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Agilent Atomic Spectroscopy solutions for routine Food & Agriculture applications
AA, MP-AES, ICP-OES,
ICP-MS.
AGENDA
Agilent Atomic Spectroscopy instruments overview
Types of applications in Food & Agriculture
Examples of available applications
1957
Built
components for
world's first AA
(as Techtron)
1971
Applies for
patent on
Zeeman
background
correction
1985
SpectrAA
instruments
released with
central
instrument
control
1987
Introduction of
the first
computer
controlled ICP-
MS, the PMS
100
1991
Releases first
sequential ICP-
OES
1994
Launch of the
4500 Series, the
world's first
benchtop ICP-
MS
1997
Fast Sequential
AA reduces
analysis times by 50%
1998
Releases first
simultaneous
ICP-OES with
full wavelength
coverage
2000
Launch of 7500
Series ICP-MS
2004
Introduction of
200 Series AA
and GTA120
GFAA with
extended tube
life
2006
Launch of the
700 Series ICP-
OES - world's
fastest ICP-
OES
2009
Launch of the
Agilent 7700
Series, with HMI,
3rd generation
ORS, and
Masshunter s/w
2011
Agilent redefines
elemental
analysis with the
introduction of
the Agilent 4100
MP-AES
2012
Agilent releases
the world's first
triple quad ICP-
MS, the Agilent
8800 ICP-QQQ
Agilent Technology Leadership, the first 55 years…
And still leading the way with recent innovative releases!
Agilent 4200 MP-AES
Safer, more cost effective elemental analysis that is uniquely suited for a wide range of sample types and applications.
- Reduce your analysis cost
- Improve your laboratory safety
- Simplify your workflow
- Increase analytical performance
Agilent 7900 ICP-MS
The most robust, sensitive, and easy to use quadrupole ICP-MS ever.
- 10x better matrix tolerance – up to 25% total dissolved solids
- 10x better signal to noise performance – improved sensitivity and detection limits
- 10x wider dynamic range – up to 11 orders of concentration from ppt to 10,000s ppm
- Software so simple yet powerful it writes your methods for you
- Enhanced customer experience – better training, easier maintenance
The new Agilent 5100 ICP-OES!
The world’s most productive, high performance ICP-OES.
- World’s first and only non-sequential dual view instrument; Synchronous Vertical Dual View (SVDV)
- Highest throughput reduces your analysis cost
- Vertical plasma runs your toughest sample
- Dichroic Spectral Combiner (DSC) simplifies method development
The Agilent Atomic Spectroscopy Instrument Family
Agilent’s 55 and 200 Series includes the
world’s fastest flame AA and
the world’s most sensitive
furnace
Agilent’s 4200 MP-AES runs on air for the lowest cost of ownership and
improved safety
Agilent’s 5100 ICP-OES is the
world’s most productive, and
only Synchronous Vertical Dual
View ICP-OES
Agilent’s 7900 is the most
robust, sensitive, and easy to use quadrupole
ICP-MS ever
Agilent’s 8800 ICP-QQQ provides accurate
measurement of difficult and
interfered elements
Types of applications in Food & Agriculture
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Typical ‘routine’ applications
Agriculture crop yield optimization
• Extractable elements in fertilizers
• High levels of active ingredients (N-P-K), low levels of secondary (Ca, Mg,
S), and micro nutrients (B, Cu, Fe, Mn, Zn)
• Extractable elements in soils (soil quality)
• Nutrient and micronutrient content to monitoring deficiencies
Plant materials and animal feed
• Nutrients for optimal livestock growth/development
• Contaminants and toxic elements that pass into the animal tissues
February 2, 2015
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Typical ‘routine’ applications
Food quality/nutrients
• Dairy, meat, fish, grain, vegetables, fruit, processed goods, etc
• Essential minerals at high levels (Na, Mg, P, S, Ca, Fe, etc)
• Essential elements at low levels (V, Cr(III), Co, Se, I, etc)
Food safety
• Dairy, meat, fish, grain, vegetables, fruit, processed goods, etc
• Toxic trace elements (As, Cd, Hg, Pb, etc)
• Chemical form can determine toxicity (Cr(VI), As(III & V), MeHg, etc)
• Elements that are toxic in excess (Al, Ni, Cu, Zn, Se, etc)
• Food profiling/authenticity
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Typical ‘routine’ applications
Other related samples
• Water for irrigation
• Food additives / flavors / colors
• Packaging materials
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Agilent restricted
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Examples of available applications
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5100 ICP-OES Applications
February 2, 2015
Confidentiality Label
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Food testing & agriculture
Neli Drvodelic
Agilent Technologies Melbourne, Australia
Publication number: 5991-4868EN
Publication date: July 2014
Analysis of bovine liver using the Agilent 5100ICP-OES
Measurement challenge
13
Challenge
How to improve sample throughput and reduce operating costs in a
food testing lab whilst maintaining analysis sensitivity and
precision.
Solution
When analyzing a Bovine Liver certified standard, the Agilent 5100
Synchronous Vertical Dual View ICP-OES delivered excellent linear
dynamic range for the major elements (Na and K, up to 500ppm),
and good agreement with certified reference values for major,
minor, and trace level elements. Sample throughput was increased
by the ability to measure both axial and radial views of the plasma
in a single measurement. This also reduced the argon consumption.
Introduction
ICP-OES is a common technique used to test food products for a range of elements including nutrients, micro-nutrients and toxic elements.
Food testing laboratories often measure samples with complex matrices, and high dissolved solids content. This can cause build up on an ICP torch, resulting in poor long term stability and accuracy, and more instrument downtime for cleaning.
These labs typically require ease of use without sacrificing measurement accuracy, and excellent linear dynamic range for both major and trace elements. Low cost of analysis and high sample throughput is also required, as is fast sample turn around.
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Results and discussion
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Recoveries• Majority of results were within 5% of the certified/reference concentration
Table 2. Results for NIST Bovine Liver 1577 SRM
Element (nm) MDL
(mg/kg)
Measured values
(mg/kg)
SD Certified value
(mg/kg)
SD Recovery(%)
K 766 7.8 9832 5.2 9700 0.06 101
Na 589 9.08 2410 2.9 2430 0.013 99
Fe 238 0.17 258 1.9 270 20 96
Cu 327 0.16 203 1.1 193 10 105
Zn 213 0.33 131 0.56 130 10 101
Mn 257 0.008 9.8 0.01 10.3 1 96
Cd 228 0.13 0.26 0.02 0.27 0.04 96
Element (nm) MDL
(mg/kg)
Measured values
(mg/kg)
SD Reference value
(mg/kg)
Recovery (%)
Ca 396 6 126 0.16 123 103
Mg 279 0.83 603 2.4 605 100
Mo 202 0.18 3.4 0.05 3.2 106
Sr 407 0.01 0.142 0.002 0.14 102
Table 3. Results for NIST Bovine Liver 1577 SRM. Certified values are not available for the elements listed.
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Conclusions
Certified bovine liver samples were analyzed using the Agilent 5100
SVDV ICP-OES.
The study found that:
• The instrument had an excellent linear dynamic range, up to 500 ppm,
for Na and K, from a single reading
• Accuracy was within 5-6% of the certified values for major and trace
elements
• Spike recoveries ranged from 99-110% when a 100 ppb spike was
performed for elements that were below the limit of quantification.
• High sample throughput was observed, with quicker sample
measurement delivering considerable gas savings
• Vertical torch resisted contamination and build-up, even with high
dissolved solids high and delivered robust analytical performance
• Features such as the plug and play torch, and intuitive software
interface, improve ease of use ensure reproducible performance
To find out more, visit agilent.com/chem
Food testing
Neli Drvodelic
Agilent Technologies Melbourne, Australia
Publication number: 5991-4900EN
Publication date: July 2014
Analysis of milk powders based on the Chinese standard method, using the Agilent 5100 ICP-OES
Measurement challenge
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Challenge
How to measure elevated levels of Na, K and Ca in milk powder, whilst
also accurately measuring trace levels of toxic elements.
Solution
The Synchronous Vertical Dual View mode of the Agilent 5100 ICP-OES
proved ideal for this application.
The major elements were measured using the radial view of the plasma
and the trace elements using the axial view. This could all be done in a
single measurement – resulting in short sample measurement times and
reduced argon consumption.
Introduction
ICP-OES is a common technique used to test food products for a range of elements including nutrients, micro-nutrients and toxic elements.
Food testing laboratories often measure samples with complex matrices, and high dissolved solids content. This can cause build up on an ICP torch, resulting in poor long term stability and accuracy, and more instrument downtime for cleaning.
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These labs typically require ease of use without sacrificing
measurement accuracy, and excellent linear dynamic range for
both major and trace elements. Low cost of analysis and high
sample throughput is also required, as is fast sample turn
around.
Results and discussion
20
Recoveries
• Recoveries ranged from
92-107%
• Wide dynamic range for
elements at ppb levels and at
% levels – in a single reading
Table 3. Recoveries from the analysis of NIST Milk Powder 8435 SRM
Element
(nm)
Certified
value
(mg/kg)
Measured
value(mg/kg)
Recovery
(%)
K 766.491 13630 13070 96
Ca 315.887 9220 9750 106
P 213.618 7800 7160 92
Na 589.592 3560 3530 99
S 181.792 2650 2650 100
Mg 279.078 814 749 92
Zn 202.548 28.0 28.9 103
Sr 421.552 4.35 4.37 101
Fe 259.940 1.8 1.9 107
Cu 327.395 0.46 0.46 100
Mo 204.598 0.29 0.27 92
Mn 257.610 0.17 0.18 103
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Conclusion
Certified whole milk powder samples were analyzed using the Agilent
5100 SVDV ICP-OES.
The study found that:
• Trace toxic and major nutrient elements were able to be measured in
a single measurement, without ionisation buffers
• Method detection limits were better than required by the method
• Excellent recoveries (92-107%) were achieved for all elements –
instrument was accurate over a large dynamic range
• High sample throughput was observed, with the quicker sample
measurement delivering considerable gas savings
• Vertical torch resisted contaminations and build-up, even with high
dissolved solids and delivered stable and robust analytical
performance
To find out more, visit agilent.com/chem
Example ICP-OES Applications (700 series)
February 2, 2015
Confidentiality Label
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• Elemental analysis of food (routine monitoring for food safety)
• “Fingerprinting” (Agilent package with MPP - chemometrics)
• Speciation
- LC-ICP-MS – As in juice
- GC-ICP-MS – pesticides, volatiles
- FFF-ICP-MS – nanoparticle characterization
Key ICP-MS Applications in Food Analysis
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Importance of Food Applications – Public Interest
Huge public interest; major news items each week relating to food safety:
1. Nutrition (5 a day, Se supplementation)
2. Toxicity (As in apple juice and brown rice syrup)
3. Contamination (Hg in seafood, melamine in baby formula)
4. Adulteration and fraud (dilution, substitution, mislabelling; horse meat in “beef” burgers; smuggling, import tax avoidance)
5. Production, additives and packaging (nanoparticle leaching)
Trace elements are complementary to DNA testing – trace elements vary by region (and sometimes method) of production, so can differentiate cases where the same foodstuff has different value depending on where it came from: olive oil, honey, juice, wine…
Toxicity, bioavailability and nutrition all depend on chemical form of the element (speciation). Agilent is WW leader in speciation with ICP-MS
Agilent offers complete solution – separation (LC, GC, CE (FFF)), inorganic and organic mass spec, chemometrics, data security and reporting
Page 24
7900 ICP-MS Applications
February 2, 2015
Confidentiality Label
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ICP-QQQ Extends Range of ApplicationsMore effective interference removal and higher sensitivity
• Accurate, low-level analysis of non-metals – Se & As
• Analysis of S, P, Cl… Quantitation of non-metal containing
biomolecules; enables monitoring of metabolic functions
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Food testing
Kazuhiro Sakai et al
Agilent Technologies Japan
Publication number: 5991-4556EN
Publication date: May 2014
Method automation for analysis of trace elements in foods by ICP-MS
ExperimentalMethod building
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Automatic mode
Based on the current instrument configuration and the
composition of the user’s own reference sample, which is
measured as part of the method setup, the Method Wizard
automatically selects the most appropriate:
• operating conditions (plasma mode and tuning conditions)
• analyte isotopes
• integration times
• cell gas modes
• internal standards
.
ExperimentalMethod building – Automatic mode
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• Sample uptake and rinse times are calculated from the tuning solution
measurement.
• Total dissolved solids (TDS) level and major element composition are
derived from the results of the semi-quantitative analysis of the typical
sample.
• The measured TDS level is used to determine the appropriate plasma
mode (Low Matrix, General Purpose, UHMI-4, -8, -25)
• The major element composition is used to identify potential matrix-based
interferences and to select the most appropriate cell mode (no gas, He,
High Energy (HE)He, H2), isotope, integration time and ISTD for each
analyte.
Results and discussionAnalytical results
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Accurate analytical results of food CRMs measured using method created by ICP-MS MassHunter's Method Automation function
Analyte UnitDORM-4 (fish protein) 7402-a (cod fish tissue) 7403-a (swordfish tissue)
Concentration Certified Concentration Certified Concentration Certified
9 Be [No gas] mg/kg 0.01 ± 0.00 N.D. (<0.0008) N.D. (<0.0008)
23 Na [No gas] g/kg 12.9 ± 0.3 3.4 ± 0.1 3.6 ± 0.2 3.57 ± 0.07 3.57 ± 0.12
24 Mg [No gas] g/kg 0.81 ± 0.01 1.29 ± 0.03 1.34 ± 0.03 1.60 ± 0.03 1.58 ± 0.04
31 P [HEHe] g/kg 7.6 ± 0.2 10.8 ± 0.1 12 14.5 ± 0.2 14.5 ± 0.4
34 S [HEHe] g/kg 8.7 ± 0.2 10.4 ± 0.1 8.43 ± 0.06
39 K [H2] g/kg 12.6 ± 0.6 21.3 ± 1.2 22.3 ± 1.0 25.5 ± 0.8 26.3 ± 1.1
40 Ca [H2] g/kg 2.18 ± 0.11 0.46 ± 0.03 0.52 ± 0.05 0.196 ± 0.014 0.189 ± 0.009
51 V [He] mg/kg 1.50 ± 0.01 N.D. (<0.014) N.D. (<0.014)
52 Cr [He] mg/kg 1.75 ± 0.09 1.87 ± 0.16 0.67 ± 0.00 0.72 ± 0.09 0.058 ± 0.001
55 Mn [He] mg/kg 3.02 ± 0.11 0.41 ± 0.03 0.41 ± 0.03 0.190 ± 0.004 0.201 ± 0.010
56 Fe [H2] mg/kg 339 ± 20 341 ± 27 11.2 ± 0.5 11.2 ± 0.9 13.6 ± 0.7 13.1 ± 0.5
59 Co [He] mg/kg 10.7 ± 0.09 0.030 ± 0.003 0.04 0.015 ± 0.001
60 Ni [He] mg/kg 1.26 ± 0.11 1.36 ± 0.02 0.40 ± 0.10 0.38 ± 0.05 0.076 ± 0.037
63 Cu [He] mg/kg 15.8 ± 0.1 15.9 ± 0.9 1.13 ± 0.02 1.25 ± 0.07 1.26 ± 0.02 1.31 ± 0.04
66 Zn [He] mg/kg 49.3 ± 0.5 52.2 ± 3.2 20.5 ± 0.2 21.3 ± 1.5 33.3 ± 0.2 33.6 ± 1.0
75 As [HEHe] mg/kg 6.73 ± 0.08 6.80 ± 0.64 36.4 ± 1.1 36.7 ± 1.8 6.77 ± 0.13 6.62 ± 0.21
78 Se [H2] mg/kg 3.47 ± 0.12 3.56 ± 0.34 1.8 ± 0.1 1.8 ± 0.2 2.11 ± 0.06 2.14 ± 0.11
88 Sr [He] mg/kg 9.72 ± 0.10 1.74 ± 0.03 2 1.08 ± 0.02 1.13 ± 0.03
95 Mo [He] mg/kg 0.261 ± 0.005 0.010 ± 0.006 0.01 N.D. (<0.0008)
107 Ag [He] mg/kg 0.022 ± 0.001 N.D. (<0.0050) N.D. (<0.0050)
111 Cd [He] mg/kg 0.304 ± 0.001 0.306 ± 0.015 0.009 ± 0.000 0.009 0.152 ± 0.003 0.159 ± 0.006
118 Sn [He] mg/kg 0.077 ± 0.004 0.056 ± 0.010 0.016 ± 0.002 0.036 ± 0.001
121 Sb [He] mg/kg 0.009 ± 0.000 0.014 ± 0.001 0.02 0.002 ± 0.001
137 Ba [He] mg/kg 5.01 ± 0.03 0.027 ± 0.002 2.4 ± 0.02
202 Hg [He] mg/kg 0.358 ± 0.004 0.410 ± 0.055 0.53 ± 0.01 0.61 ± 0.02 5.02 ± 0.02 5.34 ± 0.14
205 Tl [He] mg/kg 0.001 ± 0.002 N.D. (<0.010) N.D. (<0.010)
208 Pb [He] mg/kg 0.405 ± 0.007 0.416 ± 0.053 0.03 ± 0.00 0.04 0.006 ± 0.003
232 Th [He] mg/kg 0.177 ± 0.002 N.D. (<0.0008) N.D. (<0.0008)
238 U [He] mg/kg 0.056 ± 0.005 N.D. (<0.0010) N.D. (<0.0010)
Food testing
Wim Proper & Ed McCurdy
Eurofins Analytico; Agilent Technologies UK
Publication number: 5991-4257EN
Publication date: April 2014
Analysis of High Salt Matrices using the 7900 with UHMI
High Salt Matrix Analysis: ExperimentalAnalytical procedure
• For the performance tests on the high NaCl matrices (up to 25% NaCl),
UHMI-100 (~100x aerosol dilution) was selected because it gives the
maximum robustness and tolerance of exceptionally high matrix levels.
• The instrument settings used are shown in Table 1.
• All lens voltages were optimized using the ICP-MS MassHunter autotune
function. It is clear that most parameters are consistent for the two gas
modes used.
• Analysis of a range of trace elements of interest was performed in salt
matrices ranging from zero added NaCl to 25% NaCl solution.
• All samples were measured against simple aqueous calibration standards
(no NaCl matrix), prepared in the same acid mix as the samples (0.5%
HNO3 and 0.6% HCl).
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Results and discussionEvaluation of UHMI matrix tolerance for high NaCl
35
Low level of matrix suppression (~50%) and no long-term drift for internal standard signal for sequence including
50 samples of 25% NaCl matrix
Aqueous standards
and rinse
25% NaCl Matrix
samples
Initial signal drop due to
sample transport and
nebulization effects
Results and discussionAccurate analysis in variable NaCl matrices
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Left. Spike recovery for As, Cd,
Hg and Pb in variable NaCl
matrices up to 25% NaCl
Right. Spike recovery for interfered
elements V (ClO), Cr (ClOH), Ni
(NaCl) and Cu (ArNa) in variable
NaCl matrices up to 25% NaCl
Results and discussionAnalysis of commercial table salt samples
Commercial table salts were purchased and analyzed in order
to test the application of the method for trace element
characterization of food-grade salt.
Sea salts and rock salts were sourced from various countries.
The analytical results obtained are shown in Table 3 for
information; no reference or expected concentrations were
available for these salt samples.
For simplicity, only the elements that were found at significant
levels or showed a high degree of variation between the
samples are shown.
38
39
Units SICJ
Japan,
Mexico,
Australia
seawater
Japan, Izu,
seawater
Japan,
Mexico,
Australia
seawater
Japan, Seto,
seawater
Japan,
seawater
Mexico,
seawater
Germany,
rock
Li µg/L 14 60 140 40 160 44 1.4 100
Mg mg/L 51 430 1500 190 350 130 91 150
Al µg/L 0.22 0.13 0.38 0.15 0.23 0.16 0.048 56
S mg/L 59 520 2000 490 76 48 51 51
K mg/L 250 190 470 150 560 180 59 150
Ca mg/L 56 210 740 310 210 86 1.3 720
V µg/L 0.11 0.12 0.53 0.21 0.47 0.13 2.8 7.7
Cr µg/L 0.19 0.35 0.39 0.18 0.22 0.23 0.66 10
Mn µg/L 4 0.084 0.071 0.14 4.4 1.5 0.049 26
Fe µg/L 0.85 1.1 1.4 1.1 1.4 1 1 120
Cu µg/L 1.3 0.13 0.74 0.082 42 10 0.082 6.4
Zn µg/L 1.6 0.068 0.02 0.085 3.7 2.7 0.046 8.8
Ga µg/L 0.0079 0.021 0.04 0.033 0.017 0.013 0.0072 0.046
As µg/L 0.13 0.3 0.52 0.16 0.1 0.2 0.22 0.32
Se µg/L 1 0.6 0.43 0.56 0.71 0.45 0.66 0.8
Br mg/L 120 42 100 34 330 95 10 32
Rb µg/L 18 38 110 22 240 54 0.16 81
Sr mg/L 0.3 2.8 4 4.8 1.6 0.66 0.047 0.1
Zr µg/L 0.0093 0.0031 0 0 0 0 0.016 0.24
Mo µg/L 0.25 3.2 12 1.7 2.1 0.18 1.2 0.21
Ag µg/L 2.9 7.8 8.7 4 3.6 1.6 2.4 43
Table 3. Analytical results of commercial table salts produced in various countries from rock salt or sea salt
Results and discussionAnalysis of commercial table salt samples
40
Units SICJ
Japan,
Mexico,
Australia
seawater
Japan, Izu,
seawater
Japan,
Mexico,
Australia
seawater
Japan, Seto,
seawater
Japan,
seawater
Mexico,
seawater
Germany,
rock
Cd µg/L 0.19 0.092 0.26 0.045 0.17 0.12 0.59 1.4
Sn µg/L 0.12 0.092 0.06 0.12 0.076 0.094 0.067 0.4
Sb µg/L 0.019 0.11 0.31 0.021 0.011 0.021 0.064 0.27
Te µg/L 2.9 0.96 1 1.1 4 1.5 0.7 0.72
I µg/L 0.82 38 43 41 160 41 85 120
Cs µg/L 0.098 0.13 0.33 0.081 1 0.22 0.019 12
Ba µg/L 0.97 12 17 11 5.1 1.9 0.51 3
W µg/L 0.25 0.016 0.022 0.02 0.069 0.07 0.11 0.069
Au µg/L 0.071 0.044 0.034 0.054 0.055 0.064 0.081 0.072
Hg µg/L 0.065 0.03 0.035 0.053 0.026 0.032 0.16 0.038
Pb µg/L 1.7 0.21 0.37 0.067 0.26 0.27 0.054 2
Table 3 continued. Analytical results of commercial table salts produced in various countries from rock salt or sea salt
Results and discussionAnalysis of commercial table salt samples
Conclusion
The Agilent 7900 ICP-MS with UHMI allows ICP-MS to be used for the first
time for the direct analysis of trace elements in very high matrix samples,
without prior sample dilution. The new UHMI system extends the aerosol
dilution range up to a factor of 100, tolerating TDS levels of up to 25% (10
times higher than the previous generation HMI), a matrix level 100 times
above the accepted limit for conventional ICP-MS systems.
The 7900 ICP-MS with UHMI option was used to analyze a wide range of
elements in undiluted saturated salt water and various commercially
available table salts. The analysis demonstrates a level of matrix tolerance
that is unprecedented in ICP-MS. This capability extends the use of ICP-MS
for samples with a very high salt matrix, offering a possible alternative to AA
or ICP-OES techniques.
For additional information, please visit the Agilent 7900 ICP-MS or
Environmental, Food or Energy and Chemicals websites.
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ICP-MS and MPP for Region of Origin Analysis of Chinese Honey
Food testing
Hui Chen et al
Chinese Academy of Inspection and Testing
Publication number: 5991-4967EN
Publication date: July 2014
Mass Profiler Professional (MPP) and ICP-MSChemometrics Software for Trace Element Fingerprinting
February 2, 2015
Agilent restricted
45
ICP-MSCan analyse up to ~70 elements in a fast
screening scan (using He mode to remove
matrix-based polyatomic interferences)
Data are transferred to MPP
MPPFlexible chemometrics software can identify
main distinguishing parameters, apply
several different statistical processes and
filters, model population classification and
display results in easily interpreted graphical
plots
Honey Sample Collection, Preparation and Analysis
RF power (W) 1550
Sample depth (mm) 8
Carrier gas (L/min) 1.1
Plasma gas (L/min) 15
Spray chamber temp (oC) 2
He cell gas (mL/min) 4.3
Number of replicates 3
February 2, 2015
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Samples and Sample Preparation163 honey samples including varieties produced from linden, vitex, rape, and acacia
plants were collected from beekeepers located in 4 geographical locations in China.
The honey samples were digested using a MARS 6 microwave oven (CEM Corp.,
USA). Full details are given in Ref. 1.
InstrumentationAn Agilent 7700x ICP-MS with standard glass concentric nebulizer, quartz double-
pass spray chamber, and nickel sampler and skimmer cones was used for the
analysis. The instrument conditions are given below
Results and discussion – MPP DataIdentification of Region (botanical origin) for Chinese Honeys
47
Ref: Chemometric Determination of the Botanical Origin for Chinese Honeys on the Basis of Mineral
Elements Determined by ICP-MS, Hui Chen, Chunlin Fan, Qiaoying Chang, Guofang Pang, Xueyan
Hu, Meiling Lu, and Wenwen Wang, J. Agric. Food Chem. 2014, 62, 2443−2448
Figure 1. Two first-component scores of honeys from different botanical origins: linden
(■), vitex (▲), rape (●), and acacia (◆) honey.
LC-ICP-MS for As Speciation in Apple Juice
Food testing
Tanoshima et al
Agilent Japan
Publication number: 5991-4967EN
Publication date: July 2014
LC-ICP-MS for As Speciation in Apple Juice
February 2, 2015
Agilent restricted
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Routine LC-ICP-MS Method with simple
filtration sample prep
Linear calibrations for As(III) and As(V) shown
below. Excellent sensitivity and stability
Routine Arsenic Speciation in Apple Juice1ug/L Spike Stability and Overlaid Chromatograms (n = 7)
50
Retention Time (min) Concentration (ug/l)
Sample Name AB DMA As(III) MMA As(V) AB DMA As(III) MMA As(V)
Apple Juice 1 Spike #1 2.77 3.62 4.19 6.43 10.62 0.85 1.11 1.61 0.98 1.52
Apple Juice 1 Spike #2 2.76 3.61 4.19 6.43 10.63 0.86 1.12 1.63 1.00 1.56
Apple Juice 1 Spike #3 2.77 3.61 4.19 6.41 10.62 0.87 1.12 1.62 1.01 1.55
Apple Juice 1 Spike #4 2.77 3.61 4.18 6.41 10.63 0.89 1.12 1.63 1.00 1.55
Apple Juice 1 Spike #5 2.78 3.61 4.19 6.41 10.65 0.88 1.13 1.64 1.01 1.56
Apple Juice 1 Spike #6 2.78 3.61 4.17 6.37 10.68 0.87 1.15 1.64 1.02 1.60
Apple Juice 1 Spike #7 2.78 3.60 4.17 6.35 10.69 0.88 1.14 1.65 1.02 1.59
Average 2.78 3.61 4.18 6.41 10.65 0.87 1.13 1.63 1.00 1.56
RSD % 0.28 0.16 0.23 0.48 0.27 1.53 1.20 0.91 1.29 1.55
Excellent sensitivity
and stability
As Speciation in Six Apple Juice Samples
February 2, 2015
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Fast analysis (<12
minutes) of total and
toxic inorganic (As(III)
and As(V)) species
Simple sample prep –
filtration. No sample
digestion, so avoid
contamination and
species conversion
Easy to screen for
high As levels
Total As and species
varies according to
region of production
and historical land use
4200 MP-AES Applications
February 2, 2015
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4200 App Note Major elements in Fruit Juice…perfect for MP-AES
• Undiluted juice has 11% TDS (mainly sugars) with major
elements ranging from 20ppm (Na) -1100ppm (K)
• Diluted 20x and acidified 5% HNO3. (0.6%TDS)
• Dilution required due to high level of sugars slowly blocking
sample introduction components.
• Working range for the major elements for the MP-AES at the
20 x diluted levels was 1-55ppm. (This is much higher than
AAS)
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New 4200 App NoteMajor elements in Fruit Juice…perfect for MP-AES
Apple Juice
T0840QC
Certified Value (mg/L) Found
(mg/L)
%Recovery
Assigned Value Range
Magnesium 49.0 40.3 – 57.8 49.9 ± 0.6 101.9
Sodium 21.2 16.9 – 25.4 22.2 ± 0.5 104.7
Potassium 1044 926 -1161 1039 ± 29.7 99.5
Grapefruit
Juice
T0842QC
Certified Value (mg/L) Found
(mg/L)
%Recovery
Assigned Value Range
Calcium 145.6 123.6 – 167.6 158.3 ± 3.2 108.7
Magnesium 92.5 77.5 – 107.4 91.1 ± 0.6 98.5
Potassium 1102 979 – 1225 1100 ± 14.7 99.8
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Basic Cost Estimation applied to Fruit Juice App
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Apple and Grapefruit Juice compared to AAS
On AAS, the reduced LDR means sample needs to be diluted further compared to MP-AES
On AAS, having to run Ca and Mg on the same sample means 2 different burners required and 3 different gases. Slow throughput will not be reduced even with FS when a burner change is needed.
On AAS, as easily ionisable Na and K need to be determined, will need to add ionisation buffer to each sample and standard.
CONCLUSION:
Using the MP-AES for the major elements in fruit juice is easier, faster and is done at lower running costs compared to FAAS.
Approx $32,000 per year savings on 500 samples per week, 3 elements compared to AAS.
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Determination of major, minor and trace elements in rice flour using the 4200 (MP AES)
John Cauduro
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Sample PreparationNIES CRM 10c Rice Flour
• Digested in Milestone Ethos microwave using preloaded
method
• 0.5g in 7 mL of HNO3 and 1 mL H2O2
• Digested, cooled then diluted to 25 mL
• Final total dissolved solids of 2%
No further sample preparation required
No modifiers or ionization buffers required
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ResultsCRM Recoveries
mg/kg in
solid
Ca
422.673
Cd
228.802
Cu
324.754
Fe
438.354
K
766.491
Mg
280.271
Mn
403.076
P
214.915
Zn
213.857
Mean 96.0 1.96 4.13 11.50 2700 1174 37.35 3139 22.02
SD 2.5 0.11 0.29 1.03 105 23 1.04 92 0.48
Certified
value95 1.82 4.1 11.4 2750 1250 40.1 3350 23.1
2SD
certified2 0.06 0.3 0.8 100 80 2.0 80 0.9
%
Recovery101.0 107.7 100.8 100.9 98.2 93.9 93.1 93.7 95.3
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• Accurate determinations over a wide concentration range
• All in one sample measurement
Conclusion4200 MP-AES is the Ideal FAAS Replacement
Improved Performance
• Increased working range
• Phosphorus
• Lower detection limits
Reduced Running Costs
• Runs on Air!
• No modifiers
Increased safety
• No acetylene
• No nitrous oxide
Ease of Use
• MP Expert
• Simple sample prep
• No burner change over
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Example 4100 MP-AES Applications (applicable to 4200 also)
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Example AA Applications
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Conclusions:A portfolio to cover any Food & Ag applicationIn some cases, a sample/application may be suitable for more than one
technique, eg:
• Metals in wine: FAAS, MP-AES, ICP-OES or ICP-MS
• Heavy soil digest: ICP-OES, ICP-MS (UHMI)
Others requirements might also drive your choice, such as number of
samples, operating budget, and operator skill…
Regardless of your application needs and drivers, Agilent’s unique and
comprehensive Atomic Spectroscopy Portfolio provides the right solution for
your Food & Agriculture analysis requirements.