Standard Operation Protocol For ICP-MS Analysis TRACE Project

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Standard Operation Protocol

for ICP-MS analysis


TRACE Project
Taken from CSL SOP (John Lewis)
and adapted for WP1 FOM (Jurian Hoogewerff)

1. Scope

This document specifies a method for the determination of trace elements using
Inductively Coupled Plasma – Mass Spectrometry (ICP-MS).
The test solutions will be: simple solutions, such as water, digest liquors resulting
from the dissolution of samples into nitric acid or extractables from soils

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 by CSL. In the TRACE project however, it will be
applied to a greater range of elements, foodstuffs and sample types, but
appropriate care should be taken when interpreting the data.

For the TRACE project measurements the following element suite is required.

Element palette (31). The masses and calibration standards mentioned are for
guidance purposes only. (Merck VI refers to Merck VI Multi element standard,
Claritas refers to Spex Certiprep REE standard, Home made refers to single
element standard .

Notes have been included in this protocol (highlighted in italics), which are
intended to give additional information to the analyst, but which are not deemed
essential to the successful operation of the protocol. The protocol also describes
parameters used in the operation of key pieces of equipment, including power
settings, sample volumes, etc., However, laboratories using similar equipment,
but from a different manufacturer, should refer to their own instruments’ operating
instructions and manufacturers’ recommendations.
Information relating to the procedures preceding analysis of food-based samples
by ICP-MS, i.e., their dissolution into a suitable acid, etc., is given as an appendix
to this document but does not cover soil ‘extractables’. Also be aware that ISO
17294-1 and ISO 17294-2 have valuable suggestions on how to tune and
calibrate.
2. Principle

The use of ICP-MS to determine the multi-element composition of samples that


have either:
• had internal standard (s) added, i.e., water samples or very simple
(‘extractables’) solutions
or
• have been digested in concentrated nitric acid (with optional addition of
hydrogen peroxide, hydrochloric acid or hydrofluoric acid, depending on
matrix/analyte requirements), following a digestion procedure.

The resulting solutions will have been diluted with water, and internal standard (s)
added.

WARNING -The use of this method can involve hazardous materials, operations
and equipment. This document does not purport to address all the safety issues
associated with its use, especially HF. It is the responsibility of the user of this
method to establish appropriate health and safety practices.

3. Reagents

NOTE: The concentration of the trace elements in the reagents and water used shall be low
enough not to affect the result of the determination. Ideally, ultrapure water and high purity acids
and reagents (Ultrapure or equivalent grade) should be used. Redistillation of acids is also
acceptable.

NOTE: Sufficient reagents should be prepared to fully complete an analytical batch. New bottles
of reagents should not be started midway through an analytical batch.

3.1 Nitric acid (concentrated (Ultrapure -grade))

Not less than 65% (mass fraction), with a density of approximately 1.4 kg L-1

3.2 Nitric acid (dilute, for preparation of standards, etc.) (Ultrapure -grade)

The concentration of the acid in this solution will be dependent on the final
dilution chosen for use with the digest solution, and should be calculated to match
it as closely as possible. In the examples given below, an assumption will be
made that the acid (in which the sample was digested) was transferred, diluted,
and made up to volume, 1:1 with water (3.5), giving a nitric acid concentration in
the digest solution of 32.5% (mass fraction).
Example 1. If the digest solution is subsequently diluted (1 + 4) with water (3.5),
the acid concentration in the resulting test solution will be approximately 6.5%
(mass fraction). Therefore, to prepare dilute nitric acid for use with the calibration
standards, a ratio of 1:10 (nitric acid: water) should be used, e.g., 100 ml of nitric
acid (3.1), made to volume (1000 ml) with water (3.5).

Example 2. If the digest solution requires a higher dilution (0.1 + 4.9) because of
the levels of dissolved solids, etc., the acid concentration in the resulting test
solution will be approximately 0.65% (mass fraction). Therefore, to prepare the
dilute nitric acid for use with the calibration standards, a ratio of 1:100 (nitric acid:
water) should be used, e.g., 10 ml of nitric acid (3.1), made to volume (1000 ml)
with water (3.5).

NOTE: If the digestion procedure included the use of hydrogen peroxide or hydrochloric acid, the
dilute nitric acid required for the preparation of the standards should also contain these chemicals
at an appropriate mass fraction. However, the analyst should be aware of the potential hazard
associated with the evolution of gases from solutions containing H2O2.

3.3 Hydrogen peroxide


30% mass fraction (Ultrapure -grade)

3.4 Hydrochloric acid (Ultrapure -grade)


Not less than 31% (mass fraction), with a density of approximately 1.6 kg L-1

3.5 Hydrofluoric acid (Ultrapure -grade)


Not less than 48% (mass fraction)

NOTE: If the digestion procedure included the use of hydrofluoric acid, the dilute nitric acid
required for the preparation of the standards should also contain this chemical at an appropriate
mass fraction. However, the analyst should be aware of the potential large hazards associated
with the use of HF. Only properly trained staff should be allowed to handle HF.

3.6 Deionised water


(Greater than 18.2 MΩ resistivity)

3.7 Standard solutions

These can be prepared directly by dissolution of the metal or metal salt (traceable
to a NIST standard) in an appropriate acid solution. Prepared solutions are also
commercially available.

NOTE: If commercially prepared solutions are used, they should, where possible, be traceable to
a NIST standard or be suitably certified and should be Mass-Spec grade, i.e.¸ the quality of the
standards should reflect that they are going to be used in multi-element methods.

NOTE: Typical concentrations in the prepared stock solutions would be 1000 mg L-1 . However,
some may be higher or lower, so care should be taken to check the solution strength.

NOTE: If similar multi-elemental analyses are being performed on a routine basis, pre-prepared
multi-element solutions are commercially available from a number of suppliers, which can be
tailor-made to meet the specific needs of a particular matrix/analyte combination. However, QC
check solutions should be made from different stock standards to the calibration solutions. QC
solutions should be run after the calibration standards, at the end of the run and at regular
intervals throughout the run.
3.7.1 Example of standard solution preparation from the metal.

NOTE: Certain metals require dissolution in concentrated nitric acid, whilst other are best
dissolved in a diluted acid solution. Advice should be sought as to the appropriate method of
dissolution to be used.

The following methods for preparation of standard solutions are given as


examples.

3.7.1.1 Lead standard solution, 1000 mg L-1:


Dissolve 1.000 g Pb in 7 ml of concentrated nitric acid (3.1) in a 1000 ml
volumetric flask. Dilute to volume with water (3.5).

3.7.1.2 Cadmium standard solution, 1000 mg L-1:


Dissolve 1.000 g Cd in 20 ml of a mixture of 10 ml water (3.5) and 10 ml
concentrated nitric acid (3.1) in a 1000 ml volumetric flask. Dilute to volume with
water (3.5).

3.7.1.3 Zinc standard solution, 1000 mg L-1:


Dissolve 1.000 g Zn in 14 ml of water (3.5) and 7 ml concentrated nitric acid (3.1)
in a 1000 ml volumetric flask. Dilute to volume with water (3.5).

3.7.1.4 Calibration solutions


The relative concentrations of elements in diluted multi-element stock solutions
must be chosen to reflect the levels expected in the samples being analysed. The
calibration range should include standards both below and above the
concentration expected in the test solution.
NOTE: When preparing dilute multi-element mixtures, care should be taken to consider the
compatibility of the solubilising acid because the stability of the solution may be affected, e.g.,
ensure that none of the standards are dissolved in HCl if intending to include silver in the multi-
element standard mixture.

3.7.1.5 Example of calibration solution preparation

NOTE: The following description is given only as an example. The actual volumes and
concentrations used will reflect what is required for the analysis of specific foods and also the
equipment/facilities available to the analyst.

If wanting to prepare calibration solution containing As and Se at 100 µg L-1 and


Al, Cd, Cr, Cu, Fe, Pb, Mn, Hg, Ni, Tl and Zn at 20 µg L-1;

Pipette 1 ml of As and Se Stock Solutions (@1000 mg L-1) and pipette 0.2 ml of


and Al, Cd, Cr, Cu, Fe, Pb, Mn, Hg, Ni, Tl and Zn Stock Solutions (@1000 mg L-1)
to a volumetric flask (100 ml). Make the solution up to volume with water (3.5).
The concentration in this intermediate solution is: 10 µg ml-1 for As and Se, and 2
µg ml-1 for Al, Cd, Cr, Cu, Fe, Pb, Mn, Hg, Ni, Tl and Zn.

Transfer 1 ml of the above solution to a volumetric flask (100 ml) and make up to
volume using dilute nitric acid (3.2). The resulting concentration of elements will
be: As and Se = 0.10 µg ml-1 and Al, Cd, Cr, Cu, Fe, Pb, Mn, Hg, Ni, Tl and Zn =
0.02 µg ml-1 .
3.7.2 Internal Standards

NOTE: Although a range of internal standards are suitable for use when
performing multi-element determinations for the TRACE project the elements
suggested to be used as internal standards are Ge, Rh or In, and Re or Pt. The
choice of internal standard (s) should be made, based on the following criteria:
Are they likely to occur naturally in the matrix (if so, choose an alternative).

Mass range of analytes


− It is recommended that at least 3 internal standards, of low,
medium and high mass, be used (see table 4).

Chemistry of analytes
− If using non-routine plasma conditions, e.g., reduced forward power, mixed
gases, etc, ensure that the internal standard exhibits similar ionisation behaviour
to that of the analyte.

− In high-matrix samples, ensure that the internal standard exhibits similar


ionisation behaviour to that of the analyte.

NOTE: Ensure that the solutions are Mass-Spec grade, i.e.¸ the quality of the internal standards
should reflect that they are going to be used in multi-element methods.

NOTE: Monitor the response of the internal standard, to ensure that there are no significant
changes in its behaviour from sample to sample. If a significant difference, i.e., greater than 25%,
in the response obtained from a procedural blank and that from a sample, this should be taken as
an indication of matrix effect or interference/contamination, and would require further
investigation.
Possible ways of resolving this issue would be either to dilute the sample further, or to use a
Standard Addition Quantification procedure or Isotope Dilution MS.

The concentration of the diluted internal standard should be sufficient to produce


a significant signal response (typically between 100,000 and 500,000 cps), but
not be so concentrated as to deleteriously affect the measurement of the analyte
elements. The concentration of internal standard that gives this level of response
will vary from instrument (and element to element), but is often accepted as being
in the region of 50ppb for a fully ionised, mono-isotopic element. Higher
concentrations may be required to give the desired signal for elements which are
poorly ionised, or for which a minor isotope is measured.

3.8 Warm-up solution

An acid digest of a typical food matrix, which has been diluted in a similar way to
the test solutions.

3.9 Optimisation solution

The Optimisation Solution is suggested to contain Be, Mg, Cu, Rh, Ba, Ca, Ce,
Pb and U, at concentrations which produce count rates between 10,000 and
100,000 cps (this equates to between 1 and 10 ppb).
4. Apparatus and equipment

4.1 General
All glass and plastic ware should be cleaned and rinsed following the procedure
described in EN 13804:2002 or better.

4.2 Pipettes and pipette tips

A number of pipettes should be available, capable of dispensing a range of liquid


volumes. These should be calibrated daily, before use.
Note: It is important to establish that the pipette tips do not leach significant
amounts of the elements of interest.

4.3 Argon

Purity greater than 99.99%

4.4 ICP-MS

The instrument should be capable of measuring the mass range, from 5 to 250
amu, and should be fitted with a low-pulse peristaltic pump and autosampler
system.

NOTE: Given the presence of many of the target analytes in airborne particulate material,
consideration should be given to the use of a cover over the autosampler, to protect the samples
from contamination while they are awaiting analysis.

4.5 Cones

The material used in the construction of the cones should be compatible with the
analysis being performed, e.g. it may be beneficial to use platinum rather than
nickel cones when analysing for nickel.

NOTE: This is particularly important if the instrument/plasma configuration gives rise to a


noticeable level of cone erosion. Leaching of nickel can be established by comparing the
background Ni signal obtained when using the two cone types. Platinum cones should be used
when the acid strength is high (>10%) or where HF, H2SO4 or H3PO4 is to be used.

5. Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

5.1 General

This procedure utilises the multi-element, multi-isotope measurement capability of


ICP-MS to determine the concentration of elements over a wide mass range (5 to
250 amu.) and a large dynamic range (up to 9 orders of magnitude). However,
the technique can be prone to interferences arising from the matrix, the plasma or
elements of similar mass/charge ratios. There are a number of ways to reduce
the effect of these interferences, but each analyte/interference may require its
own approach, and is likely to require the input of an experienced ICP-MS
operator.
5.2 Obtaining a stable plasma

Allow continual nebulisation of a warm-up solution (3.8) for 20 to 30 minutes prior


to optimising the instrument. This procedure allows the components in the
interface region of the ICP-MS to become conditioned to the matrix in the test
solutions.

NOTE: The basic steps in establishing stable and appropriate plasma will differ, depending on the
instrument’s manufacturer. What is described in this document is a guide to the operational
parameters that require attention if accurate and precise data is to be obtained.

5.3 Optimisation of the ICP-MS


Following on from 5.2, optimisation of the ICP-MS plasma and nebuliser
conditions (outlined in table 1) is performed using an acidified solution (3.9)
containing elements that cover the mass range.

Table 1: Parameters for consideration when optimising the ICP-MS.


Parameter Comment

Tubing integrity Non-pulsed pumping, no blockages or leaks


Interface region Cone and torch cleanliness

Plasma stability Monitor signal drift


Tuning (signal response) Optimise for response, oxides, etc.

Oxides <3%*

Doubly-charged species <3%

• NOTE: that a lower CeO/Ce ratio equates to improved matrix decomposition and more
consistent ionisation with changing matrix levels. For this reason, reducing the CeO/Ce ratio may
be considered a priority in normal system optimisation.
5.4 Operational parameters for data acquisition

Table 2 presents typical instrument settings, as suggested by two manufactures,


and table 3 outlines operational parameters that will require additional attention.
Suggested value Agilent Suggested value PE Sciex
Instrument parameter 7500ce Elan DRC
RF – power (W) 1500 1200
Carrier gas flow (L min-1) 1.1 0.9
Plasma gas flow (L min-1) 15 15
Auxiliary gas flow (L min-1) 1.0 1.0
Nebuliser type Concentric or Babington Cross-flow
Spray chamber design Peltier cooled, double Scott double pass (no
pass cooling)
Spray chamber temp. (°C) 2 Room temp
Lens voltage 0-4V Varied, 4 to 14 V
Mass resolution 0.8 0.7 ± 0.1
Integration time (seconds/mass) 3 (total time for 100 1 (peak hopping, dwell time
sweeps) 25-100 ms)
Points per peak 3 1 (peak hopping)
Replicates 3 3
Table 2. Typical instrument settings (Agilent 7500CE and PerkinElmer Sciex Elan
DRC)

NOTE: Manufacturers recommendations should be considered when establishing data acquisition


methods.

Parameter Comment

Volume of test solution Sufficient for at least one analytical run


available
Compromise between sensitivity and consumption of test solution
Nebuliser flow rate Optimised for In “top of mountain” (TOM), and reduced to meet
CeO/Ce specification
Optimise measurement time by minimising numbers of
Numbers of elements/isotopes measured. However, it is recommended that
elements/isotopes to more than one isotope be measured, allowing the isotopic ratio to
be measured be used as an indication that the isotope being used for
quantitation is not being affected by a chemical interference.
Uptake time Sufficient to get stable plasma, but not too long to consume of the
test solution (0.5-1ml/min)

Sampling time Sufficient for measurement of elements/isotopes without


consuming all of the test solution
Washout time Sufficient to ensure that ‘between-sample’ carry-over does not
occur.
Numbers of replicate
Minimum of three
analyses
Table 3: Parameters for consideration during development of a data acquisition
method
5.5 Interferences

Table 4 details interferences that can affect the 13-analyte elements covered by
this validated part of this protocol (Al, As, Cd, Cr, Cu, Fe, Hg, Pb, Mn, Ni, Se, Tl
and Zn). The analyst must take responsibility for identifying potential additional
interferences affecting the additional elements being analysed for TRACE, which
are not in this list.

NOTE: For many elements, there is more than one isotope available for quantitation. If possible, it
is advised that at least two isotopes are measured, allowing the ratio of the responses for the two
isotopes to be used as an indication that the quantifying isotope has been measured free from
chemical interference.

Element Isotopes Interference Possible polyatomic interferences, Internal


by isobaric or assuming a nitric acid. test solution. standard (NOTE
doubly Other interferences may be present if ** hydride
charged H2O2 or HCl is used. generation, use
species e.g. Ge)
Al, 27 CN, CNH+ Sc Ga Rh
As, 75 ArCl+, CaCl+, ArSH+ Rh Ga In (Ge**)

Cd, 111 MoO+, MoOH+ Rh In


Cd, 114 Sn+ MoO+, MoOH+ Rh In
Cr, 52 ArO+, ArC+, ClOH+ Rh Ga In
Cr, 53 ArOH+, ClO+ Rh Ga In
Cu, 63 ArNa+, POO+, MgCl+, SiCl+ , Rh Ga In
Cu, 65 ZnH+, SOOH+ Rh Ga In
Fe 54 Cr+ ArN Ga Rh In
Fe, 56 CaO+, ArO+, ArNH+, KO+ Rh Ga In
Fe, 57 CaOH+, ArOH+, KOH+ Rh Ga In
Hg, 200 WO+, HgH+, RuRu+ Lu Re
Hg, 202 WO+, HgH+, RuRu+ Lu Re
Mn, 55 CaO+ NaS+, ArOH+, ArNH+, KO+ Rh Ga In
Ni, 58 Fe+ CaO+, CaN+, NaCl+, MgS+ Rh Ga In
Ni, 60 CaO+ , CaOH+ , NaCl+ , MgCl+ , Rh Ga In
CoH+
Pb, 206 RhRh Lu Re
Pb, 207 PbH+ Lu Re
Pb, 208 PbH+ Lu Re
Se, 78 Kr+ ArAr+, CaCl+ , Rh (Ge**)
Se, 80 ArAr+ , ArCa+ , CaCa+ , HBr+ , Rh (Ge**)
ArKH+, SSO+, SOOO+
Se, 82 Kr+ HBr+, SSO+, SOOO+ Rh (Ge**)
Tl 205 OsO+ Lu Re
Zn 64 Ni+ SS+, SOO+, CuH+, MgAr+ , Rh
Zn 66 Ba2+ PCl+, AlAr+, SS+, SOO+, FeC+ Rh
Zn 68 Ba2+, Ce2+ , PCl+, ArS+, SS+, ArNN+, SOO+ , Rh
CrO+, SiAr+
Table 4. The analytes covered by this protocol, their main isotopes for
quantitation, the interferences likely to be encountered and an indication as to
which internal standard is appropriate for each element.
Note: when using certain reaction/collision gases in a cell-based instrument, some Rare Earth
Elements are unsuitable for use as internal standards, as they react with the gas, producing an
apparent, but non-representative, drop in sensitivity. The use of Pt group elements should
therefore be considered, as they are totally non-reactive with cell-based gases. Alternatively, non-
reactive cell gases, which are more suitable for the analysis of multiple elements in variable
matrices, can be used.

Note: Variation in the natural isotopic abundance of lead from different geographical locations
around the world is well documented. Therefore, to avoid any inaccuracy when quantifying lead, it
is common practice to add the 3 main isotopes of the element together, using a simple equation
embedded in the instrument method software.

5.6 Measurement

Using the instrument’s software, construct a suitable ‘sample table’ to include:

− A minimum of one (5-point) calibration curve at the start of the analytical run (a
second set of standards is advisable at the end of the run).
− QC check standards should immediately follow the analysis of the standard
calibration solutions, be dispersed randomly throughout the run (with no more
than 10 sample analyses between each check standard) and be measured at the
end of the run.

Note: The nebulisation of a number of ‘warm-up’ solutions, prior to the measurement of the
calibration standards should be considered, as this can assist in stabilising the interface region of
the ICP-MS.

5.7 Calculation and assessment of data.

5.7.1 General

The following ‘quality’ parameters should be demonstrated:

− A value of at least 0.995 should be obtained from the regression fit for the
calibration standards.

− Instrumental drift, as determined by reference to the check standards, should


not exceed 15% throughout the run.

− Ensure that variation in internal standard response does not vary by more than
25% between blank and sample solutions.

− Where multiple isotopic data has been obtained, the concentration calculated
on the individual isotopes should not vary by more than 10%.

Note: If there is a significant difference between the concentrations calculated on 2 separate


isotopes, this indicates the presence of a chemical interference, which should be investigated
further.

5.7.2 Manual calculation of analyte concentrations in solution.

All ICP-MS instruments have software that, if suitable information such as sample
weight is provided, can calculate the concentration of analyte in the original
sample. However, if this approach is not taken, the following manual calculation
procedure can be used to perform the calculation, assuming that there are no
concerns regarding chemical or isobaric interferences.
Calculate the content, w, as mass fraction of the element to be determined, in
milligram per kilogram of sample, using the following equation:

w = ( a – b) V
m
where
a is the concentration in the test solution, in milligrams per litre;

b is the mean concentration in the reagent blank solutions, in milligrams


per litre;

V is the dilution factor required to obtain the test solution, in millilitres;


M is the mass of sample taken at the digestion stage, in grams.

If (a-b) is lower than the sample solution detection limit (see 5.7.2), substitute (a-
b) with the value for the detection limit in the test solution for calculation of the
limit detection in the sample.
If required, recalculate the result to fresh weight if it is based on the dry matter
content of the sample. Give the result with an applicable number of significant
figures.
5.7.3 Calculation of the limits of detection and quantification

This calculation is as follows:

Limit of Detection (LOD) = (3 x std dev blanks) x V


M

std dev blanks the standard deviation measured in at least three procedural
blanks V the dilution factor required to create the test solution M typical mass of
sample taken at the digestion stage, in grams.

6. Production of a Test report

The test report should specify at least the following:

a) All information necessary for the identification of the sample;


b) The results obtained and the units in which they are specified;
c) Any corrections applied to the final results, e.g., polyatomic interferences,
procedural blanks, and spike recovery. (PLEASE NOTE: Data should not
be corrected for the CRM, as this will be used as an assessment of the
variability within the whole dataset.)

Appendix A

Quality material and procedures associated with the TRACE ICP-MS analysis:

Each analytical batch should include sufficient QA and QC materials to allow the
accuracy of the data to be assessed, and to provide a means by which data can
be directly compared with that from another laboratory. It is suggested that each
batch should contain the following:

– a maximum of 50 ‘unknowns’ for water samples, or 35 ‘unknowns’ for


samples requiring acid digestion.
– a minimum of 3 procedural blanks
– a minimum of 1 CRM (See list for TRACE samples below!)
– a minimum of 1 spike procedural blank

Construction of an analytical batch:

All QA/QC materials, samples and replicate analyses of samples should be


randomly distributed throughout the batch, and should not be done sequentially
Definition of terms: °

– Analytical batch
o A collection of test samples (or “unknowns”), certified reference
materials (CRMs), procedural blanks and spiked procedural blanks,
which have been analysed in such a way as to have a commonality
of;
– operator
o reagents (do not replenish reagents with fresh material from
different bottles, etc). environmental and instrumental conditions
– Unknowns
o Samples (or test materials) for which the elemental composition is
unknown

– Procedural blanks
o A solution, which is quantitatively representative of all of the
reagents used in the procedure, and which has been produced by
taking the reagents through all of the stages involved in the
procedure.

– Spiked procedural blank


o A procedural blank to which an aliquot of solution, containing known
amounts of the analytes, has been quantitatively added, and which
has been taken through all of the stages involved in the procedure.

– Quality assurance (QA) material


o A material or solution containing known amounts of the analytes,
such as a CRM or a spike solution, and which are used in
assessing the accuracy of the data.

– Quality control (QC) materials/procedures


o Procedural blanks, duplicates, etc., which highlight analytical
variability within the data

– QA/QC acceptance criteria.

Within an analytical batch, the recovery of material from the ‘spike’ should fall
within the following bounds:

The recovery values for ALL the elements in a batch should be between 60 and
140%

The recovery values of 75% of the elements in a batch should be between 80 and
120%

Special for the TRACE project:

The following CRM’s have been selected as suitable reference materials for the
TRACE project: NIST1548 “Typical Diet” which is to be measured with any batch
containing wheat, olives, olive oil, honey, lamb, beef or chicken. Additionally,
NIST1640 “Natural Water” is to be measured with the water samples, NIST1567a
“Wheat Flower” is to be measured with the wheat, NIST1547 “Peach leaves”
and/or BCR-062 “Olive leaves” is to be measured with the olives and olive oil,
NIST8414 “Muscle Tissue” is to be measured together with the meat samples.

In order to attain traceability of the results within the WP each partner must
ensure that with each measurement there must be a reference to the matching
reference material(s) measured in the same batch. In this manner any intra-lab
differences can be accounted for when integrating all data set for the
interpretation and model building. Additionally the performance on the quarterly
proficiency tests will be recorded on control charts for each lab and be available
form the TRACE intranet.

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