the skeletal muscle δ13C‰ turnover can

be modelled using first order kinetics. The half-life of the turnover is defined as the time taken

for the DDM δ13C‰ value to reach half of the final value it will achieve when fully equilibrated

with the cattle’s diet. This is represented in the schematic below (Figure 7-5). If the starting

C3 diet (e.g. pasture) has an average δ13C‰ value of approximately -25‰ then the FFDM will

possess a δ13C‰ value of approximately -24‰ (shown as the solid black line in Figure 7-6

below). After a complete diet switch to a C4 diet (100% maize silage), it will take

approximately five months for the DDM to reach a δ13C‰ value of -17‰ (shown as the grey

hatched line in Figure 7-6 below).



Page 24

Figure 7-4: A cross plot of δ13C‰ and δ15N‰ values obtained from authentic British beef defa tted dry mass.

The authentic beef samples originated from England, Ireland and Brazil.

This is a relatively short time period compared to the 30 months required for the DDM

to reach full equilibrium with the C4 diet (shown as the grey hatched line in Figure 7-5 below).

However, it is still longer than the usual 3 to 4 month period when silage/fodder is used for

winter feeding. Furthermore it is unlikely that maize silage would be used exclusively as an

over-Winter diet in Northern European countries and is much more likely to form 10 to 20% of

the feed, due to nutritional requirements. These factors explain why it is highly unlikely that

English or Welsh beef DDM would possess a δ13C‰ value greater (less negative) than -20‰.

Figure 7-5: Schematic of the effect of a C 3 to C 4 diet switch on bovine skeletal muscle DDM δδδδ13C‰ values adapted from Bahar et al., 2006. The rate of change can be modelled using first order kinetics. The half-life (T1/2) value for rate of change of δδδδ13C‰ is approximately 160 days. The hatched line show s the δδδδ13C‰ value half-way between the C 3 and C4 diets.



Page 25

7.3 Evaluation of authentic British beef DDM nitrog en isotope ( δ15N‰) measurements The nitrogen isotope ratio of beef, like carbon, is determined by pasture and/or fodder

eaten by the cattle. Leguminous plants, such as clover, may form a significant part of cattle

forage. Clover can incorporate nitrogen directly from the atmosphere (nitrogen fixation) and

therefore possesses lower nitrogen-15 isotope (15N) content than other pasture plants. For

other plants, the nitrogen isotope composition of the soil nitrate determines their isotopic

composition, which they incorporate with a small offset towards higher values due to soil

processes such as denitrification (Kornexl et al., 1997). Sea plants and fishmeal are enriched

in 15N and strongly elevated values may be indicative of the inclusion of these materials in the

feed or their use as a fertilizer for forage plants (Schmidt et al., 2005). Synthetic fertiliser

application to fodder crops during cultivation leads to a reduction in their 15N content as a

consequence of the incorporation of nitrogen from air in the Haber process used in ammonia

and synthetic fertiliser production (Bateman & Kelly, 2007).

A summary of authentic British beef defatted dry mass δ15N‰ values is shown in Table



Table 7-3: Summary statistics for the δ15N‰ measurement of authentic British beef defatted d ry mass

samples

δδδδ15N [‰]AIR ENGLAND WALES SCOTLAND

mean 7.1 7.5 7.3

SD 1.1 0.8 1.2

min 4.7 5.7 4.9

max 9.9 9.7 9.8

range 5.2 4.0 4.9

N 101 101 100

There is a high degree of overlap in the mean and ranges of values observed for

English, Scottish and Welsh beef. The widest range of values (5.2‰) was measured in

English beef from 4.7‰ to 9.9‰. The narrowest range of δ15N‰ values (4.0‰) was

observed in the Welsh beef samples from 5.7‰ to 9.7‰.

The nitrogen isotope values of the authentic British beef DDM, at each of the farm

locations, were plotted onto a Google Earth map of the British Isles as polygons which varied

in colour according to the magnitude of the measured δ15N‰ values (Figure 7-6). The white

polygons show the farms that reared beef cattle with the lowest δ15N‰ values in their skeletal

muscle and the black polygons show the highest δ15N‰ values. Farms with examples of

higher beef DDM δ15N‰ values are mainly situated along the western side of the British Isles.



Page 26

Figure 7-6: The nitrogen isotope values of the auth entic British beef DDM, at each of the farm locatio ns. The polygons vary in colour according to the magnitude of the measured δ15N‰ value shown in the scale.

7.4 Evaluation of authentic British beef DDM sulphu r isotope ( δ34S‰) measurements The bulk sulphur isotope composition of the bovine skeletal muscle is related to the

feed, which in turn is related to the sulphur isotope composition of the soil. The incorporation

of sulphur isotopes into mammalian tissues occurs without significant fractionation (or offset)

from the values observed in feed. The sulphur isotope ratio of the soil is related to the δ34S‰

value of the underlying geology. However, the isotopic composition of the soil may also be

affected by sulphur that is transported onto and into the soil e.g. sea-spray sulphate, volcanic

emissions, anthropogenic emissions or fertiliser addition. It is entirely possible that recent

Icelandic volcanic emissions will have an impact on sulphur isotope patterns around Europe.

Typically δ34S‰ values of the sulphate from volcanic emissions are around +8‰ compared to

sea-spray sulphate at around +20‰ (Mather et al., 2006).

A summary of authentic British beef defatted dry mass δ34S‰ values is shown in Table





Page 27

Table 7-4: Summary statistics for the δ

34S‰ measurement of authentic British beef defatted d ry mass samples

δδδδ34S [‰]CDT ENGLAND WALES SCOTLAND

mean 5.1 5.3 8.1

SD 1.7 1.8 2.2

min 1.9 0.1 4.0

max 9.2 8.4 14.5

range 7.3 8.3 10.4

N 91 101 100

From Table 7-4 it can be seen that the mean δ34S‰ values for authentic English and

Welsh beef DDM are very similar at 5.1‰ and 5.3‰, respectively. However, the average

value for authentic Scottish beef DDM is 8.1‰. The mean δ34S‰ value for Scottish beef is

dominated by the sulphur isotope composition of Orkney beef and the marine sea-spray

sulphate signature resulting in relatively high δ34S‰ values. This was also observed in

Orkney lamb (Camin et al., 2007). The highest δ34S‰ value observed for Orkney beef was

14.5‰. This effect can be clearly seen in Figure 7-7 where the sulphur isotope values of the

authentic British beef DDM, at each of the farm locations, were plotted onto a Google Earth

map of the British Isles as polygons which varied in height and colour according to the

magnitude of the measured δ34S‰ values. The brown polygons show the farms that reared

beef cattle with the highest δ34S‰ values in their skeletal muscle and the light blue polygons

show the lowest δ34S‰ values. This aids the visualisation of the sea-spray sulphur isotopic

gradient from the Atlantic Ocean (from the South West to North East) across the British Isles.

Figure 7-7: The sulphur isotope values of the authe ntic British beef DDM, at each of the farm location s. The

polygons vary in height and colour according to the magnitude of the measured δ34S‰ value.

Orkney Isles



Page 28

7.5 Evaluation of authentic British beef DDM stront ium isotope ratio ( 87Sr/86Sr)

measurements

Strontium isotope signatures can be helpful in authenticity determinations, as they have

a different scope than the stable isotopes of the bio-elements (HCNS). This rationale applies

to all natural products including food crops and animal tissues. Thus, ideally if materials

coming from different micro-regions within the same climate zone and therefore having similar

hydrogen and oxygen isotpe values, additional strontium isotope ratio analysis may provide

an additional level of geographical resolution provided that different lithologies exist with that

region.

A total of 273 strontium isotope ratio measurements (87Sr/86Sr) were performed on

authentic beef defatted dry mass by subcontractors Professor Hölzl, Dr Rummel and Dr

Dekant at the Bavarian State Collection for Palaeontology and Geology (BSPG) using thermal

ionisation mass spectrometry (TIMS). A summary of authentic British beef defatted dry mass

δ34S‰ values is shown in Table 7-5. The sample standard deviation (σn-1), minimum,

maximum, range and number of authentic beef samples measured are shown.

Table 7-5: Summary statistics for the 87Sr/86Sr of authentic British beef defatted dry mass samp les

87Sr/86Sr ENGLAND WALES SCOTLAND

mean 0.710555 0.710407 0.711477

SD 0.001953 0.002141 0.002742

min 0.707824 0.706437 0.706815

max 0.716039 0.716671 0.717201

range 0.008215 0.010234 0.010386

N* 78 99 96

The strontium isotope ratios of the authentic British beef DDM, at each of the farm locations,

were plotted onto a Google Earth map of the British Isles as polygons which varied in height

and colour according to the magnitude of the measured 87Sr/86Sr ratio. The brown polygons

show the farms that reared beef cattle with the highest 87Sr/86Sr ratio for their skeletal muscle

and the light blue polygons show the lowest 87Sr/86Sr ratio.



Page 29

Figure 7-8: The strontium isotope values of the aut hentic British beef dry mass (DM), at each of the f arm locations. The polygons vary in height and colour a ccording to the magnitude of the measured δ

87Sr‰ value. An 87Sr/86Sr value of 0.70930 (this value can be considered a s indicative of the mean crustal 87Sr/86Sr ratio for Central-Northern Europe) was used to convert these data to a ‘delta’ scale to permit plotting in ‘GE-g raph’ software. Consequently the scale shows δ

87Sr‰ values.

It can be seen from Figure 7-8 that, for a majority of the samples, the spread of data is rather

large for a given location. In principle, the majority of cattle all over the world predominantly

graze on river flood plains that possess similar strontium values. These conditions are found

even though the soils there originate from mountain ranges with variable lithologies, chemistry

and age. The flood plain areas are mainly sediments from these mountain ranges that have

been weathered and transported from further upstream by water, ice and air. Hence, they

have undergone a thorough mixing resulting in, to a large degree, the averaging out of the

differences in the original variable lithologies and giving the neutral strontium values

associated globally with fertile flood plain regions. Furthermore, a recent study has

demonstrated that marine strontium is an important contributor to the biosphere via

precipitation and sea-spray (Evans et al., 2010). This is particularly the case on the western

coast of the British Isles, which is subjected to high rainfall and prevailing westerly winds.



Page 30

Figure 7-9: The measured strontium isotope ratio ( 87Sr/86Sr) in authentic British beef DDM is shown accordin g to the inset scale on a map of biosphere strontium isotope variation across Britain (Evans et al., 201 0)

However, Figure 7-9 illustrates that very few of the strontium isotope ratios measured in

the bovine skeletal muscle samples correspond directly with the ratios expected from the

biosphere strontium isotope map of Britain recently proposed by Evans et al., 2010. For

example, only 12 of the 78 87Sr/86Sr ratios measured in English beef skeletal muscle

correspond with the ‘isotope package’ or range predicted from the map. The map was

produced by direct measurement of strontium isotope compositions of biosphere components,

predominantly plants. If, as the data appear to indicate, the measured strontium values in



Page 31

authentic beef samples are not indicative of the cattle’s region of origin when compared to

strontium maps, then it must be suspected that in some cases extraneous fodder with

relatively lower or higher 87Sr/86Sr ratios are responsible for the observed data. However, it

should be noted that the published data from Evans et al., is not designed specifically for

tracing the origin of grazing animals. For example, the beef DDM obtained from animals

reared in the red circle in Figure 7-9 possess high 87Sr/86Sr ratios in the range 0.713 to 0.720

compared to the ‘predicted’ composition from the map of 0.709 to 0.710. High 87Sr/86Sr ratios

would be expected in feed cultivated in a neighbouring area such as Cornwall where

igneous/granitic rock is prevalent but the beef samples measured here have values that may

be too high, even for Cornish feed. One possible explanation is the consumption of imported

fodder concentrates from South America, which can possess very high 87Sr/86Sr ratios (Horn,

2005).

7.6 Multivariate analysis of authentic British beef elemental and stable isotope data

The multivariate method chosen was one that falls under the umbrella of supervised

‘pattern recognition’. The database of measured parameters from the authentic British beef

samples was the learning or training set. The specific statistical technique used was

Canonical Discriminant Analysis (CDA). CDA was applied with the aim of finding a rule that

allocated beef samples of unknown origin to the correct group, in this case English, Welsh or

Scottish origin. CDA was chosen because the constructed model can be used to predict the

origin of unknown test samples.

This statistical procedure is based on the idea of finding the directions in multivariate

space which discriminate best between the origins of beef samples. When the most important

direction is found, the method searches for the next direction with the same property, but with

the restriction that the variability along the axis is uncorrelated with the one(s) already

determined. The procedure continues until the desired number of components has been

extracted. Usually, scores for the first discriminant axis are plotted versus scores for the

second discriminant axis for visual inspection of the data.

The selection of the most significant variables was performed by forward ‘stepwise’

analysis. The variables were included in the model one by one, choosing at each step the

variable that made the most significant additional contribution to the discrimination (i.e. with

the largest F value - the value of F provides a test for the statistical significance of the

observed differences among the means of two or more groups). Measured variables were

excluded from the model if they were shown to be redundant. On the basis of the selected

variables, different independent discriminant functions were computed by CDA. Their

maximum number is equal to either the number of variables or the number of groups (in this

case geographical origins) minus one, if the latter is smaller. The statistical significance of

each discriminant function was evaluated on the basis of the Wilks’ Lambda factor after the

function was removed. This parameter ranges from 1.0 (no discriminatory power) to 0.0

(perfect discriminatory power). The separation among groups in the discriminant space was



Page 32

checked by plotting the first and the second functions shown in Figure 7-10. These two axes

represent the two-dimensional plot with the highest degree of separation among the groups.

Figure 7-10: A cross-plot showing the first two dis criminant functions obtained from the stepwise cano nical discriminant analysis of authentic British beef sta ble isotope and elemental concentration data. In t his model the samples were divided into country of orig in groups (England, Wales and Scotland)

Finally, to verify the power and the stability of the model, a ‘leave-one-out’ cross

validation discriminant analysis was performed. In this test known samples were used as

‘unknowns’ to validate the model built on the basis of a reduced set of cases. Effectively, one

sample is removed from the data set and then classified on the basis of model constructed

from the remainder (n = 300). This process is repeated for each sample in turn and the

success of the classification re-calculated by comparison with the known origin. In this model

the samples were divided into country of origin groups (England, Wales and Scotland). The

results of the CDA and cross-validation are shown in the Table 7-6. On average 76.7% of the

beef samples were correctly classified to their country of origin and on average 71.1% of

cross-validated grouped cases were correctly classified. It should be noted that the highest

correct cross-validated classification rates were obtained for Scottish and Welsh beef at

79.8% and 82.2%, respectively. These results demonstrate the reliability of the multivariate

approach in classifying the origin of beef and identifying those variables responsible for the

classification.



Page 33

Table 7-6: Results of stepwise canonical discrimina nt analysis obtained from stable isotope and trace element analyses of authentic British beef samples. In this model the samples were divided into count ry of origin (England, Wales & Scotland).

Classification Results b,c

Origin1

Predicted Group Membership

Total England Scotland Wales

Original Count England 56 4 41 101

Scotland 7 86 6 99

Wales 10 2 89 101

% England 55.4 4.0 40.6 100.0

Scotland 7.1 86.9 6.1 100.0

Wales 9.9 2.0 88.1 100.0

Cross-validateda Count England 52 5 44 101

Scotland 10 79 10 99

Wales 15 3 83 101

% England 51.5 5.0 43.6 100.0

Scotland 10.1 79.8 10.1 100.0

Wales 14.9 3.0 82.2 100.0

a. Cross validation is done only for those cases in the analysis. In cross validation, each

case is classified by the functions derived from all cases other than that case.

b. 76.7% of original grouped cases correctly classified.

c. 71.1% of cross-validated grouped cases correctly classified.

The ‘structure matrix’ of the functions showed the 9 variables chosen for the

discrimination were: Function 1 – the concentrations of strontium, magnesium, phosphorus,

niobium, holmium (in ng/g, ppb) and the stable hydrogen isotope composition (δ2H‰ defatted

dry mass); Function 2 - the concentrations of Zinc, samarium and sodium (in ng/g, ppb).

Discriminant function 1 accounted for 79.2% of the total variance and provides the separation

of the Scottish beef samples from the English and Welsh beef samples. Function 2 equates

to 20.8% of the total variance and provided the separation between the English and Welsh

samples. This explanation of the CDA is also shown diagrammatically in Figure 7-11.



Page 34

Figure 7-11: A cross-plot showing the first two dis criminant functions obtained from the stepwise cano nical discriminant analysis of authentic British beef sta ble isotope and elemental concentration data. The percentage of variation assigned to each of the two functions and the elements used in the discriminan t functions are also shown

Figure 7 -12a: The strontium conce ntration (ng/g, ppb) in the authentic British beef DM, at each of t he farm locations. The polygons vary in height and colour according to the concentration of strontium

Figure 7 -12b: The magnesium concentration (ng/g, ppb) in the authentic British beef DM, at each of t he farm locations. The polygons vary in height and colour according to the concentration of magnesium



Page 35

The existence of differences in element concentrations, identified by CDA, was

qualitatively verified through representation of significant discriminant variables in Google

Earth Graphs. Examples are shown in Figures 7-12a and 7-12b for strontium and

magnesium, respectively.

It is apparent from the first canonical discriminant analysis that distinguishing the origin

of English, Welsh and Scottish beef simultaneously gives rise to a higher rate of

misclassification than if, for example, English and Scottish beef were assessed separately.

Further CDA models produce a much better rate of correct classification when compared in a

pair-wise fashion as illustrated in Table 7-7 below, which summarises the CDA analyses

performed.

Table 7-7: Results of stepwise canonical discrimina nt analysis obtained from stable isotope and trace element analyses of authentic British beef samples. In this model the samples were divided into count ry of origin (England, Wales & Scotland) and were compare d in a pairwise fashion.

Geographical origin of beef Variables used in stepwise CDA ordered by absolute size of correlation within function.

Correct classification rate (Cross-validated)

Wales or Scotland? [δ2H‰], [δ13C‰], [δ15N‰], [Mg], [P], [Ca], [Sr],

[Mn], [Fe], [Cu], [Li], [Ru], [Cd], [Sn], [Tb] 95 %

England or Scotland? [Rb], [Sr], [Mg], [P], [K], [Ca], [Na], [Cd], [Sm],

[Pt] 91%

England or Wales? [δ15N‰], [Na], [Rb], [Ti], [Fe], [Tm], [W], [Re] 71%

Orkney or other Scottish? [δ34S‰], [δ2H‰], [Zn], [Ge], [Ti], [δ2H‰], [Te],

[P], [K], [Ca], [Mg] 95%

These discriminant analyses demonstrate that the assessment of Scottish and Welsh

beef samples separately from English and Scottish produces a superior classification of

geographical origin. The separate discriminant analysis of English and Welsh beef samples

confirmed that the highest rate of misclassification (29.2%) was a result of indistinguishable

English and Welsh samples. Orkney beef is registered as a protected denomination of origin

(PDO) product with the European Commission. Assessment of its origin as a premium

product from other Scottish beef samples resulted in a cross-validated classification rate of

95.0%. these models can be used to assess the origin of unknown test samples.



Page 36

7.7 References

Bahar, B. (2006) Development of isotopic and molecular techniques for the authentication of dietary background information in bovine tissues. PhD thesis, University College, Dublin

Boner, M. & Förstel, H. (2004) Stable isotope variation as a tool to trace the authenticity of beef. Analytical and Bioanalytical Chemistry, 378, 301–310.

Bowen,G.J.; Wassenaar,L.I.; Hobson,K.A. (2005) Global application of stable hydrogen and oxygen isotopes to wildlife forensics. Oecologia, 143 (3), 337-348.

Camin, F., Bontempo, L., Heinrich, K., Thomas, F., Kelly, S.D., et al., (2007) Multi-element (H,C,N,S) stable isotope characteristics of lamb meat from different European regions, Analytical and Bioanalytical Chemistry 389 (1), 309-320

Craig, H. (1961) Isotopic variations in meteoric waters. Science, 133, 1702-1703.

Dansgaard, W. (1964) Stable isotopes in precipitation. Tellus, XVI, 436-468.

Evans, J. A., Montgomery, J., Wildman, G. & Boulton, N. (2010) Spatial variations in biosphere 87Sr/86Sr in Britain, Journal of the Geological Society, 167, 1–4.

Fowler, J and Cohen, L. (1992) Practical statistics for field biology; John Wiley & Sons, pp 227.

Heaton, K., Kelly, S.D., Hoogewerff, J., Woolfe, M.2008, Verifying the geographical origin of beef: The application of multi-element isotope and trace element analysis. Food Chemistry, 107, p. 506-515.

Hobson, K. A. (1999). Tracing origins and migration of wildlife using stable isotopes: a review. Oecologia, 120 (3), 314-326.

Horacek, M., Eisinger, E., Papesch, W., 2009, Using δ18O from meat juice for the determination of the meat origin. Food Chemistry (2009), doi:10.1016/j.foodchem.2009.03.090.

Horn, P. (2005). δ87Sr‰ values for beef reared in a sedimentary basin north of the Alps (Bavaria). Private Communication.

Kornexl, B. E., Werner, T., Rossmann, A., Schmidt, H. L. (1997) Measurement of stable isotope abundances in milk and milk ingredients – A possible tool for origin assignment and quality control. Zeitschrift fü r Lebensmittel-Untersuchung und-Forschung A, 205, 19–24.

Mather T. A., McCabe J. R., Rai V. K., Thiemens M. H., Pyle D. M., Heaton T. H. E., Sloane H. J., Fern G. R. (2006). Oxygen and sulfur isotopic composition of volcanic sulfate aerosol at the point of emission. Journal of geophysical research, 111 (18), 1-4.

Nakashita, R., Suzuki, Y., Akamatsu, F., Iizumi, Y., Korenaga, T., Chikaraishi, Y. (2008). Stable carbon, nitrogen, and oxygen isotope analysis as a potential tool for verifying geographical origin of beef, Analytica Chimica Acta, vol. 617, p. 148–152.

Rubenstein, DR. and Hobson, KA (2004). From birds to butterflies: animal movement patterns and stable isotopes.

Trends in Ecology & Evolution 19, 256-263

Zhang B-L., Pionnier S. & Buddrus S. (2006) Deuterium NMR study of the origin of hydrogen in fatty acids produced in vivo by chicken. European Journal of Lipid Science and Technology, 108 (2), 125-133

Schmidt, O., Quilter, J. M., Bahar, B, Moloney A. P., Scrimgeour C. M., Begley, I. S., Monahan, F. J. (2005) Inferring the origin and dietary history of beef from C, N and S stable isotope ratio analysis. Food Chemistry, 91, 545-549.

Thiem, I., Lüpke, M., Seifert, H. (2004). Factors influencing the 18O/16O-ratio in meat juices Isotopes in Environmental and Health Studies, 40, 191.


Section 8: Conclusions

Page 37

8 CONCLUSIONS

Currently, stable isotope and elemental ‘finger-printing’ offers the only hypothesis-

driven approach to establish the geographical origin of food. For example, our understanding

of how hydrogen isotopes in water vary over the British Isles, due to the effects of the

hydrological cycle, have been shown in this project to be mirrored in bovine skeletal muscle

for cattle reared in Britain.

The main objective of the research described here was to apply isotopic and multi-

element analyses, in combination with statistical processing, to develop techniques to verify

the origin claims made on British beef labels. In this respect, the findings in this report

demonstrate that it is possible with a high degree of certainty to determine the origin of British

beef. The techniques described here are at their most useful when applied to specific origin

problems such as differentiating English beef from Scottish beef or Orkney (PDO) beef from

other Scottish beef. Consequently, the methodology in its current state can be used to provide

reliable origin information, but this is dependent upon the ‘intelligence’ supplied with the

sample. Furthermore, the authentic British beef database can be used to assess whether test

samples are consistent with claims for individual country origin i.e. if the isotope and

elemental results are consistent with the sample being of Scottish (or English or Welsh)

origin.

9 RECOMMENDATIONS FOR FURTHER WORK

Work is currently under way to develop Food Isotope Maps (Isoscapes) to predict the

geographical origin of beef meat produced in locations that are not present in the authentic

sample database or library. This approach is a cost effective way of ensuring the integrity of

premium British foods such as Scotch, Welsh and English beef, thus helping to support the

industry by maintaining consumer confidence in the origin of the product.

Further validation of methodology to include cooked and processed beef would also be

extremely valuable because concerns over the authenticity of the declared origin of beef in

ready meals and restaurants.

The database also lacks samples from Northern Ireland and the Republic of Ireland. As

significant quantities of beef are traded through Northern Ireland it would be prudent to

assess the isotopic and elemental profile of genuine Irish beef to detect third country imports

labelled as UK or Irish in origin.


Section 9 : Publications and other outputs

Page 38

10 PUBLICATIONS AND OTHER OUTPUTS

10.1 Papers in preparation

Kelly, S.D., Marigheto, N.A., Baxter, M., Brereton, N., Hoelzl, S., Rummel, S., Dekant, C.,

Homer, D., Matthews, K., Davies, L., Craigie, C. & Rose, M. (2010) Distinguishing between

English, Welsh and Scottish beef using stable isotope and elemental analyses.

Target Journal – Meat Science

10.2 Scientific presentations

(Presenter underlined)

Poster Presentation: Verifying the Geographical Origin of British Beef

Venue: Joint European Stable Isotope User’s Meeting, September 2008

Authors: Niusa Marigheto, Susanne Rummel, Stefan Hoelzl, Malcolm Baxter, Martin Rose, Dennis

Homer, Kim Matthews and Simon Kelly

Poster Presentation: Geographical Origin of Beef

Venue: JIFSAN, Washington, USA, May 2009

Authors: Malcolm Baxter, Stefan Hoelzl, Dennis Homer, Simon Kelly, Niusa Marigheto, Kim Matthews,

Susanne Rummel, Simon Kelly and Martin Rose

Oral Presentation: Detection of Food Adulteration: Using stable isotope analysis (SIA)

Venue: Institute of Agro-Food Science and Technology, Beijing, China, April 2009


Susanne Rummel, Martin Rose and Simon Kelly

Oral Presentation: Where in the UK did this cow graze? Using Trace technology to protect British beef

Venue: ‘TRACE - New techniques for food assurance and traceability’, Food & Environment Research

Agency, York, UK, December 2009



Oral Presentation: Where now brown cow? Tracing the geographical origin of beef using bio-element

isotope& trace element analysis

Venue: Churchill Museum & Cabinet War Rooms, London, UK, April 2010



Page 39

11 APPENDIX I – COMPLETE LIST OF AUTHENTIC BEEF SAMPLES AND DATA

The British Beef Origin Project (BBOP - Q01123) – Final ReportSection 11: Appendix I – Complete list of authentic beef samples and data

Passport Number

# Reference # MLC # Form Abattoir origin LAT LONG Date sam pled Ear Tag Number Breed Gender Born

1 05010501 0082 whole meat Yorkshire, England 54°10'45. 74"N 0°50'46.59"W 05/01/2005 UK101891300182 Charolais X M 24/08/2002

2 05010502 0083 whole meat Yorkshire, England 54°10'45. 74"N 0°50'46.59"W 05/01/2005 UK104257300084 Limousin X M 14/08/2002

3 05011001 0092 whole meat Shropshire, England 52°56'13. 85"N 2°59'47.92"W 10/01/2005 UK701706600197 British Fri esian M 27/06/2003

4 05011002 0093 whole meat Shropshire, England 52°56'13. 85"N 2°59'47.92"W 10/01/2005 UK705973200159 British Fri esian M 01/11/2002

5 05011009 0100 whole meat Shropshire, England 52°40'13. 63"N 2°18'14.18"W 10/01/2005 UK700519700141 Charolais X F 10/10/2002

6 05011010 0101 whole meat Shropshire, England 52°40'13. 63"N 2°18'14.18"W 10/01/2005 UK701598200054 Limousin X M 17/07/2002

7 05011201 0102 whole meat Cheshire, England 52°43'22.36 "N 2°56'56.52"W 12/01/2005 UK303142100490 Limousin X M 13 /10/2003

8 05011202 0103 whole meat Cheshire, England 52°43'42.12 "N 2°55'49.19"W 12/01/2005 UK303149500151 Limousin X M 19 /07/2003

9 05011204 0105 whole meat Cheshire, England 52°43'22.36 "N 2°56'56.52"W 12/01/2005 UK303142200505 Belgian Blue M 16/09/2003

10 05011206 0109 whole meat Cheshire, England 53° 1'14. 71"N 2°33'26.05"W 12/01/2005 UK200402400890 Holstein F 25/10/2002

11 05020101 0112 whole meat Dorset, England 51°10'53.93 "N 2°45'19.00"W 01/02/2005 UK344391200172 Simmental X F 18/04/2003

12 05020102 0113 whole meat Dorset, England 50°58'9.03"N 3°17'40.49"W 01/02/2005 UK361096700211 Devon X F 06/08/2 002

13 05020801 0117 whole meat Cheshire, England 51°53'47. 44"N 3° 6'21.03"W 08/02/2005 UK720191100223 Blonde D'Aq uitaine X ?? ??

14 05020802 0118 whole meat Cheshire, England 52°23'7.8 0"N 3° 4'59.58"W 08/02/2005 UK303532600224 Charolais X ?? ??

15 05021501 0130 whole meat Lancs, England 53°46'20.52" N 2°35'27.70"W 15/02/2005 UK740447300130 Charolais X F 0 5/07/2003

16 05021502 0131 whole meat Lancs, England 53°46'20.52" N 2°35'27.70"W 15/02/2005 UK181824400050 Charolais F 10 /05/2003

17 05022201 0149 whole meat Cornwall, England 50°40'29.5 8"N 4°21'25.70"W 22/02/2005 UK363056500160 Holstein Fri esian M 03/09/2002

18 09082517 AHDB 263 whole meat Whitley Bay, England 55°20'56.67"N 1°39'36.62"W 25/08/2009 UK106483100537 Simm ental X F 26/04/2007

19 05022202 0150 whole meat Cornwall, England 50°40'29.5 8"N 4°21'25.70"W 22/02/2005 UK366181700399 Limousin X F 0 5/09/2002

20 09082518 AHDB 264 whole meat Whitley Bay, England 55°18'24.82"N 1°39'10.70"W 25/08/2009 UK340854500703 Char olais X M 05/04/2007

21 05022205 0153 whole meat Cornwall, England 50°32'24.6 9"N 4°11'7.27"W 22/02/2005 UK364316100184 Limousin X M 30 /08/2002


23 09082520 AHDB 266 whole meat Whitley Bay, England 55°14'54.75"N 1°43'13.87"W 25/08/2009 UK540663300738 Limo usin X M 27/07/2007

24 05022210 0158 whole meat Cornwall, England 50°32'32.2 4"N 4°18'58.95"W 22/02/2005 UK381298700029 Limousin X F 0 3/05/2003

25 09082521 AHDB 267 whole meat Whitley Bay, England 55°18'26.92"N 1°42'13.96"W 25/08/2009 UK106352500965 Limo usin X M 16/11/2007

26 05042604 0176 whole meat Shropshire, England 52°40'13 .63"N 2°18'14.18"W 26/04/2005 UK304669200311 Limousin X F 27/07/2003

27 05042605 0179 whole meat Shropshire, England 52°40'13 .63"N 2°18'14.18"W 26/04/2005 UK304699500283 Belgian Bl ue X F 13/04/2003

28 05042801 0183 whole meat Cheshire, England 52°31'37.5 7"N 3° 1'8.64"W 28/04/2005 UK303433200282 Limousin X F 28 /04/2005

29 09082524 AHDB 270 whole meat Whitley Bay, England 55°15'22.95"N 1°36'0.33"W 25/08/2009 UK106804300698 Limou sin X F 11/01/2008

30 05042701 0187 whole meat Cheshire, England 53°11'38. 87"N 2°39'18.18"W 27/04/2005 UK160954400086 Simmental M 01/04/2004

31 09082525 AHDB 271 whole meat Whitley Bay, England 55°15'22.95"N 1°36'0.33"W 25/08/2009 UK106774400366 Limou sin X F 25/12/2007

32 05042702 0188 whole meat Cheshire, England 53°11'38. 87"N 2°39'18.18"W 27/04/2005 UK160954100076 Simmental M 24/01/2004

33 09082526 AHDB 272 whole meat Whitley Bay, England 55° 5'17.00"N 1°39'51.53"W 25/08/2009 UK106473600235 Wel sh BLack F 12/04/2007

34 05042704 0190 whole meat Cheshire, England 53°11'38. 87"N 2°39'18.18"W 27/04/2005 UK705033200358 Limousin F 25/06/2003

35 05042705 0191 whole meat Cheshire, England 53°11'38. 87"N 2°39'18.18"W 27/04/2005 UK160954500073 Limousin X F 29/08/2003

36 05050302 0207 whole meat Dorset, England 51° 1'38.50 "N 2°27'40.29"W 03/05/2005 UK345031400236 Hereford X M 12/02/2003

37 09082529 AHDB 275 whole meat Whitley Bay, England 55°38'59.45"N 1°52'24.73"W 25/08/2009 UK582311500757 Limo usin X F 10/09/2007

38 05050401 0216 whole meat Lancs, England 53°54'5.95"N 2°28'57.04"W 04/05/2005 UK182628500119 Limousin X M 02 /06/2003

39 09082530 AHDB 276 whole meat Whitley Bay, England 55°38'59.45"N 1°52'24.73"W 25/08/2009 UK106566300950 Char olais X F 10/11/2007

BBOP England Page 40


Passport Number


40 05050402 0217 whole meat Lancs, England 53°54'5.95"N 2°28'57.04"W 04/05/2005 UK182589400236 Belgian Blue X M 06/03/2003

41 09082531 AHDB 277 whole meat Whitley Bay, England 55°18'22.38"N 1°34'25.47"W 25/08/2009 UK107145600823 Belg ian Blue X M 25/07/2007



44 05051902 0237 whole meat Yorkshire, England 53°21'58. 85"N 1°16'43.51"W 19/05/2005 UK106288400052 Limousin X M 10/06/2003

45 05051904 0239 whole meat Yorkshire, England 53°21'58. 85"N 1°16'43.51"W 19/05/2005 UK107164200262 Belgian Blu e X M 18/04/2003

46 05051907 0242 whole meat Yorkshire, England 53°21'58. 85"N 1°16'43.51"W 19/05/2005 UK162504300063 Charolais X M 29/12/2002

47 05051910 0245 whole meat Yorkshire, England 53°21'58. 85"N 1°16'43.51"W 19/05/2005 UK103830700151 Limousin M 1 8/01/2003

48 05081501 0251 whole meat Yorkshire, England 54°15'38. 82"N 1° 6'7.55"W 15/08/2005 UK720041400073 Limousin X F 0 1/12/2003

49 05081508 0258 whole meat Yorkshire, England 54°15'38. 82"N 1° 6'7.55"W 15/08/2005 UK300489100042 Limousin X F 3 1/03/2003

50 05081509 0259 whole meat Yorkshire, England 54°15'38. 82"N 1° 6'7.55"W 15/08/2005 UK320812400112 Limousin X M 2 4/06/2003

51 05081602 0262 whole meat Cheshire, England 53°11'38. 87"N 2°39'18.18"W 16/08/2005 UK160954600074 Simmental F 21/01/2004


53 05081607 0268 whole meat Cheshire, England 53°10'8.6 8"N 2°46'59.79"W 16/08/2005 UK705832200143 Limousin M 24/02/2003

54 05081807 0287 whole meat Cornwall, England 50°36'52.2 3"N 4°25'7.85"W 18/08/2005 UK383029100272 South Devon M 1 1/04/200355 05081809 0289 whole meat Cornwall, England 50°36'52.2 3"N 4°25'7.85"W 18/08/2005 UK380646400017 South Devon M 0 3/03/200356 05082508 0308 whole meat Lancs, England 54°26'56.27" N 3°29'57.24"W 25/08/2005 UK100481700376 British Frie sian F 18/04/2003

57 05090704 0318 whole meat Dorset, England 51° 7'43.05 "N 2°46'59.55"W 07/09/2005 UK344578100650 Hereford X F 03/11/2003

58 05102401 0501 whole meat Cornwall, England 50°36'52.2 3"N 4°25'7.85"W 24/10/2005 UK383071700054 Limousin M 29/ 06/2003

59 05102403 0503 whole meat Cornwall, England 50°36'52.2 3"N 4°25'7.85"W 24/10/2005 UK383029600305 South Devon M 0 7/08/2003


61 05102601 0522 whole meat Dorset, England 51°28'36.80" N 2°20'40.31"W 26/10/2005 UK321802500147 Limousin X M 19/ 05/2003

62 05102602 0523 whole meat Dorset, England 51° 7'43.05 "N 2°46'59.55"W 26/10/2005 UK344578500682 Limousin X F 23/12/2003

63 05102704 0534 whole meat Lancs, England 54°26'35.66" N 2°53'42.83"W 27/10/2005 UK100408100161 Blonde D'Aqu itaine X M 06/06/2003

64 05110816 0567 whole meat Cheshire, England 53°10'8.6 8"N 2°46'59.79"W 08/11/2005 UK161427700076 Charolais X F 20/01/2004

65 05110817 0568 whole meat Cheshire, England 53°10'8.6 8"N 2°46'59.79"W 08/11/2005 UK304766600390 Limousin X F 21/08/2003

66 05112903 0807 whole meat Shropshire, England 53° 1'1 4.71"N 2°33'26.05"W 29/11/2005 UK706760200228 Simment al X M 08/06/2003

67 05112907 0812 whole meat Shropshire, England 53° 1'1 4.71"N 2°33'26.05"W 29/11/2005 UK161629300875 Belgian Blue M 09/08/2003

68 05112910 0815 whole meat Shropshire, England 53° 1'5 4.62"N 2°31'44.57"W 29/11/2005 UK305498500131 Herefor d X M 19/10/2003

69 05112911 0816 whole meat Shropshire, England 53° 1'5 4.62"N 2°31'44.57"W 29/11/2005 UK746151200176 Charola is X F 15/06/2003

70 06021501 0821 whole meat Lancs, England 54°17'41.16" N 3°23'47.56"W 15/02/2006 UK101031600390 Limousin X F 2 1/01/2004

71 06021502 0822 whole meat Lancs, England 54°10'23.31" N 2°59'23.25"W 15/02/2006 UK104058300260 Belgian Blue X M 14/03/2004

72 06021509 0829 whole meat Lancs, England 54° 8'24.87" N 3°14'19.61"W 15/02/2006 UK124988400590 Charolais X F 06/05/2004


74 06021404 0834 whole meat Dorset, England 51°10'53.93 "N 2°45'19.00"W 14/02/2006 UK344391700233 Limousin X F 26/03/2004


76 06022801 0841 whole meat Cornwall, England 50°23'3.07 "N 4°21'54.00"W 28/02/2006 UK384568400273 Aberdeen Angu s X M 15/03/2004

77 06022802 0842 whole meat Cornwall, England 50°23'3.07 "N 4°21'54.00"W 28/02/2006 UK384568400301 Aberdeen Angu s X M 29/04/2004

78 06022807 0847 whole meat Cornwall, England 50°23'3.07 "N 4°21'54.00"W 28/02/2006 UK384568700311 Blonde D'Aqui taine X M 15/10/2004



Passport Number


79 06022810 0850 whole meat Cornwall, England 50°23'3.07 "N 4°21'54.00"W 28/02/2006 UK384568500302 Aberdeen Angu s X F 29/04/2004

80 06012306 0896 whole meat Yorkshire, England 53°50'46 .19"N 0°29'50.24"W 23/01/2006 UK142186101369 Salers X M 18/03/2004

81 06012310 0900 whole meat Yorkshire, England 53°50'46 .19"N 0°29'50.24"W 23/01/2006 UK142169300798 Charolai s X M 20/04/2004

82 06050903 0918 whole meat Cheshire, England 53°11'38. 87"N 2°39'18.18"W 09/05/2006 UK160957600794 Hereford X F 21/09/2004

83 06050904 0919 whole meat Cheshire, England 53°11'38. 87"N 2°39'18.18"W 09/05/2006 UK160957600766 Hereford X F 27/06/2004

84 06060602 0942 whole meat Lancs, England 54°35'28.00" N 2°40'9.67"W 06/06/2006 UK103856200282 Holstein Frie sian X M 10/08/2004

85 06060605 0945 whole meat Lancs, England 54°59'48.80" N 2°53'51.00"W 06/06/2006 UK102656600693 Holstein Fri esian M 22/04/2005

86 06060608 0948 whole meat Lancs, England 54°21'44.84" N 2°39'37.49"W 06/06/2006 UK103374500322 Belgian Blue X M 19/03/2005

87 06060610 0950 whole meat Lancs, England 54°45'36.68" N 2°55'12.14"W 06/06/2006 UK102505100337 Meuse Rhine Issel X M 28/03/2005

88 06080201 0991 whole meat Dorset, England 50°50'30.68 "N 3°20'3.59"W 02/08/2006 UK341661300607 Aberdeen Ang us X F 20/08/2004

89 06080202 0992 whole meat Dorset, England 50°45'7.03" N 3°19'12.27"W 02/08/2006 UK363896700358 Limousin X F 0 5/04/2004

90 06080205 0995 whole meat Dorset, England 50°44'42.00 "N 3°15'14.55"W 02/08/2006 UK363904400623 Aberdeen An gus X F 12/02/2004

91 06080206 0996 whole meat Dorset, England 50°44'42.00 "N 3°15'14.55"W 02/08/2006 UK363904200642 Aberdeen An gus X F 08/04/2004



94 06081805 1015 whole meat Cornwall, England 50°45'29. 01"N 3°46'44.37"W 18/08/2006 UK366494300118 Devon X M 2 5/04/2004

95 06072706 1036 whole meat Lancs, England 54°34'50.90" N 3°26'18.81"W 27/07/2006 UK100415400360 Limousin X M 2 3/02/2004

96 E09052801 BB911 whole meat Skegness, Lincolnshire 53°10'7.16"N 0° 9'36.33"E 28/05/2009 UK141150200180 Lincol n Red X F 14/05/2007

97 E09052802 BB912 whole meat Skegness, Lincolnshire 53°10'7.16"N 0° 9'36.33"E 28/05/2009 UK141150100179 Lincol n Red X M 14/05/2007

98 E09052803 BB913 whole meat Skegness, Lincolnshire 53°10'7.16"N 0° 9'36.33"E 28/05/2009 UK141150300202 Lincol n Red X M 18/04/2008

99 E09052804 BB914 whole meat Skegness, Lincolnshire 53°20'9.20"N 0° 8'20.71"W 28/05/2009 UK140945400906 Lin coln Red F 20/04/2007

100 E09052805 BB915 whole meat Skegness, Lincolnshire 53°20'9.20"N 0° 8'20.71"W 28/05/2009 UK140945600950 Li ncoln Red X F 13/06/2007

101 E09052806 BB916 whole meat Skegness, Lincolnshire 53°20'9.20"N 0° 8'20.71"W 28/05/2009 UK140945200946 Li ncoln Red X F 27/05/2007

mean

SD

min

max

rangeN



# Reference # MLC #

1 05010501 0082

2 05010502 0083

3 05011001 0092

4 05011002 0093

5 05011009 0100

6 05011010 0101

7 05011201 0102

8 05011202 0103

9 05011204 0105

10 05011206 0109

11 05020101 0112

12 05020102 0113

13 05020801 0117

14 05020802 0118

15 05021501 0130

16 05021502 0131

17 05022201 0149

18 09082517 AHDB 263

19 05022202 0150

20 09082518 AHDB 264

21 05022205 0153

22 05022206 0154

23 09082520 AHDB 266

24 05022210 0158

25 09082521 AHDB 267

26 05042604 0176

27 05042605 0179

28 05042801 0183

29 09082524 AHDB 270

30 05042701 0187

31 09082525 AHDB 271

32 05042702 0188

33 09082526 AHDB 272

34 05042704 0190

35 05042705 0191

36 05050302 0207

37 09082529 AHDB 275

38 05050401 0216

39 09082530 AHDB 276

Protein SD/AD Protein SD/AD Protein SD/AD Protein SD/AD 87/ 86Sr 2SD(abs)

d2H [‰] [‰] n d13C [‰] [‰] n d15N [‰] [‰] n d34S [‰] [‰] n [‰]

-96.3 1.8 3 -26.12 0.10 3 7.1 0.1 3 3.7 0.3 3 0.708498 0.00002

-100.6 1.1 3 -26.11 0.06 3 6.5 0.0 3 5.5 0.6 3 0.710056 0.000078

-97.7 0.8 3 -25.90 0.05 3 6.8 0.1 3 7.1 0.4 3 0.709965 0.000245

-99.4 0.7 3 -25.98 0.06 3 8.5 0.0 3 3.1 0.6 3 0.710443 0.000245

-97.5 0.3 3 -26.51 0.06 3 7.9 0.1 3 4.7 0.3 3 0.708814 0.000116

-103.2 1.1 3 -25.59 0.08 3 6.5 0.1 3 4.3 0.2 3 0.710565 0.000112

-101.3 1.6 3 -25.43 0.04 3 5.9 0.0 3 5.6 0.6 3 0.710491 0.000145

-98.5 3.0 3 -25.38 0.12 3 6.4 0.1 3 5.5 0.6 3 0.710716 0.000079

-102.6 1.2 3 -25.50 0.06 3 5.6 0.0 3 4.8 0.3 3 0.709896 0.000496

-101.8 1.1 3 -27.60 0.14 3 9.9 0.1 3 2.0 0.2 3 0.710426 0.000125

-100.3 0.3 3 -25.89 0.10 3 6.7 0.1 3 2.2 0.1 3 0.708989 0.000112

-93.7 0.2 3 -22.96 0.05 3 7.7 0.1 3 3.6 0.3 3 0.707824 0.000259

-90.5 2.5 3 -19.64 0.03 3 6.8 0.0 3 2.8 0.2 3 0.708801 0.000087

-99.0 2.1 3 -24.35 0.04 3 6.0 0.0 3 3.2 0.1 3 0.711334 0.000162

-90.8 0.8 3 -20.34 0.11 3 9.5 0.1 3 6.2 0.3 3 0.709923 0.000095

-94.0 1.9 3 -20.95 0.06 3 9.4 0.1 3 6.7 0.1 3 0.70831 0.000066

-88.0 1.4 3 -24.74 0.09 3 6.8 0.1 3 4.1 0.5 3 0.710002 0.000245

-100.2 1.5 3 -26.00 0.07 3 5.1 0.1 3 4.8 na 1 0.711559 0.0047

-90.8 1.0 3 -24.95 0.02 3 6.5 0.1 3 8.2 0.2 3 0.710541 0.000043

-98.0 0.8 3 -26.83 0.02 3 8.0 0.0 3 5.1 na 1 0.712594 0.0057

-91.6 0.7 3 -24.51 0.00 3 6.7 0.0 3 7.9 0.3 3 0.709807 0.0082

-92.5 1.5 3 -24.07 0.03 3 6.2 0.0 3 7.8 0.2 2 0.713739 0.011500

-100.5 0.8 3 -26.93 0.02 2 5.7 0.0 2 6.0 na 1 0.709801 0.0052

-92.5 1.3 3 -25.56 0.13 3 5.5 0.1 3 7.8 0.2 3 0.707878 0.000108

-100.5 1.8 3 -25.95 0.03 2 5.8 0.1 2 4.9 na 1 0.708633 0.0046

-101.3 1.5 3 -26.57 0.08 3 6.3 0.1 3 4.3 0.1 3 0.710175 0.000104

-104.8 1.1 3 -26.64 0.03 3 7.7 0.1 3 3.9 0.3 3 0.70866 0.000083

-105.0 1.7 3 -25.85 0.04 3 7.2 0.1 3 5.5 0.2 3 0.709035 0.000059

-100.5 1.3 3 -25.38 0.04 2 5.5 0.3 2 7.2 na 1 0.709899 0.0073

-95.0 0.4 3 -20.85 0.06 3 7.1 0.1 3 4.7 0.1 3 0.710378 0.000088

-101.8 1.0 3 -25.68 0.10 2 5.4 0.3 2 4.5 na 1 0.709701 0.0053

-94.3 1.5 3 -21.16 0.03 3 7.7 0.1 3 4.9 0.1 3 0.710086 0.0005

-101.3 0.9 3 -26.70 0.08 2 7.4 0.2 2 0.710512 0.0035

-93.6 2.7 3 -21.29 0.11 3 7.7 0.0 3 2.5 0.2 3 0.710427 0.000188

-98.2 1.2 3 -21.30 0.07 3 7.5 0.0 3 3.7 0.3 3 0.70949 0.00014

-93.9 2.1 3 -26.26 0.11 3 8.7 0.1 3 4.8 0.1 3 0.709317 0.000084

-104.6 1.0 3 -25.90 0.19 2 6.2 0.2 2 4.3 0.709348 0.0035

-99.0 1.7 3 -25.75 0.10 3 6.2 0.0 3 3.9 0.3 3 0.70959 0.000166

-101.2 0.6 3 -25.83 0.11 2 6.1 0.0 2 3.1 0.709989 0.0086



# Reference # MLC #

40 05050402 0217

41 09082531 AHDB 277

42 05050404 0219

43 05050406 0221

44 05051902 0237

45 05051904 0239

46 05051907 0242

47 05051910 0245

48 05081501 0251

49 05081508 0258

50 05081509 0259

51 05081602 0262

52 05081603 0263

53 05081607 0268

54 05081807 028755 05081809 028956 05082508 0308

57 05090704 0318

58 05102401 0501

59 05102403 0503

60 05102405 0505

61 05102601 0522

62 05102602 0523

63 05102704 0534

64 05110816 0567

65 05110817 0568

66 05112903 0807

67 05112907 0812

68 05112910 0815

69 05112911 0816

70 06021501 0821

71 06021502 0822

72 06021509 0829

73 06021402 0832

74 06021404 0834

75 06021409 0839

76 06022801 0841

77 06022802 0842

78 06022807 0847


d2H [‰] [‰] n d13C [‰] [‰] n d15N [‰] [‰] n d34S [‰] [‰] n [‰]

-94.5 0.9 3 -25.89 0.02 3 6.2 0.1 3 2.6 0.2 3 0.709538 0.000286

-101.3 3.0 3 -25.96 0.09 2 6.4 0.1 2 6.3 na 1 0.710295 0.0066

-91.8 0.4 3 -25.83 0.10 3 6.1 0.1 3 4.5 0.2 3 0.710628 0.000105

-97.0 0.5 3 -25.84 0.07 3 6.0 0.1 3 3.9 0.1 3 0.709107 0.000267

-95.5 2.7 3 -25.60 0.10 3 6.5 0.0 3 3.9 0.2 3 0.7096 0.00009

-99.3 2.2 3 -25.62 0.03 3 6.3 0.1 3 4.7 0.1 3 0.710621 0.000075

-99.2 0.9 3 -25.57 0.09 3 6.4 0.1 3 4.2 0.1 3 0.710621 0.000205

-100.8 2.1 3 -25.41 0.08 3 6.6 0.0 3 4.5 0.1 3 0.70892 0.000047

-98.1 2.0 3 -25.33 0.02 3 6.6 0.1 3 5.8 0.1 3 unmeasurable na

-97.3 1.7 3 -25.43 0.09 3 6.2 0.0 3 5.1 0.1 3 unmeasurable na

-98.6 0.9 3 -25.12 0.07 3 6.2 0.1 3 5.0 0.0 2 unmeasurable na

-97.4 2.1 3 -25.46 0.01 3 9.7 0.1 3 4.9 0.1 3 0.711107 0.000106

-95.3 1.7 3 -25.14 0.13 3 9.4 0.1 3 4.8 0.1 3 unmeasurable na

-94.4 0.2 3 -25.08 0.06 3 7.3 0.0 3 4.6 0.3 3 unmeasurable na

-97.0 0.7 3 -26.98 0.07 3 6.7 0.1 3 8.1 0.0 3 0.709681 0.000059-93.2 2.6 3 -26.61 0.04 3 6.5 0.0 3 7.3 0.1 3 0.710444 0.0001-96.1 2.4 3 -26.57 0.03 3 8.6 0.0 3 8.0 0.1 2 0.709336 0.0097

-88.0 2.1 3 -24.55 0.07 3 8.4 0.1 3 2.6 0.2 3 unmeasurable na

-90.8 1.7 3 -27.04 0.14 3 8.7 0.1 3 7.5 0.1 3 0.710067 0.000079

-92.3 0.9 3 -27.09 0.09 3 8.3 0.0 3 7.7 0.1 3 unmeasurable na

-93.8 0.9 3 -26.97 0.13 3 7.3 0.0 3 7.0 0.2 3 0.708922 0.000117

-101.1 0.6 3 -25.47 0.11 3 4.7 0.1 3 2.3 0.2 3 unmeasurable na

-91.8 1.1 3 -23.66 0.07 3 8.6 0.0 3 3.3 0.1 3 unmeasurable na

-92.9 1.2 3 -25.75 0.01 3 7.1 0.0 3 7.6 0.1 2 0.715021 0.0035

-92.7 1.6 3 -26.74 0.08 3 7.9 0.1 3 4.1 0.2 3 unmeasurable na

-95.6 2.0 3 -26.58 0.12 3 7.2 0.1 3 4.2 0.1 3 unmeasurable na

-96.2 0.5 3 -26.80 0.01 3 9.1 0.1 3 4.2 0.1 3 unmeasurable na

-95.7 0.4 3 -27.00 0.10 3 8.0 0.1 3 5.0 0.0 3 unmeasurable na

-95.7 1.6 3 -25.70 0.12 3 6.7 0.1 3 4.5 0.1 3 unmeasurable na

-98.8 1.5 3 -26.10 0.06 3 7.7 0.1 3 4.4 0.1 3 unmeasurable na

-92.9 1.0 3 -26.07 0.01 3 8.6 0.0 3 7.4 0.3 2 0.709908 0.0042

-94.9 0.4 3 -25.79 0.02 3 6.5 0.0 3 7.8 0.4 2 0.710720 0.0091

-92.4 0.7 3 -25.98 0.09 3 8.0 0.0 3 4.1 0.1 3 0.708698 0.0026

-99.2 1.1 3 -26.36 0.04 3 6.7 0.1 3 5.1 0.2 3 unmeasurable na

-94.0 1.8 3 -26.40 0.05 3 8.2 0.1 3 2.0 0.1 3 unmeasurable na

-97.0 2.2 3 -26.38 0.08 3 7.8 0.1 3 5.5 0.3 3 unmeasurable na

-91.2 0.9 3 -25.62 0.03 3 6.2 0.1 3 9.2 0.1 3 0.709867 0.000046

-90.3 1.5 3 -25.47 0.07 3 6.0 0.0 3 7.7 1.1 3 0.711016 0.000089

-86.2 0.2 3 -26.17 0.06 3 6.0 0.1 3 9.1 0.2 3 0.710127 0.000046



# Reference # MLC #

79 06022810 0850

80 06012306 0896

81 06012310 0900

82 06050903 0918

83 06050904 0919

84 06060602 0942

85 06060605 0945

86 06060608 0948

87 06060610 0950

88 06080201 0991

89 06080202 0992

90 06080205 0995

91 06080206 0996

92 06080207 0997

93 06080210 1000

94 06081805 1015

95 06072706 1036

96 E09052801 BB911

97 E09052802 BB912

98 E09052803 BB913

99 E09052804 BB914

100 E09052805 BB915

101 E09052806 BB916

mean

SD

min

max

rangeN


d2H [‰] [‰] n d13C [‰] [‰] n d15N [‰] [‰] n d34S [‰] [‰] n [‰]

-90.0 1.3 3 -25.48 0.07 3 6.2 0.1 3 9.1 0.3 3 0.709633 0.000083

-97.9 1.8 3 -25.54 0.06 3 6.6 0.1 3 6.2 0.0 3 unmeasurable na

-97.1 1.7 3 -25.18 0.01 3 6.9 0.1 3 5.4 0.1 3 unmeasurable na

-97.9 1.4 3 -24.53 0.01 3 7.8 0.0 3 5.2 0.1 3 unmeasurable na

-94.3 1.1 3 -24.94 0.01 3 7.9 0.1 3 5.1 0.0 3 unmeasurable na

-98.1 1.2 3 -25.62 0.00 3 9.0 0.0 3 5.1 0.1 3 0.709164 0.0043

-97.6 0.9 3 -25.73 0.05 3 6.6 0.0 3 5.5 0.5 3 0.716039 0.0076

-96.4 0.3 3 -25.51 0.01 3 6.6 0.0 3 4.8 0.3 3 0.712338 0.0041

-98.7 1.3 3 -24.54 0.01 3 7.9 0.0 3 6.6 0.1 3 0.715883 0.0036

-96.9 0.5 3 -26.68 0.02 3 8.4 0.0 3 4.9 0.5 3 0.71339 0.0098

-93.4 0.9 3 -26.92 0.01 3 8.1 0.0 3 5.9 0.4 3 unmeasurable na

-96.2 1.3 3 -26.10 0.01 3 7.9 0.1 3 5.6 0.5 3 0.712909 0.0067

-93.8 0.6 3 -26.02 0.03 3 7.3 0.0 3 6.4 0.0 2 0.71351 0.0063

-94.5 0.4 3 -26.29 0.02 3 7.7 0.0 3 4.7 0.3 3 0.715042 0.0062

-95.4 0.9 3 -26.90 0.03 3 6.4 0.0 3 5.1 0.3 3 0.714758 0.0042

-91.9 0.4 3 -26.63 0.02 3 6.5 0.0 3 5.4 0.5 3 0.714793 0.0066

-96.0 0.5 3 -27.11 0.06 3 8.1 0.1 3 5.2 0.3 3 0.709475 0.0054

-101.02 0.68 3 -26.33 0.04 3 7.18 0.13 3 1.93 0.12 2 0.714357 0.0066

-100.42 2.03 3 -26.34 0.01 3 7.69 0.11 3 2.2 0.4 3 0.715251 0.0063

-100.28 1.75 3 -26.37 0.02 3 9.00 0.08 3 2.6 0.6 3 0.708903 0.0026

-100.40 1.12 3 -26.03 0.01 3 5.19 0.03 3 3.3 0.2 3 0.709309 0.0034

-105.85 1.10 3 -26.22 0.03 3 5.93 0.03 3 3.1 0.1 3 0.708931 0.0110

-103.82 0.40 3 -26.25 0.02 3 6.06 0.04 3 3.2 0.1 3 0.709189 0.0088

δδδδ2H [‰] δδδδ13C [‰] δδδδ15N [‰] δδδδ34S [‰] 87/86Sr

-96.68 -25.52 7.11 5.08 0.7105555

4.09 1.51 1.12 1.74 0.0019532

-105.85 -27.60 4.73 1.93 0.7078240

-86.23 -19.64 9.91 9.25 0.7160390

19.63 7.96 5.18 7.31 0.0082150101 101 101 100 78



# Reference # MLC #

1 05010501 0082

2 05010502 0083

3 05011001 0092

4 05011002 0093

5 05011009 0100

6 05011010 0101

7 05011201 0102

8 05011202 0103

9 05011204 0105

10 05011206 0109

11 05020101 0112

12 05020102 0113

13 05020801 0117

14 05020802 0118

15 05021501 0130

16 05021502 0131

17 05022201 0149

18 09082517 AHDB 263

19 05022202 0150

20 09082518 AHDB 264

21 05022205 0153

22 05022206 0154

23 09082520 AHDB 266

24 05022210 0158

25 09082521 AHDB 267

26 05042604 0176

27 05042605 0179

28 05042801 0183

29 09082524 AHDB 270

30 05042701 0187

31 09082525 AHDB 271

32 05042702 0188

33 09082526 AHDB 272

34 05042704 0190

35 05042705 0191

36 05050302 0207

37 09082529 AHDB 275

38 05050401 0216

39 09082530 AHDB 276

Na 23 Mg 24 Al 27 P 31 K 39 Ca 43 Rb 85 Sr 88 Ba 138 Sc 45 T i 48 V 51 Cr 52 Mn 55

µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg

3130829 562850 1500 4672126 8972797 219415 5644 112 83 1 622 2 25 327

2420913 572345 1566 4892042 9533082 169607 6458 60 114 2 459 2 30 278

2981716 723527 1562 6302468 11482080 445575 6716 188 118 2 1439 5 127 425

2907310 885075 1255 7087762 13798080 239100 8075 144 89 2 696 4 37 501

2939332 942767 711 7870084 15145540 176100 6768 68 69 1 354 1 5 384

2867153 955979 1579 7870702 15767140 194442 4444 66 109 1 569 3 24 269

2633766 1029562 1449 8279730 15983482 213922 8374 86 65 2 496 2 75 348

2461155 966607 2253 8167842 16317068 175156 9870 92 98 3 469 4 30 266

2127998 1003558 630 8068161 16614084 224868 7206 86 84 2 608 2 10 166

2463935 777470 1044 6718299 13592162 192719 6805 69 83 1 498 1 5 355

2272457 912746 890 7509482 14501436 230273 8390 160 53 0 538 1 24 281

2094279 747947 798 6016897 11040503 175486 4207 134 619 2 661 1 18 529

2796267 493197 1839 4372547 7801089 173206 6279 114 190 4 475 2 34 262

2799268 949962 2942 7976180 16365420 333099 15254 144 131 6 1594 4 46 225

2490668 768439 1035 6582406 13425409 198902 10253 93 50 1 559 1 50 222

2569941 905032 1178 7426007 14571291 173590 10233 65 128 3 470 1 22 308

3927577 886185 1032 7558896 13791787 246118 20471 154 66 2 560 1 38 515

2263229 1057960 1339 8933282 15470199 298969 5445 169 295 3 23 2 15 347

3365040 762524 1161 6151637 12283669 211441 14310 130 44 3 742 2 93 308

2642386 919841 2521 8071670 14535511 585355 16518 318 731 3 349 2 6 442

3415444 1001826 571 8017211 15676857 213336 10426 93 45 2 742 1 24 379

3018146 1064338 1121 8654218 17239619 222535 11185 94 120 3 1357 1 13 250

2186068 998091 772 8894932 15412317 183738 9639 120 99 1 295 1 33 366

2376200 968309 907 7952772 14855290 183211 12494 91 41 2 384 2 5 330

2278976 972996 993 8413148 14688256 214201 8794 128 403 2 295 1 10 327

2688329 1064904 703 8535207 16277303 166269 3915 50 73 1 389 1 3 267

2099497 961580 859 7780797 14566368 154938 3544 58 83 2 363 1 4 439

2953958 897516 2533 7402803 14306549 194411 11150 200 101 4 656 5 36 542

2402304 971011 507 8691201 16062768 213191 4406 111 179 3 295 1 12 360

3224787 994026 689 8038427 15464846 195960 9665 60 79 1 478 1 11 248

2687711 962970 671 7929426 15679239 330127 4389 184 201 0 738 2 34 221

3129919 943547 456 7781671 14856873 201979 9260 55 68 1 522 1 2 335

2575441 1000309 611 8591361 15058633 192084 11528 120 79 2 295 2 5 244

2389414 902863 778 7337299 15006411 205645 9525 66 106 2 723 1 9 283

2837040 920695 663 7555503 15223313 179048 9792 36 48 1 580 0 4 361

3088316 888811 604 7518782 14703787 169472 11961 64 26 1 476 0 9 387

2787086 1050744 1705 9008215 16227225 387219 4835 233 210 2 295 2 84 300

2851190 935876 1335 7874772 15683981 291008 7107 142 160 4 1033 2 14 581

2512280 1040148 3092 8929096 15341954 245604 4549 152 147 3 295 4 6 420



# Reference # MLC #

40 05050402 0217

41 09082531 AHDB 277

42 05050404 0219

43 05050406 0221

44 05051902 0237

45 05051904 0239

46 05051907 0242

47 05051910 0245

48 05081501 0251

49 05081508 0258

50 05081509 0259

51 05081602 0262

52 05081603 0263

53 05081607 0268

54 05081807 028755 05081809 028956 05082508 0308

57 05090704 0318

58 05102401 0501

59 05102403 0503

60 05102405 0505

61 05102601 0522

62 05102602 0523

63 05102704 0534

64 05110816 0567

65 05110817 0568

66 05112903 0807

67 05112907 0812

68 05112910 0815

69 05112911 0816

70 06021501 0821

71 06021502 0822

72 06021509 0829

73 06021402 0832

74 06021404 0834

75 06021409 0839

76 06022801 0841

77 06022802 0842

78 06022807 0847



2276742 924914 1244 7980489 14557127 1081150 6281 435 691 9 3309 1 4 619

3829880 953106 1285 8184676 14405386 303756 2345 238 163 0 295 2 12 391

2606676 881530 1270 7146565 14187044 156870 5333 60 78 0 438 2 13 462

2369203 878938 1042 7157730 14349468 159996 6434 69 60 1 771 2 16 244

2850269 814007 853 6928471 14002174 215663 14528 87 79 2 567 1 4 303

3177428 750601 1630 6385242 12717635 209889 14354 83 98 1 542 2 36 400

2124115 846824 617 6895717 13400417 137321 12785 36 41 4 556 2 12 465

2388978 860308 772 7176842 14300245 166507 9756 67 36 2 493 2 37 359

2446600 930688 1443 7833448 14968841 196171 5763 89 52 1 588 1 9 466

2825961 826651 2514 6790646 12593145 259332 5659 141 168 8 1956 3 73 484

2386323 886918 449 7389303 14456752 181253 6870 108 47 0 482 1 4 278

2535762 850123 1645 7100873 13337907 303594 11678 84 276 3 842 2 14 513

2162941 924254 874 7302871 14232978 219091 11764 57 131 1 772 1 32 398

2769331 991340 1235 7973386 15346348 223491 22986 82 81 2 1375 1 9 346

1717295 994253 812 8277993 16606273 169498 8398 65 20 2 453 1 4 2701862951 974854 1593 8266195 15959105 175762 7223 71 34 2 551 2 11 3342592399 981217 1641 8275888 15399554 186101 14092 94 191 3 1419 2 14 488

2237368 971208 865 8045445 16353093 220853 6055 174 43 2 636 1 18 393

2845354 795360 448 6804237 13191640 258474 7831 123 45 0 718 1 6 482

3611388 769850 633 6701368 12499608 197219 7420 93 28 3 666 1 11 462

2096398 925476 666 7823855 15676509 178385 8673 72 23 1 518 0 5 273

2648028 921628 1661 7797385 15442473 159162 38266 75 15 0 393 2 73 253

1900450 913505 717 7553797 14790819 220826 8805 168 41 0 716 1 71 385

5683590 596860 29268 5099416 8735748 461531 9270 1343 33685 36 3593 22 143 1094

2582233 920197 854 7440549 15268886 202697 10020 79 54 1 597 1 5 369

1983101 879362 615 7447174 15034797 157294 11444 63 58 2 819 2 31 447

2421176 812164 1948 6916528 13091879 189588 18579 94 40 2 542 1 9 403

2385607 857041 2099 6988590 13606032 360128 10462 261 112 3 1141 2 11 644

2598595 857661 1877 7094637 14351057 249220 23158 153 63 0 855 2 9 522

3305902 909313 1799 7270939 14453415 600227 21979 298 193 2 1788 2 4 470

2000893 877256 946 8251168 14368414 139538 15477 79 157 2 899 1 41 434

2298654 953621 916 8874212 16285411 143405 9499 102 105 2 1105 1 16 428

2787560 829097 595 7822610 14226996 163045 9429 116 55 0 1032 1 25 433

2594890 891895 714 7408682 14204803 506578 16000 202 82 1 1627 1 117 222

2107057 816548 838 6685521 12325885 284162 6390 201 106 2 898 1 9 387

2556304 843884 1826 6925967 13124800 324524 13795 136 94 1 1148 2 4 419

2336360 810240 798 6593575 12157617 145119 6323 57 22 1 406 2 6 428

2123757 1008359 662 8209704 16136309 153228 8509 48 25 0 449 2 6 435

2124508 946203 1274 7739253 15182718 210183 8126 91 41 4 1083 4 22 374



# Reference # MLC #

79 06022810 0850

80 06012306 0896

81 06012310 0900

82 06050903 0918

83 06050904 0919

84 06060602 0942

85 06060605 0945

86 06060608 0948

87 06060610 0950

88 06080201 0991

89 06080202 0992

90 06080205 0995

91 06080206 0996

92 06080207 0997

93 06080210 1000

94 06081805 1015

95 06072706 1036

96 E09052801 BB911

97 E09052802 BB912

98 E09052803 BB913

99 E09052804 BB914

100 E09052805 BB915

101 E09052806 BB916

mean

SD

min

max

rangeN



2082723 887547 689 7300963 13646551 175905 8150 59 20 1 500 2 5 369

3428180 869728 1174 7106579 13263171 202522 4952 88 36 2 718 5 26 560

3337560 959806 803 8007896 16000139 266130 5946 105 51 0 732 3 5 353

2278341 936582 918 7720552 15633688 573710 5259 242 546 0 1839 1 7 314

1841068 950543 611 8177561 16333095 138402 5591 43 71 0 376 1 7 274

4114115 743185 8375 6939954 12669559 192766 8431 143 153 4 2543 2 26 419

2741851 875386 3130 7704378 14380940 161587 7399 108 712 5 1254 2 52 478

2334820 979849 4270 8401202 16968760 181625 8775 158 705 5 1461 3 13 381

3824459 875896 7416 7572285 14037664 234227 12336 243 1646 6 2064 4 25 504

2516030 883238 998 7674509 14907105 478714 5991 220 276 1 1896 2 24 331

2798268 998689 8330 8713191 16283313 319372 9596 304 2187 10 1608 4 23 428

3517879 882588 15237 7201581 13985015 819629 16903 425 3075 13 4229 7 33 418

3180188 986025 11168 7786316 15899889 303074 17321 314 5093 11 1325 7 29 400

5094560 864442 30501 6734846 14275559 564983 17155 954 23675 19 3177 15 69 635

3789382 1051862 19632 8110396 16353560 412276 9232 590 7529 14 2408 10 48 625

2405027 975898 807 8326994 15984121 180287 5109 67 97 2 756 1 35 389

3083032 869854 852 7541209 14219874 165153 35801 78 112 1 1076 1 9 340

2608500 954337 2480 8730283 16617915 169330 5484 108 491 0 1513 1 12 234

2846231 846591 3808 7733446 14710883 152277 5508 149 961 4 968 3 12 307

3266031 903660 530 7827038 15469769 251678 6099 180 106 2 1560 1 9 338

2612443 1006428 367 8924873 16844224 161202 3677 88 42 2 767 1 6 209

2450788 1000409 627 8884683 16313709 167563 3310 100 68 0 1468 1 1 217

3005296 915546 1178 8341616 14908534 178404 3357 112 145 1 1505 1 10 313


2722437 900589 2423 7578796 14538216 250920 9832 151 897 3 942 2 24 384

621954 104523 4821 891287 1730111 144510 5902 171 4146 4 739 3 27 126

1717295 493197 367 4372547 7801089 137321 2345 36 15 0 23 0 1 166

5683590 1064904 30501 9008215 17239619 1081150 38266 1343 33685 36 4229 22 143 1094

3966295 571707 30134 4635669 9438531 943829 35922 1306 33670 36 4207 22 142 928101 101 101 101 101 101 101 101 101 101 101 101 101 101



# Reference # MLC #

1 05010501 0082

2 05010502 0083

3 05011001 0092

4 05011002 0093

5 05011009 0100

6 05011010 0101

7 05011201 0102

8 05011202 0103

9 05011204 0105

10 05011206 0109

11 05020101 0112

12 05020102 0113

13 05020801 0117

14 05020802 0118

15 05021501 0130

16 05021502 0131

17 05022201 0149

18 09082517 AHDB 263

19 05022202 0150

20 09082518 AHDB 264

21 05022205 0153

22 05022206 0154

23 09082520 AHDB 266

24 05022210 0158

25 09082521 AHDB 267

26 05042604 0176

27 05042605 0179

28 05042801 0183

29 09082524 AHDB 270

30 05042701 0187

31 09082525 AHDB 271

32 05042702 0188

33 09082526 AHDB 272

34 05042704 0190

35 05042705 0191

36 05050302 0207

37 09082529 AHDB 275

38 05050401 0216

39 09082530 AHDB 276

Fe 56 Co 59 Ni 60 Cu 63 Zn 66 Ga 69 Ge 74 As 75 Se 77 Li 7 Be 9 Y 89 Zr 90 Nb 93 Mo 98

µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg

109870 33 49 1959 168673 0 1 30 314 0.09 0.08 0.98 695.09 0.12 67.37

101445 54 295 1949 192580 0 2 91 350 0.03 0.08 0.82 2667.01 0.67 46.78

172899 12 62 3105 256805 0 3 36 432 0.00 0.00 0.84 1924.35 0.29 39.57

156186 10 26 3279 242486 1 2 35 340 0.07 0.04 0.64 691.28 0.56 48.24

158457 8 11 2782 278320 0 0 18 152 0.06 0.00 0.49 969.24 0.00 35.19

111366 3 21 2469 267959 0 1 14 103 0.03 0.03 0.48 945.03 0.25 38.65

120625 19 25 2392 260987 1 2 26 348 0.00 0.01 1.65 890.10 0.13 26.47

104964 25 65 2351 273299 1 2 52 373 0.02 0.03 0.73 1532.12 0.14 27.73

79083 18 8 2009 207874 0 1 27 273 0.06 0.12 0.51 657.10 0.63 21.18

116795 21 5 2942 169979 0 4 14 452 0.00 0.00 0.21 28.10 0.00 36.21

130418 8 38 2566 243288 0 2 10 313 0.01 0.03 0.42 656.97 0.00 36.87

87267 5 245 2451 204953 1 1 7 188 0.05 0.07 0.47 373.73 0.30 22.76

181878 10 24 1896 140624 1 2 83 240 0.03 0.08 0.50 2613.39 0.21 15.71

127570 16 36 2535 236738 1 2 8 421 0.09 0.03 3.32 1010.00 4.42 45.62

73854 4 120 1722 173240 0 1 11 256 0.04 0.01 0.27 441.92 0.15 33.95

95874 4 52 2028 207552 1 2 12 268 0.00 0.04 0.69 662.66 0.03 37.66

131676 10 84 2879 252048 0 2 38 460 0.03 0.14 0.33 782.11 0.00 54.99

36816 17 6 2792 186048 1 2 122 360 17.7 0.24 0.79 33.09 1.38 32.36

83462 8 36 2231 179812 0 3 76 450 0.03 0.11 0.59 567.64 0.23 33.83

43328 5 33 3416 199532 1 1 241 204 46.8 0.50 1.23 179.66 0.84 46.76

111873 9 2 2954 233130 0 2 154 434 7.4 0.05 0.24 4.81 0.20 56.60

92228 7 6 2310 226589 1 2 148 367 13.8 0.06 0.35 17.28 1.31 45.95

44249 6 14 4409 210790 1 2 30 305 9.7 0.09 0.28 51.48 0.74 38.03

99230 6 4 2625 257903 0 3 133 567 0.00 0.02 0.30 478.60 0.02 21.67

38928 24 42 2770 232724 1 2 63 523 8.8 0.19 0.58 58.09 0.94 29.29

88919 4 7 2528 214871 0 2 22 217 0.00 0.02 1.70 1963.95 0.26 26.67

136058 6 9 3373 258228 0 1 7 134 0.09 0.04 0.32 466.41 0.00 32.52

112217 15 29 3463 138559 1 5 7 515 0.26 0.11 2.03 33.33 1.01 42.55

33500 12 18 2762 234744 0 2 10 370 8.3 0.06 0.15 350.22 0.81 25.85

81884 19 7 2496 267604 0 1 15 250 0.00 0.00 0.26 717.65 0.00 47.13

29744 14 22 1934 229762 1 1 18 267 7.2 0.06 0.23 0.11 1.64 30.27

103565 18 14 2914 253766 0 1 13 359 0.09 0.10 0.16 613.99 0.00 31.49

37723 2 4 2822 236955 1 1 24 105 19.9 0.15 0.22 0.11 0.48 25.21

78277 9 10 2151 198335 0 6 14 263 0.00 0.01 0.18 11.26 0.15 39.28

89580 10 5 2388 163506 0 2 17 241 0.03 0.08 0.16 62.78 0.13 23.79

127274 11 57 2903 250813 1 1 6 109 0.02 0.03 0.24 288.54 0.00 58.57

38634 20 176 3025 243684 1 3 15 443 7.7 0.13 0.38 6.19 1.61 45.63

154789 8 55 4255 264828 0 3 13 241 0.09 0.07 0.53 244.15 1.81 40.09

46578 19 5 3531 230259 1 2 14 392 5.8 0.14 0.73 0.11 1.12 34.10



# Reference # MLC #

40 05050402 0217

41 09082531 AHDB 277

42 05050404 0219

43 05050406 0221

44 05051902 0237

45 05051904 0239

46 05051907 0242

47 05051910 0245

48 05081501 0251

49 05081508 0258

50 05081509 0259

51 05081602 0262

52 05081603 0263

53 05081607 0268

54 05081807 028755 05081809 028956 05082508 0308

57 05090704 0318

58 05102401 0501

59 05102403 0503

60 05102405 0505

61 05102601 0522

62 05102602 0523

63 05102704 0534

64 05110816 0567

65 05110817 0568

66 05112903 0807

67 05112907 0812

68 05112910 0815

69 05112911 0816

70 06021501 0821

71 06021502 0822

72 06021509 0829

73 06021402 0832

74 06021404 0834

75 06021409 0839

76 06022801 0841

77 06022802 0842

78 06022807 0847



116996 6 8 3323 167823 0 9 9 384 0.20 0.20 1.34 17.06 0.15 46.33

49539 5 0 2887 234299 1 2 21 276 16.7 0.15 0.46 6.93 0.51 36.80

96163 6 10 3000 173926 1 5 13 326 0.87 0.79 0.34 21.94 0.15 56.89

62521 4 9 1448 165016 0 5 14 206 0.00 0.07 0.21 14.64 0.73 35.68

84381 8 8 2221 174263 0 2 34 124 0.01 0.05 0.20 31.07 0.00 41.72

115145 7 8 2742 209984 1 2 29 114 0.00 0.01 0.25 51.32 0.49 41.88

129860 11 9 3168 216180 1 5 42 251 0.06 0.00 0.18 10.28 0.02 28.14

97955 6 6 2813 136094 0 8 26 239 0.15 0.05 0.35 21.51 0.27 32.16

126639 13 6 3521 186601 0 3 13 343 0.04 0.03 0.17 26.87 0.00 47.42

175362 5 11 4197 197034 2 2 10 223 0.09 0.08 0.34 134.79 7.35 49.50

85156 5 6 2160 171804 0 3 11 364 0.00 0.00 0.39 17.86 0.00 34.89

127936 11 83 3232 265870 1 1 14 120 0.00 0.03 1.01 1652.54 0.31 27.23

111411 11 117 3343 196951 0 3 13 151 0.00 0.00 0.34 59.16 0.00 29.45

85765 26 12 2189 143706 0 8 31 137 0.00 0.00 0.57 30.59 1.67 37.52

64174 4 9 1921 173863 0 4 20 228 0.02 0.00 0.25 26.28 0.13 18.3886075 6 15 2948 163230 0 2 38 376 0.04 0.00 0.27 49.17 1.18 28.63

120520 5 15 4748 239210 1 1 148 176 5.7 0.12 0.83 95.20 1.36 49.48

94192 7 14 2793 139733 0 9 24 352 0.55 0.48 0.37 22.54 0.00 59.61

138987 11 37 2767 152662 0 10 14 582 0.79 0.73 0.23 16.50 0.00 45.74

187430 11 13 2792 190863 0 9 22 430 0.00 0.08 0.19 14.65 0.07 36.14

55361 4 27 1957 174846 0 6 41 332 0.00 0.00 0.40 18.72 0.38 25.96

76476 3 8 2420 199130 0 0 10 46 0.55 0.51 0.20 65.13 0.00 62.12

76443 8 11 3199 123341 0 5 13 461 0.45 0.38 0.30 16.52 0.17 53.14

66714 21 72 3384 203279 15 4 7518 385 1124.0 8.27 15.77 2969.05 8.20 43.68

68612 4 20 2310 166707 0 1 36 82 0.00 0.00 0.33 16.79 0.15 37.57

98226 17 30 3276 243085 0 2 40 71 0.01 0.00 0.25 17.27 0.34 36.43

91186 9 5 2303 151964 0 2 21 196 0.00 0.03 0.26 17.93 0.04 41.52

146197 5 20 3943 251023 1 3 15 126 0.09 0.08 0.24 108.24 0.00 40.87

138895 10 31 3049 143860 0 6 14 741 0.40 0.54 0.46 23.91 0.67 38.97

130173 7 10 2581 125176 0 4 13 499 0.22 0.20 0.96 13.62 0.16 47.73

51868 8 92 3395 275341 0 1 58 310 15.3 0.14 0.44 391.52 1.59 33.59

58739 4 23 3680 287499 0 2 38 319 7.1 0.10 0.29 75.81 0.94 38.76

64473 6 46 2949 326010 0 1 10 281 4.8 0.09 0.13 101.79 1.60 40.67

80990 3 12 1743 151868 0 3 13 67 0.08 0.06 0.18 11.08 0.15 75.18

112118 16 15 3104 229907 0 4 8 290 0.11 0.10 0.29 31.39 0.14 39.68

172198 5 4 3364 201557 1 1 7 75 0.01 0.08 0.27 50.00 2.93 149.02

104980 12 30 2766 133951 0 6 16 536 0.12 0.03 0.26 15.25 0.32 66.40

95847 17 23 2800 128638 0 9 23 568 0.66 0.71 0.31 14.47 0.06 39.19

76099 23 34 2350 246574 1 11 36 445 0.03 0.10 0.41 19.89 1.22 80.72



# Reference # MLC #

79 06022810 0850

80 06012306 0896

81 06012310 0900

82 06050903 0918

83 06050904 0919

84 06060602 0942

85 06060605 0945

86 06060608 0948

87 06060610 0950

88 06080201 0991

89 06080202 0992

90 06080205 0995

91 06080206 0996

92 06080207 0997

93 06080210 1000

94 06081805 1015

95 06072706 1036

96 E09052801 BB911

97 E09052802 BB912

98 E09052803 BB913

99 E09052804 BB914

100 E09052805 BB915

101 E09052806 BB916

mean

SD

min

max

rangeN



78874 14 6 2369 163477 0 5 28 377 0.05 0.05 0.29 17.24 0.27 34.99

192166 15 6 4068 230087 0 2 79 456 0.02 0.04 0.41 67.60 1.13 38.14

87953 14 9 3340 187576 0 4 87 464 0.06 0.00 0.23 26.63 0.01 45.53

91576 6 14 2956 129964 0 8 22 326 0.41 0.39 0.40 18.93 0.10 36.75

68502 3 22 2251 143007 0 4 17 55 0.00 0.05 0.28 15.19 0.27 36.06

105094 8 43 3371 259149 1 1 93 347 12.1 0.25 0.66 341.93 2.95 78.30

57995 43 107 3502 271329 1 2 269 426 72.3 0.45 7.99 260.80 2.36 38.46

67334 21 12 2332 257899 1 2 586 219 45.2 0.76 2.75 388.87 2.45 30.80

90680 14 18 3613 267635 2 3 523 496 129.4 1.30 3.57 471.15 3.44 42.02

79883 5 43 3215 218380 0 1 69 102 69.6 0.09 0.33 53.62 0.61 64.69

75961 6 5 3564 233514 2 2 881 149 103.3 1.02 5.23 1079.27 2.47 47.87

123027 9 19 2878 226464 4 2 1839 205 115.2 1.48 7.71 480.43 4.23 44.00

94721 9 26 2457 220596 3 1 1630 120 320.1 2.25 5.82 626.09 3.51 42.38

87643 14 25 2193 225710 8 2 3909 137 888.0 4.96 14.61 401.24 5.77 41.87

95853 40 9 2898 246022 5 4 2449 366 618.2 3.62 11.14 306.30 4.91 30.45

77270 25 42 4780 219928 0 1 52 153 9.0 0.10 0.45 53.85 0.62 54.99

70724 4 16 2727 242221 0 2 34 149 4.4 0.16 0.19 71.78 1.38 30.52

44003 3 30 2498 248814 1 1 222 157 56.4 0.35 1.64 172.97 2.11 52.00

46651 4 5 1798 296769 1 1 564 108 118.8 0.60 2.27 831.83 2.19 47.50

53515 5 29 2372 315935 0 2 24 144 11.9 0.07 0.41 0.11 1.49 43.84

45782 6 17 2238 258908 0 3 13 367 7.0 0.09 0.19 2.27 0.80 41.04

48620 5 0 2429 237893 0 3 28 503 7.6 0.11 0.24 3.32 1.29 44.59

61349 7 0 2575 259473 1 2 138 434 11.3 0.19 0.75 255.43 1.59 44.65


94416 11 31 2818 213005 1 3 235 296 38.95 0.35 1.21 355.80 1.01 41.87

37187 9 45 653 46790 2 2 897 145 156.79 1.04 2.63 592.26 1.51 16.28

29744 2 0 1448 123341 0 0 6 46 0.00 0.00 0.13 0.11 0.00 15.71

192166 54 295 4780 326010 15 11 7518 741 1124.04 8.27 15.77 2969.05 8.20 149.02

162422 53 295 3331 202669 15 10 7512 695 1124.03 8.27 15.63 2968.95 8.20 133.31101 101 101 101 101 101 101 101 101 101 101 101 101 101 101



# Reference # MLC #

1 05010501 0082

2 05010502 0083

3 05011001 0092

4 05011002 0093

5 05011009 0100

6 05011010 0101

7 05011201 0102

8 05011202 0103

9 05011204 0105

10 05011206 0109

11 05020101 0112

12 05020102 0113

13 05020801 0117

14 05020802 0118

15 05021501 0130

16 05021502 0131

17 05022201 0149

18 09082517 AHDB 263

19 05022202 0150

20 09082518 AHDB 264

21 05022205 0153

22 05022206 0154

23 09082520 AHDB 266

24 05022210 0158

25 09082521 AHDB 267

26 05042604 0176

27 05042605 0179

28 05042801 0183

29 09082524 AHDB 270

30 05042701 0187

31 09082525 AHDB 271

32 05042702 0188

33 09082526 AHDB 272

34 05042704 0190

35 05042705 0191

36 05050302 0207

37 09082529 AHDB 275

38 05050401 0216

39 09082530 AHDB 276

Ru 102 Pd 106 Cd 114 Sn 120 Sb 121 Te 130 La 139 Ce 140 Pr 141 Nd 142 Sm 152 Eu 153 Gd 158 Tb 159 Dy 164


0.02 1.98 4.49 1.77 4.81 22.52 0.85 1.55 0.19 0.73 0.12 0.08 0.24 0.03 0.04

0.00 3.70 3.78 0.66 9.76 0.01 1.25 3.94 0.20 1.52 0.10 0.01 0.32 0.04 0.11

0.47 4.33 10.65 17.59 3.28 0.01 1.36 2.99 0.36 1.75 0.28 0.02 0.63 0.06 0.10

0.03 3.73 4.69 8.32 3.76 0.01 0.39 0.93 0.12 0.36 0.10 0.06 0.15 0.00 0.04

0.01 4.63 4.28 0.72 1.80 1.73 0.13 0.23 0.08 0.01 0.06 0.03 0.04 0.01 0.01

0.00 4.45 7.35 1.48 3.99 0.01 0.92 1.30 0.15 0.52 0.04 0.00 0.12 0.00 0.02

0.00 4.37 3.96 1.19 2.58 0.01 0.31 0.65 0.13 0.27 0.09 0.03 0.22 0.06 0.18

0.00 4.38 4.89 2.35 5.14 0.04 0.71 1.74 0.17 0.71 0.07 0.00 0.12 0.01 0.05

0.02 3.68 1.45 2.16 1.70 0.01 0.13 0.67 0.07 0.06 0.10 0.08 0.05 0.02 0.01

0.00 4.03 1.73 3.79 2.77 1.20 0.31 0.67 0.18 0.36 0.17 0.17 0.16 0.07 0.02

0.00 3.52 2.64 0.52 2.97 2.34 0.67 1.47 0.22 0.62 0.12 0.02 0.09 0.02 0.04

0.04 3.01 2.68 1.40 1.80 0.01 0.36 0.69 0.11 0.36 0.24 0.14 0.14 0.03 0.04

0.33 3.75 36.46 0.22 4.80 0.48 1.20 3.87 0.19 1.66 0.10 0.00 0.44 0.04 0.05

0.00 3.60 1.86 0.84 2.10 0.01 1.07 1.68 0.24 0.96 0.16 0.03 0.31 0.08 0.45

0.03 2.45 3.31 0.95 1.31 0.01 4.08 8.32 0.14 2.33 0.11 0.06 0.30 0.03 0.01

0.02 3.04 2.44 0.34 2.05 0.01 1.00 1.21 0.20 0.58 0.17 0.05 0.11 0.07 0.07

0.00 3.68 2.48 0.43 3.73 1.84 0.31 0.77 0.15 0.20 0.07 0.04 0.02 0.00 0.00

0.64 3.55 1.18 26.55 13.89 5.09 3.89 8.83 0.65 2.81 1.86 1.13 2.13 0.09 0.19

0.55 2.34 3.40 1.99 2.31 18.23 0.20 0.52 0.07 0.35 0.06 0.05 0.19 0.06 0.01

0.59 11.41 1.78 16.73 36.68 9.85 7.55 15.61 1.12 4.96 4.18 2.46 4.03 0.26 0.42

0.00 2.02 1.37 4.82 2.62 1.46 0.74 2.83 0.25 1.19 0.63 0.36 0.50 0.11 0.02

0.00 3.00 0.97 3.60 8.52 1.61 1.03 4.30 0.29 1.57 0.93 0.55 0.88 0.14 0.07

0.27 3.56 1.20 16.29 4.46 3.69 1.17 3.72 0.52 1.43 0.90 0.56 0.84 0.13 0.06

0.04 3.61 0.98 0.63 5.39 0.55 0.17 0.36 0.11 0.00 0.06 0.05 0.02 0.00 0.00

0.29 4.29 1.41 11.96 27.81 5.76 1.90 5.18 0.63 1.93 2.38 1.37 1.29 0.16 0.14

0.00 3.62 1.09 0.59 2.76 1.83 0.28 0.93 0.12 0.22 0.07 0.02 0.09 0.01 0.04

0.00 3.81 2.02 0.82 2.22 0.53 0.23 0.47 0.10 0.18 0.06 0.02 0.14 0.01 0.01

0.21 4.70 5.02 38.88 3.90 1.63 10.37 23.30 2.00 9.18 1.13 0.23 5.30 0.44 0.75

0.15 15.54 0.46 9.85 16.35 3.29 0.40 1.64 0.29 0.68 1.23 0.76 0.42 0.04 0.01

0.00 4.14 1.80 0.85 1.57 0.90 0.29 0.48 0.11 0.00 0.07 0.06 0.02 0.00 0.01

0.26 1.24 0.82 10.32 13.03 4.82 0.89 2.07 0.27 0.75 0.85 0.54 0.42 0.05 0.04

0.01 3.98 0.96 0.12 0.95 0.01 0.13 0.35 0.05 0.06 0.02 0.00 0.05 0.03 0.01

0.39 0.51 0.95 14.75 3.08 2.46 1.02 3.34 0.46 1.50 0.81 0.49 0.76 0.08 0.06

0.08 2.81 1.21 0.88 2.71 0.24 0.25 0.40 0.06 0.19 0.26 0.15 0.04 0.04 0.01

0.05 2.70 1.22 2.88 1.18 28.77 0.17 0.35 0.06 0.18 0.15 0.08 0.08 0.05 0.02

0.05 4.24 1.07 0.12 12.79 0.01 0.16 0.34 0.11 0.10 0.07 0.05 0.05 0.01 0.02

0.58 1.51 0.74 12.44 2.05 4.52 0.61 2.24 0.41 0.91 1.38 0.85 0.53 0.06 0.08

0.63 6.75 2.90 2.87 7.44 1.31 0.80 1.91 0.12 0.80 0.03 0.01 0.49 0.03 0.10

0.51 1.06 1.04 16.66 3.89 4.16 2.12 5.36 0.66 2.24 1.35 0.77 1.46 0.19 0.25



# Reference # MLC #

40 05050402 0217

41 09082531 AHDB 277

42 05050404 0219

43 05050406 0221

44 05051902 0237

45 05051904 0239

46 05051907 0242

47 05051910 0245

48 05081501 0251

49 05081508 0258

50 05081509 0259

51 05081602 0262

52 05081603 0263

53 05081607 0268

54 05081807 028755 05081809 028956 05082508 0308

57 05090704 0318

58 05102401 0501

59 05102403 0503

60 05102405 0505

61 05102601 0522

62 05102602 0523

63 05102704 0534

64 05110816 0567

65 05110817 0568

66 05112903 0807

67 05112907 0812

68 05112910 0815

69 05112911 0816

70 06021501 0821

71 06021502 0822

72 06021509 0829

73 06021402 0832

74 06021404 0834

75 06021409 0839

76 06022801 0841

77 06022802 0842

78 06022807 0847



0.12 2.92 1.14 0.12 3.38 5.20 1.40 1.44 0.32 0.88 1.44 0.85 0.50 0.07 0.06

0.57 1.56 0.98 8.74 2.25 3.37 1.10 3.33 0.40 1.41 1.13 0.62 0.92 0.07 0.07

0.04 3.26 1.32 6.65 4.29 1.43 0.53 0.96 0.39 0.63 0.47 0.34 0.30 0.20 0.02

0.05 3.19 0.98 2.70 3.51 0.34 0.26 0.34 0.08 0.26 0.00 0.01 0.16 0.03 0.02

0.13 4.63 0.90 0.73 3.11 0.87 0.25 0.66 0.12 0.40 0.09 0.04 0.28 0.02 0.01

0.00 3.90 0.91 1.29 2.95 0.83 0.34 0.52 0.08 0.23 0.09 0.05 0.26 0.00 0.02

0.00 3.06 0.66 0.43 1.92 1.93 0.18 0.41 0.08 0.17 0.19 0.12 0.03 0.05 0.01

0.57 3.79 0.59 0.12 3.68 0.01 0.32 0.58 0.14 0.64 0.10 0.05 0.47 0.15 0.04

0.00 3.87 0.99 0.87 2.30 0.38 0.20 0.39 0.12 0.24 0.09 0.10 0.17 0.03 0.02

0.39 4.98 1.93 11.02 10.48 0.27 0.51 0.73 0.04 0.40 0.04 0.03 0.31 0.00 0.04

0.06 2.92 0.39 4.80 2.06 1.50 0.21 0.39 0.12 0.20 0.21 0.24 0.07 0.13 0.00

0.02 4.44 2.15 2.46 3.35 0.06 0.63 1.07 0.12 0.57 0.16 0.04 0.17 0.05 0.05

0.00 4.00 1.34 0.12 1.94 1.96 0.27 0.66 0.16 0.32 0.24 0.21 0.21 0.05 0.02

0.04 3.70 0.92 0.90 4.18 0.55 0.38 0.66 0.12 0.49 0.10 0.05 0.24 0.08 0.09

0.07 3.29 0.40 0.12 3.60 0.01 0.10 0.16 0.11 0.16 0.07 0.07 0.09 0.03 0.000.00 3.46 0.41 0.60 2.55 0.29 0.25 0.62 0.10 0.32 0.06 0.05 0.24 0.02 0.020.11 7.37 1.31 12.22 15.97 0.01 3.18 12.93 0.85 3.83 1.39 0.82 2.53 0.30 0.19

0.16 3.49 1.27 3.54 2.82 0.77 0.31 1.07 0.35 0.81 0.37 0.20 0.25 0.19 0.03

0.08 3.20 0.69 3.24 2.83 1.29 0.12 1.17 0.27 0.54 0.36 0.23 0.25 0.20 0.01

0.00 2.96 0.94 0.64 2.20 1.50 0.11 0.27 0.11 0.24 0.21 0.13 0.09 0.04 0.01

0.00 2.56 0.69 0.76 2.94 1.23 0.16 0.29 0.12 0.20 0.13 0.07 0.09 0.08 0.03

0.00 4.48 0.43 0.30 1.24 0.16 0.62 1.31 0.17 0.79 0.06 0.04 0.35 0.02 0.03

0.11 3.35 1.17 3.06 3.30 0.89 0.20 0.94 0.35 0.71 0.39 0.20 0.26 0.20 0.04

1.28 145.61 49.38 33.86 895.45 355.28 81.37 211.08 8.27 51.62 142.28 88.01 39.53 1.73 4.88

0.14 2.71 1.11 5.93 2.62 1.50 0.33 0.73 0.24 0.37 0.35 0.18 0.23 0.15 0.05

0.00 3.04 0.78 0.75 1.97 2.32 0.20 0.46 0.05 0.15 0.20 0.13 0.09 0.06 0.04

0.00 4.24 0.78 0.97 3.22 0.12 0.26 0.41 0.09 0.35 0.18 0.12 0.16 0.05 0.02

0.98 5.93 2.58 11.28 5.80 1.33 0.30 0.34 0.04 0.25 0.00 0.00 0.42 0.00 0.01

0.26 4.37 0.95 7.26 4.29 1.10 0.43 1.17 0.22 0.74 0.09 0.00 0.41 0.10 0.02

0.08 3.23 1.06 0.12 3.66 1.57 1.67 2.68 0.52 1.58 0.81 0.45 0.90 0.20 0.21

0.21 13.74 1.64 13.44 6.49 3.39 1.83 12.34 0.67 3.50 1.10 0.63 1.74 0.25 0.08

0.30 5.47 2.12 0.12 4.47 0.47 1.12 8.84 0.78 3.03 1.17 0.69 1.08 0.33 0.08

0.48 6.93 0.97 9.00 1.59 0.50 0.30 5.59 0.88 1.90 0.47 0.27 0.74 0.39 0.04

0.00 3.56 2.21 0.99 2.28 0.62 0.40 0.76 0.13 0.39 0.13 0.09 0.16 0.05 0.01

0.00 3.55 3.14 1.10 1.71 1.71 0.24 0.46 0.09 0.09 0.15 0.11 0.09 0.04 0.02

0.09 5.03 1.19 1.09 3.06 0.26 0.23 0.41 0.04 0.27 0.00 0.00 0.24 0.00 0.07

0.05 2.82 3.61 0.12 2.60 0.01 0.23 0.87 0.39 0.73 0.26 0.09 0.21 0.24 0.02

0.08 3.64 5.40 5.25 8.48 0.34 0.26 1.09 0.21 0.49 0.31 0.21 0.22 0.20 0.00

0.00 3.02 2.27 2.49 2.80 1.99 0.28 0.64 0.12 0.32 0.14 0.15 0.14 0.06 0.02



# Reference # MLC #

79 06022810 0850

80 06012306 0896

81 06012310 0900

82 06050903 0918

83 06050904 0919

84 06060602 0942

85 06060605 0945

86 06060608 0948

87 06060610 0950

88 06080201 0991

89 06080202 0992

90 06080205 0995

91 06080206 0996

92 06080207 0997

93 06080210 1000

94 06081805 1015

95 06072706 1036

96 E09052801 BB911

97 E09052802 BB912

98 E09052803 BB913

99 E09052804 BB914

100 E09052805 BB915

101 E09052806 BB916

mean

SD

min

max

rangeN



0.60 3.56 2.33 14.52 2.40 0.01 0.17 0.22 0.05 0.43 0.04 0.00 0.41 0.02 0.02

0.17 4.83 2.52 1.19 4.13 1.29 0.31 0.51 0.05 0.40 0.06 0.03 0.30 0.00 0.07

0.00 3.39 1.72 1.03 4.43 1.41 0.25 0.58 0.21 0.27 0.25 0.16 0.18 0.12 0.02

0.18 3.60 3.50 7.23 4.13 6.84 0.50 0.96 0.34 0.71 1.25 0.77 0.28 0.19 0.04

0.00 3.56 2.04 1.55 5.37 1.38 0.15 0.28 0.06 0.12 0.20 0.10 0.10 0.01 0.01

0.34 14.30 2.37 3.89 9.87 1.28 2.60 16.10 1.39 3.76 1.81 0.99 1.94 0.39 0.20

0.22 11.59 3.07 6.25 34.06 8.99 7.95 21.75 1.44 8.29 2.14 1.12 3.30 0.35 0.40

0.13 20.69 3.24 11.54 37.30 5.42 14.62 38.26 2.10 10.50 4.04 2.21 7.47 0.56 0.74

0.22 23.34 4.17 18.59 46.86 16.62 13.10 81.52 2.15 16.24 8.13 4.60 14.53 0.53 0.91

0.05 3.97 2.13 6.54 16.32 3.14 1.40 8.09 0.57 2.38 1.65 0.99 1.12 0.21 0.11

0.04 39.58 4.71 14.70 108.84 27.71 26.81 76.22 2.86 18.49 9.37 5.50 13.03 0.66 1.25

0.14 30.30 9.05 8.82 208.54 41.58 27.70 82.35 4.18 23.01 14.25 8.18 18.49 0.80 1.76

0.08 39.20 8.76 13.95 318.67 73.14 24.26 75.60 3.55 20.41 21.93 13.30 16.60 0.76 1.47

0.58 26.90 33.54 18.36 1031.63 317.76 53.20 172.61 7.48 43.47 94.64 61.45 37.04 1.53 3.63

0.42 21.17 12.48 23.22 333.26 108.15 41.56 142.93 6.20 36.39 34.31 21.29 30.35 1.19 2.49

0.00 4.78 16.46 21.24 4.91 2.49 1.11 7.11 0.35 1.98 0.93 0.57 0.95 0.16 0.06

0.63 4.89 1.51 2.75 7.29 1.29 0.59 5.58 0.79 1.86 0.70 0.41 0.60 0.32 0.05

0.00 7.68 2.70 15.65 18.81 7.42 5.15 29.07 0.93 6.16 3.01 1.71 3.76 0.33 0.29

0.00 26.32 3.26 12.37 39.15 12.46 10.68 37.89 1.47 9.31 4.50 2.68 5.40 0.37 0.55

0.02 2.21 9.42 673.89 6.24 3.36 0.56 5.40 0.28 1.62 0.72 0.39 0.41 0.13 0.03

0.00 2.37 1.64 29.70 2.04 2.78 0.24 9.29 0.45 2.52 1.20 0.72 0.52 0.23 0.05

0.00 2.11 1.69 16.18 8.82 4.05 0.54 10.08 0.40 2.53 1.13 0.66 0.57 0.21 0.04

0.00 10.14 2.06 13.93 9.02 4.20 3.65 16.84 0.61 4.24 1.47 0.68 1.96 0.22 0.17


0.16 7.57 3.65 13.22 34.98 11.69 3.84 12.23 0.66 3.36 3.80 2.33 2.35 0.18 0.24

0.24 15.67 6.97 66.88 142.20 48.55 11.24 33.37 1.37 8.28 17.28 10.84 6.70 0.28 0.69

0.00 0.51 0.39 0.12 0.95 0.01 0.10 0.16 0.04 0.00 0.00 0.00 0.02 0.00 0.00

1.28 145.61 49.38 673.89 1031.63 355.28 81.37 211.08 8.27 51.62 142.28 88.01 39.53 1.73 4.88

1.28 145.10 48.99 673.77 1030.68 355.27 81.26 210.92 8.23 51.62 142.28 88.01 39.51 1.72 4.88101 101 101 101 101 101 101 101 101 101 101 101 101 101 101



# Reference # MLC #

1 05010501 0082

2 05010502 0083

3 05011001 0092

4 05011002 0093

5 05011009 0100

6 05011010 0101

7 05011201 0102

8 05011202 0103

9 05011204 0105

10 05011206 0109

11 05020101 0112

12 05020102 0113

13 05020801 0117

14 05020802 0118

15 05021501 0130

16 05021502 0131

17 05022201 0149

18 09082517 AHDB 263

19 05022202 0150

20 09082518 AHDB 264

21 05022205 0153

22 05022206 0154

23 09082520 AHDB 266

24 05022210 0158

25 09082521 AHDB 267

26 05042604 0176

27 05042605 0179

28 05042801 0183

29 09082524 AHDB 270

30 05042701 0187

31 09082525 AHDB 271

32 05042702 0188

33 09082526 AHDB 272

34 05042704 0190

35 05042705 0191

36 05050302 0207

37 09082529 AHDB 275

38 05050401 0216

39 09082530 AHDB 276

Ho 165 Er 166 Tm 169 Yb 174 Lu 175 Hf 180 Ta 181 W 184 Re 1 87 Ir 193 Pt 195 Hg 202

µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg µg/Kg

0.02 0.03 0.02 0.03 0.00 1.22 2.46 96.77 0.10 0.01 2.43 1.99

0.02 0.27 0.01 0.08 0.02 3.58 1.44 229.19 0.00 0.02 2.58 3.27

0.03 0.03 0.00 0.02 0.01 2.58 0.99 131.18 0.04 0.03 4.31 1.60

0.01 0.07 0.02 0.07 0.01 1.67 1.13 177.34 0.16 0.02 2.17 2.60

0.00 0.05 0.02 0.02 0.02 1.12 0.83 73.66 0.00 0.00 2.66 0.51

0.01 0.03 0.01 0.02 0.00 1.00 0.51 38.34 0.00 0.02 4.31 0.48

0.05 0.14 0.02 0.09 0.00 0.89 0.41 50.28 0.00 0.02 4.58 1.58

0.01 0.08 0.02 0.03 0.00 2.17 0.68 149.16 0.00 0.02 5.16 2.04

0.01 0.05 0.01 0.04 0.01 1.59 1.46 44.98 0.00 0.00 2.51 0.34

0.01 0.08 0.19 0.05 0.01 0.21 0.25 1.41 0.53 0.06 1.92 1.75

0.01 0.04 0.01 0.03 0.00 1.77 0.39 224.90 0.00 0.00 3.58 2.60

0.01 0.04 0.03 0.05 0.00 0.71 0.45 77.06 0.11 0.01 2.53 2.57

0.02 0.08 0.00 0.05 0.00 3.06 1.24 82.32 0.06 0.01 3.47 1.21

0.11 0.35 0.04 0.32 0.04 2.05 2.21 172.83 0.00 0.01 4.89 2.48

0.01 0.01 0.01 0.03 0.01 1.54 0.51 174.99 0.00 0.01 2.48 3.40

0.01 0.06 0.03 0.04 0.04 0.82 0.34 38.36 0.00 0.02 1.94 0.64

0.00 0.05 0.03 0.03 0.01 0.94 0.60 79.66 0.00 0.00 1.83 1.31

0.05 0.64 0.25 0.26 0.01 1.89 0.27 1.94 0.79 0.06 5.48 0.38

0.03 0.02 0.02 0.04 0.00 1.15 0.49 62.19 0.11 0.03 2.08 1.70

0.05 1.03 0.19 0.25 0.02 3.40 0.23 0.53 0.25 0.07 7.17 0.14

0.02 0.24 0.41 0.06 0.01 0.10 0.17 0.50 1.14 0.04 1.67 0.00

0.04 0.32 0.39 0.09 0.01 0.36 0.36 0.70 1.14 0.18 1.69 0.00

0.04 0.35 0.32 0.14 0.00 0.59 0.22 1.04 0.76 0.12 6.07 0.02

0.01 0.05 0.03 0.04 0.00 1.00 0.05 28.75 0.00 0.00 1.45 0.71

0.04 0.87 0.30 0.16 0.00 1.11 0.21 1.08 0.27 0.07 5.20 0.23

0.02 0.09 0.03 0.07 0.02 2.24 0.58 82.22 0.00 0.02 1.93 0.99

0.00 0.03 0.01 0.03 0.00 0.96 0.42 124.71 0.00 0.02 3.08 1.43

0.08 0.49 0.14 0.20 0.02 0.41 0.30 9.72 0.00 0.17 2.58 1.94

0.02 0.57 0.19 0.13 0.00 1.45 0.18 2.53 0.21 0.25 6.48 0.00

0.00 0.04 0.02 0.00 0.00 0.80 0.21 1.43 0.00 0.03 2.51 0.55

0.02 0.33 0.20 0.08 0.00 0.34 0.40 2.80 0.55 0.08 3.94 0.74

0.01 0.01 0.01 0.00 0.00 1.14 0.46 112.32 0.00 0.00 3.32 1.39

0.03 0.33 0.30 0.13 0.00 0.05 0.17 2.02 0.92 0.02 5.16 0.32

0.01 0.04 0.12 0.01 0.01 0.11 1.94 1.58 0.55 0.03 1.13 0.00

0.01 0.03 0.09 0.03 0.00 0.25 0.13 0.46 0.34 0.03 0.96 0.00

0.01 0.01 0.03 0.03 0.00 0.42 0.32 27.61 0.07 0.00 2.21 1.66

0.04 0.29 0.31 0.16 0.00 0.13 13.54 3.94 1.09 0.05 5.60 0.00

0.03 0.00 0.00 0.09 0.01 1.33 0.11 2.22 0.02 0.03 1.25 1.40

0.05 0.54 0.37 0.20 0.00 0.16 0.20 3.85 1.20 0.06 3.66 0.04



# Reference # MLC #

40 05050402 0217

41 09082531 AHDB 277

42 05050404 0219

43 05050406 0221

44 05051902 0237

45 05051904 0239

46 05051907 0242

47 05051910 0245

48 05081501 0251

49 05081508 0258

50 05081509 0259

51 05081602 0262

52 05081603 0263

53 05081607 0268

54 05081807 028755 05081809 028956 05082508 0308

57 05090704 0318

58 05102401 0501

59 05102403 0503

60 05102405 0505

61 05102601 0522

62 05102602 0523

63 05102704 0534

64 05110816 0567

65 05110817 0568

66 05112903 0807

67 05112907 0812

68 05112910 0815

69 05112911 0816

70 06021501 0821

71 06021502 0822

72 06021509 0829

73 06021402 0832

74 06021404 0834

75 06021409 0839

76 06022801 0841

77 06022802 0842

78 06022807 0847



0.00 0.24 0.43 0.08 0.06 0.21 0.13 0.78 1.35 0.06 0.34 1.91

0.05 0.32 0.24 0.12 0.00 0.41 0.21 1.28 0.46 0.05 7.16 0.00

0.05 0.12 0.43 0.06 0.01 0.22 0.18 1.26 1.14 0.17 3.07 2.56

0.03 0.04 0.06 0.06 0.00 0.14 0.24 0.73 0.00 0.00 1.14 0.42

0.01 0.07 0.03 0.03 0.01 0.21 0.19 1.41 0.00 0.01 1.12 0.51

0.01 0.02 0.01 0.06 0.01 0.28 0.14 1.47 0.00 0.07 0.66 0.30

0.01 0.03 0.17 0.03 0.01 0.06 0.05 0.81 0.78 0.04 1.08 0.31

0.02 0.13 0.00 0.05 0.04 0.23 0.11 0.87 0.00 0.08 2.27 0.09

0.01 0.03 0.08 0.03 0.01 0.19 0.51 1.13 0.27 0.06 1.21 0.42

0.02 0.06 0.00 0.04 0.01 0.99 0.21 9.15 0.00 0.02 1.15 0.44

0.01 0.11 0.27 0.08 0.01 0.29 0.12 0.27 1.12 0.00 2.37 2.76

0.01 0.02 0.02 0.03 0.03 1.99 18.40 98.57 0.01 0.02 1.57 1.39

0.00 0.11 0.21 0.04 0.02 0.42 1.56 1.95 0.56 0.03 1.58 1.13

0.03 0.08 0.09 0.05 0.00 0.32 0.33 0.71 0.00 0.05 1.32 0.00

0.02 0.01 0.08 0.03 0.00 0.30 0.10 0.39 0.00 0.05 1.03 0.150.01 0.04 0.03 0.04 0.02 0.26 0.18 1.17 0.00 0.02 0.87 1.220.07 0.84 0.12 0.21 0.06 2.00 0.50 0.69 0.43 0.18 0.53 0.00

0.02 0.18 0.38 0.11 0.01 0.21 0.16 0.76 0.81 0.23 2.50 0.72

0.03 0.14 0.39 0.09 0.00 0.25 0.25 0.42 0.99 0.09 3.41 1.36

0.01 0.04 0.18 0.03 0.00 0.14 0.19 1.08 0.71 0.05 0.98 0.33

0.02 0.01 0.14 0.03 0.00 0.15 0.13 0.50 0.52 0.07 1.35 0.00

0.02 0.01 0.00 0.03 0.01 0.34 0.23 0.72 0.00 0.02 1.06 1.51

0.04 0.16 0.29 0.06 0.01 0.29 0.19 0.82 0.63 0.16 2.76 0.98

0.54 24.79 0.21 1.82 0.43 47.51 1.12 6.38 0.12 0.86 0.34 0.00

0.02 0.17 0.30 0.06 0.01 0.19 0.30 2.02 1.37 0.00 2.17 2.37

0.01 0.05 0.15 0.01 0.01 0.13 0.28 2.02 0.88 0.05 0.81 1.15

0.01 0.06 0.11 0.06 0.00 0.25 0.17 1.87 0.35 0.00 0.58 0.66

0.03 0.00 0.00 0.03 0.01 0.65 0.32 1.34 0.03 0.00 0.91 1.73

0.01 0.04 0.00 0.10 0.01 0.29 0.07 1.09 0.00 0.09 2.07 2.24

0.05 0.38 0.38 0.11 0.04 0.17 0.28 2.16 1.19 0.07 0.34 2.54

0.05 0.55 0.04 0.13 0.07 1.85 0.66 2.35 0.00 0.06 0.34 1.49

0.08 0.73 0.10 0.20 0.07 0.46 0.64 0.31 0.00 0.06 0.34 0.00

0.07 0.44 0.01 0.14 0.04 0.81 0.77 1.42 0.00 0.00 1.60 0.00

0.01 0.05 0.11 0.03 0.01 0.13 2.79 0.58 0.27 0.01 1.05 0.59

0.00 0.03 0.12 0.03 0.01 0.16 6.26 3.12 0.43 0.02 0.59 0.75

0.01 0.00 0.00 0.04 0.00 0.38 0.15 6.63 0.00 0.06 1.19 1.19

0.02 0.08 0.18 0.04 0.01 0.08 0.14 1.31 0.00 0.18 2.17 0.47

0.02 0.17 0.35 0.10 0.02 0.19 0.10 0.49 0.98 0.21 2.82 1.69

0.02 0.01 0.16 0.04 0.00 0.24 6.77 3.10 0.61 0.04 1.55 0.44



# Reference # MLC #

79 06022810 0850

80 06012306 0896

81 06012310 0900

82 06050903 0918

83 06050904 0919

84 06060602 0942

85 06060605 0945

86 06060608 0948

87 06060610 0950

88 06080201 0991

89 06080202 0992

90 06080205 0995

91 06080206 0996

92 06080207 0997

93 06080210 1000

94 06081805 1015

95 06072706 1036

96 E09052801 BB911

97 E09052802 BB912

98 E09052803 BB913

99 E09052804 BB914

100 E09052805 BB915

101 E09052806 BB916

mean

SD

min

max

rangeN



0.02 0.11 0.00 0.03 0.04 0.20 0.20 2.41 0.00 0.03 1.61 0.00

0.01 0.03 0.03 0.05 0.02 0.41 0.20 1.92 0.00 0.03 0.99 1.28

0.01 0.10 0.17 0.05 0.02 0.14 2.20 1.49 0.56 0.05 0.93 1.14

0.02 0.26 0.38 0.10 0.02 0.15 0.21 4.74 0.74 0.23 2.81 1.76

0.01 0.02 0.08 0.03 0.01 0.14 1.37 1.18 0.33 0.03 1.16 0.15

0.12 1.10 0.05 0.17 0.11 3.57 0.86 0.71 0.01 0.16 0.01 0.00

0.09 1.15 0.09 0.26 0.10 4.39 1.82 1.07 0.07 0.00 0.04 0.52

0.11 1.58 0.23 0.43 0.11 7.77 0.40 0.67 0.54 0.32 0.98 0.00

0.14 2.36 0.21 0.49 0.11 8.17 0.49 1.01 0.49 0.41 1.29 0.00

0.03 0.66 0.28 0.10 0.04 0.69 0.32 2.16 0.49 0.08 0.47 0.00

0.19 2.88 0.32 0.72 0.17 19.51 0.33 2.76 0.44 0.44 0.09 0.00

0.26 4.95 0.40 0.91 0.17 10.91 0.23 2.70 0.95 0.40 1.82 0.00

0.18 6.31 0.49 0.63 0.11 11.22 0.22 3.10 1.09 0.25 1.92 0.00

0.38 22.57 0.56 1.61 0.35 8.52 0.24 4.02 1.03 0.47 0.98 0.00

0.34 8.23 0.52 1.36 0.26 6.29 0.23 4.12 0.95 0.46 2.61 0.00

0.04 0.46 0.25 0.11 0.04 0.52 0.32 4.28 0.48 0.02 0.21 0.21

0.06 0.62 0.05 0.09 0.06 0.60 1.31 0.08 0.00 0.00 1.04 0.00

0.09 1.15 0.18 0.21 0.12 2.59 0.61 1.54 0.00 0.32 0.34 0.00

0.13 1.82 0.28 0.39 0.10 9.32 0.43 1.34 0.03 0.24 0.34 0.39

0.05 0.41 0.12 0.09 0.04 0.06 0.81 1.09 0.09 0.08 0.40 0.06

0.05 0.71 0.41 0.10 0.06 0.01 0.50 2.33 0.14 0.00 0.34 1.47

0.06 0.84 0.13 0.15 0.10 0.25 0.50 1.42 0.00 0.17 0.34 1.13

0.08 0.91 0.18 0.20 0.06 3.09 0.69 0.99 0.00 0.22 0.34 0.00


0.05 0.96 0.15 0.16 0.03 2.06 0.96 25.02 0.35 0.09 2.06 0.87

0.08 3.46 0.15 0.29 0.07 5.41 2.39 51.31 0.41 0.13 1.65 0.89

0.00 0.00 0.00 0.00 0.00 0.01 0.05 0.08 0.00 0.00 0.01 0.00

0.54 24.79 0.56 1.82 0.43 47.51 18.40 229.19 1.37 0.86 7.17 3.40

0.54 24.79 0.56 1.82 0.43 47.49 18.35 229.10 1.37 0.86 7.16 3.40101 101 101 101 101 101 101 101 101 101 101 101


The British Beef Origin Project (BBOP - Q01123) - Final ReportSection 11: Appendix I - Complete list of authentic beef samples and data

Passport Number Protein

# Reference # MLC # Form Abattoir origin LAT LONG Date sam pled Ear Tag Number Breed Gender Born d2H [‰]

1 S08030401 S0001 whole meat Orkney, Scotland 58°54'3.83 "N 2°52'18.64"W 04/03/2008 UK523675702032 Limousin ? 25/0 4/2006 -96.3

2 S08030402 S0002 whole meat Orkney, Scotland 59° 1'56.4 9"N 3°10'37.89"W 04/03/2008 UK523593500648 Limosin X ? 08 /11/2005 -100.4

3 S08030403 S0003 whole meat Orkney, Scotland 59° 0'2.74 "N 3°17'12.20"W 04/03/2008 UK523924500743 Limousin ? 12/0 1/2006 -100.1

4 S08030404 S0004 whole meat Orkney, Scotland 58°54'43.9 3"N 2°54'10.16"W 04/03/2008 UK523677200841 Simmental ? 06 /06/2006 -96.4

5 S08030405 S0005 whole meat Orkney, Scotland 59° 0'2.74 "N 3°17'12.20"W 04/03/2008 UK523924100809 Charolais ? 08/ 04/2006 -97.8

6 S08030406 S0006 whole meat Orkney, Scotland 58°58'16.4 6"N 3°13'12.05" 04/03/2008 UK523879100369 Simmental ? 14/ 01/2006 -96.0

7 S08030407 S0007 whole meat Orkney, Scotland 58°58'16.4 6"N 3°13'12.05" 04/03/2008 UK523879600416 Aberdeen Angu s ? 04/05/2006 -97.4

8 S08030408 S0008 whole meat Orkney, Scotland 58°55'7.4 8"N 2°48'52.26"W 04/03/2008 UK52377440414 Limousin ? 14/0 3/2006 -99.8

9 S08030409 S0009 whole meat Orkney, Scotland 59° 0'2.74 "N 3°17'12.20"W 04/03/2008 UK523924400756 Limousin ? 28/0 1/2006 -100.3

10 S08030410 S0010 whole meat Orkney, Scotland 59° 6'36. 82"N 3° 5'59.70"W 04/03/2008 UK523615200577 Salers ? 28/0 2/2006 -101.1

11 S08030411 S0011 whole meat Orkney, Scotland 59° 3'52 .27"N 2°49'33.87"W 04/03/2008 UK524017500418 Limousin ? 0 1/05/2006 -95.1

12 S08030412 S0012 whole meat Orkney, Scotland 58°54'3.8 3"N 2°52'18.64"W 04/03/2008 UK523675402071 Limousin ? 06/ 06/2006 -97.6

13 S08030413 S0013 whole meat Orkney, Scotland 59° 0'2.7 4"N 3°17'12.20"W 04/03/2008 UK523924200796 Charolais ? 30 /03/2006 -96.3

14 S08030414 S0014 whole meat Orkney, Scotland 59° 2'17 .20"N 3°12'54.83"W 04/03/2008 UK523576101149 Simmental ? 20/07/2006 -92.6

15 S08030415 S0015 whole meat Orkney, Scotland 59° 2'17 .20"N 3°12'54.83"W 04/03/2008 UK523576501123 Charolais ? 09/06/2006 -96.2



18 S08030418 S0018 whole meat Orkney, Scotland 59° 6'4. 77"N 3° 4'20.95"W 04/03/2008 UK523606300532 Limousin ? 1 8/01/2006 -96.3



21 S08090801 S0021 whole meat Moray, Scotland 57°34'9.27 "N 3°29'51.20"W 18/09/2008 UK523460400612 ? ? ? -105.2




25 S08101401 S0025 whole meat Orkney, Scotland 58°56'38. 52"N 2°46'8.81"W 14/10/2008 UK523927500042 Charolais X F 06/06/2007 -92.7


27 S08101403 S0027 whole meat Orkney, Scotland 58°56'38. 52"N 2°46'8.81"W 14/10/2008 UKO021700322 Charolais X M 06 /06/2007 -95.0

28 S08092502 S0028 whole meat Lanarkshire, Scotland 55°37'22.58"N 3°31'42.10"W 25/09/2008 UK560899300701 ? ? ? -104.3



31 S08031101 S0031 whole meat Scottish Borders 55°51'37.04"N 3°12'28.30"W 11/03/2008 UK561500101243 Ab erdeen Angus X F 31/03/2007 -105.3

32 S09041401 S0032 whole meat Scottish Borders 55°51'37.04"N 3°12'28.30"W 14/04/2009 UK561500701305 Ab erdeen Angus X F 12/04/2007 -102.0

33 S09051201 S0033 whole meat Scottish Borders 55°51'37.04"N 3°12'28.30"W 12/05/2009 UK561500601367 Ab erdeen Angus X M 13/05/2007 -101.9


35 S09072702 S0035 whole meat Orkney, Scotland 58°59'31. 00"N 2°58'33.90"W 27/07/2009 UK523589301241 Charolais X M 11/03/2008 -94.8



BBOP Scotland 58




38 S09072705 S0038 whole meat Orkney, Scotland 58°59'31. 00"N 2°58'33.90"W 27/07/2009 UK523859501236 Limousin X M 09/03/2008 -97.4



41 S09072708 S0041 whole meat Orkney, Scotland 58°59'31. 00"N 2°58'33.90"W 27/07/2009 UK523612401203 Simmental X M 26/04/2007 -95.7

42 S09072709 S0042 whole meat Orkney, Scotland 58°59'31. 00"N 2°58'33.90"W 27/07/2009 UK523612401210 Simmental X M 28/04/2007 -96.1








50 S09072717 S0050 whole meat Orkney, Scotland 58°59'31. 00"N 2°58'33.90"W 27/07/2009 UK523539600359 Aberdeen An gus X F 19/04/2007 -97.2

51 S09072718 S0051 whole meat Orkney, Scotland 58°59'31. 00"N 2°58'33.90"W 27/07/2009 UK523539600345 Aberdeen An gus X F 17/03/2007 -97.3

52 none S0052 whole meat Scottish Borders 55°51'37.04"N 3°12'28.30"W 17/08/2009 UK561500701480 Ab erdeen Angus X F 02/04/2008 -100.5

53 none S0053 whole meat PE Anglo Beef, Perth 56° 6'30.7 0"N 3°25'57.96"W 30/09/2009 UK542763200737 LimousinX F 24 (9) -92.4



56 none S0056 whole meat Scottish Borders 55°51'37.04"N 3°12'28.30"W 17/08/2009 UK561500401407 Ab erdeen Angus X F 28/03/2008 -102.4

57 none S0057 whole meat PE Anglo Beef, Perth 55°51'9.59 "N 2°23'20.14"W 03/09/2009 UK560001500370 WB F 28 (0) -105 .8

58 none S0058 whole meat PE Anglo Beef, Perth 56°19'31.0 7"N 4°21'59.86"W 13/04/2009 UK582391300376 LimousinX S 29 (18) -95.6

59 none S0059 whole meat PE Anglo Beef, Perth 56°19'31.0 7"N 4°21'59.86"W 13/04/2009 UK542717301752 Charolais X S 23 (2) -99.1




63 none S0063 whole meat PE Anglo Beef, Perth 56°18'49.0 1"N 3° 8'58.15"W 02/09/2009 UK561455500723 Charolais S 24 (6) -100.2

64 none S0064 whole meat PE Anglo Beef, Perth 56°18'49.0 1"N 3° 8'58.15"W 02/09/2009 UK561843500771 Charolais X S 23 (18) -100.4







71 none S0071 whole meat -104.7

72 none S0072 whole meat PE Anglo Beef, Perth 56°14'3.11 "N 3°13'0.30"W 13/04/2009 UK583177100504 Charolais X F 29 (0) -105.0

73 none S0073 whole meat PE Anglo Beef, Perth 56°22'3.60 "N 3°50'57.43"W 13/04/2009 UK542071200571 Charolais X F 2 4 (23) -96.8

74 none S0074 whole meat PE Anglo Beef, Perth 56°22'3.60 "N 3°50'57.43"W 13/04/2009 UK542071600589 Charolais X S 2 4 (3) -94.9

BBOP Scotland 59




75 none S0075 whole meat PE Anglo Beef, Perth 56°22'3.60 "N 3°50'57.43"W 13/04/2009 UK542164500361 LimousinX S 24 (18) -97.1

76 00000001 S0076 whole meat Lockerbie 54°50'43.92"N 4° 5 '30.88"W 04/11/2009 UK582996100989 Charolais X ? ?? -91.6

77 00000002 S0077 whole meat Lockerbie 54°50'43.92"N 4° 5 '30.88"W 04/11/2009 UK582996400943 Charolais X F 05/09/2007 -95.7

78 00000003 S0078 whole meat Lockerbie 55° 5'36.12"N 3°3 1'2.71"W 04/11/2009 UK561761700336 LimousinX F 26/03/2008 -98.9

79 00000004 S0079 whole meat Lockerbie 54°59'17.35"N 3° 4 '34.16"W 04/11/2009 UK581743100268 LimousinX F 15/06/2007 -95.5

80 00000005 S0080 whole meat Lockerbie 55°20'48.04"N 3° 26'6.40"W 04/11/2009 UK582149700323 Limousin F 21/05/2007 -94.9

81 00000006 S0081 whole meat Lockerbie 55° 9'20.22"N 3°4 7'58.57"W 04/11/2009 UK582301700403 LimousinX F 07/05/2007 -98.9

82 00000007 S0082 whole meat Lockerbie 55° 3'7.52"N 3°44' 32.28"W 04/11/2009 UK582595200965 LimousinX F 11/09/2007 -96.8

83 00000008 S0083 whole meat Lockerbie 54°57'41.11"N 5° 9 '48.91"W 02/11/2009 UK583609300950 Hereford M 16/10/2007 -90.7

84 00000009 S0084 whole meat Lockerbie 55° 9'35.38"N 3°33 '20.78"W 02/11/2009 UK560448301220 Charolais X M 10/09/2007 -99.6

85 00000010 S0085 whole meat Lockerbie 55° 0'58.36"N 2°42 '12.51"W 02/11/2009 UK110767300182 Belted Galloway M 15/05/2007 -96.6

86 00000011 S0086 whole meat Lockerbie 55° 9'20.22"N 3°4 7'58.57"W 04/11/2009 UK582301400407 Limousin X F 10/05/2007 -97.8

87 00000012 S0087 whole meat Lockerbie 55°12'47.74"N 3°58 '26.90"W 04/11/2009 UK582306401642 Charolais X F 28/06/2007 -95.0

88 00000013 S0088 whole meat Lockerbie 55° 5'28.59"N 3°41 '54.24"W 04/11/2009 UK582283301518 Charolais X F 22/10/2007 -100.5

89 00000014 S0089 whole meat Lockerbie 55°13'53.64"N 2°58 '22.40"W 02/11/2009 UK5819848100174 Galloway M 20/06/2007 -98.6

90 00000015 S0090 whole meat Lockerbie 55° 9'34.19"N 3°16 '51.95"W 02/11/2009 UK582054300031 Herford X F 29/11/2007 -100.1

91 00000016 S0091 whole meat Lockerbie 55°19'33.45"N 3°1 2'16.69"W 02/11/2009 UK583842600677 Aberdeen Angus X M 15/05/2007 -95.1

92 00000017 S0092 whole meat Lockerbie 55° 8'37.24"N 3°33 '21.56"W 02/11/2009 UK581714400304 Limousin X F 12/05/2007 -97.4

93 00000018 S0093 whole meat Lockerbie 54°52'3.22"N 4°21' 11.67"W 02/11/2009 UK582521700633 South Devon X M 02/05/2007 -96.0



96 00000021 S0096 whole meat Lockerbie 55°10'45.52"N 3°35 '50.00"W 04/11/2009 UK581669300437 Limousin X F 03/06/2007 -100.1

97 00000022 S0097 whole meat Lockerbie 55° 5'36.12"N 3°3 1'2.71"W 04/11/2009 UK583874100099 Limousin X M 18/05/2007 -100.5


99 00000024 S0099 whole meat Lockerbie 55°10'45.52"N 3°35 '50.00"W 04/11/2009 UK581669400452 Limousin X F 18/06/2007 -97.0

100 00000025 S0100 whole meat Lockerbie 54°51'5.37"N 4°16 '48.06"W 04/11/2009 UK582494200392 Limousin X M 25/10/2007 -98.3

δδδδ2H [‰]

mean -98.04

SD 3.39

min -107.04

max -90.72

range 16.33

N 100

BBOP Scotland 60


# Reference # MLC #

1 S08030401 S0001

2 S08030402 S0002

3 S08030403 S0003

4 S08030404 S0004

5 S08030405 S0005

6 S08030406 S0006

7 S08030407 S0007

8 S08030408 S0008

9 S08030409 S0009

10 S08030410 S0010

11 S08030411 S0011

12 S08030412 S0012

13 S08030413 S0013

14 S08030414 S0014

15 S08030415 S0015

16 S08030416 S0016

17 S08030417 S0017

18 S08030418 S0018

19 S08030419 S0019

20 S08030420 S0020

21 S08090801 S0021

22 S08092501 S0022

23 S08091801 S0023

24 S08091601 S0024

25 S08101401 S0025

26 S08101402 S0026

27 S08101403 S0027

28 S08092502 S0028

29 S08091001 S0029

30 S08102401 S0030

31 S08031101 S0031

32 S09041401 S0032

33 S09051201 S0033

34 S09072701 S0034

35 S09072702 S0035

36 S09072703 S0036

37 S09072704 S0037

SD/AD Protein SD/AD Protein SD/AD Protein SD/AD 87/86Sr 2SD (abs) Na 23 Mg 24 Al 27 P 31 K 39

[‰] n d13C [‰] [‰] n d15N [‰] [‰] n d34S [‰] [‰] n [‰] [ug/kg] [ ug/kg] [ug/kg] [ug/kg] [ug/kg]

1.4 3 -27.15 0.07 3 7.02 0.10 3 8.3 1.2 3 0.70874 0.000119 2622250 881776 709 7186629 14389174

1.2 3 -26.82 0.04 3 8.11 0.12 3 10.4 0.1 3 0.709844 0.000127 2161391 890468 1698 7139698 13756812

1.2 3 -27.09 0.05 3 7.97 0.12 3 5.6 0.7 3 0.70836 0.000029 2322934 897889 1101 7379196 14534642

2.6 3 -27.11 0.03 3 6.73 0.01 3 4.0 1.0 3 0.70788 0.00004 2658449 926045 545 7932226 16662825

1.7 3 -27.02 0.02 3 8.08 0.06 3 6.7 0.9 3 0.708934 0.000043 2406311 876415 1032 7207356 14417944

0.8 3 -26.56 0.04 3 8.12 0.02 3 11.7 0.2 3 0.709244 0.000037 2539017 887368 992 6995548 13881771

2.8 3 -26.50 0.02 3 7.57 0.02 3 11.2 0.3 3 0.708994 0.000027 2550647 998285 1853 7991521 14764944

0.5 3 -27.22 0.01 3 8.12 0.11 3 11.0 0.2 3 0.709779 0.000015 1987491 792112 4934 6522489 13044019

0.2 3 -27.13 0.01 3 7.79 0.02 3 11.3 1.2 3 0.708435 0.000028 2399304 874103 1116 7319733 14016192

2.5 3 -26.57 0.05 3 9.41 0.10 3 13.1 0.2 3 0.709607 0.000021 3039088 794264 740 6346922 12316688

2.1 3 -27.02 0.02 3 9.20 0.08 3 14.5 0.4 3 0.708716 0.000066 2332561 787678 493 6454947 12438731

1.1 3 -27.16 0.01 3 7.37 0.05 3 14.3 0.1 3 0.708606 0.000044 2307130 890232 908 6979108 13691356

2.3 3 -27.14 0.09 3 8.22 0.11 3 13.2 0.1 3 0.708782 0.000026 3175216 829466 582 6751161 13315008

0.2 3 -25.62 0.01 3 7.64 0.05 3 11.3 0.2 3 0.708644 0.000049 2192109 632373 4390 5402190 10215570

2.0 3 -25.85 0.04 3 7.55 0.05 3 9.6 0.6 3 0.709152 0.000059 2656758 790060 1225 6431446 12336951

1.4 3 -27.19 0.05 3 7.60 0.03 3 10.2 0.2 3 0.709244 0.000059 3260290 753487 1095 6235390 12341203

0.7 3 -27.58 0.05 3 8.09 0.08 3 10.8 0.1 3 0.70894 0.000045 2878470 837416 1696 6910217 13172004

1.4 3 -26.59 0.00 3 8.39 0.08 3 9.6 0.3 3 0.70891 0.000068 2615661 854127 696 7006007 13762366

2.1 3 -26.60 0.06 3 7.63 0.09 3 10.1 0.0 3 0.709094 0.00012 2773870 865928 674 7159530 15286975

2.8 3 -26.67 0.02 3 8.67 0.10 3 10.4 0.2 3 0.708536 0.000056 2797764 813557 729 6862642 13396342

1.0 3 -27.36 0.03 3 7.55 0.01 3 8.3 0.3 3 0.712126 0.000044 3096705 931132 3138 7554049 13973400

0.8 3 -26.95 0.02 3 7.75 0.06 3 7.2 0.3 3 0.713957 0.000041 3513011 946267 7047 7836964 14355513

1.9 3 -27.23 0.03 3 8.38 0.01 3 8.5 0.1 3 0.707825 0.00003 3269672 985716 1029 8057534 14672854

0.4 3 -27.01 0.03 2 6.71 0.01 2 8.6 0.3 3 0.710914 0.000093 3303449 971843 1162 8200821 15172659

1.9 3 -26.64 0.06 3 8.17 0.04 3 9.3 0.3 3 0.709545 0.000048 2508310 984099 2082 8298458 14870700

1.1 3 -26.65 0.04 3 7.91 0.05 3 9.9 0.1 3 0.711214 0.000027 2006694 1016648 2599 8336846 16135694

1.3 3 -26.58 0.05 3 7.19 0.03 3 9.1 0.1 3 0.711041 0.000025 2424783 1054400 1806 8618710 15515486

1.4 3 -26.67 0.01 3 5.63 0.04 3 7.9 0.3 3 0.716148 0.00002 3550419 948707 11898 7668780 14429331

0.8 3 -26.73 0.01 3 5.82 0.02 3 7.6 0.1 3 0.714667 0.000037 3512031 974413 6724 8001973 14435615

0.6 3 -26.67 0.03 3 5.12 0.02 3 7.6 0.2 3 0.711848 0.000033 2682141 935941 1464 7566240 13867569

1.0 3 -26.40 0.01 3 6.78 0.02 3 5.8 0.4 3 0.714977 0.0116 1722600 896493 4097 8124202 14538788

1.6 3 -26.20 0.03 3 6.51 0.06 3 5.2 0.1 2 0.711557 0.0103 2110346 842314 777 7989435 13858729

5.2 3 -26.07 0.02 3 6.48 0.08 3 5.3 0.3 3 0.712312 0.0083 1939670 901541 2527 8387512 15906070

1.2 3 -26.00 0.04 3 7.2 0.0 3 10.5 0.4 3 0.708243 0.0086 1682039 574776 1908 5232001 7991215

1.6 3 -25.92 0.06 3 7.6 0.1 3 11.3 0.2 3 0.712511 0.0077 3301519 719965 2034 6442946 9992562

0.7 3 -26.07 0.08 3 7.8 0.2 3 8.2 0.6 3 0.710554 0.0071 1977844 852416 1762 6925459 12323444

0.8 3 -26.10 0.03 3 7.3 0.0 3 12.1 0.6 3 0.708952 0.0086 2534713 735651 852 6526165 10488048

BBOP Scotland 61


# Reference # MLC #

38 S09072705 S0038

39 S09072706 S0039

40 S09072707 S0040

41 S09072708 S0041

42 S09072709 S0042

43 S09072710 S0043

44 S09072711 S0044

45 S09072712 S0045

46 S09072713 S0046

47 S09072714 S0047

48 S09072715 S0048

49 S09072716 S0049

50 S09072717 S0050

51 S09072718 S0051

52 none S0052

53 none S0053

54 none S0054

55 none S0055

56 none S0056

57 none S0057

58 none S0058

59 none S0059

60 none S0060

61 none S0061

62 none S0062

63 none S0063

64 none S0064

65 none S0065

66 none S0066

67 none S0067

68 none S0068

69 none S0069

70 none S0070

71 none S0071

72 none S0072

73 none S0073

74 none S0074



1.6 3 -25.79 0.05 3 8.0 0.1 3 7.6 0.7 3 0.712137 0.0075 2099953 763981 8802 6485412 10934573

1.2 3 -25.77 0.07 3 7.4 0.1 3 13.1 0.7 3 0.708797 0.0020 2508647 788192 1502 6838507 11462068

na 1 -27.27 0.02 3 9.7 0.0 3 7.8 0.3 3 0.710848 0.0032 1717742 687739 1238 6167790 9527211

1 3 -27.27 0.06 3 9.5 0.0 3 7.0 0.6 3 0.709252 0.0033 1755804 765250 3868 6850922 10562228

0.8 3 -27.28 0.05 3 9.0 0.1 3 10.6 0.7 3 0.712192 0.0065 2012234 694187 1971 6810774 8501009

0.9 3 -27.08 0.02 3 9.6 0.0 3 9.6 0.2 3 0.709760 0.0023 2230239 710667 884 6318712 9139462

0.4 3 -27.19 0.02 3 8.8 0.1 3 8.2 0.7 3 0.709856 0.0072 1908641 824428 1812 6948697 12400654

1.3 3 -27.29 0.06 3 9.1 0.1 3 9.9 0.1 3 0.716658 0.0031 2045876 833642 6817 7480889 12292140

2 3 -27.20 0.08 3 9.4 0.1 3 7.9 0.8 3 0.709821 0.0081 2320399 661116 1747 5887639 9155831

2.5 3 -27.11 0.07 3 8.2 0.0 3 8.3 0.4 3 0.709472 0.0041 2614629 870054 2095 7872833 12199976

2.1 3 -27.13 0.04 2 9.8 0.1 2 9.9 0.5 3 0.716758 0.0033 2355506 457444 34657 3865984 5785019

1.5 3 -27.21 0.01 3 9.7 0.0 3 9.4 0.6 3 0.709847 0.0063 2022326 808680 2102 7140135 11270725

1.6 3 -27.37 0.05 3 7.0 0.2 3 9.4 0.3 3 0.713062 0.0054 2784412 784458 8831 7380367 11556786

1 3 -27.43 0.02 3 7.1 0.1 3 7.3 0.3 3 0.715440 0.0117 2108764 671322 4556 6200962 9274280

1.0 3 -26.32 0.30 2 6.1 0.2 2 6.0 0.3 3 0.713558 0.0076 1647702 1070366 1134 9618578 18706384

2.1 3 -25.92 0.03 2 8.2 0.1 2 6.8 0.6 3 0.713250 0.0056 2290439 861156 1931 7716620 15288258

1.3 3 -25.80 0.08 2 8.2 0.2 2 6.8 0.8 3 0.709602 0.0105 2450731 960901 943 9080897 17445264

0.6 3 -25.76 0.06 2 7.8 0.1 2 6.6 0.6 3 0.709733 0.0026 2303874 884617 1418 8046416 15701506

2.9 3 -26.44 0.08 2 6.7 0.1 2 5.8 0.7 3 0.714121 0.0048 2869124 917000 22760 8442437 16501726

2.0 3 -26.87 0.01 2 6.1 0.1 2 6.9 0.7 3 0.713713 0.0125 2597755 886995 19027 8999788 15503902

1.4 3 -25.28 0.01 2 7.6 0.1 2 7.0 0.3 3 0.708801 0.0067 2022371 840911 1092 7390111 14639063

0.4 3 -25.31 0.06 2 7.1 0.0 2 4.4 0.4 3 0.712794 0.0076 2344150 847302 2427 7433440 15126153

2.4 3 -25.20 0.00 2 6.9 0.1 2 5.9 0.4 3 0.709373 0.0078 2174918 879213 1539 8013486 16290722

2.8 3 -25.25 0.05 2 7.1 0.1 2 5.8 0.7 3 0.709002 0.0054 2266301 867078 743 7837921 15768625

0.7 3 -25.13 0.04 2 7.7 0.1 2 6.2 0.4 3 0.710085 0.0079 2340497 860091 1129 7769389 14920196

0.6 3 -26.53 0.01 2 5.1 0.0 2 5.2 0.8 3 0.712934 0.0056 2694564 695175 24230 5827829 11535409

1.0 3 -26.14 0.03 2 4.9 0.0 2 5.9 0.4 3 0.717145 0.0041 3695122 411913 38320 3420523 6633407

1.4 3 -26.38 0.08 2 5.7 0.0 2 5.7 0.4 3 0.716602 0.0047 4975044 620446 42839 4652347 9574058

1.3 3 -26.14 0.05 2 4.9 0.1 2 6.2 0.4 3 0.713096 0.0039 1526635 840911 17283 7058518 13449971

0.5 3 -26.15 0.03 2 5.4 0.2 2 4.7 0.4 3 0.716480 0.0071 4153925 532304 37468 4405796 8139233

0.6 3 -26.03 0.03 2 5.5 0.2 2 6.2 0.7 3 0.714042 0.0049 1887135 779517 6247 6944806 14671509

1.1 3 -25.76 0.01 2 5.5 0.2 2 5.1 0.1 3 0.706815 0.0051 1738760 787664 2623 6822729 13148556

0.5 3 -26.21 0.22 2 5.5 0.2 2 5.2 0.3 3 0.716590 0.0026 3187899 444717 36874 3577958 7307972

0.6 3 -27.17 0.01 2 7.1 0.1 2 4.8 0.5 3 0.708272 0.0031 2850706 884574 2488 7580892 14233572

1.2 3 -26.25 0.06 2 7.4 0.1 2 5.1 0.7 3 0.710078 0.0035 2575857 894531 14569 8241001 15261291

1.0 3 -25.41 0.08 2 7.3 0.2 2 6.2 0.3 3 unmeasurable na 1851831 791469 1639 7149205 14030051

0.9 3 -25.10 0.17 2 7.7 0.4 2 7.0 0.5 3 unmeasurable na 2269028 872011 6824 9213489 15206944

BBOP Scotland 62


# Reference # MLC #

75 none S0075

76 00000001 S0076

77 00000002 S0077

78 00000003 S0078

79 00000004 S0079

80 00000005 S0080

81 00000006 S0081

82 00000007 S0082

83 00000008 S0083

84 00000009 S0084

85 00000010 S0085

86 00000011 S0086

87 00000012 S0087

88 00000013 S0088

89 00000014 S0089

90 00000015 S0090

91 00000016 S0091

92 00000017 S0092

93 00000018 S0093

94 00000019 S0094

95 00000020 S0095

96 00000021 S0096

97 00000022 S0097

98 00000023 S0098

99 00000024 S0099

100 00000025 S0100

mean

SD

min

max

range

N



0.5 3 -24.54 0.00 2 7.0 0.4 2 4.8 0.8 3 unmeasurable na 4749858 696826 26562 5953476 11990195

2.2 3 -26.89 0.08 2 7.1 0.1 2 7.4 0.1 3 0.709934 0.0062 1960230 822683 709 7835507 14730682

2.4 3 -26.07 0.02 2 8.0 0.0 2 8.2 0.4 3 0.712740 0.0036 2135433 751045 3851 6902760 12857968

1.8 3 -26.24 0.01 2 6.3 0.0 2 6.8 0.6 3 0.714774 0.0070 2022575 800884 3812 7289523 13582628

1.7 3 -26.03 0.01 2 7.0 na 1 7.3 0.5 3 unmeasurable na 2580583 858998 2032 7861016 14920870

0.2 3 -26.97 0.06 2 7.7 0.2 2 8.2 0.2 3 0.717201 0.0064 2248556 791568 8160 7242005 13647975

0.8 3 -26.15 0.02 2 5.7 0.2 2 6.9 0.3 3 0.714622 0.0046 2021543 835105 1433 7943998 14806547

2.6 3 -27.32 0.07 2 5.7 0.1 2 6.7 0.1 3 0.716476 0.0027 3013574 783253 23123 6667049 13620413

1.3 3 -26.66 0.04 2 8.8 0.1 2 7.2 0.7 3 0.714317 0.0031 3215184 676256 5098 6787876 12473500

1.0 3 -26.69 0.11 2 6.4 0.1 2 5.9 0.5 3 0.707729 0.0032 2099039 880048 448 8008108 14869736

0.9 3 -26.81 0.10 2 8.2 0.2 2 8.3 0.5 3 0.712689 0.0054 3282709 715555 1122 6829744 11504371

1.3 3 -26.88 0.04 2 6.1 0.1 2 8.5 0.2 3 0.709306 0.0199 1924822 855661 742 7944954 15202305

1.8 3 -26.11 0.07 2 6.9 0.1 2 7.6 0.6 3 0.711187 0.0075 2381412 807982 805 7554166 14288475

0.9 3 -26.41 0.02 2 6.3 0.0 2 7.6 0.1 3 0.708917 0.0027 2417164 927839 844 8775947 16446278

0.5 3 -27.11 0.04 2 4.9 0.1 2 7.3 0.6 3 0.713367 0.0022 2995521 809041 17828 7465662 14084904

0.9 3 -27.15 0.02 2 6.9 0.0 2 7.4 0.8 3 0.716674 0.0024 2010044 828204 385 7570054 14113584

1.4 3 -25.60 0.05 2 6.8 0.2 2 8.2 0.7 3 0.712363 0.0034 4058401 638447 14100 6102765 11367576

4.2 3 -26.15 0.02 2 7.6 0.0 2 8.7 0.6 3 0.715442 0.0059 2955294 777260 12455 7280130 13066932

5.0 3 -26.81 0.03 2 5.4 0.0 2 8.2 0.2 3 0.712906 0.0159 3036345 773434 12227 7623792 14239928

2.5 3 -25.33 0.03 2 7.1 0.3 2 7.9 0.2 3 0.712203 0.0039 2218631 836931 5750 7703411 14404484

1.6 3 -26.41 0.08 2 6.7 0.1 2 7.8 0.3 3 0.711301 0.0030 2440186 855035 1123 7794409 15124556

1.2 3 -26.37 0.05 2 7.0 0.2 2 8.3 0.1 3 0.713421 0.0033 1957623 847609 692 8066773 15179929

0.9 3 -26.28 0.02 2 6.7 0.1 2 8.4 0.5 3 0.714437 0.0023 2545932 849982 2861 7545483 15333640

1.0 3 -26.43 0.02 2 5.9 0.1 2 8.7 0.6 3 0.708769 0.0020 2311776 848182 677 8204641 15105394

1.3 3 -26.72 0.03 2 7.2 0.1 2 8.3 0.7 3 0.712201 0.0026 2773569 867859 3973 8509292 15920084

1.0 3 -26.21 0.02 2 7.5 0.1 2 8.4 0.5 3 0.711991 0.0054 2121181 841633 443 7931531 14900306

δδδδ13C [‰] δδδδ15N [‰] δδδδ34S [‰] 87/86Sr Na 23 Mg 24 Al 27 P 31 K 39

-26.49 7.30 8.10 0.7114769 2534894 818747 5978 7208699 13351982

0.64 1.18 2.24 0.0027424 629586 118444 9359 1103785 2417022

-27.58 4.87 4.05 0.7068150 1526635 411913 385 3420523 5785019

-24.54 9.78 14.50 0.7172010 4975044 1070366 42839 9618578 18706384

3.04 4.91 10.45 0.01 3448409 658453 42454 6198055 12921365

100 100 100 96 100 100 100 100 100

BBOP Scotland 63


# Reference # MLC #

1 S08030401 S0001

2 S08030402 S0002

3 S08030403 S0003

4 S08030404 S0004

5 S08030405 S0005

6 S08030406 S0006

7 S08030407 S0007

8 S08030408 S0008

9 S08030409 S0009

10 S08030410 S0010

11 S08030411 S0011

12 S08030412 S0012

13 S08030413 S0013

14 S08030414 S0014

15 S08030415 S0015

16 S08030416 S0016

17 S08030417 S0017

18 S08030418 S0018

19 S08030419 S0019

20 S08030420 S0020

21 S08090801 S0021

22 S08092501 S0022

23 S08091801 S0023

24 S08091601 S0024

25 S08101401 S0025

26 S08101402 S0026

27 S08101403 S0027

28 S08092502 S0028

29 S08091001 S0029

30 S08102401 S0030

31 S08031101 S0031

32 S09041401 S0032

33 S09051201 S0033

34 S09072701 S0034

35 S09072702 S0035

36 S09072703 S0036

37 S09072704 S0037

Ca 43 Rb 85 Sr 88 Ba 138 Sc 45 Ti 48 V 51 Cr 52 Mn 55 F e 56 Co 59 Ni 60 Cu 63 Zn 66 Ga 69 Ge 74 As 75

[ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [u g/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/ kg] [ug/kg] [ug/kg]

159213 44269 210 45 0 416 1 5 351 113051 5 10 2432 176249 0 3 12

191905 22560 103 48 0 295 1 6 390 106212 11 3 3291 201651 0 1 20

238074 19476 234 74 1 658 2 141 394 124615 8 102 2744 156802 0 5 14

187782 24008 256 36 0 565 1 4 271 74281 40 1 2399 169530 0 9 12

157335 19269 224 42 0 378 1 1 380 89311 27 3 2622 181407 0 3 13

151134 13189 231 70 2 965 3 20 391 115491 4 21 3109 206488 0 12 16

281745 11703 385 97 3 813 2 6 423 119950 2 14 4065 208749 0 2 16

228776 25293 246 99 1 691 2 18 464 119979 8 4 2201 169451 0 4 9

356281 17985 471 101 1 1371 2 19 548 99943 5 19 2770 186780 0 6 13

274638 10786 305 68 2 909 1 4 410 139197 27 9 2760 166607 0 3 11

538846 15242 619 265 2 1883 1 4 361 94853 41 11 2378 146127 0 5 10

227987 41314 271 91 1 690 1 8 382 135323 6 1090 2651 192933 0 1 13

182571 19011 241 48 0 557 0 4 392 102953 54 10 2743 140901 0 2 8

147648 9871 204 28 0 387 1 1 282 79327 6 5 1912 142813 1 4 14

234867 12716 355 82 3 1146 2 12 448 154886 12 51 3238 161415 0 4 16

300223 18127 338 85 2 1049 0 7 362 175522 7 12 2303 173978 1 0 18

227540 17466 345 85 4 721 3 1 341 135840 10 14 2756 244811 0 1 44

193065 14971 198 41 1 636 1 7 429 107833 27 18 2578 172416 0 7 20

180905 14367 161 30 2 595 1 8 337 89615 28 5 2320 136718 0 5 21

184434 14587 172 30 2 584 2 11 434 114183 33 7 2797 205133 0 4 27

286724 12854 242 577 3 1312 3 84 276 88263 6 1 2418 216062 0 1 296

434035 17823 531 1669 4 2626 4 83 458 116866 16 44 3042 281906 1 3 398

228033 16825 231 172 0 1295 0 2 403 103472 8 0 2624 295872 0 1 16

216860 27512 235 155 1 1330 1 35 439 86796 6 11 2648 189566 0 2 34

337578 14857 352 180 0 609 4 50 448 97498 13 28 3287 195417 0 2 70

391127 14294 364 476 9 2083 4 11 463 81029 11 4 2683 223309 2 3 230

335548 12497 302 168 2 1873 4 15 414 85876 16 10 2484 181069 0 2 63

305076 17603 279 3772 6 1555 7 31 447 103518 13 8 2535 266486 3 3 1210

228861 17429 116 777 10 2840 6 33 449 86076 11 25 3261 211988 1 1 158

236854 14615 111 261 0 295 2 62 408 98005 6 7 2462 202840 0 1 70

142676 4574 100 818 5 1458 2 12 315 44195 27 15 2236 197304 1 1 401

124089 5455 48 53 1 414 2 21 392 50054 64 47 2951 242467 1 3 14

144687 7733 94 498 4 1200 2 6 258 53523 45 0 1903 168140 1 1 244

583537 8438 575 217 2 280 2 30 277 23333 10 15 2053 172977 1 1 28

500905 13579 440 1301 4 24 4 37 444 38630 18 17 3084 208862 1 2 192

350584 11761 227 116 6 527 3 70 447 41614 21 21 3622 237868 0 2 25

660557 11722 632 323 2 698 2 29 289 24657 11 1 2347 186975 1 1 20

BBOP Scotland 64


# Reference # MLC #

38 S09072705 S0038

39 S09072706 S0039

40 S09072707 S0040

41 S09072708 S0041

42 S09072709 S0042

43 S09072710 S0043

44 S09072711 S0044

45 S09072712 S0045

46 S09072713 S0046

47 S09072714 S0047

48 S09072715 S0048

49 S09072716 S0049

50 S09072717 S0050

51 S09072718 S0051

52 none S0052

53 none S0053

54 none S0054

55 none S0055

56 none S0056

57 none S0057

58 none S0058

59 none S0059

60 none S0060

61 none S0061

62 none S0062

63 none S0063

64 none S0064

65 none S0065

66 none S0066

67 none S0067

68 none S0068

69 none S0069

70 none S0070

71 none S0071

72 none S0072

73 none S0073

74 none S0074



803946 13306 734 2409 10 1799 20 918 484 29353 19 342 2917 225087 13 3 982

597566 12499 514 242 2 943 5 667 473 34423 18 37 2797 235968 1 1 45

429776 6655 326 191 1 0 2 3 496 41669 11 0 3940 230231 1 1 41

307404 7265 235 95 2 0 3 54 613 44522 10 0 4982 147743 2 1 67

2765232 6054 2466 1330 4 10798 2 31 403 30619 6 17 2739 225960 1 1 131

662806 6237 610 162 2 816 2 7 607 47107 10 3 4683 234763 1 2 19

352987 7882 260 100 2 517 2 51 632 42219 10 35 3474 226909 0 1 22

573637 8330 516 2458 7 587 5 28 646 44533 11 33 3657 166517 2 1 496

550806 6192 521 161 2 297 2 7 598 35886 11 3 3662 164772 1 0 15

762142 7457 677 284 3 956 5 198 504 32253 6 53 4008 202145 1 1 47

491938 4040 798 8934 25 1359 19 51 619 27507 11 17 2587 178912 9 4 3488

602884 7596 542 168 3 518 3 97 853 47464 10 65 4069 202520 1 1 37

526535 18647 447 2177 13 299 9 44 705 37185 9 5 3365 176093 4 1 1102

541478 14608 457 2591 5 278 6 52 647 39453 5 4 3829 172263 2 1 198

154162 9837 73 124 5 507 2 17 214 49334 16 8 1961 121713 1 1 16

478543 28691 276 761 3 1414 4 5 461 129279 20 0 21187 307053 0 3 130

1643090 27949 722 689 2 4635 3 5 447 114725 18 0 4154 340147 0 2 0

876414 23733 454 481 1 2918 2 0 439 125378 15 0 3857 303634 4 1 30

292666 17763 436 4840 19 3145 11 101 557 64090 28 349 3476 245442 0 7 1329

3183675 6716 1345 3104 17 12627 8 44 539 120880 8 46 3364 332338 18 2 1208

564038 13792 451 403 2 1760 2 28 374 94591 9 15 3385 294087 0 1 13

305479 11300 274 835 3 558 4 2 383 112909 8 0 3852 286214 0 0 201

357602 13461 283 276 7 1227 2 11 404 110510 11 44 3691 314966 0 0 92

353215 12700 283 290 2 1076 1 2 443 126176 7 0 3979 320515 5 1 26

465271 12828 385 377 2 1450 2 7 494 98511 11 22 4113 295207 13 0 15

283070 10310 584 44364 21 2156 10 41 433 72376 10 8 2721 241322 25 2 3171

446502 6951 1150 17310 27 5824 17 135 621 42937 13 81 1220 120703 19 3 7915

572995 9872 1506 51737 32 5145 23 204 910 68113 18 335 2374 226496 33 1 4976

150109 11590 129 375 19 433 14 49 420 156954 11 57 2609 139777 76 2 74

438641 8889 1080 35854 33 3980 70 164 1726 71040 18 631 33391 167529 0 1 4252

152656 13256 106 164 6 791 7 39 299 83427 8 51 2238 350038 1 0 29

133491 11412 95 308 3 1045 4 6 152 48196 7 0 1833 164413 0 0 103

386514 7959 981 36367 23 3860 22 1011 588 46609 28 574 2100 180781 0 2 4354

226942 11151 263 23667 3 255 2 24 382 74070 6 0 3120 232477 0 1 21

1098561 23054 710 6642 11 4199 7 87 586 130840 15 174 3832 305628 0 3 1301

400974 12537 375 533 2 1614 2 8 371 106633 6 0 3500 310127 25 1 46

2869117 13715 2458 4762 15 9319 4 44 496 123024 11 148 4830 299900 0 1 715

BBOP Scotland 65


# Reference # MLC #

75 none S0075

76 00000001 S0076

77 00000002 S0077

78 00000003 S0078

79 00000004 S0079

80 00000005 S0080

81 00000006 S0081

82 00000007 S0082

83 00000008 S0083

84 00000009 S0084

85 00000010 S0085

86 00000011 S0086

87 00000012 S0087

88 00000013 S0088

89 00000014 S0089

90 00000015 S0090

91 00000016 S0091

92 00000017 S0092

93 00000018 S0093

94 00000019 S0094

95 00000020 S0095

96 00000021 S0096

97 00000022 S0097

98 00000023 S0098

99 00000024 S0099

100 00000025 S0100

mean

SD

min

max

range

N



732355 12805 1351 32031 24 5817 16 95 967 112919 19 58 4147 278042 0 5 3345

148755 9951 159 57 2 873 1 9 345 37870 4 14 3428 219113 1 1 19

501752 11983 440 691 6 2456 4 61 437 69868 7 6 3326 175063 2 2 358

169992 5899 179 493 6 1108 2 8 316 33987 5 7 2609 227100 2 2 321

624634 20275 496 482 5 3006 4 18 283 47412 4 2 2630 210589 2 1 150

199798 13205 265 2275 8 1458 4 12 437 59082 11 0 3143 216258 3 3 550

197398 22947 160 236 1 1042 1 6 314 41962 4 0 3123 232015 2 2 67

320118 11521 597 7471 22 2580 12 47 494 29897 30 31 2771 218588 7 2 2077

207080 5960 184 1078 8 1206 4 13 456 47370 11 1 2513 185493 3 2 476

163183 5768 81 48 1 838 0 6 306 33506 3 0 2864 184703 1 1 14

235009 20220 145 193 2 1185 1 9 393 45973 7 0 3267 222670 1 1 36

165787 27696 116 54 1 857 1 7 399 40252 7 0 3701 209251 1 2 15

167845 15278 106 86 0 865 2 106 270 32008 6 2 2630 206004 1 1 32

209847 12370 129 88 3 1097 1 6 327 38008 4 36 3335 242927 2 2 23

319995 3291 730 6930 18 3037 13 56 696 35793 14 66 3323 192513 6 4 2267

160184 12561 99 111 2 918 2 8 424 35339 3 25 3574 218290 1 2 15

742045 16228 704 5007 15 4374 10 50 437 44280 8 18 2454 195090 4 4 1139

535891 13951 535 3545 11 3143 8 24 562 78238 8 5 3886 260375 4 3 748

258272 37114 472 3355 8 2036 7 24 465 32755 6 3 2733 207770 4 4 1439

202752 5715 183 1193 5 1177 5 11 264 30376 5 9 3764 218906 2 2 206

172435 5659 79 126 1 914 2 367 278 33827 6 10 2468 214402 1 2 49

157004 8668 79 67 2 778 1 64 395 37272 6 4 3543 215322 1 2 29

181788 8375 125 430 2 963 6 31 239 38392 20 6 2441 254687 1 1 134

175900 5611 79 66 2 847 1 8 286 30614 10 10 2745 206390 1 1 35

319959 11200 186 356 6 1596 7 28 651 61795 9 62 4610 200804 2 3 134

163201 9041 76 33 1 964 1 22 419 36872 6 2 3537 200269 1 1 72


433885 13953 417 3351 6 1700 5 62 453 73862 13 52 3538 215231 3 2 543

501432 7487 413 9215 7 2057 8 153 189 37852 11 146 3589 50631 9 2 1242

124089 3291 48 28 0 0 0 0 152 23333 2 0 1220 120703 0 0 0

3183675 44269 2466 51737 33 12627 70 1011 1726 175522 64 1090 33391 350038 76 12 7915

3059586 40978 2418 51709 33 12627 70 1011 1574 152189 63 1090 32171 229335 76 12 7915

100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100

BBOP Scotland 66


# Reference # MLC #

1 S08030401 S0001

2 S08030402 S0002

3 S08030403 S0003

4 S08030404 S0004

5 S08030405 S0005

6 S08030406 S0006

7 S08030407 S0007

8 S08030408 S0008

9 S08030409 S0009

10 S08030410 S0010

11 S08030411 S0011

12 S08030412 S0012

13 S08030413 S0013

14 S08030414 S0014

15 S08030415 S0015

16 S08030416 S0016

17 S08030417 S0017

18 S08030418 S0018

19 S08030419 S0019

20 S08030420 S0020

21 S08090801 S0021

22 S08092501 S0022

23 S08091801 S0023

24 S08091601 S0024

25 S08101401 S0025

26 S08101402 S0026

27 S08101403 S0027

28 S08092502 S0028

29 S08091001 S0029

30 S08102401 S0030

31 S08031101 S0031

32 S09041401 S0032

33 S09051201 S0033

34 S09072701 S0034

35 S09072702 S0035

36 S09072703 S0036

37 S09072704 S0037

Se 77 Li 7 Be 9 Y 89 Zr 90 Nb 93 Mo 98 Ru 102 Pd 1 06 Cd 114 Sn 120 Sb 121 Te 130 La 139 Ce 140 Pr 141 Nd 142


65 0.01 0.06 0.20 24.30 0.00 41.65 0.06 4.46 0.31 0.53 1.49 0.40 0.12 0.33 0.13 0.24

202 0.07 0.07 0.09 34.76 0.00 41.62 0.00 4.68 0.39 0.30 0.35 1.25 0.13 0.38 0.08 0.16

300 0.16 0.12 0.16 218.51 0.25 39.70 0.04 4.94 0.67 1.60 2.22 0.76 0.22 0.62 0.28 0.46

506 0.88 0.73 0.27 14.45 0.04 50.31 0.23 3.06 0.83 4.39 1.78 1.34 0.19 0.84 0.44 0.50

218 0.55 0.51 0.10 20.33 0.00 26.47 0.04 4.06 0.43 0.12 1.94 0.32 0.12 0.21 0.09 0.13

91 0.02 0.04 0.26 13.03 0.73 50.84 0.00 4.08 0.76 0.71 2.94 2.34 0.28 0.48 0.12 0.22

77 0.90 0.83 0.22 41.10 1.35 30.25 0.00 5.21 1.20 0.66 1.96 0.62 0.26 0.43 0.09 0.20

246 0.00 0.00 0.31 55.14 0.13 31.24 0.12 2.27 1.54 40.51 2.22 24.09 0.52 1.25 0.18 0.66

326 0.15 0.09 0.35 44.80 0.33 25.05 0.27 4.05 0.29 3.55 2.88 1.37 0.56 0.86 0.07 0.49

403 0.00 0.03 0.55 78.50 0.25 49.15 0.10 3.36 0.78 2.08 1.59 0.01 0.18 0.19 0.04 0.22

368 0.04 0.07 2.86 55.85 0.11 48.75 0.33 3.09 0.47 0.64 0.90 49.11 0.17 0.36 0.06 0.27

77 0.08 0.02 0.19 58.83 0.00 37.39 0.01 4.09 0.38 0.59 1.15 7.51 0.18 0.46 0.09 0.21

362 0.25 0.26 0.17 44.02 0.00 38.94 0.17 3.11 0.84 4.15 1.00 0.01 0.10 0.42 0.19 0.35

113 0.00 0.08 0.17 8.34 0.00 24.16 0.03 2.02 0.84 0.12 1.64 0.50 0.19 0.38 0.22 0.31

142 0.42 0.49 0.25 29.63 1.03 35.76 0.12 2.90 0.67 1.66 1.13 0.28 0.26 0.48 0.08 0.25

88 0.53 0.64 0.16 71.06 0.12 29.90 0.23 1.60 0.37 1.45 0.40 37.33 0.12 0.49 0.08 0.34

108 0.42 0.45 0.49 61.14 2.37 33.94 0.14 5.80 0.70 0.88 3.19 0.01 0.40 0.73 0.08 0.56

425 0.00 0.00 0.23 9.14 0.03 27.12 0.12 2.59 1.15 2.22 2.02 0.21 0.24 0.66 0.26 0.38

497 0.32 0.32 0.22 98.55 0.36 32.37 0.10 2.59 0.85 2.04 1.34 0.01 0.18 0.96 0.24 0.57

532 0.00 0.03 0.13 9.07 0.01 52.21 0.00 3.06 0.72 1.09 2.52 0.80 0.12 0.44 0.09 0.24

73 0.46 0.52 1.68 0.11 1.62 27.99 0.10 20.71 1.61 6.68 22.26 7.27 6.99 15.31 0.83 5.13

255 0.58 0.63 4.81 0.11 8.22 52.77 0.19 15.61 3.06 7.16 49.43 20.30 8.44 28.87 1.10 8.27

90 0.07 0.06 0.26 7.34 1.44 37.26 0.13 3.26 0.67 1.49 2.75 4.59 0.50 2.17 0.23 0.73

132 0.11 0.12 0.30 0.11 1.34 36.01 0.07 3.16 1.13 3.12 4.63 4.51 0.80 2.97 0.33 1.02

207 0.13 0.13 1.92 0.11 1.14 46.61 0.14 5.92 1.33 2.34 6.35 3.38 2.42 4.88 0.48 2.15

209 0.30 0.38 4.37 0.11 1.76 36.11 0.11 10.75 1.28 0.12 20.59 3.84 9.88 17.74 1.41 8.54

227 0.18 0.20 1.90 0.11 2.61 32.27 0.14 2.67 1.01 3.42 4.40 3.08 1.66 4.63 0.34 1.64

178 1.56 1.74 5.65 0.11 3.31 36.88 0.17 40.79 6.75 8.04 156.61 45.21 19.83 65.02 2.33 18.33

126 0.35 0.23 5.24 0.11 8.92 41.31 0.09 8.85 1.47 3.67 29.19 9.04 4.11 17.93 0.75 5.04

149 0.17 0.12 0.41 0.11 1.50 45.45 0.10 4.88 1.17 0.22 8.30 1.57 1.49 4.04 0.30 1.47

345 67.1 0.53 2.25 577.46 2.05 21.73 0.20 21.40 2.52 2.61 34.54 8.80 8.65 35.46 1.34 8.83

432 3.5 0.10 0.20 223.06 0.34 25.78 0.00 9.02 1.38 20.69 1.24 1.66 0.47 7.97 0.89 2.22

302 23.5 0.37 1.43 602.37 1.71 21.94 0.12 21.89 1.71 9.15 29.14 6.07 7.36 26.11 1.42 6.61

296 6.6 0.09 2.32 0.00 0.40 30.38 0.69 0.17 0.80 15.28 4.71 3.37 2.12 4.27 0.39 1.65

399 40.4 0.54 3.90 64.15 0.76 38.38 0.50 4.64 1.56 0.86 20.10 12.76 8.99 14.48 1.29 5.14

406 6.4 0.19 4.57 0.00 2.25 33.91 0.04 1.31 0.75 6.59 13.48 2.65 1.99 2.74 0.45 1.51

312 6.6 0.13 3.17 0.00 0.37 28.88 0.67 0.02 18.70 6.50 6.36 4.52 2.47 3.85 0.54 1.96

BBOP Scotland 67


# Reference # MLC #

38 S09072705 S0038

39 S09072706 S0039

40 S09072707 S0040

41 S09072708 S0041

42 S09072709 S0042

43 S09072710 S0043

44 S09072711 S0044

45 S09072712 S0045

46 S09072713 S0046

47 S09072714 S0047

48 S09072715 S0048

49 S09072716 S0049

50 S09072717 S0050

51 S09072718 S0051

52 none S0052

53 none S0053

54 none S0054

55 none S0055

56 none S0056

57 none S0057

58 none S0058

59 none S0059

60 none S0060

61 none S0061

62 none S0062

63 none S0063

64 none S0064

65 none S0065

66 none S0066

67 none S0067

68 none S0068

69 none S0069

70 none S0070

71 none S0071

72 none S0072

73 none S0073

74 none S0074



364 125.7 1.99 8.41 500.96 2.82 60.58 0.78 28.66 4.23 44.18 162.29 30.63 41.75 78.61 4.72 22.52

375 10.7 0.49 3.07 4.33 1.36 39.53 0.58 1.68 0.89 13.32 8.34 4.48 3.96 6.82 0.63 2.80

202 7.7 0.17 2.22 0.67 0.10 37.17 0.48 1.56 0.85 16.82 8.69 2.28 1.98 3.15 0.38 1.56

303 5.2 0.11 2.25 0.00 0.41 33.92 2.27 1.15 0.64 3.73 8.16 2.05 4.36 11.49 0.87 3.94

160 61.0 0.46 2.21 76.20 0.52 31.15 2.55 5.22 1.68 16.30 28.65 16.84 3.36 11.43 0.63 3.33

171 3.2 0.13 2.10 0.00 0.61 41.59 0.68 0.15 0.94 7.28 2.05 2.18 1.61 3.33 0.44 1.65

183 2.4 0.15 1.95 0.00 0.71 42.12 0.09 0.70 2.38 25.41 4.16 3.31 2.02 2.89 0.38 1.61

213 201.9 0.95 5.71 282.12 1.48 31.99 0.63 16.94 4.24 14.92 148.38 30.35 11.28 40.97 1.69 10.04

189 4.9 0.25 2.62 0.00 0.68 41.86 2.01 1.32 0.76 6.36 6.57 3.25 2.25 4.11 0.44 3.75

187 6.1 0.16 3.08 0.00 0.67 54.72 0.82 0.47 1.32 12.96 5.30 4.38 3.13 5.74 0.67 2.45

155 831.7 5.96 19.80 1590.07 7.07 37.13 1.57 86.36 20.63 60.71 380.86 108.95 91.91 286.69 11.24 66.09

212 4.8 0.18 3.66 0.00 0.96 42.31 0.81 1.03 5.27 38.34 4.10 3.06 2.81 6.09 0.60 2.24

57 150.6 2.88 8.90 995.84 2.41 50.67 0.49 52.02 4.50 21.05 132.00 27.32 36.90 69.54 4.67 20.99

68 109.9 1.10 5.23 173.71 1.24 32.92 1.91 10.72 1.74 6.47 90.29 29.63 7.54 43.58 1.70 9.84

596 4.7 0.14 1.23 229.55 1.63 22.22 0.00 4.05 0.56 0.00 0.00 0.94 0.66 1.87 0.18 0.74

522 30.6 0.57 0.78 45.45 0.52 48.22 1.85 3.51 0.95 0.00 34.26 7.11 1.50 7.26 0.32 2.96

411 3.8 2.24 0.44 60.83 0.00 67.27 0.51 3.72 1.26 0.00 0.00 5.17 0.26 0.06 0.13 0.00

457 5.7 0.08 0.66 0.00 0.43 56.91 0.00 2.55 0.85 5.84 0.13 5.17 0.91 2.63 0.28 0.92

602 360.0 2.52 8.38 1413.17 7.83 39.02 1.25 25.47 7.93 21.72 68.48 53.21 29.56 118.72 3.80 39.94

100 278.4 1.45 5.14 564.48 6.71 37.99 1.93 13.38 9.31 5.85 51.66 26.16 13.35 54.02 1.67 18.71

246 1.2 0.08 0.20 11.86 0.15 47.10 0.03 2.15 1.26 7.81 2.66 6.86 0.28 0.85 0.14 0.65

284 30.5 0.37 1.12 587.62 0.12 38.57 0.00 9.09 1.87 13.35 38.32 10.43 4.26 12.40 0.60 4.30

312 3.5 0.21 0.76 185.19 1.23 52.84 0.00 4.42 1.10 4.71 23.37 3.65 2.11 8.24 0.31 2.68

240 3.9 0.16 0.37 48.46 0.00 46.52 0.00 2.73 0.85 8.65 4.25 6.12 0.50 1.30 0.12 0.42

281 4.1 0.25 0.21 318.85 0.18 58.23 0.00 5.27 1.71 6.88 3.83 5.80 0.36 1.49 0.08 0.31

144 388.9 3.38 12.48 1071.09 12.73 56.84 0.00 24.03 25.99 49.43 1910.86 535.13 50.22 175.48 6.19 62.15

103 2377.8 8.20 13.23 1204.82 31.94 38.24 0.22 31.06 58.53 49.09 292.81 188.62 55.12 118.53 7.40 68.62

133 2762.2 10.77 17.87 1424.86 41.68 83.06 0.00 44.60 70.55 113.57 1437.18 606.54 67.37 166.75 10.82 100.97

246 12.9 0.55 4.78 82.23 0.76 39.54 0.00 2.52 7.50 45.04 1.56 10.24 10.17 26.55 2.00 12.06

142 2425.2 6.38 14.78 888.98 20.68 35.50 0.00 26.78 49.08 164.27 687.43 420.91 59.32 174.66 8.89 95.67

194 8.3 0.27 0.99 0.00 2.68 44.01 0.00 2.22 3.33 23.52 1.51 4.40 3.13 7.21 0.59 3.38

291 13.2 0.39 0.77 103.64 2.56 38.43 0.00 2.75 2.11 11.11 14.32 6.98 4.47 8.50 0.56 3.29

146 1884.7 6.47 14.82 383.02 20.68 56.46 0.00 17.61 38.73 64.23 972.73 439.44 65.50 141.29 8.80 74.27

142 6.3 0.75 1.01 336.52 0.00 27.88 0.57 7.33 2.67 58.02 1225.64 248.26 2.11 3.37 0.37 1.17

460 594.7 1.85 5.99 645.02 4.64 64.23 0.00 12.76 11.46 19.09 265.02 73.79 18.80 88.69 2.55 28.53

563 10.0 0.45 0.81 25.76 2.98 47.49 0.00 2.67 1.48 1.56 11.62 8.04 1.70 4.68 0.25 1.57

371 49.7 0.75 3.43 1780.37 2.81 48.19 0.00 23.85 3.10 32.76 129.57 52.42 12.72 31.57 1.71 11.18

BBOP Scotland 68


# Reference # MLC #

75 none S0075

76 00000001 S0076

77 00000002 S0077

78 00000003 S0078

79 00000004 S0079

80 00000005 S0080

81 00000006 S0081

82 00000007 S0082

83 00000008 S0083

84 00000009 S0084

85 00000010 S0085

86 00000011 S0086

87 00000012 S0087

88 00000013 S0088

89 00000014 S0089

90 00000015 S0090

91 00000016 S0091

92 00000017 S0092

93 00000018 S0093

94 00000019 S0094

95 00000020 S0095

96 00000021 S0096

97 00000022 S0097

98 00000023 S0098

99 00000024 S0099

100 00000025 S0100

mean

SD

min

max

range

N



630 1569.9 7.60 13.48 623.59 22.47 54.84 1.26 22.02 23.79 41.35 909.62 355.08 56.69 181.39 7.00 70.31

118 3.5 0.19 0.25 0.00 0.88 47.57 0.26 0.19 1.47 0.11 2.82 0.00 0.68 2.00 0.50 0.96

202 52.2 0.89 2.82 448.62 1.96 36.67 1.16 19.75 1.89 3.62 25.97 20.05 13.34 26.94 1.93 9.06

226 45.8 0.45 2.22 443.87 2.05 40.58 0.32 18.79 2.70 0.00 19.12 5.42 4.12 16.81 1.02 4.59

81 13.4 0.37 2.55 261.79 2.66 40.87 0.48 13.27 1.44 18.72 13.81 8.32 6.10 13.97 0.96 4.45

370 313.1 1.60 4.29 978.26 3.16 39.00 0.25 38.23 5.13 10.78 39.45 33.55 12.21 67.54 1.80 15.00

273 27.2 0.26 0.71 105.64 1.39 33.78 0.39 6.15 1.07 1.83 9.91 2.39 1.78 7.87 0.65 2.36

137 869.8 3.49 10.55 690.43 9.98 30.69 0.12 36.17 20.81 25.76 109.95 111.41 25.88 110.44 3.84 34.33

107 89.3 0.93 3.55 1384.54 2.08 88.90 0.24 53.11 2.65 4.80 39.94 12.68 13.02 39.39 1.64 10.48

174 9.6 0.13 0.25 0.00 0.74 93.74 0.07 0.00 0.77 0.00 0.88 0.00 0.67 1.54 0.31 0.68

259 9.6 0.27 0.60 83.57 1.12 55.90 0.12 4.53 1.15 1.17 3.55 3.22 1.66 6.12 0.46 1.81

256 2.0 0.12 0.27 0.00 0.90 35.36 0.07 0.00 0.94 1.14 1.79 0.00 0.67 2.00 0.34 0.78

357 9.5 0.13 0.32 0.00 0.76 31.75 0.20 0.42 0.86 1.19 6.16 2.83 0.56 3.88 0.42 1.31

148 5.0 0.54 0.48 0.00 1.12 37.17 0.17 1.42 1.16 7.82 3.13 0.14 0.78 2.91 0.42 1.09

321 697.2 5.63 12.74 1968.40 10.95 40.05 0.61 85.80 14.99 37.45 132.52 120.08 66.55 143.63 7.57 42.88

199 80.9 0.34 0.17 0.00 1.08 37.70 0.76 0.00 0.93 0.00 2.25 7.28 0.40 1.85 0.63 0.87

297 521.6 3.61 8.25 1529.22 7.44 36.62 0.58 62.04 7.33 28.03 77.20 86.80 29.87 125.44 3.69 30.17

360 376.6 1.92 6.93 632.80 5.33 24.29 0.46 28.20 9.22 8.59 49.74 60.08 19.76 109.59 2.88 23.19

261 350.1 2.75 9.97 1104.55 6.62 41.98 0.70 50.47 7.71 30.70 84.99 51.06 46.53 102.71 5.66 29.57

276 75.7 0.95 3.21 529.35 2.54 48.42 0.26 21.87 2.19 14.98 22.50 21.07 9.25 50.85 1.53 11.65

268 7.3 0.30 0.62 62.44 1.25 35.28 0.00 4.65 1.67 3.19 4.78 2.84 2.21 7.42 0.46 2.05

277 6.1 0.19 0.40 0.00 0.89 24.54 0.03 0.78 1.18 0.00 1.95 0.00 1.03 3.02 0.32 1.05

269 27.5 0.38 1.14 234.79 1.53 36.65 0.00 10.20 1.46 5.79 10.75 4.40 4.07 16.48 0.71 4.83

320 19.8 0.31 0.39 0.00 0.87 44.50 1.22 0.84 1.11 0.00 3.39 8.65 0.97 3.38 0.56 1.50

377 28.0 1.09 1.72 212.72 1.58 43.46 0.99 12.00 2.95 5.18 9.17 11.28 5.24 12.74 1.19 4.59

175 2.3 0.10 0.32 0.00 1.05 40.08 0.13 0.13 1.06 0.00 2.74 0.00 0.58 1.76 0.40 0.80


258 181.62 1.09 3.21 287.96 3.23 41.33 0.38 12.20 5.31 14.14 102.04 41.94 10.37 30.62 1.51 10.85

135 505.53 1.93 4.28 460.78 6.41 12.80 0.55 17.18 11.47 23.78 300.00 107.80 18.54 52.84 2.38 20.59

57 0.00 0.00 0.09 0.00 0.00 21.73 0.00 0.00 0.29 0.00 0.00 0.00 0.10 0.06 0.04 0.00

630 2762.22 10.77 19.80 1968.40 41.68 93.74 2.55 86.36 70.55 164.27 1910.86 606.54 91.91 286.69 11.24 100.97

573 2762.22 10.77 19.71 1968.40 41.68 72.01 2.55 86.36 70.25 164.27 1910.86 606.54 91.81 286.63 11.20 100.97

100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100

BBOP Scotland 69


# Reference # MLC #

1 S08030401 S0001

2 S08030402 S0002

3 S08030403 S0003

4 S08030404 S0004

5 S08030405 S0005

6 S08030406 S0006

7 S08030407 S0007

8 S08030408 S0008

9 S08030409 S0009

10 S08030410 S0010

11 S08030411 S0011

12 S08030412 S0012

13 S08030413 S0013

14 S08030414 S0014

15 S08030415 S0015

16 S08030416 S0016

17 S08030417 S0017

18 S08030418 S0018

19 S08030419 S0019

20 S08030420 S0020

21 S08090801 S0021

22 S08092501 S0022

23 S08091801 S0023

24 S08091601 S0024

25 S08101401 S0025

26 S08101402 S0026

27 S08101403 S0027

28 S08092502 S0028

29 S08091001 S0029

30 S08102401 S0030

31 S08031101 S0031

32 S09041401 S0032

33 S09051201 S0033

34 S09072701 S0034

35 S09072702 S0035

36 S09072703 S0036

37 S09072704 S0037

Sm 152 Eu 153 Gd 158 Tb 159 Dy 164 Ho 165 Er 166 Tm 169 Yb 174 Lu 175 Hf 180 Ta 181 W 184 Re 187 Ir 193 Pt 195 Hg 202


0.02 0.04 0.20 0.04 0.02 0.01 0.01 0.07 0.04 0.01 0.12 0.17 0.87 0.00 0.04 0.90 0.25

0.02 0.01 0.29 0.00 0.02 0.00 0.04 0.02 0.03 0.00 0.16 0.42 0.73 0.00 0.02 0.96 0.80

0.23 0.12 0.23 0.14 0.01 0.02 0.15 0.13 0.06 0.01 0.74 0.16 0.94 0.25 0.13 1.73 0.72

0.37 0.20 0.19 0.23 0.04 0.01 0.16 0.37 0.10 0.00 0.12 0.27 1.30 1.24 0.19 3.15 2.71

0.01 0.04 0.15 0.04 0.01 0.00 0.03 0.04 0.01 0.00 0.15 0.44 5.31 0.00 0.01 0.88 0.00

0.19 0.12 0.08 0.06 0.02 0.00 0.04 0.14 0.01 0.01 0.14 0.12 0.72 0.71 0.06 1.32 0.15

0.09 0.03 0.16 0.03 0.04 0.01 0.03 0.02 0.04 0.01 0.23 0.08 2.83 0.00 0.02 0.84 0.00

0.28 0.20 0.33 0.13 0.06 0.02 0.11 0.13 0.06 0.01 0.19 0.23 3.76 0.53 0.05 1.97 1.22

0.14 0.07 0.32 0.00 0.05 0.00 0.05 0.00 0.05 0.01 0.29 0.40 1.21 0.00 0.00 2.24 4.84

0.43 0.06 0.07 0.02 0.03 0.02 0.04 0.01 0.04 0.00 0.32 0.19 2.58 0.12 0.04 0.97 1.20

0.39 0.41 0.15 0.04 0.01 0.02 0.05 0.00 0.02 0.01 0.17 0.15 0.90 0.00 0.01 1.01 0.97

0.13 0.05 0.18 0.05 0.03 0.01 0.03 0.02 0.03 0.00 0.21 0.40 0.75 0.00 0.05 1.08 0.81

0.31 0.15 0.10 0.14 0.02 0.02 0.09 0.22 0.03 0.01 0.52 0.24 109.32 0.65 0.08 2.46 2.89

0.45 0.22 0.09 0.12 0.00 0.01 0.24 0.28 0.02 0.01 0.06 0.17 0.35 1.13 0.02 0.46 0.80

0.25 0.12 0.10 0.04 0.03 0.01 0.05 0.07 0.04 0.01 0.18 0.11 1.64 0.48 0.06 0.42 0.65

0.23 0.16 0.09 0.09 0.03 0.02 0.00 0.03 0.02 0.01 0.25 0.29 1.25 0.23 0.02 0.74 0.01

0.00 0.00 0.33 0.03 0.01 0.03 0.00 0.00 0.08 0.01 0.36 0.26 17.39 0.00 0.03 1.18 2.06

0.27 0.25 0.20 0.18 0.02 0.01 0.14 0.23 0.08 0.01 0.08 0.13 1.70 1.10 0.11 1.41 0.69

0.22 0.13 0.23 0.16 0.01 0.02 0.14 0.17 0.05 0.02 0.46 0.67 7.26 0.20 0.09 2.34 1.76

0.13 0.16 0.06 0.08 0.01 0.01 0.02 0.16 0.01 0.00 0.15 0.11 31.51 0.47 0.00 1.34 0.50

0.85 0.42 2.24 0.10 0.32 0.03 0.67 0.05 0.22 0.04 17.97 3.57 0.77 0.00 0.04 59.04 0.50

1.75 1.02 4.36 0.15 0.73 0.13 1.66 0.07 0.50 0.08 12.03 1.40 1.44 0.00 0.07 54.02 0.74

0.27 0.21 0.39 0.04 0.02 0.02 0.20 0.11 0.07 0.00 0.08 0.47 1.21 0.00 0.02 39.95 0.23

0.32 0.25 0.48 0.06 0.05 0.01 0.21 0.09 0.05 0.02 1.19 0.55 0.02 0.00 0.03 43.39 0.71

0.48 0.22 0.96 0.09 0.20 0.03 0.34 0.07 0.15 0.02 2.64 1.47 0.33 0.00 0.04 53.58 0.32

1.23 0.59 3.39 0.21 0.60 0.10 0.99 0.13 0.29 0.07 8.63 0.55 0.02 0.00 0.07 0.34 0.80

0.31 0.19 0.84 0.07 0.18 0.04 0.24 0.04 0.12 0.02 1.04 0.96 0.02 0.00 0.03 36.19 0.00

4.30 2.40 9.82 0.27 1.02 0.15 4.25 0.15 0.63 0.10 34.48 0.78 1.49 0.00 0.15 50.60 0.00

0.91 0.58 2.84 0.16 0.78 0.17 1.14 0.10 0.56 0.08 6.61 1.86 0.96 0.01 0.12 73.07 0.00

0.45 0.23 0.66 0.06 0.08 0.02 0.41 0.11 0.06 0.01 3.09 0.55 0.02 0.00 0.08 37.53 0.00

4.13 2.41 5.81 0.48 0.55 0.11 1.68 0.00 0.35 0.14 7.95 0.56 1.67 0.00 0.33 0.00 1.12

0.93 0.54 0.61 0.34 0.03 0.03 0.63 0.11 0.16 0.06 0.76 0.53 1.19 0.00 0.07 0.00 1.49

3.00 1.75 4.48 0.49 0.45 0.07 1.56 0.04 0.31 0.10 6.36 0.51 0.30 0.00 0.28 0.00 0.10

1.43 0.81 1.27 0.16 0.25 0.06 0.43 0.21 0.19 0.01 0.14 0.13 12.66 0.57 0.04 4.51 0.14

6.51 3.77 4.16 0.44 0.62 0.08 0.98 0.19 0.26 0.09 1.45 0.02 2.08 0.28 0.08 0.00 0.00

0.60 0.28 0.90 0.17 0.51 0.12 0.53 0.16 0.42 0.04 0.44 1.81 13.23 0.25 0.06 5.23 0.97

1.90 1.21 1.20 0.20 0.33 0.08 0.47 0.21 0.23 0.01 0.10 0.13 8.38 0.50 0.00 6.69 0.78

BBOP Scotland 70


# Reference # MLC #

38 S09072705 S0038

39 S09072706 S0039

40 S09072707 S0040

41 S09072708 S0041

42 S09072709 S0042

43 S09072710 S0043

44 S09072711 S0044

45 S09072712 S0045

46 S09072713 S0046

47 S09072714 S0047

48 S09072715 S0048

49 S09072716 S0049

50 S09072717 S0050

51 S09072718 S0051

52 none S0052

53 none S0053

54 none S0054

55 none S0055

56 none S0056

57 none S0057

58 none S0058

59 none S0059

60 none S0060

61 none S0061

62 none S0062

63 none S0063

64 none S0064

65 none S0065

66 none S0066

67 none S0067

68 none S0068

69 none S0069

70 none S0070

71 none S0071

72 none S0072

73 none S0073

74 none S0074



12.95 7.23 19.13 1.24 2.29 0.20 4.09 0.32 0.82 0.09 12.77 1.67 6.96 0.50 0.32 7.84 0.84

1.58 0.90 2.01 0.19 0.31 0.06 0.52 0.20 0.24 0.02 0.29 0.23 6.27 0.36 0.09 6.01 1.10

1.15 0.65 1.02 0.17 0.27 0.03 0.37 0.08 0.22 0.02 0.41 0.02 4.79 0.00 0.00 1.27 0.01

0.68 0.28 2.95 0.47 0.28 0.04 0.32 0.00 0.21 0.03 0.18 0.32 3.28 0.00 0.02 13.16 0.00

6.31 3.88 2.84 0.21 0.33 0.04 0.83 0.11 0.20 0.09 1.37 0.10 18.74 0.24 0.00 2.38 0.79

1.01 0.57 0.94 0.16 0.22 0.04 0.31 0.11 0.15 0.00 0.00 0.16 4.13 0.23 0.01 3.73 0.61

0.55 0.27 0.72 0.13 0.19 0.06 0.25 0.17 0.15 0.00 0.00 0.33 0.98 0.31 0.13 4.99 0.96

12.38 7.16 9.80 0.55 1.08 0.14 3.37 0.15 0.56 0.08 5.00 0.31 10.22 0.03 0.15 4.22 0.68

0.85 0.51 1.49 0.27 0.32 0.08 0.31 0.00 0.20 0.15 0.24 0.22 1.39 0.00 0.06 23.62 0.27

1.74 1.05 1.68 0.25 0.38 0.08 0.48 0.19 0.23 0.02 0.29 0.22 2.72 0.34 0.00 5.93 1.20

47.04 27.01 65.40 2.97 5.44 0.52 9.07 0.22 2.10 0.38 32.00 0.65 8.33 0.00 0.72 9.91 0.00

1.26 0.73 1.74 0.23 0.43 0.09 0.54 0.26 0.34 0.05 0.16 0.22 2.54 0.58 0.05 2.85 0.00

12.00 6.89 18.00 1.18 2.18 0.21 3.84 0.22 0.90 0.14 15.69 0.42 3.13 0.18 0.34 5.87 0.08

12.01 7.73 10.21 0.71 0.82 0.12 2.15 0.00 0.43 0.08 2.94 0.40 0.49 0.00 0.15 11.19 0.00

0.14 0.09 0.14 0.12 0.18 0.04 0.14 0.12 0.15 0.00 1.51 0.42 12.93 0.56 0.08 4.13 2.82

0.32 0.19 1.09 0.18 0.10 0.02 0.89 0.00 0.07 0.02 1.40 0.14 53.35 0.00 0.00 3.72 1.79

0.31 0.28 0.00 0.10 0.01 0.01 0.04 0.07 0.04 0.04 0.68 0.12 83.42 0.17 0.00 2.41 2.21

0.27 0.16 0.26 0.12 0.07 0.01 0.11 0.09 0.08 0.00 0.63 0.18 23.83 0.43 0.04 3.55 1.53

3.65 1.83 11.34 0.40 1.11 0.24 1.72 0.14 0.95 0.13 28.45 0.48 23.67 0.00 0.00 3.88 2.00

1.88 0.96 5.57 0.23 0.56 0.12 0.97 0.04 0.45 0.15 10.30 0.27 4.77 0.00 0.00 1.75 0.19

0.24 0.14 0.14 0.08 0.01 0.00 0.01 0.06 0.05 0.00 0.22 0.75 5.11 0.26 0.08 4.07 0.38

0.58 0.33 0.99 0.08 0.21 0.03 1.31 0.08 0.17 0.00 6.91 0.20 1.86 0.63 0.24 4.96 0.71

0.26 0.13 0.37 0.06 0.13 0.01 0.56 0.13 0.07 0.00 2.49 0.21 2.00 0.72 0.13 5.82 1.00

0.25 0.13 0.10 0.06 0.03 0.01 0.18 0.09 0.04 0.00 0.71 0.13 2.77 0.63 0.17 5.89 0.54

0.21 0.14 0.00 0.09 0.02 0.00 0.09 0.10 0.05 0.00 1.43 0.12 7.00 0.79 0.21 5.41 0.46

20.43 13.20 14.57 0.45 4.83 0.33 66.63 0.27 1.47 0.25 38.15 0.77 3.64 0.52 0.36 5.07 0.44

10.20 6.25 17.63 0.54 1.76 0.37 2.83 0.28 1.40 0.30 30.28 1.90 8.39 0.21 0.00 0.00 1.07

25.03 16.81 25.94 0.61 4.56 0.53 39.75 0.36 2.31 0.39 54.15 2.56 23.65 0.79 0.72 5.72 1.19

1.61 0.39 2.54 0.27 0.92 0.14 0.54 0.18 0.45 0.00 2.31 0.10 5.16 1.30 0.81 8.16 0.54

17.80 10.76 22.25 0.59 3.43 0.45 23.50 0.30 1.76 0.26 40.58 0.85 9.00 0.44 0.51 2.94 0.57

0.40 0.10 0.66 0.09 0.17 0.04 0.13 0.07 0.13 0.00 0.33 0.13 6.54 0.61 0.32 5.60 1.24

0.40 0.14 0.52 0.09 0.13 0.02 0.32 0.07 0.13 0.00 2.11 0.23 11.03 0.47 0.61 4.16 2.02

20.30 12.58 20.59 0.61 3.76 0.40 35.55 0.24 1.61 0.28 33.08 6.20 8.61 0.19 0.22 2.73 0.17

10.23 7.17 0.07 0.02 1.68 0.04 32.15 0.10 0.11 0.04 2.46 0.10 16.46 0.12 0.00 0.00 0.95

3.88 2.12 7.43 0.29 1.03 0.17 6.10 0.15 0.69 0.12 14.59 0.40 101.97 0.35 0.16 2.92 2.63

0.29 0.20 0.36 0.10 0.14 0.04 0.39 0.09 0.10 0.00 1.00 0.38 6.23 0.62 0.32 4.13 1.22

2.43 1.50 2.55 0.20 0.64 0.10 3.16 0.12 0.51 0.12 20.36 0.22 7.75 0.42 0.03 1.78 1.66

BBOP Scotland 71


# Reference # MLC #

75 none S0075

76 00000001 S0076

77 00000002 S0077

78 00000003 S0078

79 00000004 S0079

80 00000005 S0080

81 00000006 S0081

82 00000007 S0082

83 00000008 S0083

84 00000009 S0084

85 00000010 S0085

86 00000011 S0086

87 00000012 S0087

88 00000013 S0088

89 00000014 S0089

90 00000015 S0090

91 00000016 S0091

92 00000017 S0092

93 00000018 S0093

94 00000019 S0094

95 00000020 S0095

96 00000021 S0096

97 00000022 S0097

98 00000023 S0098

99 00000024 S0099

100 00000025 S0100

mean

SD

min

max

range

N



17.01 10.81 16.98 0.54 2.72 0.37 21.89 0.20 1.46 0.29 35.67 0.89 5.08 0.00 0.00 2.14 0.68

0.56 0.31 0.39 0.10 0.04 0.02 0.33 0.23 0.11 0.02 0.21 0.76 0.13 0.00 0.02 0.93 0.65

2.73 1.52 6.52 0.41 0.54 0.07 0.71 0.02 0.37 0.08 6.15 1.63 1.66 0.00 0.13 0.68 0.48

1.82 1.07 3.62 0.26 0.30 0.06 0.58 0.06 0.31 0.06 5.27 1.52 0.55 0.00 0.19 0.72 0.18

1.98 1.18 3.15 0.23 0.31 0.08 0.70 0.26 0.31 0.06 4.36 1.59 2.42 0.56 0.03 0.59 0.72

7.05 4.61 13.82 0.42 0.72 0.11 1.52 0.24 0.52 0.09 9.62 1.52 1.06 0.00 0.17 0.95 0.37

1.06 0.65 1.70 0.20 0.12 0.03 0.37 0.17 0.18 0.04 2.05 1.24 1.73 0.12 0.04 0.62 1.41

15.85 9.43 20.82 0.62 1.73 0.29 2.99 0.25 1.20 0.21 23.48 2.87 3.00 0.00 0.25 2.08 0.36

4.02 2.25 8.50 0.33 0.67 0.10 1.09 0.26 0.43 0.08 14.46 1.39 2.46 0.20 0.18 1.40 0.70

0.47 0.35 0.44 0.10 0.03 0.02 0.31 0.30 0.09 0.03 0.44 0.57 0.67 0.80 0.00 0.00 2.27

0.90 0.54 1.28 0.13 0.10 0.03 0.27 0.16 0.11 0.02 1.20 1.04 0.54 0.26 0.04 0.70 1.18

0.47 0.35 0.47 0.15 0.05 0.02 0.34 0.34 0.10 0.02 0.38 0.55 1.01 0.71 0.00 0.11 1.34

0.62 0.32 0.81 0.12 0.05 0.02 0.25 0.21 0.12 0.02 0.63 0.91 0.69 0.25 0.00 1.03 0.63

0.66 0.38 0.59 0.13 0.04 0.02 0.35 0.27 0.13 0.02 0.79 1.03 4.18 0.47 0.00 0.55 0.59

23.36 13.95 33.02 1.41 2.81 0.36 4.03 0.42 1.51 0.27 38.16 1.95 4.27 0.54 0.41 1.03 1.34

0.40 0.23 0.47 0.16 0.02 0.01 0.17 0.00 0.11 0.03 0.41 0.73 1.89 0.00 0.06 1.77 0.46

16.07 8.74 26.54 0.82 1.69 0.23 2.79 0.23 1.02 0.17 22.97 1.70 3.39 0.05 0.32 1.25 0.67

12.17 7.61 22.49 0.62 1.27 0.18 2.16 0.41 0.74 0.17 11.91 1.03 5.63 0.92 0.09 0.00 1.06

10.41 6.74 22.36 1.12 1.84 0.24 2.98 0.25 1.11 0.19 27.63 1.96 13.00 0.00 0.42 0.86 1.22

4.22 2.63 10.29 0.34 0.57 0.10 1.45 0.27 0.39 0.07 8.04 23.29 10.73 0.37 0.09 0.93 0.99

0.72 0.51 1.61 0.14 0.15 0.03 0.44 0.28 0.13 0.03 2.31 1.15 12.82 0.57 0.00 0.01 1.11

0.68 0.43 0.72 0.11 0.05 0.02 0.48 0.31 0.10 0.03 0.74 0.69 5.67 0.92 0.00 0.00 0.51

1.21 0.68 2.90 0.14 0.20 0.04 0.44 0.18 0.18 0.02 4.03 1.02 74.00 0.15 0.07 2.47 2.42

0.55 0.32 0.68 0.20 0.05 0.04 0.35 0.07 0.13 0.04 0.82 0.94 5.47 0.00 0.08 1.16 0.78

1.71 0.94 3.13 0.33 0.34 0.05 0.67 0.15 0.29 0.05 3.63 1.31 29.15 0.00 0.06 0.44 1.23

0.45 0.23 0.39 0.11 0.03 0.02 0.26 0.20 0.09 0.02 0.40 0.86 8.93 0.20 0.00 0.64 1.45


3.93 2.37 5.25 0.28 0.64 0.09 3.09 0.15 0.36 0.06 7.01 0.97 9.41 0.29 0.12 7.06 0.90

7.22 4.37 9.53 0.38 1.07 0.12 9.36 0.10 0.48 0.09 11.60 2.42 18.98 0.32 0.17 14.27 0.80

0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.01 0.00 0.00 0.02 0.02 0.00 0.00 0.00 0.00

47.04 27.01 65.40 2.97 5.44 0.53 66.63 0.42 2.31 0.39 54.15 23.29 109.32 1.30 0.81 73.07 4.84

47.04 27.01 65.40 2.97 5.43 0.54 66.63 0.42 2.31 0.39 54.15 23.27 109.30 1.30 0.81 73.07 4.84

100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100

BBOP Scotland 72


Passport Number


1 W08022101 W0001 whole meat St Merryn 53°19'1.06"N 3°18 '47.04"W 21/02/2008 UK707244500779 Blonde D'Aquitaine X M 21/09/2005

2 W08022102 W0002 whole meat St Merryn 53°19'1.06"N 3°18 '47.04"W 21/02/2008 UK707244500793 Blonde D'Aquitaine X M 11/11/20053 W08022103 W0003 whole meat St Merryn 52°55'56.47"N 3° 5'51.62"W 21/02/2008 UK700012700611 Holstein Friesian M 19/06/20064 W08022104 W0004 whole meat St Merryn 52° 1'17.30"N 3°15 '43.70"W 21/02/2008 UK720071200068 Limousin X M 17/09/20055 W08022105 W0005 whole meat St Merryn 52° 1'17.30"N 3°15 '43.70"W 21/02/2008 UK720616600056 Charolais X M 13/10/20056 W08022106 W0006 whole meat St Merryn 52° 1'17.30"N 3°15 '43.70"W 21/02/2008 UK720667500185 Limousin X M 28/08/20057 W08022701 W0007 whole meat Llanidloes, Powys 51°53'11. 39"N 4°31'53.72"W 27/02/2008 UK740254500502 Charolais X F 03/07/20068 W08022702 W0008 whole meat Llanidloes, Powys 52°24'26. 97"N 3°32'34.74"W 27/02/2008 UK701202200347 Charolais M 29/07/20069 W08022703 W0009 whole meat Llanidloes, Powys 52°31'12. 08"N 3°17'10.47"W 27/02/2008 UK701564300078 Simmental M 16/10/2006

10 W08022704 W0010 whole meat Llanidloes, Powys 51°53'11 .39"N 4°31'53.72"W 27/02/2008 UK740254400508 Charolais X F 10/07/200611 W08022705 W0011 whole meat Llanidloes, Powys 51°53'11 .39"N 4°31'53.72"W 27/02/2008 UK740254100484 Charolais X F 29/04/2006

12 W08022706 W0012 whole meat Llanidloes, Powys 51°53'11 .39"N 4°31'53.72"W 27/02/2008 UK720718100297 Blonde D'Aquitaine X M 18/04/200613 W08030301 W0014 whole meat Conway Valley Meats 53°14 '56.56"N 3°19'23.75"W 03/03/2008 UK705249700151 Charolais X F 25/09/200515 W08030303 W0016 whole meat Conway Valley Meats 53°17' 58.99"N 3°47'6.94"W 04/03/2008 UK702358600185 Charolais X M 12/12/200516 W08030304 W0017 whole meat Conway Valley Meats 53° 3' 44.30"N 3°44'37.16"W 04/03/2008 UK704981600272 Beef Sho rthorn M 01/02/200617 W08030305 W0018 whole meat Conway Valley Meats 53°12' 20.02"N 3°46'57.32"W 04/03/2008 UK704898100052 Welsh Bl ack M 14/09/200518 W08050601 W0020 whole meat Conwy Valley Meats 53°11'4 1.79"N 3°14'5.42"W 06/05/2008 UK705446300268 Charolais X F 14/12/200519 W08050602 W0021 whole meat Conwy Valley Meats 53° 2'5 1.97"N 3°23'21.97"W 06/05/2008 UK705071400709 Limousin F 10/01/200620 W08050603 W0022 whole meat Conwy Valley Meats 53°16'2 7.13"N 3°15'56.11"W 06/05/2008 UK701771300632 Limousin X F 12/01/200621 W08050701 W0024 whole meat Conwy Valley Meats 53° 2'2 .85"N 3°15'43.90"W 07/05/2008 UK705695700056 Limousin X F 25/03/200622 W08050702 W0025 whole meat Conwy Valley Meats 53° 9'5 9.56"N 3°35'11.64"W 07/05/2008 UK705977400302 Belgian B lue F 04/02/200623 W08050703 W0026 whole meat Conwy Valley Meats 53°11' 28.27"N 3°26'12.73"W 07/05/2008 UK721428700260 Charolai s X F 11/02/200624 W08050704 W0027 whole meat Conwy Valley Meats 53° 3'4 4.30"N 3°44'37.16"W 07/05/2008 UK704946500173 Charolais X M 13/05/2006

25 W08052201 W0028 whole meat St Merryn Meats 52°14'49.4 4"N 3°24'13.43"W 22/05/2008 UK305012300018 Charolais X F 05/05/2006

26 W08052202 W0029 whole meat St Merryn Meats 53°12'21.0 8"N 3°16'38.87"W 22/05/2008 UK707206200644 Holstein Fri esian M 01/03/200627 W08052203 W0030 whole meat St Merryn Meats 52°14'49.4 4"N 3°24'13.43"W 22/05/2008 UK305012200017 Charolais X F 01/05/200628 W08052204 W0031 whole meat St Merryn Meats 52°14'49.4 4"N 3°24'13.43"W 22/05/2008 UK305012700015 Charolais X F 29/04/200629 W08052205 W0032 whole meat St Merryn Meats 52°14'49.4 4"N 3°24'13.43"W 22/05/2008 UK160292100215 Simmental X M 21/04/200630 W08052206 W0033 whole meat St Merryn Meats 53°19'1.06 "N 3°18'47.04"W 22/05/2008 UK707244500800 Blonde D'Aqu itaine X F 12/12/200531 W08052207 W0034 whole meat St Merryn Meats 51°28'13.5 4"N 3°37'26.48"W 22/05/2008 UK720309100459 Limousin X F 0 2/07/200632 W08052208 W0035 whole meat St Merryn Meats 51°28'13.5 4"N 3°37'26.48"W 22/05/2008 UK722312100139 Limousin X M 0 1/06/200633 W08052209 W0036 whole meat St Merryn Meats 51°28'13.5 4"N 3°37'26.48"W 22/05/2008 UK722312400142 Limousin X F 1 2/07/200634 W08052210 W0037 whole meat St Merryn Meats 53°19'1.06 "N 3°18'47.04"W 22/05/2008 UK707244200804 Blonde D'Aqu itaine X F 28/12/200535 W08073101 W0038 whole meat Conwy Valley Meats 53°16'7 .11"N 4°12'25.83"W 31/07/2008 UK743633600254 South Devo n X M 07/05/200636 W08073102 W0039 whole meat Conwy Valley Meats 53° 5'3 2.27"N 3°47'19.18"W 31/07/2008 UK701956700292 Limousin X F 08/04/200637 W08073103 W0040 whole meat Conwy Valley Meats 53° 7'5 8.53"N 3°44'58.70"W 31/07/2008 UK722846200207 Simmental X M 31/01/200638 W08073104 W0041 whole meat Conwy Valley Meats 53° 7'5 8.53"N 3°44'58.70"W 31/07/2008 UK722131100295 Limousin X F 03/04/200639 W08073105 W0042 whole meat Conwy Valley Meats 53° 7'8 .25"N 3°44'20.88"W 31/07/2008 UK710804700012 Salers F 10/ 08/2006

BBOP Wales Page 73


Passport Number

# Reference # MLC # Form Abattoir origin LAT LONG Date sam pled Ear Tag Number Breed Gender Born40 W08090301 W0043 whole meat Llanidloes 52°29'18.50"N 3° 30'16.10"W 03/09/2008 UK701295500333 Charolais X F 04/09/200641 W08090302 W0044 whole meat Llanidloes 52°29'18.50"N 3° 30'16.10"W 03/09/2008 UK743308400288 Aberdeen Angus X F 09/03/200642 W08090303 W0045 whole meat Llanidloes 52°21'26.11"N 3 °28'35.72"W 03/09/2008 UK742861100448 Holstein Friesia n M 26/05/200743 W08090304 W0046 whole meat Llanidloes 52°21'58.30"N 3° 28'49.70"W 03/09/2008 UK721648200002 Charolais X M 29/03/200744 W08090201 W0048 whole meat Llanidloes 52°14'47.13"N 3° 23'32.02"W 02/09/2008 UK721020200545 Limousin X M 16/09/200645 W08090202 W0049 whole meat Llanidloes 52°26'28.65"N 3° 34'47.76"W 02/09/2008 UK701226300802 Charolais X F 10/03/200746 W08090203 W0050 whole meat Llanidloes 52°27'31.22"N 3° 33'35.22"W 02/09/2008 UK701226300844 Charolais X M 09/05/200747 W08091001 W0051 whole meat Merthyr Tydfil 51°31'14.96 "N 3°40'17.93"W 10/09/2008 UK722396400660 Belgian Blue X F 07/05/200648 W08091002 W0052 whole meat Merthyr Tydfil 51°31'14.96 "N 3°40'17.93"W 10/09/2008 UK722396400709 Limousin X M 19 /11/200649 W08091003 W0053 whole meat Merthyr Tydfil 51°31'14.96 "N 3°40'17.93"W 10/09/2008 UK722396600711 Limousin X M 20 /11/200650 W08091004 W0054 whole meat Merthyr Tydfil 51°31'14.96 "N 3°40'17.93"W 10/09/2008 UK722396400688 Limousin X M 04 /09/200651 W08091005 W0055 whole meat Merthyr Tydfil 51°31'14.96 "N 3°40'17.93"W 10/09/2008 UK722396200658 Belgian Blue X M 04/05/200652 W08091006 W0056 whole meat Merthyr Tydfil 10/09/2008 UK702868400104 Limousin X F 10/04/200653 W08091007 W0057 whole meat Merthyr Tydfil 10/09/2008 UK706886701234 Hereford X M 30/11/200654 W08091008 W0058 whole meat Merthyr Tydfil 10/09/2008 UK706056202194 Charolais X M 28/05/200655 W08110401 W0059 whole meat Conway Valley Meats 53° 3' 44.30"N 3°44'37.16"W 04/11/2008 UK702534100413 Welsh Bl ack F 08/05/200656 W08110402 W0060 whole meat Conway Valley Meats 53° 7' 36.36"N 3°46'50.20"W 04/11/2008 UK705013500118 Charola is X F 01/01/200757 W08110403 W0061 whole meat Conway Valley Meats 53°16' 39.62"N 4°29'58.80"W 04/11/2008 UK703591600516 Limousin X M 24/07/200658 W08110404 W0062 whole meat Conway Valley Meats 53°16' 34.97"N 4°34'32.11"W 04/11/2008 UK703880100298 Simmenta l X M 29/09/200659 W08110405 W0063 whole meat Conway Valley Meats 52°53' 46.41"N 4°33'21.68"W 04/11/2008 UK702796600088 Limousin X M 24/08/200660 W08111401 W0064 whole meat Merthyr Tydfil 51°54'45.62 "N 3°17'12.62"W 14/11/2008 UK720499500486 Limousin X F 11 /09/200661 W08111402 W0065 whole meat Merthyr Tydfil 51°57'2.24" N 3°25'35.80"W 14/11/2008 UK740166301346 Limousin X F 09/ 11/200662 W08111403 W0066 whole meat Merthyr Tydfil 51°57'2.24" N 3°25'35.80"W 14/11/2008 UK740088100901 Limousin F 23/05 /200663 W08111404 W0067 whole meat Merthyr Tydfil 51°57'2.24" N 3°25'35.80"W 14/11/2008 UK746163100612 Limousin X F 28/ 10/2006

64 W08111405 W0068 whole meat Merthyr Tydfil 51°24'44.20 "N 3°12'21.40"W 14/11/2008 UK722125700198 Limousin X F 05 /06/200665 W08111406 W0069 whole meat Merthyr Tydfil 51°24'44.20 "N 3°12'21.40"W 14/11/2008 UK721770700538 Simmental X F 1 4/04/200766 W08111407 W0070 whole meat Merthyr Tydfil 51°24'44.20 "N 3°12'21.40"W 14/11/2008 UK723394400724 Limousin X M 22 /06/200667 W08111408 W0071 whole meat Merthyr Tydfil 51°24'44.20 "N 3°12'21.40"W 14/11/2008 UK722134600201 Aberdeen Angu s F 30/04/200768 W08111409 W0072 whole meat Merthyr Tydfil 51°24'44.20 "N 3°12'21.40"W 14/11/2008 UK721669300115 Blonde D'Aqui taine X M 16/05/200669 W08111410 W0073 whole meat Merthyr Tydfil 51°24'44.20 "N 3°12'21.40"W 14/11/2008 UK721669700119 Blonde D'Aqui taine X M 09/08/200670 W08111411 W0074 whole meat Merthyr Tydfil 53°12'21.08 "N 3°16'38.87"W 14/11/2008 UK705801400524 British Fries ian M 06/07/200671 W08111412 W0075 whole meat Merthyr Tydfil 53°12'21.08 "N 3°16'38.87"W 14/11/2008 UK160435300601 Holstein M 17/0 5/200689 W09052703 W0093 whole meat Merthyr Tydfil 51°44'57.20 "N 5° 6'3.05"W 27/05/2009 UK746416200097 Simmental X M 23 /12/2006

90 W09052704 W0094 whole meat Merthyr Tydfil 51°44'57.20 "N 5° 6'3.05"W 27/05/2009 UK746454500015 Welsh Black X F 10/08/200791 W09052705 W0095 whole meat Merthyr Tydfil 51°44'57.20 "N 5° 6'3.05"W 27/05/2009 UK742679600628 Limousin X M 12/ 02/200792 W09052706 W0096 whole meat Merthyr Tydfil 51°44'57.20 "N 5° 6'3.05"W 27/05/2009 UK746562100150 Limousin X F 01/ 07/2007

93 05020801 0117 whole meat Cheshire, England 51°53'47.4 4"N 3° 6'21.03"W 08/02/2005 UK720191100223 Blonde D'Aqu itaine X ?? ??

93 W09052707 W0097 whole meat Merthyr Tydfil 51°44'57.20 "N 5° 6'3.05"W 27/05/2009 UK722882400316 British Friesi an M 03/04/2007

BBOP Wales Page 74


Passport Number

# Reference # MLC # Form Abattoir origin LAT LONG Date sam pled Ear Tag Number Breed Gender Born94 05020802 0118 whole meat Cheshire, England 52°23'7.80 "N 3° 4'59.58"W 08/02/2005 UK303532600224 Charolais X ?? ??94 W09052708 W0098 whole meat Merthyr Tydfil 51°44'57.20 "N 5° 6'3.05"W 27/05/2009 UK744632200176 Limousin X F 15/ 04/2007

95 05020803 0119 whole meat Cheshire, England 52° 9'6.06 "N 4° 7'31.77"W 08/02/2005 UK748776400080 Blonde D'Aqui taine X ?? ??

95 W09052709 W0099 whole meat Merthyr Tydfil 51°44'57.20 "N 5° 6'3.05"W 27/05/2009 UK745006300092 Limousin X M 02/ 02/2007

96 W09052710 W0100 whole meat Merthyr Tydfil 51°44'57.20 "N 5° 6'3.05"W 27/05/2009 UK744632300177 Belgian Blue X F 19/04/2007

97 W09052711 W0101 whole meat Merthyr Tydfil 51°44'57.20 "N 5° 6'3.05"W 27/05/2009 UK722826400239 Limousin X F 31/ 05/2007

98 W09052712 W0102 whole meat Merthyr Tydfil 51°44'57.20 "N 5° 6'3.05"W 27/05/2009 UK742951500646 Simmental F 19/1 2/2006

99 W09052713 W0103 whole meat Merthyr Tydfil 51°44'57.20 "N 5° 6'3.05"W 27/05/2009 UK745815300408 Limousin X M 13/ 05/2007

136 05042801 0183 whole meat Cheshire, England 52°31'37. 57"N 3° 1'8.64"W 28/04/2005 UK303433200282 Limousin X F 2 8/04/2005


217 05081610 0271 whole meat Cheshire, England 16/08/2005 UK704194400341 Charolais X F 26/06/2003


219 05081612 0273 whole meat Cheshire, England 53°10'45. 56"N 4° 9'5.16"W 16/08/2005 UK703805100295 Hereford X F 1 0/07/2003


237 05082401 0291 whole meat Shropshire, England 53°15'5 9.70"N 4°10'38.34"W 24/08/2005 UK702346500300 Limousin X F 02/03/2003

238 05082402 0292 whole meat Shropshire, England 53°24'4 4.09"N 4°22'58.82"W 24/08/2005 UK703668300254 Charolais X M 07/05/2003

309 05110801 0551 whole meat Cheshire, England 53°15'59. 70"N 4°10'38.34"W 08/11/2005 UK703273400431 Charolais X F 09/05/2003

310 05110802 0552 whole meat Cheshire, England 53°15'59. 70"N 4°10'38.34"W 08/11/2005 UK703273200443 Charolais X F 14/05/2003


312 05110804 0554 whole meat Cheshire, England 52°55'9.2 4"N 4°24'31.11"W 08/11/2005 UK702865200068 Charolais X F 29/04/2004

491 06083005 0986 whole meat Shropshire, England 53°14'4 6.18"N 4° 9'37.20"W 30/08/2006 UK703196500292 Limousin X M 05/05/2004

492 06083006 0987 whole meat Shropshire, England 53°14'4 6.18"N 4° 9'37.20"W 30/08/2006 UK340470500047 Simmental X M 13/08/2004


494 06083008 0989 whole meat Shropshire, England 53°14'4 6.18"N 4° 9'37.20"W 30/08/2006 UK340175500472 Charolais X M 21/05/2004


meanSD

minmax

rangeN

BBOP Wales Page 75


# Reference # MLC #

1 W08022101 W0001

2 W08022102 W00023 W08022103 W00034 W08022104 W00045 W08022105 W00056 W08022106 W00067 W08022701 W00078 W08022702 W00089 W08022703 W0009

10 W08022704 W001011 W08022705 W0011

12 W08022706 W001213 W08030301 W001415 W08030303 W001616 W08030304 W001717 W08030305 W001818 W08050601 W002019 W08050602 W002120 W08050603 W002221 W08050701 W002422 W08050702 W002523 W08050703 W002624 W08050704 W0027

25 W08052201 W0028

26 W08052202 W002927 W08052203 W003028 W08052204 W003129 W08052205 W003230 W08052206 W003331 W08052207 W003432 W08052208 W003533 W08052209 W003634 W08052210 W003735 W08073101 W003836 W08073102 W003937 W08073103 W004038 W08073104 W004139 W08073105 W0042

Protein SD/AD Protein SD/AD Protein SD/AD Protein SD/AD 87/ 86Sr 2SD(abs) Na 23 Mg 24 Al 27 P 31

d2H [‰] [‰] n d13C [‰] [‰] n d15N [‰] [‰] n d34S [‰] [‰] n [‰] [ ug/kg] [ug/kg] [ug/kg] [ug/kg]

-101.4 0.91 3 -26.05 0.04 3 6.51 0.08 3 5.4 0.2 3 0.709824 0.000068 2675591 955860 805 7778242

-99.1 0.97 3 -25.96 0.03 3 7.25 0.08 3 5.7 0.2 3 0.709935 0.000031 3156035 791963 1209 6675028-97.1 0.75 3 -24.21 0.02 3 7.55 0.04 3 5.1 0.1 3 0.710380 0.000087 3041420 875845 1781 7241675-92.3 1.87 3 -25.95 0.01 3 7.16 0.05 3 7.0 0.2 3 0.711979 0.000049 3896159 894495 1801 7561578-97.7 1.24 3 -26.17 0.02 3 7.28 0.05 3 2.7 0.3 3 0.710412 0.000071 2480581 900283 741 7878404-95.0 2.73 3 -26.16 0.01 3 6.84 0.05 3 6.7 0.5 3 0.708804 0.000031 2600981 930142 602 7954792-96.5 1.12 3 -26.67 0.02 3 8.27 0.02 3 6.9 0.2 3 0.707460 0.000055 2615846 822081 1112 6645958-93.9 1.47 3 -25.84 0.02 3 7.19 0.04 3 6.6 0.2 3 0.709908 0.000035 2297007 842953 720 7177636-99.9 2.56 3 -25.80 0.02 3 7.07 0.14 3 7.3 0.9 3 0.711568 0.000060 3214459 871032 4057 7155191-99.9 1.59 3 -26.76 0.03 3 8.68 0.09 3 6.4 0.3 3 0.707229 0.000093 2142043 857067 672 6859725-98.0 1.91 3 -26.67 0.09 3 8.33 0.02 3 4.5 0.3 3 0.707114 0.000057 2748564 906896 1155 7376076

-96.4 1.23 3 -26.28 0.03 3 8.99 0.04 3 4.5 0.3 3 0.707615 0.000064 3305671 914734 630 7407302-102.5 1.32 3 -27.44 0.01 3 8.59 0.11 3 6.2 0.0 3 0.710631 0.000029 2291917 814868 784 6761924-95.4 0.92 3 -25.66 0.01 3 8.36 0.10 3 5.9 0.1 3 0.709744 0.000083 2179757 957027 746 8054118-97.7 2.47 3 -25.98 0.03 3 7.20 0.03 3 6.5 0.0 3 0.710444 0.000039 1741555 807267 2292 6698304-96.7 0.95 3 -26.08 0.26 3 7.97 0.04 3 6.2 0.0 3 0.709555 0.000040 2691416 873670 2835 7841973-99.9 1.78 3 -24.59 0.03 3 7.33 0.03 3 4.7 0.2 3 0.711509 0.000123 2409433 897455 2545 7520853-98.9 1.23 3 -25.00 0.01 3 8.91 0.02 3 5.2 0.1 3 0.709473 0.000089 2505659 982134 4535 8033155

-100.8 0.49 3 -26.46 0.02 3 9.71 0.01 3 5.8 0.1 3 0.709431 0.000088 2883863 848562 4773 7077335-99.6 0.38 3 -26.30 0.02 3 7.40 0.05 3 6.0 0.2 3 0.710153 0.000090 2311911 943664 2038 7383421

-101.7 0.45 3 -26.13 0.01 3 7.01 0.04 3 7.0 0.3 3 0.710786 0.000077 2378944 865599 2521 7154997-101.9 0.83 3 -26.10 0.05 3 7.10 0.05 3 5.9 0.2 3 0.710253 0.000119 2234441 1005725 2581 8101900-93.6 1.25 3 -25.00 0.02 3 8.39 0.03 3 7.0 0.3 3 0.709060 0.000088 2148166 764693 1534 6371336

-98.3 1.17 3 -25.02 0.04 3 6.91 0.01 3 6.5 0.2 3 0.709714 0.000095 2265180 863874 4692 7554078

-100.0 0.84 2 -24.90 0.00 3 8.26 0.06 3 6.1 0.1 3 0.711055 0.000082 2562342 960108 1609 8165455-97.4 1.27 3 -25.11 0.03 3 7.59 0.07 3 5.8 0.2 3 0.711213 0.000083 2877004 806258 1784 6606414-96.2 1.67 3 -25.09 0.02 3 7.35 0.02 3 5.3 0.1 3 0.711525 0.000080 2147742 796414 2135 6639894-98.7 1.19 3 -25.27 0.01 3 7.29 0.04 3 4.5 0.3 3 0.710693 0.000042 3182738 778125 938 6464844

-100.9 0.89 3 -25.02 0.03 3 6.65 0.00 3 3.2 0.2 3 0.710048 0.000048 2485017 918436 1829 7585549-94.7 0.81 3 -25.95 0.01 3 7.16 0.06 3 4.2 0.2 3 0.708589 0.000059 2102915 898598 2631 7645145-93.6 1.27 3 -25.25 0.02 3 5.89 0.02 3 4.2 0.1 3 0.708216 0.000037 2890974 946423 1916 8094420-97.4 1.81 3 -25.93 0.92 3 5.75 0.05 3 4.9 0.2 3 0.708216 0.000065 2583067 959967 1114 7882678-95.9 0.98 3 -25.02 0.01 3 7.08 0.07 3 4.1 0.1 3 0.710416 0.000057 2329127 898204 2187 7411175-99.9 0.25 3 -27.22 0.02 3 7.83 0.14 3 6.0 0.1 3 0.711603 0.000281 2251887 1077234 2940 8869314-99.6 0.57 3 -27.71 0.02 3 7.65 0.06 3 7.3 0.8 3 0.707855 0.000044 2483425 1127085 760 9168552-96.8 0.71 3 -25.44 0.05 3 6.32 0.05 3 4.1 0.5 3 0.708879 0.000041 2442116 1066772 1441 8430151-94.9 1.02 3 -25.58 0.01 3 7.29 0.03 3 4.1 1.2 3 0.708692 0.000073 2180345 1084246 870 8434515-96.3 0.47 3 -26.57 0.06 3 6.33 0.03 3 6.5 0.3 3 0.710543 0.000035 3147435 1025393 1145 8193474

BBOP Wales Page 76


# Reference # MLC #40 W08090301 W004341 W08090302 W004442 W08090303 W004543 W08090304 W004644 W08090201 W004845 W08090202 W004946 W08090203 W005047 W08091001 W005148 W08091002 W005249 W08091003 W005350 W08091004 W005451 W08091005 W005552 W08091006 W005653 W08091007 W005754 W08091008 W005855 W08110401 W005956 W08110402 W006057 W08110403 W006158 W08110404 W006259 W08110405 W006360 W08111401 W006461 W08111402 W006562 W08111403 W006663 W08111404 W0067

64 W08111405 W006865 W08111406 W006966 W08111407 W007067 W08111408 W007168 W08111409 W007269 W08111410 W007370 W08111411 W007471 W08111412 W007589 W09052703 W0093

90 W09052704 W009491 W09052705 W009592 W09052706 W0096

93 05020801 0117

93 W09052707 W0097


d2H [‰] [‰] n d13C [‰] [‰] n d15N [‰] [‰] n d34S [‰] [‰] n [‰] [ ug/kg] [ug/kg] [ug/kg] [ug/kg]-92.3 0.38 3 -25.31 0.01 3 7.92 0.02 3 5.0 0.6 3 0.713872 0.000021 3162379 1012262 7497 8249896-96.2 0.59 3 -26.89 0.04 3 8.32 0.11 3 6.2 0.3 3 0.710006 0.000029 2363584 1023763 2610 8248111-92.8 1.72 3 -22.88 0.02 3 6.69 0.03 3 3.7 0.5 3 0.709327 0.000030 2406187 948138 1478 7882415-93.5 0.50 3 -23.31 0.01 3 6.92 0.03 3 2.8 0.1 3 0.708372 0.000024 3049182 889038 1695 7113494-97.7 1.34 3 -25.81 0.03 3 6.27 0.11 3 2.6 0.1 3 0.710503 0.000029 2123086 1061532 901 9014291-96.7 0.43 3 -25.77 0.02 3 5.85 0.08 3 3.2 0.1 3 0.709721 0.000031 3068784 1016135 2659 8174733-96.3 0.21 3 -24.95 0.01 3 5.73 0.02 3 3.9 0.4 3 0.710235 0.000024 2773317 987783 797 8222767-95.2 0.54 3 -27.35 0.01 3 7.29 0.02 3 4.8 0.6 3 0.716666 0.000031 3325523 830382 14832 6751416-96.5 1.34 3 -27.78 0.02 3 6.87 0.13 3 3.2 0.1 3 0.706987 0.000022 2173499 1072541 1349 8633962-94.7 1.89 3 -28.03 0.04 3 7.73 0.04 3 3.1 0.4 3 0.706437 0.000028 2765194 993781 1033 8208782-91.6 1.60 3 -27.86 0.05 3 7.72 0.03 3 2.7 0.5 3 0.706828 0.000076 2917546 957844 1020 7858165-96.0 1.65 3 -27.06 0.02 3 6.70 0.03 3 3.0 0.2 3 0.706861 0.000035 3600865 958540 1095 7614851

-102.4 0.18 3 -27.42 0.00 3 8.20 0.04 3 3.7 0.1 3 0.711360 0.000111 1992688 969558 774 8046199-103.2 0.71 3 -27.21 0.01 3 8.18 0.03 3 2.7 0.2 3 0.709663 0.000362 2338362 986364 1233 8324691-100.9 0.46 3 -27.08 0.01 3 8.60 0.05 3 2.7 0.3 3 0.709832 0.000048 2596508 976236 985 8202385-96.3 0.46 3 -25.89 0.05 3 8.20 0.12 3 6.0 0.1 2 0.710197 0.007400 2683723 943453 6181 8129202-97.0 2.06 3 -26.34 0.03 3 8.56 0.07 3 6.8 0.1 3 0.709829 0.005300 2864385 1027184 664 8074081

-101.2 1.58 3 -27.70 0.03 3 7.31 0.12 3 6.8 0.1 3 0.711441 0.011900 2337466 991393 1536 8589868-98.9 1.01 3 -27.28 0.04 3 8.07 0.03 3 7.3 0.2 2 0.710672 0.008000 2526027 925956 1326 7630339-99.6 1.99 3 -27.02 0.07 3 8.05 0.09 3 8.0 0.1 3 0.708521 0.006400 2479703 1048833 704 8440322-99.8 0.93 3 -26.11 0.01 3 6.81 0.11 3 4.3 0.4 3 0.708296 0.008700 2219873 1171837 1314 9159432-93.6 1.06 3 -26.30 0.02 3 6.43 0.09 3 4.5 0.3 3 0.708518 0.004800 2459908 1079658 873 8594887-94.7 0.86 3 -26.41 0.03 3 7.43 0.06 3 4.8 0.4 3 0.716152 0.006400 3013746 890862 846 7403986-94.0 1.89 3 -26.34 0.04 3 6.17 0.12 3 4.3 0.3 3 0.711604 0.038600 2715215 1034253 360 8792173

-95.7 1.69 3 -27.41 0.01 3 8.46 0.03 3 1.9 0.4 3 unmeasurable na 2936304 955701 846 7986744-96.5 2.29 3 -27.63 0.04 3 7.22 0.05 3 2.6 0.2 3 0.711835 0.011300 2565089 962155 884 8044127-94.0 1.52 3 -27.20 0.04 3 7.60 0.08 3 0.1 0.2 3 0.709636 0.011400 3033893 999639 654 8346219-93.2 1.60 3 -27.25 0.04 3 7.64 0.07 3 1.7 0.2 3 0.716040 0.003800 2866685 969233 3576 7925682-97.0 0.63 3 -27.25 0.05 3 7.20 0.04 3 1.7 0.1 3 0.710845 0.007100 3318904 998286 2742 8098158

-100.5 2.26 3 -27.14 0.02 3 6.51 0.06 3 2.4 0.1 3 0.708391 0.007400 2638138 1083948 263 9317838-100.6 0.76 3 -26.54 0.02 3 7.84 0.02 3 4.5 0.3 3 0.710251 0.004600 2973352 994856 860 7837081-98.1 1.48 3 -26.25 0.01 3 7.59 0.06 3 4.9 0.2 3 unmeasurable na 3105714 1079258 694 8914913-91.3 1.70 3 -23.40 0.02 3 7.80 0.08 3 7.0 0.2 3 0.712487 0.002400 2260551 792809 2802 7614070

-95.5 1.83 3 -23.44 0.03 3 7.26 0.04 3 7.5 0.5 3 0.710270 0.006300 2126062 898340 818 7934264-90.3 2.16 3 -22.84 0.03 3 7.45 0.06 3 7.0 0.5 3 0.706919 0.004300 2310133 883838 449 8331248-92.6 2.42 3 -22.82 0.04 3 7.37 0.09 3 7.3 0.6 3 0.709999 0.008600 2708416 915517 564 8552545

-90.5 2.48 3 -19.64 0.03 3 6.81 0.03 3 2.8 0.2 3 0.708801 0.000087 2796267 493197 1839 4372547-92.2 0.47 3 -23.75 0.04 3 7.86 0.14 3 6.0 0.4 3 0.709539 0.005800 2028432 913865 931 8514167

BBOP Wales Page 77


# Reference # MLC #94 05020802 011894 W09052708 W0098

95 05020803 0119

95 W09052709 W0099

96 W09052710 W0100

97 W09052711 W0101

98 W09052712 W0102

99 W09052713 W0103

136 05042801 0183

216 05081609 0270

217 05081610 0271

218 05081611 0272

219 05081612 0273

220 05081613 0274

237 05082401 0291

238 05082402 0292

309 05110801 0551

310 05110802 0552

311 05110803 0553

312 05110804 0554

491 06083005 0986

492 06083006 0987

493 06083007 0988

494 06083008 0989

495 06083009 0990

meanSD

minmax

rangeN


d2H [‰] [‰] n d13C [‰] [‰] n d15N [‰] [‰] n d34S [‰] [‰] n [‰] [ ug/kg] [ug/kg] [ug/kg] [ug/kg]-99.0 2.14 3 -24.35 0.04 3 5.98 0.04 3 3.2 0.1 3 0.711334 0.000162 2799268 949962 2942 7976180-93.9 2.60 3 -23.03 0.04 3 7.03 0.10 3 4.6 0.6 3 0.709953 0.004200 2468988 956983 1067 8954954

-95.7 0.16 3 -24.05 0.01 3 6.48 0.03 3 5.0 0.4 3 0.709250 0.009100 3773512 950726 2808 7901425

-88.9 1.74 3 -23.38 0.03 3 8.02 0.09 3 6.4 0.5 3 0.708273 0.003100 2765619 844680 524 8071159

-92.8 0.62 3 -23.37 0.04 3 7.09 0.13 3 5.7 0.2 3 0.708260 0.002800 2291262 976323 4856 8935686

-89.7 0.23 3 -22.95 0.04 3 7.47 0.15 3 5.6 0.4 3 0.710433 0.015700 2503550 918027 761 7863786

-94.4 0.32 3 -25.40 0.03 3 6.89 0.06 3 6.6 0.1 3 0.710505 0.005700 2454462 874663 208 8280087

-92.8 2.37 3 -23.59 0.02 3 7.91 0.07 3 7.5 0.3 3 0.711334 0.006500 2582169 927931 790 8577674

-105.0 1.74 3 -25.85 0.04 3 7.23 0.06 3 5.5 0.2 3 0.709035 0.000059 2953958 897516 2533 7402803

-92.4 2.33 3 -27.42 0.01 3 8.98 0.04 3 6.6 0.6 3 0.712243 0.008100 3292320 787483 917 6397695

-98.5 3.38 3 -27.10 0.01 3 7.70 0.04 3 8.2 0.1 3 0.712613 0.004100 2513002 930731 5071 7604204

-94.3 1.35 3 -27.27 0.01 3 7.69 0.10 3 7.0 0.4 3 0.710342 0.008100 2209110 882784 412 8130272

-97.3 0.88 3 -26.77 0.03 3 8.07 0.02 3 7.8 0.3 2 0.713012 0.009300 1983646 917584 3066 8083875

-97.1 1.15 3 -27.11 0.03 3 7.50 0.02 3 6.8 0.1 3 0.711926 0.010700 2483303 1066109 480 8546095

-98.8 1.52 3 -27.21 0.01 3 9.14 0.04 3 6.9 0.3 3 0.710567 0.006500 2764771 1006940 410 8294710

-93.7 0.33 3 -27.40 0.03 3 8.32 0.10 3 7.4 0.2 3 0.710651 0.010300 2585534 901822 1458 8386071

-95.4 0.11 3 -26.74 0.02 3 7.98 0.04 3 6.9 0.3 3 0.712761 0.005800 2034701 915398 1320 8771176

-95.2 2.29 3 -27.06 0.06 3 8.37 0.05 3 8.4 0.7 3 0.714111 0.005800 3356564 769068 2239 6523825

-93.9 1.27 3 -27.15 0.02 3 9.70 0.04 3 8.0 0.2 3 0.710936 0.005000 2113473 712252 966 6613168

-95.9 0.62 3 -27.77 0.03 3 7.56 0.09 3 6.0 0.2 3 0.713983 0.009700 2229971 938527 1447 7937793

-90.7 1.61 3 -26.45 0.02 3 8.14 0.05 3 7.3 0.8 3 0.714966 0.009200 3792826 944706 6207 7643373

-89.1 1.09 3 -26.28 0.01 3 8.68 0.03 3 6.7 0.1 2 0.716671 0.009800 2706237 555313 14024 5222017

-94.6 1.09 3 -26.79 0.03 3 8.31 0.03 3 6.9 0.7 3 0.714164 0.003400 3365619 862644 13281 7242016

-92.5 1.57 3 -27.02 0.01 3 8.62 0.03 3 6.7 0.1 3 0.711756 0.009800 2396058 725290 1094 6872735

-93.5 0.73 3 -26.25 0.02 3 8.20 0.05 3 6.4 0.1 3 0.713755 0.083100 3234423 1018997 2950 8157149

δδδδ2H [‰] δδδδ13C [‰] δδδδ15N [‰] δδδδ34S [‰] 87/86Sr Na 23 Mg 24 Al 27 P 31-96.3 -25.91 7.55 5.34 0.7104068 2645166 925758 2119 77960063.4 1.48 0.83 1.76 0.0021412 436669 106105 2518 812839

-105.0 -28.03 5.73 0.12 0.7064370 1741555 493197 208 4372547-88.9 -19.6 9.7 8.4 0.7166710 3896159 1171837 14832 931783816.1 8.39 3.98 8.32 0.01 2154604 678640 14624 4945292101 101 101 101 99 101 101 101 101

BBOP Wales Page 78


# Reference # MLC #

1 W08022101 W0001


10 W08022704 W001011 W08022705 W0011


25 W08052201 W0028


K 39 Ca 43 Rb 85 Sr 88 Ba 138 Sc 45 Ti 48 V 51 Cr 52 Mn 55 Fe 56 Co 59 Ni 60 Cu 63 Zn 66 Ga 69

[ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [u g/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/ kg] [ug/kg]

15574734 331934 14927 117 119 3 1304 2 43 375 104755 6 45 2219 175156 0

13027942 195338 10325 71 73 2 582 1 5 469 140716 8 46 3497 200133 014192844 361117 10509 162 130 2 1451 2 103 308 136653 10 56 2428 177046 115798213 493796 17675 175 231 4 1634 2 13 522 105636 15 14 2541 157374 115983245 195154 19177 71 119 1 612 1 5 439 88182 8 15 2803 183250 016065296 167454 17772 65 61 1 363 1 18 317 56517 11 26 1604 99872 013590703 252788 9601 139 69 1 767 2 18 466 213034 8 25 2905 220907 114231999 205886 13311 106 33 1 662 1 21 271 67518 7 25 1881 148040 014946208 248254 12049 172 84 3 782 3 73 535 134273 12 39 2723 130609 113885586 291999 10771 155 39 1 909 1 8 375 127628 6 10 2453 148114 014542296 197260 11836 125 43 1 807 1 2 401 144989 8 5 3013 194665 0

14000467 268248 11814 138 93 2 915 1 61 657 189880 6 16 3397 244409 013767871 156025 14282 47 34 1 449 1 7 412 103874 8 7 2590 174731 016656555 179019 16435 29 11 1 822 1 6 266 68395 8 11 1545 131439 013576456 184629 20793 46 35 2 673 1 8 333 94316 7 6 1909 138485 114774904 154534 26879 42 25 0 347 2 8 378 100910 21 4 2643 268882 214789898 189300 26375 73 71 1 1182 3 19 372 90580 29 28 2883 152011 116053599 453117 12308 178 186 6 2079 6 23 444 102821 18 31 2926 145897 113775685 195307 8766 95 93 4 2013 4 16 312 96696 11 39 2254 139955 114447291 342894 8371 99 75 3 1786 2 8 389 113012 14 18 2075 146653 014073901 436803 20520 109 106 9 2324 3 55 468 198236 12 51 3224 218935 216140260 169524 16252 61 47 3 1505 3 24 394 91435 26 15 2828 183587 112154312 300164 16657 98 61 2 1288 2 19 399 144114 11 20 2669 139559 1

15435240 255659 24919 89 78 6 1785 6 63 303 96514 50 20 1799 187102 1

16343681 292534 9133 103 107 2 1903 2 16 327 90608 6 13 2005 144114 012513387 240808 14548 97 61 5 1275 3 22 538 131828 13 18 3462 195654 112727856 263949 20541 99 91 1 1456 2 22 415 116447 12 17 2465 175436 011791058 360963 21589 125 98 1 1064 2 25 375 190195 23 10 2577 158597 015272823 256658 16085 80 64 2 1701 1 33 330 107755 6 30 2096 134919 015458425 226788 12174 80 69 5 1419 5 18 264 68704 10 9 1941 133408 015050513 231622 11846 91 61 2 1219 4 9 444 102559 22 114 3491 188904 015499397 183233 11916 54 32 0 841 2 36 340 71493 9 19 2410 164111 114453151 285950 16259 81 64 2 1445 2 15 339 117128 146 21 2512 134633 015813218 198970 11437 72 106 8 1712 5 17 914 143613 6 24 4316 219053 115781625 217447 11172 107 74 0 994 1 1 718 100828 7 2 3915 205063 016011976 195646 12980 135 94 0 1160 2 7 363 96859 12 0 2813 225848 016684760 212281 14636 146 59 1 697 2 1 529 121357 11 10 3647 245649 014837360 263983 21098 129 141 1 1167 1 11 685 132840 4 27 4188 209109 0

BBOP Wales Page 79




90 W09052704 W009491 W09052705 W009592 W09052706 W0096

93 05020801 0117

93 W09052707 W0097


[ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [u g/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/ kg] [ug/kg]15017745 849697 14968 291 644 13 3051 12 164 737 130502 11 9 3609 239722 215778717 248775 10085 94 91 4 1388 5 12 633 127648 12 9 3311 251357 113496643 222386 17477 90 72 4 1275 3 40 379 95605 8 54 3088 208426 013197266 299816 16886 168 114 2 1125 3 44 464 279714 6 13 3298 220181 0

202725 13391 68 64 0 935 1 9 400 72012 5 0 3194 176675 014790386 286195 20547 147 85 3 1102 6 12 619 167740 12 1 3796 211792 015304324 233454 28155 92 75 0 1020 1 27 357 71561 8 16 2528 193151 011997669 464692 14412 471 3336 11 2273 8 2775 654 218052 8 17 3880 179293 416510560 188671 18057 91 38 2 979 2 3 435 93204 4 1 3010 191036 014912426 258335 15398 165 67 1 986 1 6 613 129931 7 92 3340 221576 014195703 254287 17007 144 63 1 1361 2 7 713 137070 6 0 4146 231719 013927405 437643 13584 219 122 2 1733 1 22 503 231381 5 0 3312 216913 014274453 171838 11073 52 46 2009 13075 38 10527 1581 5781 182 68826 5756 23492 380414952449 183987 4769 56 46 0 906 1 4 454 109049 3 2 3490 157093 014951307 313873 5938 116 104 0 1137 1 46 582 143187 4 3 3179 250699 016517272 154632 14819 73 103 10 1331 10 19 477 103850 18 24 3490 239828 217644463 184631 14919 68 47 2 1189 1 31 550 124701 12 22 3229 163420 016629731 226930 32881 101 62 9 1191 2 25 513 74765 3 9 3013 221459 014933287 248365 12828 174 118 2 1294 2 14 617 85812 9 7 3949 229079 017732127 190673 11268 79 33 1 714 1 23 381 95441 8 27 3033 208587 019091948 193242 9108 47 44 1 1151 2 7 429 103718 2 13 3224 232138 117714553 178408 8906 69 54 1 596 2 15 439 92011 3 43 3632 219639 014709755 224360 7184 91 118 1 698 1 39 460 123371 10 133 3580 176187 016954910 183428 8923 74 59 2 785 1 6 440 72680 3 10 3480 229838 0

15621256 359356 9884 125 169 2 2052 2 13 596 139708 11 28 3575 153043 016310592 201597 8996 51 92 2 895 1 9 419 74874 4 266 3674 217974 017438753 329600 11304 126 97 2 1907 1 13 358 106404 6 19 2856 209345 016055966 716263 10814 320 905 4 3116 3 17 591 133270 12 17 3604 199721 116374102 224500 11291 65 113 6 1185 5 213 492 134691 8 27 3117 220664 118212534 190776 10674 41 37 54 698 2 19 283 57182 3 3 2644 177194 116034555 267935 3688 88 109 1 1528 1 15 379 116219 4 5 2984 219126 018379484 225297 4385 85 723 0 1371 1 6 399 129446 4 0 3480 238309 014111910 159832 3523 107 692 3 812 2 7 372 68900 9 0 2866 299446 0

15886916 176922 3985 83 74 3 1122 12 8 277 46501 8 0 2612 271135 015223518 168686 4113 66 50 1 1108 1 11 316 53382 6 30 2812 267088 015833356 154384 3737 66 80 2 998 1 3 295 48738 6 18 2560 270369 0

7801089 173206 6279 114 190 4 475 2 34 262 181878 10 24 1896 140624 115755059 189134 3619 81 227 1 1483 1 9 417 58406 6 21 3224 288070 0

BBOP Wales Page 80


# Reference # MLC #94 05020802 011894 W09052708 W0098

95 05020803 0119

95 W09052709 W0099

96 W09052710 W0100

97 W09052711 W0101

98 W09052712 W0102

99 W09052713 W0103

136 05042801 0183

216 05081609 0270

217 05081610 0271

218 05081611 0272

219 05081612 0273

220 05081613 0274

237 05082401 0291

238 05082402 0292

309 05110801 0551

310 05110802 0552

311 05110803 0553

312 05110804 0554

491 06083005 0986

492 06083006 0987

493 06083007 0988

494 06083008 0989

495 06083009 0990

meanSD

minmax

rangeN


[ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [u g/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/ kg] [ug/kg]16365420 333099 15254 144 131 6 1594 4 46 225 127570 16 36 2535 236738 116332605 331693 3904 140 156 2 2324 1 16 288 57888 6 46 3229 249791 0

15909416 488779 13129 227 179 5 1983 7 46 643 175862 15 10 2946 150904 3

14566686 207708 4361 92 53 2 955 1 3 303 63635 7 2 2902 299778 0

16438504 189248 4380 122 691 5 1408 3 12 361 48961 6 9 2987 249792 2

14765290 272932 3620 138 86 1 1142 1 1 279 63876 5 3 2635 272310 0

15044144 138654 5042 56 30 0 606 1 94 401 53116 6 23 2978 300854 0

15915771 165222 3691 70 101 1 845 1 1 316 54046 6 0 2546 265636 0

14306549 194411 11150 200 101 4 656 5 36 542 112217 15 29 3463 138559 1

13087901 680597 16910 210 412 3 3318 2 15 497 178640 6 0 3124 154421 0

15092425 306946 18840 165 618 3 1847 3 41 465 119151 7 63 3314 208198 2

15214677 184238 7924 72 78 1 1233 1 8 379 48771 3 15 2460 292227 0

15048842 162435 12409 103 402 5 896 3 14 431 76264 5 15 3503 222719 3

16797297 244969 25091 94 74 0 822 1 3 378 153490 4 21 2595 208945 1

17211619 249561 20450 157 66 2 916 1 26 444 102132 3 18 3222 208289 1

15684975 174400 11558 125 195 3 1454 2 12 509 63038 4 16 4459 259181 1

16161349 160691 20045 79 341 3 1038 2 17 441 54533 6 17 3390 298435 1

13221256 250356 14607 137 466 1 1117 2 15 372 163491 6 25 3120 235428 0

12267243 131346 8620 68 66 5 1064 2 6 644 77294 12 13 3810 322574 3

15238793 168264 34825 96 337 2 674 2 11 413 101592 5 17 2850 186203 1

15246295 391691 11240 251 1579 7 1573 4 27 382 196996 14 53 3211 194334 2

9620206 397412 13119 434 4459 14 2862 7 42 519 56110 10 36 2405 240569 4

14899944 311243 15251 351 3113 13 1945 8 37 588 175100 10 34 3328 198967 4

12508270 170541 16733 101 142 5 1051 3 33 539 86818 14 12 2954 325019 1

16635367 300088 12203 215 816 5 1384 2 14 569 177711 4 20 3841 172910 1K 39 Ca 43 Rb 85 Sr 88 Ba 138 Sc 45 Ti 48 V 51 Cr 52 Mn 55 Fe 56 Co 59 Ni 60 Cu 63 Zn 66 Ga 69

15075798 259427 13277 120 266 23 1385 3 155 455 111184 12 705 3029 203955 381704112 118920 6371 75 643 200 1310 4 1078 169 46922 23 6846 660 51967 3787801089 131346 3523 29 11 0 347 1 1 225 5781 2 0 1545 23492 0

19091948 849697 34825 471 4459 2009 13075 38 10527 1581 279714 182 68826 5756 325019 380411290860 718351 31302 442 4447 2009 12729 37 10526 1356 273933 180 68825 4212 301527 3804

100 101 101 101 101 101 101 101 101 101 101 101 101 101 101 101

BBOP Wales Page 81


# Reference # MLC #

1 W08022101 W0001


10 W08022704 W001011 W08022705 W0011


25 W08052201 W0028


Ge 74 As 75 Se 77 Li 7 Be 9 Y 89 Zr 90 Nb 93 Mo 9 8 Ru 102 Pd 106 Cd 114 Sn 120 Sb 121 Te 130 La 139 Ce 140


5 24 254 0.00 0.05 4.61 183.42 0.14 56.78 0.00 6.92 1.96 1.82 2.83 2.90 0.25 0.60

1 9 209 0.09 0.07 1.67 159.76 0.00 98.60 0.00 5.64 2.27 0.38 1.89 0.99 0.21 0.388 20 497 0.36 0.29 1.28 91.94 2.61 54.31 0.00 5.30 0.84 2.74 3.38 2.14 0.54 1.115 19 371 0.11 0.12 1.13 22.79 0.29 40.57 0.05 3.42 1.21 10.21 2.77 1.82 1.42 3.053 18 343 0.03 0.03 0.76 47.59 0.00 36.83 0.03 3.84 0.44 0.12 1.86 0.33 0.19 0.455 16 222 0.00 0.03 0.26 7.72 0.07 21.76 0.00 2.13 0.52 0.23 1.07 1.57 0.12 0.321 9 195 0.09 0.12 0.57 46.01 0.00 32.81 0.00 4.46 0.21 0.12 1.37 0.24 0.40 0.87

11 14 369 0.79 0.44 0.64 26.00 0.22 18.89 0.26 2.94 0.35 5.92 2.68 0.01 0.37 1.133 9 232 0.48 0.40 0.43 36.12 0.47 48.25 0.09 4.13 1.57 3.59 1.30 0.56 0.51 1.686 8 182 0.07 0.06 0.41 18.74 0.11 32.50 0.00 4.36 0.48 0.12 2.28 0.88 0.17 0.243 7 232 0.05 0.07 0.36 26.22 0.15 39.59 0.03 4.32 0.43 0.19 1.12 0.94 0.20 0.46

4 15 363 0.08 0.01 0.21 24.38 0.00 38.18 0.00 4.80 1.09 1.08 1.98 1.11 0.14 0.355 40 125 0.00 0.00 0.35 19.96 0.00 29.33 0.11 3.08 0.57 3.61 3.12 1.12 0.34 0.546 12 407 0.06 0.10 0.32 20.79 0.59 18.89 0.38 3.85 0.15 0.12 2.17 0.01 0.21 0.308 10 494 0.72 0.74 0.31 21.34 0.51 22.06 0.19 3.76 0.55 2.64 2.56 1.05 0.31 0.801 31 387 0.09 0.13 0.19 41.06 0.00 41.68 0.00 5.58 1.13 3.29 2.51 1.03 0.30 0.518 10 159 0.22 2.75 0.56 28.24 2.21 33.14 0.08 3.16 1.36 8.87 3.33 0.53 0.83 2.207 19 611 0.20 0.23 1.24 29.80 2.87 27.18 0.12 4.13 1.49 12.89 4.39 2.51 1.70 3.58

12 14 205 0.23 0.19 1.54 66.85 4.23 34.99 0.37 5.91 2.56 4.10 4.92 0.10 1.27 2.103 20 285 0.00 0.04 0.54 24.22 1.88 29.78 0.00 4.57 1.18 5.89 2.84 0.01 0.80 1.242 21 337 0.05 0.12 0.34 103.19 5.05 54.98 0.00 5.34 1.07 5.31 5.18 0.53 0.62 0.756 12 255 0.03 0.00 1.69 77.94 3.58 31.52 0.00 4.80 1.13 5.37 2.49 0.99 1.70 2.969 16 548 0.68 0.54 0.36 27.47 1.38 28.77 0.06 3.30 1.59 7.45 2.76 1.03 0.41 1.13

7 47 302 3.03 3.13 1.44 32.00 2.37 41.68 0.06 3.56 4.36 30.53 1.83 0.99 2.28 10.03

4 15 215 0.01 0.09 1.11 72.38 1.84 31.29 0.00 4.66 2.13 0.66 2.09 2.29 0.57 1.012 31 411 0.07 0.08 0.49 54.27 1.03 44.61 0.00 3.82 1.79 5.89 1.92 1.26 0.69 1.337 40 406 0.58 0.42 0.32 30.99 1.14 29.36 0.09 3.31 2.88 6.39 1.80 1.83 0.49 0.904 44 586 0.02 0.00 0.22 11.91 0.01 37.76 0.11 2.52 2.58 26.29 1.04 1.28 0.51 1.117 12 159 0.21 0.14 0.39 32.74 3.23 26.72 0.16 5.98 4.55 3.20 4.09 0.01 0.62 0.762 42 242 0.12 0.13 0.55 33.40 1.87 35.16 0.00 4.34 2.07 1.03 2.38 0.48 0.82 1.213 46 309 0.08 0.04 0.63 91.13 0.90 49.28 0.00 4.54 2.54 1.49 3.13 0.66 0.91 1.068 46 352 0.25 0.12 0.28 14.42 0.38 25.00 0.00 2.76 2.31 1.84 1.30 0.01 0.25 0.416 9 207 1.34 2.47 0.64 31.96 1.15 32.77 0.11 3.95 3.29 7.27 2.41 1.94 1.09 1.881 39 157 0.05 0.09 2.50 0.11 2.95 33.05 0.00 2.71 2.26 0.12 3.79 0.01 5.42 7.772 52 372 0.01 0.04 0.23 0.11 0.77 43.44 0.11 8.17 1.99 1.76 3.05 3.04 0.72 2.334 57 350 0.09 0.08 1.00 0.11 1.35 34.84 0.00 4.05 2.00 1.23 5.56 0.01 1.29 3.093 26 326 0.02 0.09 0.40 0.11 1.22 32.78 0.06 4.02 1.18 1.09 2.33 2.96 0.45 1.971 21 115 0.13 0.09 0.38 0.11 0.92 34.01 0.01 2.96 1.11 3.80 4.11 1.17 0.85 2.59

BBOP Wales Page 82




90 W09052704 W009491 W09052705 W009592 W09052706 W0096

93 05020801 0117

93 W09052707 W0097


[ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [u g/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/ kg] [ug/kg] [ug/kg]2 178 279 0.40 0.47 2.47 0.11 1.03 54.32 0.15 14.90 2.46 3.61 22.26 11.34 5.17 12.372 149 208 0.05 0.14 0.55 0.11 1.27 45.80 0.18 6.49 1.08 1.95 5.71 9.87 0.87 3.572 23 342 0.05 0.07 2.56 1.41 3.29 27.82 0.02 2.95 1.41 0.13 2.18 2.10 1.01 2.393 17 407 0.02 0.13 0.45 0.11 0.73 28.67 0.26 6.90 1.12 3.86 4.01 2.67 0.91 2.773 46 323 0.11 0.13 0.41 0.54 0.73 39.65 0.01 2.32 0.67 5.74 3.08 1.02 0.49 1.683 77 358 0.15 0.14 0.44 0.11 0.66 38.62 0.14 3.90 0.60 2.18 3.16 3.11 1.09 3.732 36 363 0.05 0.06 0.29 0.11 0.82 29.83 0.11 2.82 0.32 0.12 2.03 1.90 0.64 2.514 1544 303 2.20 2.11 7.29 0.11 3.87 88.02 0.26 26.84 11.74 12.52 64.24 38.60 25.24 88.823 40 341 0.09 0.17 0.85 0.11 1.08 30.84 0.03 1.90 10.06 7.86 2.30 2.05 1.51 3.462 47 299 0.00 0.06 0.27 2.14 0.64 52.76 0.05 2.71 1.18 0.66 1.66 2.20 0.52 1.423 43 332 0.09 0.08 0.34 0.11 1.61 38.75 0.15 3.61 0.72 0.40 1.83 4.76 0.91 2.663 70 425 0.06 0.15 0.49 8.44 1.08 34.73 0.00 2.45 0.89 5.33 2.97 1.30 0.61 1.25

414 11686 705897 0.05 0.09 0.33 0.11 1.32 36.28 0.32 3.05 0.64 9.15 1.66 5.66 0.47 1.431 37 127 0.05 0.08 0.22 0.11 1.07 51.31 0.08 2.15 0.95 0.12 2.59 3.59 0.51 2.091 19 103 0.05 0.09 0.31 0.11 0.57 51.00 0.11 4.07 1.42 6.16 2.08 2.84 0.56 2.112 59 503 22.4 0.25 1.95 306.36 1.90 47.68 0.00 13.59 2.36 7.41 5.38 0.24 4.29 14.252 34 451 9.4 0.06 0.32 4.14 1.00 46.82 0.00 2.30 1.08 3.78 2.03 3.74 0.74 2.891 28 134 3.3 0.07 0.39 59.92 0.87 44.69 0.00 3.37 0.96 16.71 1.92 3.24 0.70 6.012 27 232 8.4 0.09 0.69 6.81 1.37 39.44 0.20 1.99 0.82 0.12 7.80 1.84 1.23 2.591 28 268 5.3 0.00 0.15 1.85 0.21 29.82 0.00 1.78 0.90 1.04 0.68 0.14 0.33 2.220 28 251 4.6 0.04 0.29 7.25 1.09 42.32 0.00 2.24 3.60 4.23 1.42 0.57 0.65 2.441 42 259 12.4 0.04 0.28 4.99 0.42 34.85 0.00 2.06 3.76 8.52 1.79 1.02 0.71 3.031 53 231 19.8 0.04 0.27 9.29 0.28 48.13 0.00 2.80 3.63 8.78 4.20 1.69 0.75 2.681 40 212 14.7 0.03 0.17 14.44 0.46 40.07 0.00 2.26 1.60 11.08 1.75 1.25 0.22 5.43

2 42 256 9.9 0.04 0.32 14.16 1.64 66.56 0.00 3.35 11.21 3.43 2.25 3.28 0.78 2.712 34 277 18.7 0.08 0.22 19.01 2.04 50.40 0.11 2.30 1.76 4.49 8.93 0.01 0.51 1.931 41 191 27.9 0.06 0.22 16.14 1.47 60.68 0.00 2.76 1.77 3.91 3.34 1.89 0.56 2.792 344 327 103.8 0.44 1.64 104.76 1.43 47.25 0.00 8.13 4.00 2.41 24.98 9.12 4.58 19.031 13 233 18.1 0.09 1.70 8.55 2.26 80.30 0.00 2.22 1.07 1.41 1.09 0.01 1.02 3.571 14 269 12.8 0.05 0.12 38.95 0.17 55.49 0.00 2.19 1.59 8.06 0.85 1.21 0.25 5.321 24 125 5.1 0.08 0.24 11.76 1.17 47.76 0.00 2.35 3.32 4.85 6.04 0.32 0.58 2.891 38 128 10.1 0.06 1.14 22.81 1.37 70.34 0.00 3.15 1.84 3.93 95.47 10.28 0.88 3.271 377 354 72.7 0.44 1.48 706.27 0.85 38.92 0.04 28.14 2.29 13.79 46.50 8.47 7.45 29.57

2 25 296 4.3 0.16 0.65 1.69 1.19 29.98 0.01 2.37 1.00 7.22 6.31 2.46 1.40 6.652 19 401 3.3 0.11 0.17 43.32 0.60 43.73 0.00 3.69 1.70 12.21 1.69 2.23 0.62 8.121 34 310 6.3 0.06 0.28 35.57 0.70 42.47 0.00 3.50 1.54 25.53 3.04 3.36 1.16 10.99

2 83 240 0.03 0.08 0.50 2613.39 0.21 15.71 0.33 3.75 36.46 0.22 4.80 0.48 1.20 3.872 53 398 6.3 0.11 0.37 118.60 1.16 36.68 0.00 6.16 1.55 20.37 21.14 4.05 1.45 10.54

BBOP Wales Page 83


# Reference # MLC #94 05020802 011894 W09052708 W0098

95 05020803 0119

95 W09052709 W0099

96 W09052710 W0100

97 W09052711 W0101

98 W09052712 W0102

99 W09052713 W0103

136 05042801 0183

216 05081609 0270

217 05081610 0271

218 05081611 0272

219 05081612 0273

220 05081613 0274

237 05082401 0291

238 05082402 0292

309 05110801 0551

310 05110802 0552

311 05110803 0553

312 05110804 0554

491 06083005 0986

492 06083006 0987

493 06083007 0988

494 06083008 0989

495 06083009 0990

meanSD

minmax

rangeN


[ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [u g/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/ kg] [ug/kg] [ug/kg]2 8 421 0.09 0.03 3.32 1010.00 4.42 45.62 0.00 3.60 1.86 0.84 2.10 0.01 1.07 1.682 81 384 6.9 0.25 0.53 164.53 1.52 40.31 0.00 7.63 2.06 10.09 6.74 3.31 2.22 12.37

3 23 399 16.0 0.16 0.97 7.45 0.54 36.06 1.44 2.94 0.92 4.47 6.49 5.99 1.51 3.22

2 11 327 5.4 0.08 0.11 78.98 0.22 41.68 0.05 5.72 0.62 7.58 1.42 0.84 0.26 5.63

2 616 326 48.1 0.76 3.14 708.99 1.80 34.09 0.00 26.74 3.46 54.22 33.16 9.06 17.28 46.41

1 12 312 2.4 0.09 0.45 9.18 0.51 24.09 0.04 2.31 1.01 6.92 2.12 3.86 0.77 4.42

0 6 166 5.2 0.08 0.11 22.86 0.24 51.71 0.00 3.31 1.42 13.40 1.44 2.24 0.20 6.20

1 82 263 7.3 0.09 0.42 152.12 0.84 36.45 0.00 7.06 0.88 27.32 12.20 3.12 2.00 10.13

5 7 515 0.26 0.11 2.03 33.33 1.01 42.55 0.21 4.70 5.02 38.88 3.90 1.63 10.37 23.30

2 78 67 9.0 0.12 0.73 37.38 1.08 28.50 0.00 3.97 0.69 0.12 6.70 3.69 2.58 6.87

2 496 148 21.3 0.39 2.36 282.35 2.59 40.92 0.12 19.11 1.89 20.02 76.19 9.55 9.88 28.25

1 16 107 3.6 0.10 0.13 3.56 1.65 31.56 0.50 4.03 1.35 0.12 4.81 0.01 0.58 6.04

2 715 196 24.9 0.35 1.70 850.22 0.97 47.68 0.78 27.23 1.39 10.31 26.05 6.53 7.09 21.69

1 24 343 2.7 0.02 0.17 4.89 0.28 35.10 0.00 1.79 0.13 8.71 3.92 4.01 0.41 1.93

1 26 168 4.5 0.08 0.21 3.11 0.25 45.36 1.02 1.90 0.16 0.12 2.56 2.37 0.46 3.57

1 208 139 5.9 0.09 0.66 140.44 1.37 48.56 0.56 9.03 2.63 33.05 22.55 0.60 2.39 10.94

1 137 226 17.2 0.27 0.67 262.69 1.31 41.43 0.30 13.26 1.92 3.53 17.58 2.98 3.25 12.07

1 104 174 22.4 0.29 0.90 57.73 1.65 45.56 0.51 4.70 1.08 8.20 22.41 7.82 2.42 11.13

1 30 225 2.7 0.09 0.20 68.57 1.32 48.50 0.29 7.68 0.27 2.77 3.56 0.03 0.60 1.54

1 87 97 16.3 0.20 0.67 40.73 0.41 41.73 1.74 4.49 0.09 2.31 19.42 6.68 1.87 6.54

1 424 122 111.6 1.00 4.72 273.83 2.33 46.49 0.25 18.01 5.95 16.83 55.91 25.38 6.79 40.59

2 1902 111 594.4 2.14 8.27 1503.79 4.14 28.67 0.26 49.35 12.83 15.29 156.90 45.13 35.35 121.14

1 1776 158 211.4 2.19 8.42 157.20 3.16 42.33 0.26 11.89 14.46 21.93 206.64 38.66 37.05 93.54

1 66 125 6.7 0.19 0.57 126.84 0.52 34.97 0.73 9.48 7.51 0.12 10.33 0.22 1.16 2.67

2 272 199 37.0 0.22 1.32 188.71 1.31 35.77 0.14 12.70 6.15 9.85 28.29 13.82 5.31 15.25Ge 74 As 75 Se 77 Li 7 Be 9 Y 89 Zr 90 Nb 93 Mo 9 8 Ru 102 Pd 106 Cd 114 Sn 120 Sb 121 Te 130 La 139 Ce 140

7 234 7267 15.81 0.29 1.03 118.12 1.25 40.67 0.14 6.11 2.59 7.22 11.98 3.88 2.53 8.3841 1192 70212 64.12 0.58 1.51 332.72 1.09 13.16 0.27 6.99 4.30 9.11 29.02 7.44 5.91 18.290 6 67 0.00 0.00 0.11 0.11 0.00 15.71 0.00 1.78 0.09 0.12 0.68 0.01 0.12 0.24

414 11686 705897 594.41 3.13 8.42 2613.39 5.05 98.60 1.74 49.35 36.46 54.22 206.64 45.13 37.05 121.14413 11680 705829 594.41 3.13 8.31 2613.28 5.05 82.89 1.73 47.57 36.37 54.09 205.96 45.12 36.92 120.91101 101 101 101 101 101 101 101 101 101 101 101 101 101 101 101 101

BBOP Wales Page 84


# Reference # MLC #

1 W08022101 W0001


10 W08022704 W001011 W08022705 W0011


25 W08052201 W0028


Pr 141 Nd 142 Sm 152 Eu 153 Gd 158 Tb 159 Dy 164 Ho 165 Er 166 Tm 169 Yb 174 Lu 175 Hf 180 Ta 181 W 184 Re 187 Ir 193


0.13 0.34 0.26 0.13 0.13 0.06 0.02 0.01 0.05 0.18 0.05 0.00 2.37 0.13 1.19 0.64 0.06

0.15 0.17 0.04 0.01 0.12 0.00 0.03 0.01 0.02 0.02 0.02 0.01 0.87 0.23 0.97 0.00 0.080.27 0.72 0.35 0.17 0.33 0.09 0.07 0.02 0.17 0.21 0.07 0.01 0.78 0.19 1.82 0.31 0.120.53 1.51 0.94 0.53 0.88 0.19 0.16 0.04 0.35 0.42 0.10 0.02 0.26 0.51 0.85 1.22 0.060.15 0.37 0.07 0.06 0.20 0.04 0.02 0.00 0.04 0.03 0.03 0.00 0.39 0.13 0.34 0.00 0.000.06 0.20 0.08 0.08 0.08 0.04 0.01 0.00 0.02 0.10 0.01 0.00 0.04 0.05 0.29 0.48 0.020.15 0.51 0.13 0.02 0.21 0.01 0.08 0.01 0.03 0.04 0.04 0.01 0.27 0.23 0.51 0.00 0.060.32 0.65 0.11 0.02 0.33 0.14 0.04 0.02 0.06 0.00 0.10 0.00 0.33 0.13 0.87 0.00 0.050.52 1.07 0.52 0.29 0.38 0.28 0.07 0.05 0.15 0.32 0.08 0.01 0.38 0.16 0.61 0.37 0.190.10 0.25 0.09 0.03 0.14 0.08 0.01 0.01 0.05 0.08 0.01 0.00 0.26 0.10 0.38 0.16 0.040.11 0.20 0.15 0.11 0.18 0.02 0.01 0.01 0.03 0.09 0.02 0.00 0.19 0.30 0.70 0.27 0.05

0.13 0.16 0.15 0.12 0.14 0.06 0.01 0.00 0.03 0.16 0.02 0.01 0.13 0.90 0.56 0.49 0.010.24 0.41 0.21 0.15 0.21 0.11 0.04 0.00 0.17 0.24 0.07 0.01 0.28 0.13 0.66 0.92 0.020.08 0.39 0.02 0.02 0.22 0.05 0.03 0.02 0.04 0.05 0.02 0.01 0.16 0.94 0.08 0.00 0.010.23 0.53 0.35 0.18 0.27 0.12 0.03 0.03 0.17 0.26 0.08 0.01 0.14 0.13 0.35 0.73 0.190.13 0.31 0.13 0.08 0.19 0.06 0.05 0.01 0.04 0.02 0.01 0.00 0.25 0.25 0.02 0.00 0.050.50 1.23 0.29 0.19 0.55 0.23 0.08 0.04 0.16 0.23 0.15 0.00 0.36 0.18 6.42 0.00 0.170.40 1.53 0.71 0.41 1.04 0.18 0.20 0.06 0.28 0.24 0.11 0.02 0.38 0.61 6.12 1.05 0.100.27 1.55 0.17 0.04 0.54 0.03 0.19 0.06 0.18 0.00 0.14 0.03 0.78 0.44 4.74 0.00 0.070.20 0.83 0.14 0.05 0.36 0.03 0.08 0.03 0.06 0.02 0.07 0.01 0.31 0.33 4.28 0.00 0.010.12 0.44 0.12 0.00 0.40 0.03 0.05 0.01 0.00 0.00 0.02 0.01 0.56 0.16 5.02 0.00 0.050.44 1.61 0.45 0.17 0.77 0.14 0.29 0.06 0.28 0.17 0.17 0.03 0.84 0.30 4.50 0.49 0.070.49 1.25 0.44 0.16 0.45 0.30 0.09 0.03 0.20 0.27 0.06 0.00 0.37 0.09 3.57 0.56 0.23

1.05 3.93 0.46 0.18 0.60 0.14 0.19 0.04 0.14 0.15 0.13 0.02 0.41 0.19 7.94 0.50 0.01

0.16 0.64 0.33 0.15 0.19 0.10 0.06 0.02 0.06 0.13 0.04 0.00 0.87 0.23 3.84 0.47 0.020.22 0.90 0.11 0.02 0.41 0.00 0.09 0.03 0.10 0.02 0.03 0.03 0.32 0.20 12.43 0.00 0.070.19 0.51 0.25 0.16 0.22 0.06 0.04 0.02 0.10 0.13 0.06 0.01 0.23 0.50 2.11 0.24 0.110.24 0.48 0.47 0.33 0.29 0.10 0.03 0.03 0.18 0.33 0.05 0.01 0.12 0.12 0.55 1.04 0.000.10 1.18 0.35 0.18 0.95 0.25 0.11 0.02 0.22 0.00 0.08 0.15 0.36 0.55 2.21 0.00 0.000.20 0.79 0.22 0.11 0.31 0.06 0.07 0.02 0.06 0.08 0.10 0.00 0.42 0.33 11.24 0.28 0.030.17 0.53 0.15 0.06 0.19 0.04 0.05 0.02 0.03 0.05 0.07 0.01 0.68 0.30 6.17 0.00 0.010.30 0.39 0.43 0.31 0.14 0.12 0.02 0.02 0.32 0.43 0.06 0.02 0.15 0.18 0.65 1.25 0.010.38 1.14 0.45 0.24 0.50 0.19 0.11 0.03 0.16 0.30 0.09 0.02 0.35 0.19 3.71 0.95 0.151.05 4.95 0.99 0.41 1.90 0.12 0.40 0.07 0.63 0.14 0.22 0.06 0.59 1.41 0.02 0.00 0.030.25 0.74 0.08 0.10 0.39 0.09 0.03 0.00 0.03 0.07 0.06 0.00 2.21 0.53 0.02 0.00 0.020.34 1.02 0.35 0.21 0.63 0.03 0.06 0.02 0.33 0.09 0.07 0.01 1.85 0.41 0.02 0.00 0.050.22 0.67 0.21 0.12 0.36 0.08 0.03 0.00 0.14 0.02 0.07 0.00 0.59 12.08 0.57 0.00 0.000.35 0.87 0.37 0.27 0.42 0.04 0.08 0.02 0.23 0.05 0.03 0.00 0.68 0.37 0.02 0.00 0.00

BBOP Wales Page 85




90 W09052704 W009491 W09052705 W009592 W09052706 W0096

93 05020801 0117

93 W09052707 W0097


[ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [u g/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/ kg] [ug/kg] [ug/kg]0.82 4.50 0.91 0.45 2.23 0.10 0.28 0.04 0.71 0.06 0.22 0.04 10.09 0.44 0.02 0.00 0.000.20 1.35 0.02 0.00 0.50 0.05 0.05 0.01 0.01 0.00 0.07 0.00 3.05 0.78 0.39 0.00 0.010.32 1.13 0.29 0.20 0.55 0.09 0.36 0.08 0.52 0.12 0.24 0.05 0.41 0.98 1.78 0.00 0.000.10 1.11 0.00 0.00 0.43 0.04 0.07 0.02 0.00 0.00 0.06 0.00 3.96 1.06 0.39 0.00 0.030.20 0.62 0.15 0.16 0.26 0.05 0.03 0.00 0.13 0.09 0.05 0.00 0.49 0.46 0.36 0.00 0.030.28 1.61 0.16 0.09 0.53 0.05 0.09 0.01 0.13 0.01 0.08 0.01 1.42 0.75 0.02 0.00 0.010.16 0.99 0.14 0.06 0.25 0.04 0.01 0.02 0.06 0.00 0.06 0.00 0.84 0.58 0.02 0.00 0.032.99 23.81 3.91 2.12 12.58 0.33 1.08 0.21 1.85 0.03 0.78 0.13 34.38 0.89 4.43 0.00 0.160.46 1.56 0.41 0.31 0.63 0.08 0.14 0.03 0.26 0.15 0.10 0.02 0.62 6.53 5.98 0.00 0.050.18 0.47 0.10 0.13 0.26 0.02 0.03 0.01 0.08 0.03 0.05 0.01 0.54 0.44 0.02 0.00 0.000.09 0.87 0.00 0.00 0.37 0.08 0.05 0.01 0.00 0.00 0.06 0.00 1.14 0.70 0.03 0.00 0.090.30 0.62 0.27 0.26 0.25 0.03 0.02 0.02 0.20 0.08 0.04 0.01 0.05 0.33 5.50 0.00 0.050.04 0.51 0.00 0.00 0.23 0.00 0.03 0.00 0.00 0.00 0.03 0.00 3.97 0.87 0.02 0.00 0.000.18 0.75 0.12 0.09 0.22 0.05 0.01 0.01 0.06 0.05 0.02 0.01 0.55 0.51 0.02 0.00 0.070.18 0.82 0.09 0.08 0.37 0.04 0.02 0.01 0.08 0.00 0.06 0.00 0.78 6.48 0.02 0.00 0.041.52 5.41 1.59 0.80 3.07 0.56 0.45 0.11 1.12 0.29 0.26 0.09 1.98 0.43 1.77 0.09 0.160.84 1.51 0.73 0.41 0.56 0.36 0.03 0.04 0.41 0.41 0.14 0.03 0.09 0.14 1.58 0.00 0.080.78 2.30 0.91 0.54 0.72 0.31 0.06 0.05 0.47 0.22 0.13 0.05 0.25 0.30 1.40 0.00 0.110.44 1.58 0.54 0.36 0.66 0.14 0.11 0.03 0.34 0.14 0.11 0.06 0.27 1.29 1.39 0.00 0.000.45 0.99 0.57 0.38 0.43 0.22 0.01 0.02 0.37 0.43 0.08 0.02 0.07 0.16 1.10 0.36 0.040.44 1.57 0.77 0.47 0.54 0.15 0.05 0.02 0.34 0.48 0.11 0.01 0.18 0.16 1.76 0.93 0.130.65 1.66 0.84 0.49 0.60 0.21 0.06 0.03 0.35 0.47 0.09 0.00 0.11 0.17 3.24 1.02 0.040.26 1.09 0.84 0.53 0.63 0.04 0.09 0.02 0.29 0.30 0.08 0.01 0.21 0.19 4.31 0.62 0.040.63 1.75 1.05 0.54 0.43 0.18 0.02 0.04 0.47 0.38 0.11 0.03 0.05 0.35 0.61 0.34 0.01

0.58 1.60 1.30 0.73 0.64 0.23 0.05 0.04 0.36 0.49 0.11 0.00 0.25 0.25 1.25 0.62 0.100.38 0.92 0.54 0.27 0.48 0.10 0.02 0.05 0.23 0.21 0.08 0.00 0.62 1.76 1.84 0.13 0.000.40 1.20 0.97 0.58 0.52 0.14 0.03 0.03 0.35 0.51 0.12 0.01 0.43 0.23 0.56 0.96 0.151.33 5.67 3.99 2.35 3.79 0.38 0.30 0.07 1.07 0.34 0.24 0.05 1.83 0.18 0.79 0.00 0.170.64 2.09 1.20 0.60 0.89 0.26 0.25 0.09 0.51 0.49 0.25 0.02 0.18 0.27 1.64 0.75 0.060.57 1.71 0.71 0.53 0.41 0.23 0.01 0.03 0.44 0.29 0.08 0.05 0.17 0.34 0.33 0.10 0.060.35 1.54 0.80 0.57 0.59 0.16 0.03 0.04 0.44 0.44 0.13 0.01 0.21 0.21 0.84 0.84 0.120.60 1.47 3.16 2.08 0.69 0.13 0.29 0.07 2.55 0.48 0.18 0.03 0.50 0.18 0.52 0.80 0.131.31 7.94 3.65 2.14 4.87 0.38 0.44 0.11 1.71 0.10 0.31 0.10 6.98 0.53 0.42 0.00 0.15

0.45 2.34 0.73 0.42 0.83 0.17 0.17 0.04 0.50 0.13 0.14 0.04 0.17 1.19 0.02 0.07 0.000.51 2.29 0.88 0.52 0.68 0.17 0.05 0.05 0.58 0.11 0.11 0.06 0.31 0.39 1.06 0.00 0.100.52 2.87 1.26 0.72 0.89 0.27 0.07 0.07 0.75 0.23 0.14 0.06 0.50 2.13 0.39 0.00 0.07

0.19 1.66 0.10 0.00 0.44 0.04 0.05 0.02 0.08 0.00 0.05 0.00 3.06 1.24 82.32 0.06 0.010.46 3.40 1.63 0.97 1.09 0.19 0.12 0.06 1.19 0.08 0.13 0.09 1.10 0.42 0.98 0.00 0.11

BBOP Wales Page 86


# Reference # MLC #94 05020802 011894 W09052708 W0098

95 05020803 0119

95 W09052709 W0099

96 W09052710 W0100

97 W09052711 W0101

98 W09052712 W0102

99 W09052713 W0103

136 05042801 0183

216 05081609 0270

217 05081610 0271

218 05081611 0272

219 05081612 0273

220 05081613 0274

237 05082401 0291

238 05082402 0292

309 05110801 0551

310 05110802 0552

311 05110803 0553

312 05110804 0554

491 06083005 0986

492 06083006 0987

493 06083007 0988

494 06083008 0989

495 06083009 0990

meanSD

minmax

rangeN


[ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [u g/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/kg] [ug/ kg] [ug/kg] [ug/kg]0.24 0.96 0.16 0.03 0.31 0.08 0.45 0.11 0.35 0.04 0.32 0.04 2.05 2.21 172.83 0.00 0.010.77 3.72 1.39 0.82 1.56 0.30 0.17 0.07 0.77 0.16 0.19 0.10 1.73 0.53 1.31 0.00 0.19

0.32 1.99 0.83 0.47 1.33 0.17 0.20 0.06 0.18 0.00 0.13 0.14 0.20 0.28 1.16 0.00 0.01

0.49 2.06 0.61 0.32 0.43 0.27 0.03 0.04 0.35 0.06 0.11 0.02 0.21 0.47 0.19 0.00 0.00

2.09 12.26 4.15 2.19 7.50 0.57 0.85 0.18 1.96 0.17 0.54 0.15 12.42 0.59 1.03 0.00 0.38

0.27 1.61 0.64 0.33 0.37 0.11 0.04 0.03 0.28 0.13 0.06 0.02 0.02 1.36 0.02 0.16 0.00

0.34 2.34 0.71 0.46 0.30 0.19 0.01 0.06 0.50 0.25 0.11 0.05 0.09 0.40 0.39 0.05 0.00

0.42 3.29 0.99 0.48 1.07 0.20 0.11 0.04 0.60 0.18 0.14 0.02 1.47 0.50 0.06 0.02 0.02

2.00 9.18 1.13 0.23 5.30 0.44 0.75 0.08 0.49 0.14 0.20 0.02 0.41 0.30 9.72 0.00 0.17

0.78 2.29 1.97 1.35 1.57 0.23 0.09 0.01 0.52 0.35 0.09 0.19 0.68 0.05 1.19 0.00 0.15

1.80 8.26 3.45 1.69 6.21 0.34 0.61 0.09 1.89 0.32 0.37 0.04 5.97 0.29 4.06 0.88 0.24

0.99 1.86 1.24 0.78 1.06 0.56 0.03 0.06 0.93 0.10 0.20 0.12 0.50 0.45 0.39 0.00 0.00

1.32 5.79 1.99 1.08 3.47 0.40 0.36 0.09 0.94 0.01 0.31 0.10 8.71 1.74 1.63 0.00 0.23

0.16 0.92 0.68 0.40 0.32 0.10 0.04 0.02 0.17 0.33 0.06 0.01 0.16 0.12 0.75 0.97 0.07

1.13 1.79 0.47 0.20 0.63 0.47 0.02 0.03 0.30 0.05 0.12 0.04 0.17 0.51 0.05 0.00 0.03

1.07 3.37 1.26 1.06 1.98 0.52 0.19 0.07 1.27 0.09 0.26 0.13 2.23 0.73 0.31 0.00 0.12

1.49 4.57 2.81 1.70 2.34 0.77 0.19 0.10 1.58 0.24 0.28 0.12 3.21 0.47 0.82 0.00 0.12

0.48 3.72 1.25 0.72 1.96 0.13 0.17 0.04 0.57 0.14 0.12 0.01 1.59 0.97 1.61 0.46 0.00

0.08 0.32 0.00 0.00 0.99 0.34 0.06 0.02 0.07 0.00 0.16 0.11 0.97 0.21 1.13 0.00 0.00

0.97 2.45 1.26 0.75 1.57 0.34 0.10 0.02 0.44 0.00 0.16 0.07 0.74 0.27 0.04 0.00 0.06

1.08 8.80 7.32 4.44 8.67 0.20 0.58 0.08 1.65 0.25 0.33 0.06 5.31 0.19 3.86 0.95 0.17

3.72 26.75 18.19 10.44 21.81 0.92 2.05 0.28 5.08 0.11 0.97 0.26 21.99 0.56 3.51 0.00 0.70

5.25 26.82 14.37 8.55 20.89 0.99 2.00 0.27 5.46 0.44 1.16 0.19 2.75 0.14 3.46 0.92 0.30

0.65 1.57 0.76 0.41 1.25 0.52 0.11 0.05 0.46 0.00 0.17 0.11 1.90 0.26 0.50 0.00 0.00

0.79 4.59 3.99 2.37 3.30 0.25 0.39 0.06 0.87 0.39 0.24 0.04 3.74 0.19 0.81 1.07 0.11Pr 141 Nd 142 Sm 152 Eu 153 Gd 158 Tb 159 Dy 164 Ho 165 Er 166 Tm 169 Yb 174 Lu 175 Hf 180 Ta 181 W 184 Re 187 Ir 1930.60 2.69 1.17 0.67 1.54 0.19 0.17 0.04 0.52 0.17 0.14 0.04 1.80 0.72 4.32 0.25 0.080.75 4.59 2.46 1.44 3.39 0.19 0.32 0.05 0.84 0.15 0.17 0.05 4.39 1.48 18.89 0.38 0.100.04 0.16 0.00 0.00 0.08 0.00 0.01 0.00 0.00 0.00 0.01 0.00 0.02 0.05 0.02 0.00 0.005.25 26.82 18.19 10.44 21.81 0.99 2.05 0.28 5.46 0.51 1.16 0.26 34.38 12.08 172.83 1.25 0.705.21 26.65 18.19 10.43 21.73 0.98 2.04 0.28 5.46 0.51 1.15 0.26 34.36 12.03 172.81 1.25 0.70101 101 101 101 101 101 101 101 101 101 101 101 101 101 101 101 101

BBOP Wales Page 87


# Reference # MLC #

1 W08022101 W0001


10 W08022704 W001011 W08022705 W0011


25 W08052201 W0028


Pt 195 Hg 202

[ug/kg] [ug/kg]

1.41 0.69

1.05 0.192.01 0.920.34 2.271.02 0.610.65 0.770.72 0.451.66 1.662.96 0.40

174.52 0.360.80 0.36

0.83 0.551.72 2.841.72 0.003.07 1.161.05 1.772.35 1.542.98 1.431.73 0.001.29 0.001.02 0.541.41 1.562.49 0.53

0.85 0.33

0.76 0.131.01 0.501.81 0.670.96 2.112.58 6.831.27 1.380.75 0.730.34 2.022.92 0.620.34 1.04

69.02 0.255.16 0.66

53.15 0.0630.31 0.00

BBOP Wales Page 88




90 W09052704 W009491 W09052705 W009592 W09052706 W0096

93 05020801 0117

93 W09052707 W0097

Pt 195 Hg 202

[ug/kg] [ug/kg]54.37 0.34

107.75 0.0021.05 0.40

126.47 0.0038.66 0.7681.42 0.0090.17 0.0078.02 0.0337.03 0.0059.02 0.00

118.76 0.007.07 0.35

151.28 0.0080.42 0.0081.29 0.001.02 0.000.20 0.000.34 0.000.34 0.001.42 0.001.83 0.151.24 0.001.73 0.000.34 0.00

2.05 0.000.84 0.000.39 0.240.69 0.001.88 0.000.38 0.001.36 0.002.73 0.000.34 2.14

0.56 0.660.34 1.720.34 1.34

3.47 1.210.34 1.70

BBOP Wales Page 89


# Reference # MLC #94 05020802 011894 W09052708 W0098

95 05020803 0119

95 W09052709 W0099

96 W09052710 W0100

97 W09052711 W0101

98 W09052712 W0102

99 W09052713 W0103

136 05042801 0183

216 05081609 0270

217 05081610 0271

218 05081611 0272

219 05081612 0273

220 05081613 0274

237 05082401 0291

238 05082402 0292

309 05110801 0551

310 05110802 0552

311 05110803 0553

312 05110804 0554

491 06083005 0986

492 06083006 0987

493 06083007 0988

494 06083008 0989

495 06083009 0990

meanSD

minmax

rangeN

Pt 195 Hg 202

[ug/kg] [ug/kg]4.89 2.480.34 1.13

9.17 1.34

0.34 0.61

0.34 2.45

1.02 0.32

0.34 0.33

0.34 1.92

2.58 1.94

0.34 0.00

0.57 0.00

1.16 0.00

3.10 0.00

1.31 0.21

5.95 23.27

1.29 0.00

0.45 0.94

2.17 0.17

3.51 0.56

4.22 0.11

1.90 0.31

0.34 0.00

1.90 0.10

2.44 0.00

2.59 0.00Pt 195 Hg 20215.74 0.8635.02 2.440.20 0.00

174.52 23.27174.33 23.27

101 101

BBOP Wales Page 90


Section 12: Appendix II – SOP for the measurement of HCNS stable isotope ratios in beef

Page 91

STANDARD OPERATING PROCEDURE (SOP)

Version 1.1, October, 2011

STANDARD OPERATING PROCEDURE FOR THE DETERMINATION OF

THE HYDROGEN, CARBON, NITROGEN AND SULPHUR STABLE ISOTOPE COMPOSITION OF UNCOOKED BEEF MEAT

Prepared by _________________________ Date October 2011

Dr Simon Kelly, Food & Environment research Agency

Approved by Authenticity Methodology Working Group Date 14th July 2011



Page 92

CONTENTS

HISTORY / BACKGROUND ....................................................................................................93

Background............................................................................................................................................................ 93

PURPOSE .................................................................................................................................93

SCOPE ......................................................................................................................................93

DEFINITIONS AND ABBREVIATIONS ..................................................................................93

PRINCIPLE OF THE METHOD ..............................................................................................95

Preparation of the beef for isotope analysis ................................................................................................................ 95

Simultaneous carbon and nitrogen stable isotope analysis ............................................................................................ 95

Hydrogen stable isotope analysis .............................................................................................................................. 95

Sulphur stable isotope analysis ................................................................................................................................. 95

MATERIALS AND EQUIPMENT ............................................................................................96

Chemicals .............................................................................................................................................................. 96

Standards and reference materials ............................................................................................................................. 97

Equipment ............................................................................................................................................................. 97

PROCEDURES .........................................................................................................................98

Sample preparation ................................................................................................................................................. 98

Measurement of δ13C‰ and δ15N‰........................................................................................................................... 98

Preparation of combustion and reduction reactors ...................................................................................................... 99

Preparation of Reference Materials and samples for δ13C and δ15N analysis................................................................... 99

δ13C‰ and δ15N‰ analysis - Batch protocol .............................................................................................................. 99

Correction of measured δ13C‰ and δ15N‰ data ....................................................................................................... 100

Quality Assurance of δ13C‰ and δ15N‰ analyses ..................................................................................................... 100

Quality of ‘fat free dry mass’ .................................................................................................................................. 100

Absolute difference between duplicate δ13C‰ and δ15N‰ measurements ..................................................................... 101

δ13C‰ and δ15N‰ Measurement of Bovine milk casein Inter-lab Comparison material (casein ICM) ............................. 101

Measurment of L-glutamic acid reference material (USGS40) .................................................................................... 101

Measurement of δ2H‰ .......................................................................................................................................... 101

Preparation of the high temperature elemental analyser reaction tube ......................................................................... 101

Preparation of Reference Materials and samples for δ2H‰ analysis ........................................................................... 102

Comparative equilibration of protein samples for δ2H‰ analysis ............................................................................... 102

δ2H‰ analysis - Batch protocol .............................................................................................................................. 103

H3+ correction of measured δ2H‰ results ................................................................................................................ 103

Correction for protein exchangeable hydrogen ......................................................................................................... 103

Quality Assurance of δ2H‰ analyses ...................................................................................................................... 104

Standard deviation (σn-1) of triplicate δ2H‰ measurements ...................................................................................... 104

δ2H‰ Measurement of collagen Inter-comparison Material (collagen ICM) ................................................................ 104

IAEA primary standards ........................................................................................................................................ 104

Measurement of δ34S‰ .......................................................................................................................................... 105

Preparation of combustion/reduction reactor ........................................................................................................... 105

Preparation of Reference Materials and samples for δ34S analysis .............................................................................. 105

δ34S‰ analysis - Batch protocol ............................................................................................................................. 106

Correction of measured δ34S‰ data ........................................................................................................................ 106

Quality Assurance of δ34S‰ analyses ...................................................................................................................... 107

Standard deviation (σn-1) of triplicate δ34S‰ measurements ...................................................................................... 107

δ34S‰ Measurement of collagen Inter-comparison Material (collagen ICM) ................................................................ 107



Page 93

HISTORY / BACKGROUND

Background

The introduction of pan-European compulsory beef labelling rules, from the 1st September 2000

onwards [(EC) No 2772/1999] was designed to provide consumer’s with correct, complete and transparent information to enable them to make an informed choice on the type and origin of beef they purchased1. The natural variation, or fractionation, that occurs in the isotopic content of the bio-elements, hydrogen carbon, nitrogen, and oxygen may be exploited to determine the geographical origin of beef and dietary patterns that can act as proxies for the identification of provenance. In addition, multi-element screening may be used to identify macro-, micro- or trace-elements that indicate origin. In some instances comparison of one or two variables is sufficient to discriminate geographical origins; for example, carbon stable isotope ratios of beef fat-free dry mass indicate the quantity of maize in the diet and this leads to useful ‘screening’ discrimination of UK and Brazilian beef. Discriminant analysis of the stable isotope and multi-element data permits simultaneous

comparison of several origins on a global and regional scale and quantitative assessment of correct classification and identification of the most useful elements for geographical discrimination.

PURPOSE

The SOP is designed to provide a reliable measurement of the hydrogen, carbon, nitrogen and sulphur stable isotope composition of defatted, uncooked beef skeletal muscle.

SCOPE

The methods described in this SOP are for the measurement of the δ2H‰, δ13C‰, δ15N‰ and δ34S‰ value of beef defatted dry mass to aid in the determination of its geographical origin. The supplementary determination of 87Sr/86Sr ratio and/or trace element composition may serve as further confirmation of origin.

DEFINITIONS AND ABBREVIATIONS

δ2H‰, δ2H‰VSMOW "Delta deuterium per mil''. The 2H/1H ratio expressed relative to the

international standard VSMOW.

2H/1H The ratio of the isotope of hydrogen with atomic mass 2 to the isotope of

hydrogen with atomic mass 1.

VSMOW Vienna Standard Mean Ocean Water used as an international standard for

which the 2H/1H ratio is precisely known and is defined as 0 ‰ on the δ2H

scale.

δ13C‰, δ13C‰PDB "Delta carbon-13 per mil''. The 13C/12C ratio expressed relative to the

international standard Pee Dee Belemnite.

1 Council Regulation (EC) No 2772/1999, Official Journal, 1999, L334, 0001–0002.



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13C/12C The ratio of the isotope of carbon with atomic mass 13 to the isotope of

carbon with atomic mass 12

PDB Pee Dee Belemnite - Calcium carbonate used as an international standard for which the 13C/12C ratio is precisely known and is defined as 0 ‰ on the δ13C scale.

δ15N‰, δ15N‰AIR "Delta nitrogen-15 per mil''. The 15N/14N ratio expressed relative to the

international standard AIR.

15N/14N The ratio of the isotope of nitrogen with atomic mass 15 to the isotope of

nitrogen with atomic mass 14.

δ34S‰, δ34S‰CDT "Delta sulphur-34 per mil''. The 34S/32S ratio expressed relative to the

international standard CDT.

34S/32S The ratio of the isotope of sulphur with atomic mass 34 to the isotope of

sulphur with atomic mass 32.

CDT Cañon Diablo Troilite used as an international standard for which the

34S/32S ratio is precisely known and is defined as 0 ‰ on the δ34S scale.

AIR AIR - atmospheric air used as an international standard for which the 15N/14N ratio is precisely known and is defined as 0 ‰ on the δ15N scale.

EA Elemental Analyser

ICM Inter-Comparison Material

sd The sample standard deviation of the mean, (n - 1)

IRMS Isotope Ratio Mass Spectrometry



Page 95

PRINCIPLE OF THE METHOD

Preparation of the beef for isotope analysis

The beef is cut into small pieces and is dried completely with the aid of a lyophiliser (freeze-drier).

The dried pieces are homogenized with a suitable grinder. The resultant dry powder is extracted with petroleum ether for 6 hours in a Soxhlet-apparatus. Afterwards the fat free dry mass (FFDM) can be stored in an appropriate container in a vacuum desiccator until measurement.

Simultaneous carbon and nitrogen stable isotope analysis

Approximately 1 milligram of FFDM is placed in a tin capsule to provide sufficient carbon and nitrogen for the isotope analysis. The tin capsule is sealed and dropped into an elemental analyser reaction tube containing chromium oxide maintained at 1020˚C. The sample is quantitatively

converted into carbon dioxide, nitrogen oxides and water in the presence of an excess of oxygen. The combustion products pass into a second reactor at 650˚C that quantitatively coverts nitrogen oxides to dinitrogen gas. Water is then removed from the carrier stream by a chemical trap containing drying agent and the carbon dioxide and nitrogen are separated on a packed GC column. The GC effluent then flows into the stable isotope ratio mass spectrometer via an interface and the ratio of the isotopologues of nitrogen and carbon dioxide are determined against nitrogen and carbon dioxide reference materials or gasses of known 15N/14N and 13C/12C ratios versus accepted international standards.

Hydrogen stable isotope analysis

Approximately 1 milligram of FFDM is placed in a silver capsule to provide approximately 100 µg and 100 µg of hydrogen. The capsule is equilibrated with appropriate standards to allow for exchange of labile hydrogen with ambient lab air. The capsules are then dried over phosphorous pentoxide in a vacuum desiccator. The capsule is then sealed and dropped into a high temperature elemental analyser reaction tube, lined with glassy carbon and containing glassy carbon chips as a support material. Depending on the system in use the furnace will be maintained between 1260˚C to 1450˚C. Depending on the elemental composition, the sample is converted into hydrogen, carbon monoxide, nitrogen, nitrogen monoxide and elemental carbon. The pyrolysis products pass through a packed GC column that separates hydrogen from the other gaseous pyrolysis products. The GC effluent then

flows into the stable isotope ratio mass spectrometer via an interface and the ratio of the isotopologues of hydrogen are determined against a reference material or gas of known 2H/1H ratio versus accepted international standards.

Sulphur stable isotope analysis

Sufficient test material is placed in a tin capsule to provide approximately 100 µg of sulphur. The tin capsule is sealed and dropped into an elemental analyser reaction tube containing tungstic oxide in the upper section and copper in the lower section. The reactor is maintained at 1050˚C. The sample is

quantitatively converted, in an oxygen atmosphere, in the upper part of the tube into carbon dioxide, nitrogen oxides, sulphur oxides and water. The combustion products pass into the lower part of the reactor containing copper, which quantitatively converts sulphur oxides into copper sulphate. The copper sulphate thermally decomposes to form sulphur dioxide gas. Water is then removed from the carrier stream by a chemical trap containing phosphorous pentoxide and the carbon dioxide and nitrogen are separated from sulphur dioxide on a packed PTFE GC column. The GC effluent then



Page 96

flows into the stable isotope ratio mass spectrometer via an interface and the ratio of the isotopologues of sulphur dioxide are determined against reference materials or gasses of known 34S/32S ratios versus accepted international standards.

MATERIALS AND EQUIPMENT

Chemicals

5.1.1 Petroleum ether, boiling range 40-60°C Supplier: Riedel-de Haën, Cat. no. 32246-2.5L Directions for Safe Handling: Do not breathe vapor. Avoid contact with eyes, skin, and clothing. Avoid prolonged or repeated exposure. Conditions of Storage: Keep container closed. Keep away from heat, sparks, and open flames.

5.1.2 Chromium oxide Empirical Formula (Hill Notation): Cr2O3, Formula Weight: 151.99 Supplier: Elemental Microanalysis, Cat. No. B1179 Directions for Safe Handling: Avoid inhalation. Avoid contact with eyes, skin, and clothing. Avoid prolonged or repeated exposure. Conditions of Storage: Keep tightly closed.

5.1.3 Tungstic oxide Empirical Formula (Hill Notation): WO3, Formula Weight: 231.84 Supplier: Elemental Microanalysis, Cat. No. B1025 Directions for Safe Handling: Avoid inhalation. Avoid contact with eyes, skin, and clothing. Avoid prolonged or repeated exposure. Conditions of Storage: Keep tightly closed.

5.1.4 Silvered copper oxide Supplier: Elemental Microanalysis, Cat. No. B1070 Directions for Safe Handling: Avoid breathing dust. Do not get in eyes, on skin, on clothing. Avoid prolonged or repeated exposure. Conditions of Storage: Keep tightly closed. Store in a cool dry place.

5.1.5 Copper wires, reduced Empirical Formula (Hill Notation): Cu, Formula Weight: 63.55 Supplier: Elemental Microanalysis, Cat. No. B1213 Not hazardous according to Directive 67/548/EEC.

5.1.6 Magnesium perchlorate (dessicant) Linear Formula: Mg(ClO4)2, Formula Weight: 223.21 Supplier: Elemental Microanalysis, Cat. No. B1101 Directions for Safe Handling: Avoid breathing dust. Do not get in eyes, on skin, on clothing. Avoid prolonged or repeated exposure. Conditions of Storage: Keep tightly closed. Store in a cool dry place. Unsuitable: Do not store near, nor allow contact with, clothing and other combustible material.

5.1.7 Phosphorous pentoxide (dessicant) Linear Formula: P2O5, Formula Weight: 283.89 Supplier: Elemental Microanalysis, Cat. No. B1197 Directions for Safe Handling: Avoid generation of dusts. Avoid contact with skin an eyes. Wear appropriate protective clothing. Wash hands and face thoroughly after working with material. Contaminated clothing should be removed and washed before re-use. Conditions of Storage: Store at room temperature (15 to 25˚C recommended). Keep well closed and protected from direct sunlight and moisture. Store away from combustible materials.



Page 97

5.1.8 Gassy carbon Supplier: Elemental Microanalysis, Cat. No. C7002 Not hazardous according to Directive 67/548/EEC.

Standards and reference materials

L-glutamic acid is a non-essential amino acid, supplied by the International Atomic Energy Agency, with an accepted δ13C‰ value of -26.39‰ versus PDB and a δ15N‰ value of -4.5‰ versus AIR. Supplier: IAEA (Vienna), Cat. No. USGS40 Storage: At room temperature, under vacuum over anhydrous silica gel.

Casein Inter-laboratory Comparison Material (casein ICM working standard). This industrial bovine milk casein material has been characterised by TRACE participant stable isotope laboratories and has a nominal δ

13C‰ versus PDB of -23.35‰; a δ15N‰ value of +6.15‰ versus AIR; a δ2H‰ value of -113.0‰ versus V-SMOW and a δ34S‰ value of 4.4‰ versus CDT Storage: At room temperature, under vacuum over anhydrous silica gel.

Collagen Inter-laboratory Comparison Material (collagen ICM working standard). This industrial porcine collagen material has been characterised by TRACE participant stable isotope laboratories and has a nominal δ

13C‰ versus Pee Dee Belemnite of -17.98‰; a δ

15N‰ value of +6.12‰ versus AIR; a δ2H‰ value of -65.9‰ versus V-SMOW and a δ34S‰ value of 5.2‰ versus CDT Storage: At room temperature, under vacuum over anhydrous silica gel.

Equipment

5.3.1 Teflon chopping board

5.3.2 Knives(ceramic)

5.3.3 Wide neck bottles with filter cap (600ml) for freeze-drying

5.3.4 Freeze-dryer, e.g. Christ, Alpha 1-4 e.g. Christ Cat. No. 127415

5.3.5 Mulinette food processor with insert

5.3.6 Pair of scissors (ceramic)

5.3.7 Agate pestle and mortar

5.3.8 Quartz extraction thimble, 33 x 118mm, e.g. Schleicher & Schuell Cat. No. 10350245

5.3.9 Quartz wool e.g. Microelemental Analysis Cat. No. B1017

5.3.10 Quartz filters, 150 mm, e.g. Schleicher & Schuell Cat. No. 312545

5.3.11 Soxhlet- extraction apparatus (with 150ml extractor)

5.3.12 Iso-mantle heater

5.3.13 round-bottomed flask (250ml)

5.3.14 Analytical mill, e. g. Fa. IKA

5.3.15 Securitainers, 35ml

5.3.16 Rotating evaporator

5.3.17 Evaporator with heating module and nitrogen facility, e.g. Barkey

5.3.18 Tin capsules for solid samples (3,3 x 5 m); e.g. Microelemental Analysis

5.3.19 Flat-nose tweezers



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5.3.20 Elemental analyser (EA)

5.3.21 Isotope Ratio Mass Spectrometer (IRMS)

5.3.22 Silver capsules for solid samples (3,3 x 5 m); e.g. Microelemental Analysis

PROCEDURES

Sample preparation

Cut 100g of lean beef meat into small pieces of approximately 1cm3 using a clean ceramic knife and a

Teflon chopping board (5.3.1; 5.3.2). The chopping process is aided by using partially rather than fully thawed meat. These pieces are placed in a suitable receptacle (5.3.3) and connected to/placed in a freeze dryer (5.3.4). The beef is freeze dried for 48 hours. Conditions will vary according to Freeze-dryer manufacturer and vacuum system performance. Consequently, completeness of drying can be determined by removing samples from the freeze drier and checking the temperature of the sample container (by hand): a cold container indicates remnants of ice in the sample. Alternatively, in a gas-tight freeze-drier system the vacuum may be temporarily iso-lated from the drier and a sharp rise in pressure indicates a significant vapour pressure from the samples. The dry meat is homogenized afterwards with the help of a Mulinette (5.3.5) [IRMS only] or ceramic scissors (5.3.6) and an agate pestle and

mortar (5.3.7) if the subsample is to be used for elemental profiling or strontium isotope analysis. Approximately 40g of the beef dry mass is placed in an extraction thimble (5.3.8) and closed with quartz wool (5.3.9) in a folded filter (5.3.10). NOTE 1: The quartz wool has to be separated from the sample with a piece of filter paper to prevent quartz wool fibres contaminating the beef sample. NOTE 2: The quartz wool should be placed tightly into the extraction thimble to prevent the petroleum ether, and therefore the lipid, becoming contaminated with the "dry matter" of the sample. The meat is extracted for a minimum of 6 h with 200ml of boiling and condensed petroleum ether (5.1.1) in a Soxhlet apparatus (5.3.11; 5.3.12) with round bottomed flask (5.3.13) or equivalent Soxtech instrument.

The round-bottomed flask with the extracted fat is stored and the extraction thimble containing the fat free dry mass (FFDM) stays over-night in the Soxhlet apparatus until the solvent has completely evaporated. Alternatively, to speed-up the drying process, remove the thimble from the Soxhlet apparatus, remove the quartz wool and filter paper, and leave the thimble containing the FFDM to stand for several hours in a fume cupboard to allow any remaining solvent to evaporate. Drying is also facilitated by breaking-up the compacted mass of FFDM before leaving it to air dry.. The solvent-free FFDM is homogenized in an analytical mill (5.3.14) [IRMS only] or homogenised using ceramic scissors and an agate pestle and mortar (5.3.6; 5.3.7). The samples are stored in air-tight container (4.15) until measurement.

Measurement of δ13C‰ and δ15N‰

The information given in this section is for general guidance only. For example, it is accepted that the configuration of specific elemental anlaysers and gas isotope ratio mass spectrometers will vary according to manufacturer’s requirements. Similarly the quantity of test material required to obtain reliable δ13C‰ and δ15N‰ results will vary according to the instrument manufacturer and the age of the instrument.



Page 99

Consequently it is recognised that demonstration of and adherence to agreed Quality Assurance

principles outlined below are essential.

Preparation of combustion and reduction reactors

Combustion reactor Reduction reactor Moisture trap

Figure 1: Configuration of combustion, reduction and drying tubes for production of CO2 and N2 from bulk organic materials

Preparation of Reference Materials and samples for δ13C and δ15N analysis

Into a pressed tin capsule (5.1.1), weigh accurately about 1 ± 0.2 mg of solid test or reference material,

or sufficient to give an equivalent of 100 µg of nitrogen for δ15N analysis or 100 µg of carbon (after

dilution) for δ13C analysis. Fold and seal the capsule with a pair of flat nosed tweezers (5.3.1.9).

δ13C‰ and δ15N‰ analysis - Batch protocol

Blank capsules must be included in the batch of samples for analysis. A duplicate anlysis of the

collagen Inter-Comparison Material (5.2.2) should be included every 20 analyses. This standard is

included after every 10th sample pair (as shown in section 6.2.4 below). Sufficient standards should be

located in the batch to permit reliable drift correction over the duration of the analysis. Batches consist

of multiples of this standard/samples/standard sequence. Every 10th batch must also include at least

Quartz wool (1 cm)

Quartz wool (1 cm)

Chromium oxide (11 cm)

Quartz wool (1 cm)

Silvered cobalt

oxide (6 cm)

Quartz wool ( 4 cm)

Copper wires,

(reduced)

Quartz wool ( 4 cm)

Quartz wool (1 cm)

Quartz wool (1 cm)

Magnesium

perchlorate

(anhydrous)



Page 100

one duplicate measurement of International Atomic Energy Association reference material L-glutamic

acid (USGS 40) (5.2.1).

Correction of measured δ13C‰ and δ15N‰ data

The measured δ13C‰ and δ15N‰ of the FFDM samples should be corrected according to the

difference between the measured δ13C‰ and δ15N‰ values of the collagen ICM working standard and

its accepted values of -17.98 ‰PDB and +6.12‰AIR respectively2. In the example below the accepted

δ13C‰ of the collagen ICM is subtracted from the measured δ13C‰ values across the analytical batch.

These ‘correction factors’ are then plotted against corresponding positions (line numbers) at which the

collagen ICMs were measured in the analytical batch. A correction for each of the 10 samples between

consecutive collagen ICMs is then calculated by substituting the sample position (line number) into the

equation of the regression line.

Raw Correction Corrected mean absolute

Line Identifier 1 δδδδ13C‰PDB Linear interploation factor δδδδ13C‰PDB δδδδ13C‰PDB difference n

1 Dummy -25.892 empty capsule not detected3 empty capsule not detected4 collagen ICM -17.50 0.35 -17.855 collagen ICM -17.62 0.35 -17.976 sample A replicate 1 -22.84 0.34 -23.18 -23.22 0.06 27 sample A replicate 2 -22.91 0.34 -23.258 sample B replicate 1 -17.08 0.33 -17.41 -17.45 0.07 29 sample B replicate 2 -17.16 0.33 -17.48

10 sample C replicate 1 -23.42 0.32 -23.75 -23.80 0.11 211 sample C replicate 2 -23.54 0.32 -23.8612 sample D replicate 1 -17.46 0.32 -17.78 -17.78 0.00 213 sample D replicate 2 -17.47 0.31 -17.7814 sample E replicate 1 -16.98 0.31 -17.28 -17.27 0.03 215 sample E replicate 2 -16.95 0.30 -17.2516 collagen ICM -17.66 0.30 -17.9517 collagen ICM -17.74 0.29 -18.03

y = -0.0048x + 0.3727

0.0

0.1

0.1

0.2

0.2

0.3

0.3

0.4

0.4

0.5

0.5

0 20 40 60

Line number (sample position)

Diff

eren

ce fr

om a

ccep

ted

colla

gen

ICM

valu

e δδ δδ13

C‰

The mean of the two δ13C‰ corrected values is then calculated and the absolute difference between the

two results. δ15N‰ data are corrected in the same way by making a linear interpolation between the

values of the differences between the accepted value of +6.12‰ for the collagen ICM and the

measurements.

Quality Assurance of δ13C‰ and δ15N‰ analyses

Quality of ‘fat free dry mass’

In general the quality of the FFDM (‘protein fraction’) can be checked by measuring the carbon:

nitrogen ratio (C:N, which should be about 3.45 for meat protein and casein (46 –47 % carbon and 14

% nitrogen). A good homogenisation ensures acceptable repeatability of the isotopic measurements as

the FFDM still contains material of different isotopic and elemental composition (muscle tissue

protein, soluble protein and collagen). This can be achieved routinely by taking the ratio of the

combined area (‘area all [Vs]’) value for CO2 and N2 gas measured by the isotope ratio mass

2 Jamin E et al., (2004) AOAC International, 87 (3) 621-631



Page 101

spectrometer. If these criteria are not met then the samples should be re-prepared from the original

tissue.

Absolute difference between duplicate δ

13C‰ and δ15N‰ measurements

The absolute difference between duplicate measurements of FFDM and reference materials, should be

less than or equal to 0.2‰ for δ13C‰ and less than or equal to 0.3‰ for δ

15N‰. If these criteria are

not met the sample should be re-analysed in duplicate.

δ13C‰ and δ15N‰ Measurement of Bovine milk casein Inter-lab Comparison material (casein ICM)

The absolute difference between the measured values for the casein ICM and the accepted δ13C‰

value of -23.35‰ PDB and δ15N‰ value of +6.15 AIR should be less than or equal to 0.2‰ and 0.3‰

respectively. If these criteria are not met the analytical batch should be repeated.

Measurment of L-glutamic acid reference material (USGS40)

The absolute difference between the measured values for the USGS40 reference material and the

accepted δ13C‰ value of -26.39‰PDB and δ15N‰ value of -4.5‰AIR should be less than or equal to

0.2‰ and 0.3‰ respectively. If these criteria are not met the analytical batch should be repeated.

Measurement of δ2H‰

As with the measurement of carbon and nitrogen stable isotopes above, the information given in this

section is for general guidance only. For example, it is accepted that the maximum operating

temperatures and configurations of specific high temperature elemental anlaysers and gas isotope ratio

mass spectrometers respectively, will vary with different manufacturer’s specifications. Similarly the

quantity of test material required to obtain reliable δ2H‰ results will vary according to the instrument

manufacturer and the age of the instrument.

Preparation of the high temperature elemental analyser reaction tube

There are a number of acceptable reactor tube configurations that can be used to pyrolyse organic

samples. Temperatures may also vary depending on instrument manufacturer. It is not possible to

specify one set of conditions because there will be temperature and configuration restraints specific to

each manufacturer. Some of reactor configurations and temperatures are summarised below with the

corresponding literature reference.



Page 102

45 cm

1 cm quartz wool

4 cm quartz wool

17.5 cm glassy

carbon

Werner et al (1996)1080°C

4 cm quartz wool

glassy

carbon

quartz tube Glassy carbon

tube

Graphite crucible

Carbon powder

Koziet et al (1997)1300°C

1 cm Nickel wool

4 cm quartz wool

14.5 cm glassy

carbon

Farquhar et al (1996)1080°C

quartz tube

1 cm quartz wool

2 cm Nickelised

carbon

Carbon felt

4 cm quartz wool

glassy

carbon

Glassy carbon

tube

Graphite crucible

Nickelised Carbon

Kornexl et al (1999)1450°C

Carbon felt

55 cm

quartz tube

1 cm quartz wool

5 cm graphite chips

Inside graphite liner

Costech(2004)1700°C

Preparation of Reference Materials and samples for δ2H‰ analysis

Weigh accurately about 1 mg of solid test or reference material ± 0.2 mg, or sufficient to give an

equivalent of 100 μg of hydrogen for δ2H‰ analysis (see comparative equilibration below). Fold and

seal the capsule with a pair of flat nosed tweezers. Prepare samples and reference materials in

triplicate.

Comparative equilibration of protein samples for δ2H‰ analysis

Hydrogen stable isotope analysis of proteins has to take into account that about ~17 % of the total

hydrogen present is exchangeable. This requires specific methods to account for the variability of

hydrogen isotopic ratios from labile positions depending on the hydrogen isotopic ratio of ambient air

humidity. This problem can be solved using the recently described “comparative equilibration

technique” 3. After the sample and reference capsules have been weighed they are left unsealed in a

covered sample tray in ambient lab air for 96 hours. The capsules are then dried over phosphorous

pentoxide in a vacuum desiccator for 24 hours. The capsule is then sealed and placed in a helium

purged zero-blank auto-sampler prior to analysis.

3 Wassenar LI, Hobson KA (2003). Comparative equilibration and online technique for determination of non-exchangeable

hydrogen of keratins for use in animal migration studies. Isotopes Environm. Health Stud. 39 (3), 211-217.



Page 103

δ2H‰ analysis - Batch protocol

Blank capsules must be included. A triplicate casein ICM must be included every 15 analyses to

normalise the effects exchangeable hydrogen in protein samples. A triplicate analysis of the collagen

inter-comparison material (collagen ICM) should be included every 20 samples to ensure the

comparative equilibration has worked correctly. This standard is included after every 10th sample pair

(as shown below). Sufficient casein ICMs should be located in the batch to permit reliable drift

correction over the duration of the analysis. Batches consist of multiples of this

standard/samples/standard sequence (shown below).

1 Dummy (conditioning sample) 2 blank (empty tin capsule) 3 blank (empty tin capsule) 4 casein ICM 5 casein ICM 6 casein ICM 7 sample 1a 8 sample 1b 9 sample 1c 10 sample 2a 11 sample 2b 12 sample 2c 13 collagen ICM 14 collagen ICM 15 collagen ICM 16 sample 3a 17 sample 3b 18 sample 3c 19 sample 4a 20 sample 4b 21 sample 4c 22 casein ICM 23 casein ICM 24 casein ICM 25 sample 5a 26 sample 5b 27 sample 5c etc.

H3+ correction of measured δ2H‰ results

The presence of hydrogen gas in the electron impact source of the mass spectrometer causes the

formation of H3+ (m/z 3), which is a direct isobaric interference with minor beam measuring species

2H1H+ (m/z 3). The formation of H3+ is dependent upon the pressure of hydrogen in the source and

consequently sample size. The IRMS manufacturer’s proprietary software will usually be equipped

with a facility to calibrate and compensate for the effect of for H3+ formation. It is good practice to

determine the H3+ correction prior to each batch of samples analysed. This correction must be applied

to all reported data.

Correction for protein exchangeable hydrogen

The measured δ2H‰ of the protein samples should be corrected according to the difference between

the measured δ2H‰ (H3+ corrected) values of the bovine milk casein ICM working standard and its

accepted values of -113.0‰ V SMOW. In the example below the accepted δ2H‰ of the casein ICM is



Page 104

subtracted from the measured δ2H‰ values across the analytical batch. These ‘correction factors’ are

then plotted against corresponding positions (line numbers) at which the casein ICMs were measured in

the analytical batch. A correction for each of the 15 samples between consecutive casein ICMs is then

calculated by substituting the sample position (line number) into the equation of the regression line.

The mean of the three δ2H‰ corrected values is then calculated and the sample standard deviation

(σn-1) of the results reported.

H3

+ corrected Linear interploation Correction Corrected me an standardLine Identifier 1 δδδδ2H‰V-SMOW factor δδδδ2H‰V-SMOW δδδδ2H‰V-SMOW deviation n

1 Dummy2 Blank3 Blank4 Casein IHR -108.8 4.2 3.9 -112.7 -113.3 0.5 35 Casein IHR -109.7 3.3 3.9 -113.66 Casein IHR -109.7 3.3 3.9 -113.67 sample 1a -78.3 3.9 -82.1 -82.3 0.5 38 sample 1b -79.0 3.9 -82.89 sample 1c -78.1 3.8 -81.910 sample 2a -78.2 3.8 -82.0 -84.5 2.2 311 sample 2b -82.2 3.8 -86.012 sample 2b -81.8 3.8 -85.613 collagen ICM -62.1 3.8 -65.9 -63.9 1.8 314 collagen ICM -58.7 3.7 -62.515 collagen ICM -59.6 3.7 -63.316 sample 3a -80.3 3.7 -83.9 -85.1 2.2 317 sample 3b -83.9 3.7 -87.618 sample 3c -80.0 3.6 -83.619 sample 4a -80.7 3.6 -84.3 -83.3 1.7 320 sample 4b -77.7 3.6 -81.321 sample 4c -80.7 3.6 -84.322 Casein IHR -108.5 4.5 3.6 -112.1 -112.3 0.8 323 Casein IHR -109.7 3.3 3.5 -113.224 Casein IHR -108.1 4.9 3.5 -111.6

y = -0.021x + 4.0892

0.0

1.0

2.0

3.0

4.0

5.0

6.0

0 10 20 30 40 50 60

Line number (sample position)

Diff

eren

ce fr

om a

ccep

ted

colla

gen

ICM

val

ue

δδ δδ13C

‰

Quality Assurance of δ2H‰ analyses

Standard deviation (σn-1) of triplicate δ2H‰ measurements

The standard deviation of triplicate δ2H‰ measurements of the same sample or the same reference

material (recorded as σn-1) should be less than or equal to 3.0‰ and this will be the action limit for

repeating the triplicate analysis of the sample or reference material.

δ2H‰ Measurement of collagen Inter-comparison Material (collagen ICM)

Collagen ICM δ2H‰ results are set at ± 3‰ of the mean of replicate analyses of this reference material

from the TRACE project (mean δ2H‰ = -65.9‰). After comparative equilibration and normalisation

against the casein ICM, these will be the action limits for repeating samples within the batch.

IAEA primary standards

Analysis of NBS22 should give a δ2H‰ value between -118‰ and -122‰. These will be the action

limits for repeating samples within the batch.



Page 105

Measurement of δ34S‰

The information given in this section is for general guidance only. Sulphur dioxide gas is reactive and great care must be taken to ‘pacify’ the elemental analyser gas train. This is usually achieved through the use of PTFE tubing wherever possible and a shorter PTFE Porapak column. The quantity of test

material required to obtain reliable δ34S‰ results will vary from sample to sample and according to the instrument manufacturer and the age of the instrument. Consequently, it is recognised that demonstration of and adherence to agreed Quality Assurance principles outlined below are essential. Preparation of combustion/reduction reactor

Combustion/reduction reactor Moisture trap

45 cm

Preparation of Reference Materials and samples for δ34S analysis

Weigh accurately about 8 mg of solid test or reference material ± 0.2 mg, or sufficient to give an

equivalent of 100 μg of sulphur for δ34S‰ analysis, into a pressed tin capsule. Samples should be

prepared in triplicate. Fold and seal the capsule with a pair of flat nosed tweezers.

Quartz wool (1 cm)

Quartz wool ( 2 cm)

Copper wires

(11 cm)

Quartz wool ( 4 cm)

Tungstic oxide (5cm) Phosphorus pentoxide



Page 106

δ34S‰ analysis - Batch protocol

Blank capsules must be included in the batch of samples for analysis. A triplicate analysis of the casein

Inter-laboratory Comparison Material (casein ICM) should be included batch. Alternatively this ICM

may be included after every 15th analysis (as shown below). Sufficient ICMs should be located in the

batch to permit reliable drift correction over the duration of the analysis. Batches consist of multiples

of this standard/samples/standard sequence.

1 Dummy (conditioning sample) 2 blank (empty tin capsule) 3 blank (empty tin capsule) 4 casein ICM 5 casein ICM 6 casein ICM 7 sample 1a 8 sample 1b 9 sample 1c 10 sample 2a 11 sample 2b 12 sample 2c 13 collagen ICM 14 collagen ICM 15 collagen ICM 16 sample 3a 17 sample 3b 18 sample 3c 19 sample 4a 20 sample 4b 21 sample 4c 22 casein ICM 23 casein ICM 24 casein ICM 25 sample 5a 26 sample 5b 27 sample 5c etc.

Correction of measured δ34S‰ data

The measured δ34S‰ of the FFDM samples should be corrected according to the difference between

the measured δ34S‰ value of the casein ICM working standard and its accepted values of 4.4 ‰CDT.

This process is analogous to that shown above for the accepted δ13C‰ of the collagen ICM. The

correction factors for δ34S‰ are then subtracted from the measured δ

34S‰ values across the analytical

batch. These ‘correction factors’ are then plotted against corresponding positions (line numbers) at

which the casein ICMs were measured in the analytical batch. A δ34S‰ correction for each of the 15

samples between consecutive casein ICMs is then calculated by substituting the sample position (line

number) into the equation of the regression line. The mean of the three δ34S‰ corrected values is then

calculated and the sample standard deviation (σn-1) of the results.



Page 107

Quality Assurance of δ34S‰ analyses

Standard deviation (σn-1) of triplicate δ34S‰ measurements

The standard deviation of triplicate δ34S‰ measurements of the same sample or the same reference

material (recorded as σn-1) should be less than or equal to 0.6‰ and this will be the action limit for

repeating the triplicate analysis of the sample or reference material.

δ34S‰ Measurement of collagen Inter-comparison Material (collagen ICM)

Collagen ICM δ34S‰ results are set at ± 0.6‰ of the mean of replicate analyses of this reference

material from the TRACE project (mean δ34S‰ = 5.2‰). These will be the action limits for repeating

samples within the batch.


Section 12: Appendix III – SOP for the determinati on of beef 87Sr/86Sr isotope ratios

Page 108



STANDARD OPERATING PROCEDURE FOR THE DETERMINATION OF STRONTIUM ISOTOPE RATIOS (87Sr/86Sr) IN UNCOOKED BEEF MEAT






Page 109

CONTENTS

HISTORY / BACKGROUND ..................................................................................................110

Background.......................................................................................................................................................... 110

PURPOSE ...............................................................................................................................110

SCOPE ....................................................................................................................................110

DEFINITIONS AND ABBREVIATIONS ................................................................................110

PRINCIPLE OF THE METHOD ............................................................................................111

MATERIALS AND EQUIPMENT ..........................................................................................111

Chemicals ............................................................................................................................................................ 111

Water .................................................................................................................................................................. 111

Standards and reference materials ........................................................................................................................... 111

Equipment ........................................................................................................................................................... 112

PROCEDURES .......................................................................................................................112

Sample preparation ............................................................................................................................................... 112

Dry-ashing and dissolution of ash ........................................................................................................................... 112

Preparation of Strontium-resin columns ............................................................................................................... 113

Loading, washing and elution of the Strontium-resin columns ................................................................................ 113

Thermal ionisation mass spectrometry ................................................................................................................. 113

Quality assurance of strontium isotope ratio measurements ....................................................113



Page 110


Background




PURPOSE

The SOP is designed to provide a reliable measurement of the strontium isotope ratio (87Sr/86Sr) of freeze dried uncooked beef skeletal muscle.

SCOPE

The methods described in this SOP are for the measurement of 87Sr/86Sr ratio of beef to aid in the determination of its geographical origin. The supplementary determination of the bio-element stable isotope ratios (HCNS) and/or trace element composition may serve as further confirmation of origin.


87Sr/86Sr The ratio of the isotope of strontium with atomic mass 87 to the isotope of

strontium with atomic mass 86.

TIMS Thermal Ionisation Mass Spectrometry




Page 111


The beef sample is dry-ashed and the residue dissolved in nitric acid. The nitric acid solution is then passed through a strontium-selective resin to remove interferences. The strontium is eluted and loaded onto a filament for thermal ionisation mass spectrometric analysis. The sample is gradually

heated to selectively remove any 87-Rubidium interference and the ratio of the isotope of strontium with atomic mass 87 to the isotope of strontium with atomic mass 86 (87Sr/86Sr) is determined. As mass fractionation takes place during the analysis the measured Sr-isotope ratios have to be corrected. For that purpose the naturally invariant 88Sr/86Sr ratio is used.


Chemicals

5.1.1 Nitric acid (concentrated (Ultrapure -grade)) Not less than 65% (mass fraction), with a density of approximately 1.4 kg L-1 Empirical Formula (Hill Notation): HNO3; Molecular Weight: 63.01 Supplier: Sigma-Aldrich, Cat. no. 02650 Directions for Safe Handling: Avoid inhalation of vapour or mist. Keep/Store away from clothing/ combustible materials/wear protective gloves/protective clothing/eye protection/face protection. Conditions of Storage: Keep container tightly closed in a dry and well-ventilated place. Containers which are opened must be carefully resealed and kept upright to prevent leakage. Store in cool place.

5.1.2 Strontium-selective resin 1.0M 4,4'(5')-di-t-butylcyclohexano 18-crown-6 (crown ether) in 1-octanol. Supplier: Eichrom, Cat. No. SR-B25-A Directions for Safe Handling: Avoid inhalation. Avoid contact with eyes, skin, and clothing. Avoid prolonged or repeated exposure. Conditions of Storage: Keep tightly closed.

Water

Ultra-pure deionised water (Greater than 18.2 MΩ resistivity)


National Bureau of Standards Strontium Carbonate (NBS987) Supplier: http://www.nist.gov/srm/ Cat. No. SRM 987 Absolute abundance ratios 88Sr/86Sr = 8.378 61 ± 0.003 25 87Sr/86Sr = 0.710 34 ± 0.000 26 84Sr/86Sr = 0.056 55 ± 0.000 14 Storage: At room temperature, under vacuum over anhydrous silica gel.



Page 112

Equipment








5.3.8 Quartz crucible (50ml capacity)

5.3.9 Muffle furnace capable of maintaining temperatures of 500˚C

5.3.10 pipette tips (Gilson D-200) for use as ion exchange columns

5.3.11 Perfluoroalkoxy (PFA) vials (7 ml) with caps (Savillex Inc.)

5.3.12 Ceramic tweezers

5.3.13 2.4 mm PTFE frit

5.3.14 4.0 mm PTFE frit

5.3.15 5ml syringe barrel

PROCEDURES

Sample preparation


Teflon chopping board (5.3.1; 5.3.2). The chopping process is aided by using partially rather than

fully thawed meat. These pieces are placed in a suitable receptacle (5.3.3) and connected to/placed in

a freeze dryer (5.3.4). The beef is freeze dried for 48 hours. Conditions will vary according to Freeze-

dryer manufacturer and vacuum system performance. Consequently, completeness of drying can be

determined by removing samples from the freeze drier and checking the temperature of the sample

container (by hand): a cold container indicates remnants of ice in the sample. Alternatively, in a gas-

tight freeze-drier system the vacuum may be temporarily iso-lated from the drier and a sharp rise in

pressure indicates a significant vapour pressure from the samples. The dry meat is homogenized

afterwards with an agate pestle and mortar (5.3.6) and with ceramic scissors (5.3.5) and stored in an

airtight container (5.3.7).

Dry-ashing and dissolution of ash

Weigh accurately about 200mg of the freeze dried beef into a quartz crucible (5.3.8) and place the

crucible in a muffle furnace (5.3.9). Heat the sample to 500°C for 6 hours to remove all organic

compounds. After cooling, the residual white ash is dissolved in 3M ultrapure HNO3 before being

applied to the Strontium selective resin (5.1.2).



Page 113

Preparation of Strontium-resin columns

The strontium resin (5.1.2) is slurried with 3M ultrapure HNO3 in an acid-cleaned 7 ml PFA vial

(5.3.11). Using the ceramic tweezers (5.3.12), a 2.4 mm PTFE frit (5.3.13) is dropped into a D-200

pipette tip (5.3.10). The frit is pushed down to a tight fit using a clean 200 ul pipette tip. 100-200 ul of

the resin slurry is pipetted into the column and allowed to settle for several minutes. Any air bubbles

must be expelled and there must be no air gap between the resin and the bottom frit. The resin must not

be allowed to dry out. Once sufficient resin has settled for its top surface to be about 2-3 mm above the

main joint of the D-200 tip, a 4mm PTFE frit (5.3.14) is dropped into the column (using the ceramic

tweezers) and is carefully pushed down to eliminate any air gap between it and the resin. 3M ultrapure

HNO3 is used to fill the space above the top frit to prevent drying out of the column.

Loading, washing and elution of the Strontium-resin columns

An acid-cleaned 7 ml PFA vial is placed under the tip of each column to catch the outflow. Each

sample is pipetted into a syringe barrel (5.3.15) connected to the resin filled pipette tip. The open top of

the syringe is covered with Clingfilm to prevent entry of dust. The sample is allowed to drain through

the column under gravity until about 0.1 – 0.05 ml remains, at which point 1 ml of 3M ultrapure HNO

is then pipetted into the syringe barrel and allowed to drain onto the column to wash off unbound ions.

The strontium is then eluted from the column using 1.6ml of 0.05M ultrapure HNO3 .

Thermal ionisation mass spectrometry

The strontium eluate is loaded onto a single tungsten filament and the 87Sr/86Sr measurement is

carried out on a thermal ionisation mass spectrometer (TIMS).

QUALITY ASSURANCE OF STRONTIUM ISOTOPE RATIO MEASUREMENTS

To control the quality of the measurements an international strontium standard reference material

(SrCO3, NBS 987) is analysed under the same conditions as the samples at least once a day or every 50

samples. As mass fractionation takes place during the analysis the measured Sr-isotope ratios have to

be corrected. For that purpose the naturally invariant 88Sr/86Sr = 8,37521 is used.


Section 12: Appendix IV – SOP for the measurement of elemental concentrations in beef

Page 114

FOOD STANDARDS AGENCY



STANDARD OPERATING PROCEDURE FOR THE MEASUREMENT OF

ELEMENTAL CONCENTRATIONS IN UNCOOKED BEEF MEAT






Page 115

CONTENTS

HISTORY / BACKGROUND ..................................................................................................116

Background.......................................................................................................................................................... 116

PURPOSE ...............................................................................................................................116

SCOPE ....................................................................................................................................116

DEFINITIONS AND ABBREVIATIONS ................................................................................116

PRINCIPLE OF THE METHOD ............................................................................................117

MATERIALS AND EQUIPMENT ..........................................................................................117

Chemicals ............................................................................................................................................................ 117

Water .................................................................................................................................................................. 117

Standards and reference materials ........................................................................................................................... 118

Equipment ........................................................................................................................................................... 118

PROCEDURES .......................................................................................................................118

Sample preparation ............................................................................................................................................... 118

Microwave digestion procedure .............................................................................................................................. 119

ICP-MS Measurement procedure ............................................................................................................................ 119

Quality Assurance ................................................................................................................................................. 120

APPENDIX 1 ..........................................................................................................................121



Page 116


Background




PURPOSE

The SOP is designed to provide a reliable measurement of the elemental composition of freeze dried, uncooked beef skeletal muscle.

SCOPE

This document specifies a method for the determination of elemental concentrations using Inductively

Coupled Plasma – Mass Spectrometry (ICP-MS). The test solutions will be the digest liquors resulting from the dissolution of homogenised freeze dried uncooked beef samples into nitric acid, using microwave-assisted digestion, or similar, procedures. The method has been validated for the determination of Al, As, Cd, Cr, Cu, Fe, Hg, Pb, Mn, Ni, Se, Tl and Zn in various types of food, including composite diets, cereals, rice, fish and offal. However, it can be applied to a greater range of elements, foodstuffs and sample types, but appropriate care should be taken when interpreting the data. These data may be used to aid in the determination of the geographical origin of beef. The supplementary determination of 87Sr/86Sr ratio and/or bio-element stable isotope ratios (HCNS) may serve as further confirmation of origin.


ICPMS Inductively Couple Plasma Mass Spectrometry




Page 117


The beef is cut into small pieces and is dried completely with the aid of a lyophiliser (freeze-drier). The dried pieces are homogenized with an agate pestle and mortar and/or ceramic scissors/knives. The resultant dry powder is digested in concentrated nitric acid with the aid of a microwave digester,

following EN 14804:2003. The resulting solutions are diluted with water, internal standard (s) added, and their multi-element composition determined by ICP-MS.

WARNING - The use of this method can involve hazardous materials, operations and equipment. This document does not address the safety issues associated with its use. It is the responsibility of the user of this method to establish appropriate health and safety practices.


Chemicals

5.1.1 Nitric acid (concentrated (Ultrapure -grade)) Not less than 65% (mass fraction), with a density of approximately 1.4 kg L-1 Empirical Formula (Hill Notation): HNO3; Molecular Weight: 63.01 Supplier: Sigma-Aldrich, Cat. no. 02650 Directions for Safe Handling: Avoid inhalation of vapour or mist. Keep/Store away from clothing/ combustible materials/wear protective gloves/protective clothing/eye protection/face protection. Conditions of Storage: Keep container tightly closed in a dry and well-ventilated place. Containers which are opened must be carefully resealed and kept upright to prevent leakage. Store in cool place.

5.1.2 Hydrochloric acid (Ultrapure -grade) Not less than 31% (mass fraction), with a density of approximately 1.6 kg L-1 Empirical Formula (Hill Notation): HCl; Molecular Weight: 36.46 Supplier: Sigma-Aldrich, Cat. no. 96208 Directions for Safe Handling: Avoid inhalation. Avoid contact with eyes, skin, and clothing. Avoid prolonged or repeated exposure. Conditions of Storage: Keep container tightly closed in a dry and well-ventilated place. Containers which are opened must be carefully resealed and kept upright to prevent leakage. Store in cool place.

Water

Ultra-pure deionised water (Greater than 18.2 MΩ resistivity)



Page 118


National Institute of Standards and Technology, Standard Reference Material 1547 – Peach Leaves (NIST SRM 1547) Supplier: http://www.nist.gov/srm/ Cat. No. SRM 1547 Storage: At room temperature, under vacuum over anhydrous silica gel.

National Institute of Standards and Technology, Standard Reference Material 1577a bovine liver (NIST SRM 1577a) Supplier: http://www.nist.gov/srm/ Cat. No. SRM 1577a Storage: At room temperature, under vacuum over anhydrous silica gel.

National Institute of Standards and Technology, Standard Reference Material 8414 bovine muscle (NIST SRM 8414) Supplier: http://www.nist.gov/srm/ Cat. No. SRM 8414 Storage: At room temperature, under vacuum over anhydrous silica gel.

Equipment








5.3.8 Anton Paar ‘Multiwave’ digestion system consisting of a microwave oven and a six position carrousel containing high pressure quartz vessels (or equivalent)

5.3.9 Agilent 7500ce Quadrupole Inductively Coupled Plasma-Mass Spectrometer (or equivalent)

PROCEDURES

Sample preparation


Teflon chopping board (5.3.1; 5.3.2). The chopping process is aided by using partially rather than

fully thawed meat. These pieces are placed in a suitable receptacle (5.3.3) and connected to/placed in

a freeze dryer (5.3.4). The beef is freeze dried for 48 hours. Conditions will vary according to Freeze-

dryer manufacturer and vacuum system performance. Consequently, completeness of drying can be

determined by removing samples from the freeze drier and checking the temperature of the sample

container (by hand): a cold container indicates remnants of ice in the sample. Alternatively, in a gas-

tight freeze-drier system the vacuum may be temporarily iso-lated from the drier and a sharp rise in

pressure indicates a significant vapour pressure from the samples. The dry meat is homogenized

afterwards with an agate pestle and mortar (5.3.6) and with ceramic scissors (5.3.5) and stored in an

airtight container (5.3.7).



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NOTE: All apparatus that come into contact with the sample or diluted digests are acid cleaned prior

to use (typically submerged overnight in 5% nitric acid, then rinsed carefully with Ultra-pure water

and dried in a dust free area).

Microwave digestion procedure

All samples are processed in discrete batches consisting of samples and quality control checks. The

QC checks include analytical blanks, certified reference materials and spiked blanks and/or samples,

which are randomised within the batch. The batch size is a multiple of six (the microwave capacity),

typically 24 or higher. The certified reference materials used for this work are; NIST1547 peach

leaves, NIST1577a bovine liver and reference material NIST8414 bovine muscle. Prior to starting a

batch, the quartz vessels are acid cleaned by heating 3 ml nitric acid using the microwave programme

given in Appendix 1 of this SOP. The acid is rinsed out with Ultra-pure water and the vessels/caps

shaken ‘dry’ ready for analysis.

Aliquots of sample or CRM (0.5 g dry or up to 4 g fresh weight equivalent) are weighed into their

allotted quartz vessels then 4.5 ml nitric acid (concentrated) and 0.5 ml hydrochloric acid (75%v/v)

added. Analytical blanks consist of the digestion acids only, and where appropriate, spikes are added

in a minimum amount of solution (preferably less than 1 ml). The vessels are sealed and the contents

digested in the microwave digester (5.3.8) using the programme given in Appendix 1 of this SOP.

After completion of the microwave programme, the acid digests are transferred to pre-marked plastic

test tubes and diluted to 10 ml with Ultra-pure water. The contents are vortex mixed and stood covered

until measurement. The quartz vessels and caps are rinsed with water, shaken ‘dry’ and used

immediately for the next samples until the batch is completed.

Seven calibration standards are prepared from certified stocks via serial dilution to provide three orders

of magnitude calibration in the expected concentration range for each element. Both single element

and multi-element stocks are used to create the final element cocktail and the acid strength is matched

to the diluted digest solutions above. Just prior to measurement, the standards and digest solutions are

diluted further with a solution containing internal standards (typically indium or rhodium) in dilute

nitric acid (1%v/v).

ICP-MS Measurement procedure

A method is set up to give optimum resolution settings for each element taking into consideration

spectral interferences and expected analyte levels. Typically the settings are 400 resolution for ultra

trace levels where maximum signal is required, then between 2,000 and 10,000 resolution depending

on the severity of interference, thus ensuring an accurate analyte signal. In total, a 66 element list was

selected.



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The mass spectrometer is tuned using indium in dilute acid (1% v/v) to obtain maximum signal at 400

resolution, then fine tuned to achieve clean peak shape at 10,000 resolution. After adjustments are

completed, a mass calibration is performed at specific points across the mass range from lithium to

uranium to ensure accuracy.

The diluted standards and samples are then measured and from the response curve of the standards, the

concentrations in the diluted samples can be estimated. All sample and CRM results are then corrected

for analytical blank contribution, recovery, dilution and sample weight to an estimate of the element in

the original sample.

Quality Assurance

The calibration linearity for standard metal solutions should be better than 0.99 (correlation

coefficient). Instrument drift should be less than ±20% across the analytical run. The limit of detection

is based on three standard deviations of the analytical blank variation, corrected for dilution and sample

weight. The limit of quantification is based on five standard deviations of the analytical blank

variation, corrected for dilution and sample weight. The recovery of added analyte should be within 60

to 140% for all accepted elements whilst the majority of these (75%) should be within 80 to 120%.

Agreement with certified CRM values should be within ±20% of the target value and between -50 to

100% for indicative values.



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APPENDIX 1

PE MULTIWAVE PROGRAMMES

SAMPLE DIGESTION PROGRAMME (user001h)

6 vessels 75 bar.

Step Heating power/W Time/mins Fan

1 0-500 2:00 1

2 500 5:00 1

3 500-1000 2:00 1

4 1000 20:00 1

5 0 15:00 3

Total 44:00

CLEANING PROGRAMME (user002h)

6 vessels 75 bar.

Step Heating power/W Time/mins Fan

1 1000 20:00 1

2 0 15:00 3

Total 35:00

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ACKNOWLEDGEMENTS

This research was financed by the UK Food Standards Agency as part of the Food Authenticity

Programme (Q01). The views expressed here are those of the authors and do not necessarily reflect

the views of the UK Food Standards Agency. The authors would also like to thank the Agriculture &

Horticulture Development Board/EBLEX, Hybu Cig Cymru (Meat Promotion Wales) and Quality Meat

Scotland for their involvement in this project.

Documents

THE BRITISH BEEF ORIGIN PROJECT (BBOP)