July 9, 2014

Confidentiality Label

1

Steven Pang

Agilent Technologies,

Singapore

14th April 2014

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

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

Sample

Microwave excited

Plasma

Monochromator

& Detector

Quantitation

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

Mass flow control of

nebulizer gas and

robust sample

introduction:

Enhanced accuracy

and long term

stability in tough

samples.

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.

7

8

Higher Performance

• Ideal flame AA alternative

• Handles major, minor & most trace levels

• Wider linear dynamic range

• Lower detection limits

Easy Operation

New generation software

• Simultaneous auto background correction

• Plug & Play torch

Safer Laboratory Operation

• No flammable gases

• Unattended multi-element operation

Key Benefits of the 4200 MP-AES

Lowest cost of ownership

• Runs on air!

• Eliminates on-going gas supply costs

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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

10

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.

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Element Flame AA 4200 MP-

AES

K 0.8 0.65

Ca 0.4 0.04

Mg 0.3 0.09

Na 0.3 0.12

Au 5 2.1

Pt 76 6.1

Pd 15 1.6

Ag 1.7 1.2

Rh 4 0.5

DL’s in ppb, clean water samples

4200 MP-AES Performance – Detection Limits

Element Flame AA 4200 MP-

AES

As* 60 57

Cd 1.5 1.4

Cr 5 0.3

Mn 1.0 1.05

Pb 14 2.5

Sb 37 12

Se* 500 77

Zn 1.6 3.1

* 30 seconds integration time used for these

elements

4200 MP-AES Performance Working concentration range

Linear range comparison

between FAAS and MP-AES

Element 4200 MP-AES,

mg/L

Linear correlation

coeff. MP-AES

FAAS, mg/L

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

Example: Au 242.8nm calibration for 4200 MP-AES

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4200 MP-AES Performance in Complex Matrix

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Analysis stability is ensured with robust sample introduction

components and mass flow control on the nebulizer gas line.

0

0.2

0.4

0.6

0.8

1

1.2

1.4

0 20 40 60 80 100 120 140

no

rmalised

co

ncen

trati

on

mins

2hr stability graph of 5 target analytes in presence of >3% TDS Gp I+II matrix

Cu MP

Ag MP

Ni MP

Fe MP

Pb MP

Ease of Use

Simple hardware

• Torch installation

• Sample Introduction System

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Ease of Use

Simple software

• Applet quick start methods

• Auto optimization tools

• FLIC and IEC tools

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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

interferences

FAAS specific sample

preparation

MP-AES specific

sample preparation Calcium Refractory compounds

with phosphorus.

Ionization effects from

sodium, potassium

Lanthanum or strontium

releasing agent on

air/acetylene flame.

Potassium ionization buffer

on a nitrous oxide/acetylene

flame

None

Potassium Ionization effects Cesium ionization buffer None

Magnesium Refractory compounds,

ionization effects

Lanthanum or strontium

releasing agent

None

Sodium Ionization effects Potassium nitrate of chloride None

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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

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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

Agilent 4200 MP-AES Nitrogen Generator OneNeb SPS3

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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

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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4200 MP-AES Performance - Stability

Analysis stability is ensured with robust sample introduction

components and mass flow control on the nebuliser gas line.

July 9, 2014

Agilent Confidential

22

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

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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

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

Table 2. Method parameters

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Wavelength selection and calibration 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

• 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

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Results CRM 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

value 95 1.82 4.1 11.4 2750 1250 40.1 3350 23.1

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

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• 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.

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Long term stability <3% RSD for all elements over 8 hours in 2% TDS

9 July 2014

27

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

1.1

1.2

1.3

1.4

1.5

0 33 66 99 132

No

rmalized

Co

nc.

No. of Samples

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

The combination of improved waveguide and torch, robust

plasma and sample introduction gives excellent long term

stability.

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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Agilent Technologies – The Market Leader in Atomic Spectroscopy

Agilent MP-AES

Agilent ICP-QMS/-QQQ Agilent ICP-OES Agilent AAS

Thank You!

Page 29

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US/promotions/Pages/4200mp-aes.aspx