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Analytical strategies to confirm Scotch whisky

authenticity. Part II: Mobile brand
authentication

Article in The Analyst · August 2004

DOI: 10.1039/b403068k · Source: PubMed

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 Analytical strategies to confirm Scotch whisky authenticity.

Part II:† Mobile brand authentication

W. M. MacKenzie and R. I. Aylott
Diageo PLC, Brand Technical Centre, Menstrie, Clackmannanshire, Scotland, UK FK11 7ES

Received 1st March 2004, Accepted 5th May 2004

First published as an Advance Article on the web 8th June 2004

Whilst the authentication of Scotch whisky brands using laboratory based gas chromatography is well established, there
is a need for authentication methods for use under field test conditions. The UV/visible absorbance spectra of specific
brands of Scotch whisky were found to produce consistent absorbance ranges which allowed the development of a faster,
cheaper and more mobile test method. Test samples with spectra outside the acceptable ranges for genuine reference
samples were therefore deemed suspect, enabling their authenticity to be later confirmed in the laboratory by GC. This
novel application allowed brand authenticity analyses to be undertaken at remote sites where gas chromatography was
unavailable and has also allowed the introduction of field testing using a small portable hand held spectrophotometer.

Introduction Experimental
Absorbance spectra of test samples were collected using two
As part of its worldwide popularity, blended Scotch whiskies can be
different spectrophotometers, one laboratory based and one
subject to illegal counterfeiting and substitution. Consumer protec-
portable. Absorbance data at set wavelengths from both instru-
tion agencies and producers require analytical laboratories to
ments were transferred electronically via RS232 interfaces into
support their consumer and brand protection programmes with
Microsoft® Excel spreadsheets.
effective brand authenticity analyses.
Initial laboratory development was conducted on a WPA
Current authenticity analysis is based upon the gas chromato-
graphic determination of the major volatile congeners present in Lightwave® S2000 UV/visible diode-array spectrophotometer
(Walden Precision Apparatus Ltd., The Old Station, Linton,
Scotch whisky. Normal concentration ranges are first set for
Cambridge, UK CB1 6NW) fitted with deuterium and tungsten
genuine product, against which the results for suspect samples may
lamps. Samples were introduced by drawing liquid up into a 1 mm-
be compared. Suspect samples are then analysed for alcoholic
path length flow cell using a 5 ml plastic syringe. Absorbance data
strength and major volatile congeners. If the suspect sample’s
was collected at 1 nm intervals between 200 and 500 nm and
alcoholic strength and congener results fall within the normal
transferred into the spreadsheet using WPA Lightwave® software.
ranges for the genuine brand, then the sample is considered
authentic. If the results are outside the normal ranges, the sample is At the start of operation, the spectrophotometer was referenced
against 40% vol. ethanol in water.
not authentic. These analyses may then form part of the evidence
The development of mobile authentication was conducted on a
used in the prosecution of offenders.1,2
However, investigations are enhanced when supported by fast SAD Brand Authenticator® (Spectroscopic and Analytical De-
vices, West Grinstead, West Sussex, UK RH13 8LH. http://
and reliable forensic information, ideally based on field tests.
www.spectroscopic.co.uk). This small novel instrument was de-
Whilst the current gas chromatographic approach provides accurate
signed and built specifically by SAD for the purpose of enabling
and precise results which enable reliable conclusions, it can take
authenticity analysis to be conducted under field conditions. The
significant time and cost to locate and utilise local laboratories with
instrument measures 27 cm long 3 9 cm wide 3 10 cm deep,
appropriate equipment and expertise. Spectroscopic techniques
weighs 1.75 kg and is shown in Fig. 1. It is powered by a 20 V
were therefore considered as an alternative means of authenticating
whiskies. rechargeable battery that enables approximately 2 h continuous use.
UV and visible absorbency in Scotch whisky is primarily derived
from three sources. First, the Scotch whisky maturation process
results in the addition of a range of congeners, which are extracted
from the oak cask into liquid through the interaction of ethanol with
wood lignin. Secondly, volatile phenolic compounds are found in
whiskies where peat is used in the kiln drying of the malted barley
used in the fermentation. The spectroscopic properties of the
maturation and phenolic congeners are employed in their high
performance liquid chromatographic determination with UV and
fluorescence detection. Thirdly, batch to batch colour consistency
is often maintained through the addition of trace spirit caramel
(E150a). Indeed, the colour consistency of Scotch whisky is
DOI: 10.1039/b403068k

monitored at the blending and bottling stage by visible spectros-

copy typically around 500nm.3 Maturation congeners in brandies
have been shown to result in similar spectra.4

Fig. 1 Photograph of a test sample being injected into the SAD Brand
† For Part 1 see ref. 1. Authenticator®.

This journal is © The Royal Society of Chemistry 2004 Analyst, 2004, 129, 607–612 607
 The Brand Authenticator® was fitted with a deuterium lamp and a
diode array detector. Samples were introduced by either injecting or
drawing liquids into the 1 mm-path flow cell using a plastic syringe.
Absorbance data was collected at defined intervals at approx-
imately 1 nm resolution between 200 and 460 nm. Four patents
have been applied for covering various features of this instrument,
which is designed to be simple to operate in stand-alone mode
controlled by internal software. There are five control keys, a two-
line text screen and three result lights. Reference data for genuine
brands is uploaded to the authenticator via its electronic interface.
Similarly, result data from field measurements may be downloaded
to the result spreadsheet for onward transmission and critical
examination at a central laboratory.
A process for drawing conclusions on sample authenticity was
devised. An algorithm was constructed based on the sum of squared
scores (S z2) for absorbance results at 10 pre-selected wavelengths
ranging from 230 to 500 nm for the WPA Lightwave® S2000 and
between 220 and 360 nm for the SAD Brand Authenticator®. The
absorbance of the test sample and the average and standard
deviation of at least 10 reference samples were entered into the
calculation. The z-score5 was calculated from z = (x 2 X)/s for
absorbance data at 10 wavelengths chosen to reflect changes in the
slope of the spectral curve, where x is the determined value, X is the
average of the reference values and s is the standard deviation of
the reference values. For example, the Brand Authenticator® used
wavelengths at 220, 230, 240, 250, 260, 280, 300, 320, 340 and
360nm. The formula for the z score at each given wavelength (l
nm) was therefore
Finally, S z2 = Sum of squared scores (z(l)) at each monitored
wavelength.
The same test samples were subjected to brand authenticity
analysis by gas chromatographic methods previously described.1
Methanol, n-propanol, isobutanol and the combined value for 2-
and 3-methyl butanol were determined. For the gas chromato-
graphic process a similar algorithm was applied to each of the 4
congeners.
Results
Initial stages of this spectroscopic method development determined
the consistency and specificity of the spectral characteristics of a
range of Scotch whisky brands. The brands were selected to
Fig. 2 Absorbance spectra of 10 samples from different production batches of five different brands of Scotch whisky collected using the WPA Lightwave®
S2000 spectrophotometer.
608 Analyst, 2004, 129, 607–612
represent blend compositions containing increasing proportions of
malt whiskies. Compositions may be shown from their 2- and
3-methylbutanol concentrations, congeners primarily associated
with the malt whisky contents of blended whiskies.3
The spectra for single samples taken from 10 different batches
representing five different brands (labelled A to E) produced over
a two-year period are shown in Fig. 2. There were clear separations
between the spectra of certain brands, particularly brands A, B, C
and E. There was partial overlap between others (such as brands C
and D) particularly at higher wavelengths. Whiskies of known
authenticity were then analysed in a similar way. Fig. 3 shows that
a sample of genuine brand B (sample T1) fitted, as expected, within
the minimum and maximum ranges for that brand, whereas four
non-authentic samples (samples T2–T5), which were known
counterfeits, each had spectra outside these ranges.
The principles of this spectroscopic method were then trans-
ferred from the laboratory WPA Lightwave® spectrophotometer to
the portable SAD Brand Authenticator®. Brand range data were
generated on the Brand Authenticator® in the same way as that
used for the laboratory instrument. Fig. 4 shows equivalent spectra
for 10 samples of each of the five Scotch whisky brands A to E.
Minor differences in the absorbencies at higher wavelengths
between the two instruments (Figs. 2 and 4) were thought to arise
from secondary transmissions caused by the higher excitation
energy used in the Brand Authenticator®. This highlighted the
necessity to establish brand ranges on each model of instrument
used at this stage of method development.
Analytical precision was investigated on the Brand Authentica-
tor® over the range 220 to 360nm. The repeatability of 10
measurements on one sample of brand C (expressed as ±2s/mean 3
100%) ranged from ±0.32% at 260nm to ±1.43% at 360nm (Table
1). The equivalent confidence limits for brand authenticity analysis
by gas chromatography were approximated double the spectral
limits and ranged from ±1.6% (for methanol analysis) to ±2.7% (for
2-methyl butanol analysis).1 The spectral confidence limits for 10
production batches of brand C analysed once ranged from ±9.8 to
±10.9%, indicating that variation in instrument repeatability was
very small compared to batch to batch variation.
The authenticities of a series of samples were then assessed both
by the spectroscopic method on the Brand Authenticator® and by
gas chromatography. Reference samples of the same five brands
were analysed for their major volatile congeners. Minimum and
maximum range data, shown in Table 2, indicated that similar
analytical overlap of certain congeners used in authenticity
assessment occurs and therefore specific congeners, such as 2- and
3-methyl butanols, are particularly important in reaching au-
Fig. 3 Absorbance spectra of five samples of known authenticity (one genuine brand B [T1] and four counterfeits [T2–T5]) shown against minima and
maxima of genuine brand B collected using the WPA Lightwave® S2000 spectrophotometer.

Fig. 4 Absorbance spectra of 10 samples from different production batches of five different brands of Scotch whisky collected using the SAD Brand
Authenticator®.

Table 1 Precision of spectral analyses for brand C using the Brand Authenticator®. The repeatability of ten measurements on one sample and the results
obtained from single analyses on ten production batches of brand C

Wavelength/ Confidence Confidence 2s/

nm Absorbance range Mean limit (2s) 2s/mean,% Absorbance range Mean limit (2s) mean,%

Ten measurements on one sample of brand C Single analyses on ten production batches of brand C.

220 1.141–1.150 1.145 ±0.0066 ±0.58% 1.109–1.302 1.205 ±0.118 ±9.8%

230 0.947–0.953 0.951 ±0.0038 ±0.40% 0.922–1.091 1.002 ±0.103 ±10.3%
240 0.819–0.825 0.822 ±0.0033 ±0.40% 0.782–0.934 0.853 ±0.090 ±10.6%
250 0.734–0.742 0.738 ±0.0047 ±0.64% 0.720–0.857 0.780 ±0.081 ±10.4%
260 0.740–0.744 0.743 ±0.0023 ±0.32% 0.723–0.855 0.781 ±0.079 ±10.1%
280 0.714–0.731 0.726 ±0.0103 ±1.43% 0.707–0.836 0.760 ±0.076 ±10.0%
300 0.507–0.513 0.509 ±0.0038 ±0.74% 0.491–0.584 0.525 ±0.056 ±10.7%
320 0.356–0.361 0.359 ±0.0030 ±0.82% 0.357–0.425 0.384 ±0.042 ±10.9%
340 0.279–0.282 0.280 ±0.0023 ±0.81% 0.279–0.328 0.297 ±0.029 ±9.8%
360 0.229–0.235 0.232 ±0.0033 ±1.43% 0.229–0.270 0.244 ±0.024 ±9.8%

Analyst, 2004, 129, 607–612 609

 thenticity conclusions.1 Interestingly, brands B and E showed
similar congener ranges while their spectral characteristics were
quite different (Fig. 2 and 4). In an opposite way, brands C and D
exhibited overlapping spectra while their congener ranges were
quite distinct.
The spectra of twenty suspect samples purporting to be brand B
(labelled S1 to S20 in Table 2) and 15 other brands of Scotch
whisky (labelled X1 to X15) were collected and compared against
the known spectral ranges of brand B. Their spectra, shown in Fig.
5, indicated that suspect samples S2, S4, S7, S11, S12, S14 and S20
each had spectra within the ranges for genuine brand B. Their
resulting spectral S z2 scores are shown in Table 3 together with
equivalent results, S z2 scores and conclusions by gas chromatog-
raphy. These results, plotted on Fig. 6, indicated that the
spectroscopic and gas chromatographic methods came to the same
conclusions that these seven samples were authentic. The remain-
ing suspect samples each had spectra outside the ranges for genuine
brand B indicating that they were not genuine. These conclusions
were confirmed by gas chromatography.
The spectra for the 15 brands of other Scotch whiskies also
exhibited spectra outside the normal ranges for brand B, except for
sample X14. However, the gas chromatographic results for this
sample indicated that it was not brand B but was a Scotch whisky
with a higher malt whisky content than brand B. The spectral
conclusions for whiskies X4 and X12 indicated that they were not
brand B, whereas gas chromatography found both samples to have
certain congener results only slightly out of range. These results
demonstrated the complementary value of the two techniques
working together to highlight differences between brands based on
colour and/or congener concentrations.
Whilst the reference spectra were collected from up to ten
production batches of each brand, many more production batches of
these brands had been produced during the two year time frame in
which the reference samples were collected. Suspect samples taken
Table 2 Maximum and minimum range data for major volatile congeners
in five blended Scotch whisky brands A to E
2- and
3-Methyl
Brand Methanol n-Propanol Isobutanol butanol
Volatiles/g (100 l absolute alcohol)21
Brand A 6.8–8.4 58–77 69–77 101–115
Brand B 6.0–9.2 58–89 63–76 80–96
Brand C 6.3–9.8 44–76 63–76 70–83
Brand D 6.4–9.9 50–58 61–70 42–53
Brand E 7.2–10.5 51–62 63–72 75–93
for authenticity analyses could also have been produced prior to the
reference period or be derived from production batches other than
those used for the reference data. The robust performance of this
methodology was then demonstrated by authenticating other brands
in a similar way.
An authenticity decision process was established based upon S z2
values. Pass/fail limits were initially based upon values obtained
from chi-squared tables. For 10 data points the limits were set at
18.6 and 26.9 for 95.5% and 99.7% confidence limits, respectively.
From experience and observation during testing of the WPA
Lightwave® instrument, these limits were found to fail genuine
samples at a higher frequency than would have been expected. A
decision was taken to increase these limits, as these would only
have been appropriate if multiple reference samples from the same
batch/period as the suspect sample were available to use to establish
the baseline figures for comparison. A pragmatic decision was
made to apply more usable limits, based on less rigorous
application of statistical concepts, using the following calcula-
tions:
Lower limit = S(2la)2 + (2lb)2 + …
Upper limit = S(3la)2 + (3lb)2 + …
Therefore for 10 data points the limits and decision points were as
follows: If S z2 was < 40, the sample was deemed authentic. If S z2
was > 40 and < 90, the sample was deemed suspect and if S z2 was
> 90, the sample was deemed to be not authentic. S z2 values in
these categories resulted in the Brand Authenticator® showing a
green (genuine), yellow (suspect) or red light (not authentic) at the
completion of each test.
A similar decision process was applied to the gas chromato-
graphic results. If S z2 for four data points was < 16, the sample was
deemed authentic. If S z2 was > 16 and < 36, the sample was
deemed suspect and if S z2 was > 36, the sample was deemed to be
not authentic. The validity of the chosen limits was confirmed by
the complimentary results obtained by the two analytical tech-
niques (Fig. 6). The potential to refine the numerical analysis and
judgement criterion will be investigated on an on-going basis as
more range data for a particular product is gathered.
Various criteria were considered when selecting acceptance
limits for these spectroscopic and chromatographic methods. As
already reported, the reference samples used to establish normal
ranges were taken from retained genuine samples representing at
least 10 production batches produced during the last two years.
However, for brand B this represented only 5 to 10% of the total
production batches produced for market. Suspect samples collected
in the field could have been produced prior to the reference period

Fig. 5 Absorbance spectra of 20 suspect samples purporting to be brand B collected using the SAD Brand Authenticator®.

610 Analyst, 2004, 129, 607–612

Table 3 The sum of squared scores (S z2) results on 20 suspect samples (S1 to S20) and 15 other Scotch whisky brands (X1 to X15) each determined using
the SAD Brand Authenticator® and by gas chromatography

2- and
Sample Isobutyl 3-Methyl Authenticity S z2 by Authenticity
number Methanol n-Propanol alcohol butanol S z2 by GC by GC UV/VIS by UV/VIS

Volatiles/g (100 litres absolute alcohol)21

S1 4.3 31.9 33.0 39.2 401 Fail 629 Fail

S2 9.2 67.7 68.9 79.9 11 Pass 7 Pass
S3 1.4 2.2 3.4 8.5 1190 Fail 869 Fail
S4 7.2 62.1 66.1 87.3 6 Pass 25 Pass
S5 2.7 17.6 23.2 37.2 563 Fail 233 Fail
S6 3.3 35.3 14.2 18.8 804 Fail 619 Fail
S7 8.0 62.3 68.3 82.4 6 Pass 9 Pass
S8 7.0 36.1 39.9 44.0 283 Fail 387 Fail
S9 2.5 9.5 14.1 33.9 715 Fail 995 Fail
S10 5.2 32.6 33.5 39.6 381 Fail 626 Fail
S11 7.4 62.5 67.7 85.5 4 Pass 31 Pass
S12 6.4 65.6 70.9 83.2 7 Pass 7 Pass
S13 70.8 2.7 0.4 0.0 10672 Fail 475 Fail
S14 7.1 75.1 68.3 81.9 3 Pass 16 Pass
S15 3.1 18.8 24.1 28.0 628 Fail 820 Fail
S16 16.9 57.8 52.9 23.7 581 Fail 247 Fail
S17 0.0 0.1 4.6 11.4 1186 Fail 1215 Fail
S18 0.0 1.0 0.5 5.1 1329 Fail 1252 Fail
S19 0.0 1.0 0.5 5.0 1330 Fail 1256 Fail
S20 9.0 63.6 68.4 91.0 9 Pass 9 Pass
X1 6.7 79.1 51.4 31.8 298 Fail 469 Fail
X2 5.9 114.9 52.6 50.7 175 Fail 325 Fail
X3 6.4 69.9 60.1 53.2 110 Fail 531 Fail
X4 7.8 60.6 68.2 84.2 5 Pass 231 Fail
X5 6.3 66.5 64.1 63.9 54 Fail 236 Fail
X6 4.8 94.1 53.6 31.7 311 Fail 477 Fail
X7 11.2 57.2 55.8 61.6 112 Fail 377 Fail
X8 8.1 93.3 53.0 62.1 88 Fail 238 Fail
X9 11.1 55.7 60.5 57.5 119 Fail 272 Fail
X10 4.8 33.6 55.3 65.7 112 Fail 522 Fail
X11 5.0 83.7 53.6 50.1 160 Fail 721 Fail
X12 5.4 50.9 63.6 92.4 30 Suspect 326 Fail
X13 5.3 51.6 60.2 63.4 80 Fail 499 Fail
X14 5.7 51.7 96.3 221 1652 Fail 44 Suspect
X15 4.7 52.7 58.3 75.1 56 Fail 606 Fail

Fig. 6 The sum of squared scores (S z2) for 20 suspect samples and 15 other brands of Scotch whisky determined both spectrally, using the SAD Brand
Authenticator®, and by gas chromatography.

Analyst, 2004, 129, 607–612 611

 or be derived from batches produced during this two-year period
but out with the reference set. Older suspect samples may also have
been exposed to harsh environmental conditions such as bright
sunlight that can cause colour fading (with a resulting impact of
lowering their UV/visible spectra). These effects could result in a
risk of higher values for spectral standard deviations for genuine
product collected in the field compared to those for genuine product
retained at production. Conversely, methanol and higher alcohol
concentrations in such samples remain stable and therefore the gas
chromatographic standard deviations for retained and field samples
of genuine product are similar. To allow for these affects, S z2
values greater than the equivalent chi-squared limits were chosen,
this being a factor easily reset for individual brands within the
Brand Authenticator® software. An alternative approach would be
to take an inflated standard deviation value, which would result in
a correspondingly lower S z2 value closer to the chi-squared
statistical limits.
As greater experience is gained with the Brand Authenticator®
under field conditions and brand ranges extend over longer time
periods, it may be possible to tighten the S z2 acceptance criteria.
However, the width and consistency of the spectral ranges of
genuine product will vary from brand to brand depending on that
brand owner’s specific blend formulation. Therefore, during the
initial deployment of the Brand Authenticator®, it is recommended
that appropriate acceptance limits are established brand by brand,
with the instrument used as a screening tool prior to gas
chromatographic confirmation.
For consistency within this project, the gas chromatographic chi-
squared statistical limits were inflated in the same way as those
applied to the Brand Authenticator®. Review of the gas chromato-
graphic result trends for brand B over a 20-year period indicated
that chi-squared statistical limits are appropriate for the GC method
if the correct production period segments are selected for the range
data. A similar approach for the Brand Authenticator® will be used,
as spectral trends become available.
Finally, an operational process was then configured for the use of
this mobile instrument under field test conditions. First, average
and standard deviation spectral data for the required brands (up to
a memory capacity of 16 brands) were collected and held in the
Brand Authenticator® memory. The procedure for analysing a test
sample was established as follows:
1. After the instrument has completed its initial warm-up
procedure, flush and load the flow cell with 2 ml 40% ethanol in
order to reference the instrument.
2. The quality control procedure is then automatically activated.
Check the instrument calibration against a quality control whisky of
known spectral characteristics. Once the sample passes this test, the
spectrophotometer progresses to test samples.
3. Select the brand whose authenticity is to be tested from the
brand list held within instrument memory. Introduce liquid as
previously described.
4. The instrument records the spectra, calculates a S z2 score for
the test sample, compares it against the acceptance criteria
described above and displays its decision on sample authenticity.
5. Samples whose authenticity is deemed “pass” (green light) are
considered authentic. Samples whose authenticity is deemed “fail”
(red light) or “suspect” (yellow light) are retained and returned to
the central laboratory for confirmation by gas chromatography.
6. Continue with the next suspect sample.
612 Analyst, 2004, 129, 607–612
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Conclusions
This spectroscopic method has enabled the deployment of a novel
method for Scotch whisky brand authentication in the field. It
clearly distinguishes counterfeits, most of which, are combinations
of cheap local alcohol flavoured with a smaller proportion of
whisky and colouring. It can also distinguish other Scotch whiskies
and, in particular, compliment gas chromatographic authentication
where two distinct brands have similar malt whisky contents.
Subsequent confirmation by gas chromatography not only confirms
the spectroscopic result, it also gives compositional information on
the non-authentic liquid.3
This method has three distinct benefits. First, the methodology
enables laboratories not equipped with gas chromatography to
conduct Scotch whisky brand authenticity analysis. Secondly, the
handheld spectrophotometer enables field-testing with the added
benefit of speeding up investigation processes (for example,
enabling suspect goods to be seized pending full forensic
examination). Thirdly, this fast screening technique can enable only
those samples which failed the spectroscopic analysis to go forward
for confirmatory analysis by gas chromatography, thus saving both
time and analysis cost. The Brand Authenticator® takes less than
one minute to analyse each sample compared to at least 20 min by
gas chromatography, thus offering advantages of speed, cost and
mobility.
This spectroscopic method has the potential to be used for brand
authenticating other categories of distilled spirit that have suitable
UV/visible spectra such as other whiskies, brandy, rum and
flavoured spirits. It also has the potential to find application in the
authentication of beers, wines and non-alcoholic beverages (al-
though sample filtration and degassing may be required prior to
spectral analysis). There are also opportunities to develop more
sophisticated data handling post analysis using derivative spectros-
copy and chemometric techniques.
Acknowledgements
The authors wish to thank John Ferguson, Bill Considine and Jon
Considine of Spectroscopic and Analytical Devices for designing
and manufacturing the Brand Authenticator® to our design brief.
Thanks are due to colleagues Jennifer Yeh (Diageo Taiwan),
Margarita Calderon (Diageo Colombia), Maria Camacho (Diageo
Venezuela) and Marcial Cid Nieto (Diageo Spain) for their
contributions to the field-testing of prototype instruments. Finally
thanks to John Wilson (Diageo Scotland) for statistical advice and
Brand Technical Centre colleagues who contributed to in-house
testing.
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