Application of a Second

Generation Microwave
Plasma Atomic Emission
Spectrometer (MP-AES) in
the Analysis of Food
Samples

Steven Pang
Agilent Technologies,
Singapore
14th April 2014

Confidentiality Label
July 9, 2014
1
 Agenda

• Change is in the air

• How does the 4200 MP-AES work?
• Technology inclusions
• Key Benefits
• Ease of Use benefits over FAAS
• Instrument and analytical performance
• Analysis of Food Samples
• Summary

2
Introducing the Agilent 4200 MP-AES

The 4200 MP-AES is the second generation of proven MP-AES

technology.
The 4200 offers safe, cost effective elemental analysis, and
expands the application range of MP-AES.

3
 Microwave Plasma Emission Overview

Ground State Excited State Emission

Monochromator Quantitation
& Detector

Microwave excited
Plasma

Sample

Page 4
How does the MP-AES work?
• 4200 MP-AES runs from Nitrogen extracted from air using
Agilent 4107 nitrogen generator

• Axial magnetic and radial electrical fields generated by a

magnetron sustain the nitrogen plasma
• Sample aerosol is introduced into nitrogen plasma.

5
How does the MP-AES work?
• Axial emission from the nitrogen plasma is directed into the
fast scanning monochromator optics

• Wavelength specific emissions are detected using a high

efficiency CCD.

6
Introducing the Second Generation Agilent 4200 MP-AES
Optimized, second generation plasma system and new torch design:
Superior analytical performance and torch robustness suiting a
broader range of complex matrix samples.

MP Expert v1.2:
Intuitive software
interface, now
with advanced
features in the
‘PRO’ pack. Mass flow control of
nebulizer gas and
robust sample
introduction:
Enhanced accuracy
and long term
stability in tough
samples.

7
Key Benefits of the 4200 MP-AES
• Runs on air!
Lowest cost of • Eliminates on-going gas
ownership supply costs

Safer • No flammable gases

Laboratory • Unattended multi-element
Operation operation

• Ideal flame AA alternative

Higher • Handles major, minor
& most trace levels
Performance • Wider linear dynamic range
• Lower detection limits

New generation software

Easy • Simultaneous auto background correction
Operation • Plug & Play torch

8
Low cost of ownership
• Supply of gases is the major on going cost for any routine
elemental spectrometer.
• 4200 MP-AES uses Nitrogen extracted from air using
Agilent 4107 nitrogen generator.
• Example, big USA fruit juice manufacturer doing 100 FAAS
samples per day, 3 elements per sample.

Online cost estimator available at:

www.agilent.com/chem/runsonair

9
Safety
• Using inert Nitrogen gas to sustain the
atomization/ionization source eliminates the
need to use combustible gases like
acetylene.

• Not having to ever replace a gas cylinder

reduces manual handling issues.

10
4200 MP-AES Performance – Detection Limits
DL’s in ppb, clean water samples
Element Flame AA 4200 MP- Element Flame AA 4200 MP-
AES AES
K 0.8 0.65 As* 60 57
Ca 0.4 0.04 Cd 1.5 1.4
Mg 0.3 0.09 Cr 5 0.3
Na 0.3 0.12 Mn 1.0 1.05
Au 5 2.1 Pb 14 2.5
Pt 76 6.1 Sb 37 12
Pd 15 1.6 Se* 500 77
Ag 1.7 1.2 Zn 1.6 3.1
Rh 4 0.5 * 30 seconds integration time used for these
elements

11
4200 MP-AES Performance
Working concentration range

Linear range comparison

between FAAS and MP-AES Example: Au 242.8nm calibration for 4200 MP-AES

Element 4200 MP-AES, Linear correlation FAAS, mg/L

mg/L coeff. MP-AES
Au 242.8 0-50 0.9999 0.1 – 30
Ca 422.6 0-20 0.9999 0.01-10
Mg 518.3 0-100 0.9999 0.15-20 (202.6nm)
Na 589.5 0-20 1.0000 0.01-2
K 767.8 0-100 0.9997 1-6

12
4200 MP-AES Performance in Complex Matrix
Analysis stability is ensured with robust sample introduction
components and mass flow control on the nebulizer gas line.
2hr stability graph of 5 target analytes in
presence of >3% TDS Gp I+II matrix

1.4

1.2 Cu MP
normalised concentration

Ag MP
1
Ni MP
0.8 Fe MP
Pb MP
0.6

0.4

0.2

0
0 20 40 60 80 100 120 140 mins

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Ease of Use

Simple hardware
• Torch installation
• Sample Introduction System

14
Ease of Use

Simple software
• Applet quick start methods
• Auto optimization tools
• FLIC and IEC tools

15
Ease of Use - MP-AES verses FAAS
• Simple sample preparation
- Reduced chemical and ionization interferences minimizes need for
addition of extra reagents
• Lower costs
• Reduces introduction of possible contaminants

Element Possible Chemical FAAS specific sample MP-AES specific

interferences preparation sample preparation
Calcium Refractory compounds Lanthanum or strontium None
with phosphorus. releasing agent on
Ionization effects from air/acetylene flame.
sodium, potassium Potassium ionization buffer
on a nitrous oxide/acetylene
flame

Potassium Ionization effects Cesium ionization buffer None

Magnesium Refractory compounds, Lanthanum or strontium None
ionization effects releasing agent
Sodium Ionization effects Potassium nitrate of chloride None

16
Determination of Major Elements in Fruit Juices

Major elements such as calcium, magnesium, sodium and

potassium are essential nutrients in food and the routine
monitoring of the levels of these elements in fruit juices is a
common quality control process.

July 9, 2014
17
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)

• Easier sample preparation compared to FAAS.

• Reduced dilution
• No ionisation buffer required to be added in

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 Experimental
Instrumentation
Instrument: Agilent 4200 MP-AES with 4107 Nitrogen Generator
Sample introduction system: a double-pass cyclonic spray chamber and
the OneNeb nebulizer and SPS3
Software: Agilent MP Expert software

Nitrogen Generator SPS3 OneNeb Agilent 4200 MP-AES

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Experimental
Instrumentation
Parameter Value
Element Ca Mg Na K
Wavelength 422.673 518.360 589.592 769.897
Nebulizer OneNeb
Nebulizer flow rate Default (0.75 L/min)
Spay chamber Double pass cyclonic glass
Pump rate 15 rpm
Sample pump tubing Orange/ Green
Waste pump tubing Blue/blue
Autosampler Agilent SPS 3
Read time 1 second
Number of replicates 3
Fast pump during uptake On
Sample uptake delay 30 seconds
Rinse time 40 seconds
Stabilization time 20 seconds
Background correction Auto
Gas source Nitrogen generator

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Major Elements in Fruit Juice
Apple Juice Certified Value (mg/L) Found %Recovery
T0840QC Assigned Value Range (mg/L)
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 Certified Value (mg/L) Found %Recovery

Juice Assigned Value Range (mg/L)
T0842QC

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

21
4200 MP-AES Performance - Stability

Analysis stability is ensured with robust sample introduction

components and mass flow control on the nebuliser gas line.

0.6% TDS fruit juice (with 5% HNO3) run over 6 hrs.

Agilent Confidential
July 9, 2014
22 22
Analysis of Rice Flour Samples

Analysis of major, minor and trace elements in rice flour is

important for food safety, measurement of nutrient elements,
and also product origin testing.

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4200 MP-AES
General method parameters

Table 2. Method parameters

Parameter Value
Replicates 3
Pump rate 15 rpm
Sample uptake delay 30 seconds
Rinse time 60 seconds
Stabilization time 10 seconds
Fast Pump during Uptake and Rinse On (80 rpm)
Nebulizer OneNeb
Spray chamber Double pass cyclonic
Autosampler Agilent SPS 3
Sample pump tubing Orange/green
Waste pump tubing Blue/blue

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Wavelength selection and calibration range
• Continuous wavelength coverage allows lines to be chosen that have
appropriate sensitivity for the concentration range, and avoid spectral
interferences.
• Only 1 dilution is required for the complete set of elements
Table 3. Working calibration concentration range
Element Calibration range for this application

P 214.915 0 – 100 ppm

Cd 228.802 0 – 1.0 ppm
Mg 280.271 0 – 40 ppm
Zn 213.857 0 – 4.0 ppm
Mn 403.076 0 – 1.0 ppm
K 766.491 0 – 100 ppm
Cu 324.754 0 – 1.0 ppm
Fe 438.354 0 – 1.0 ppm
Ca 422.673 0 – 4.0 ppm

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Results
CRM recoveries

• Accurate determinations over a wide concentration range

• All in one sample measurement

Table 5. Results of NIES No.10c Rice Flour. All results in mg/kg in the solid sample.
mg/kg in Ca Cd Cu K Mg Mn P
Fe 438.354 Zn 213.857
solid 422.673 228.802 324.754 766.491 280.271 403.076 214.915

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
95 1.82 4.1 11.4 2750 1250 40.1 3350 23.1
value
2SD certified 2 0.06 0.3 0.8 100 80 2.0 80 0.9

% Recovery 101.0 107.7 100.8 100.9 98.2 93.9 93.1 93.7 95.3

9 July 2014
26 26
Long term stability
<3% RSD for all elements over 8 hours in 2% TDS
The combination of improved waveguide and torch, robust
plasma and sample introduction gives excellent long term
stability.
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
1.5
1.4
1.3
1.2
1.1
Normalized Conc.

1
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0 33 66 99 132
No. of Samples

9 July 2014
27 27
 Summary
• The Agilent 4200 MP-AES is a second generation of
proven MP-AES technology.
• The 4200 offers safe, cost effective elemental
analysis, and expands the application range of MP-
AES.
• The 4200 MP-AES is very easy to use and has
simple sample preparation relative to the AAS
technique.
• 4200 has an expanded application range due to
increased component robustness and excellent %
recoveries in complex matrix samples.
• Through the displacement of fuel gases such as
acetylene and nitrous oxide, the MP-AES leads in the
area of environment-friendly (green) technology. This
ties in the CSR initiatives of today’s businesses.

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 Thank You!

http://www.chem.agilent.com/en-
US/promotions/Pages/4200mp-aes.aspx
Agilent MP-AES

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