MPAES Accessories Applications

Geochemistry, Mining
Chemical and Petrochemical

and Minerals
Agilent 4100 MP-AES
Applications,
Accessories,
Software
and
Food and Agriculture Environmental
Questions
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Page11
Agenda for IDO SPS sales training
• Software Overview
•Auto & FLIC Background Correction Overview

• OneNeb Overview
– Examples in Geochemistry, Mining and Minerals Applications
• EGCM Overview
– Examples in Chemical and Petrochemical Applications
• MSIS Overview
– Examples of Food/Agriculture and Environmental Applications
• Questions
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Key Benefits by Market
• Improved performance
• Matrix handing to match
Chemical / flame AA
Petrochem • Low running costs
• Ease of use
• Fast sequential measurement

Food and • Ease of use
Agriculture • Improved performance
• No flammable gases
• Runs on air
• Improved performance
• Improved Geochemistry/
• No flammable gases
Environmental performance
• Runs on air
Metals • Unattended operation
(non –regulated • Moderate pricing
methods) • Unattended
operation
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4100 MP-AES Software
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Auto/FLIC Background Correction &
OneNeb Overview
Examples in Geochemistry, Mining and Minerals
Applications
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MP-AES Auto Background Correction
Auto uses the spectrum around the peak of interest to create

models.
1. Models of the background (the blank) and the analyte (the
standards) are created during the calibration block
2. For every sample the amount of blank model and the
amount of analyte model in the spectrum is calculated
3. Once the amount of analyte is known the intensity can be
determined
4. Because of very stable plasma structures no need for
correction lamps
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Example – Blank, 3 Replicates
Measured spectrum Blank substracted spectrum
Variation is below 20 counts/sec
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Example - Standard , 3 Replicates
1ppm Pb is 3200 counts/sec
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Example - Sample , 3 Replicates
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Example - Sample , 3 Replicates
BG correction left/right
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Detection Limit Comparison
Element Wavelength (nm) DL Auto (ppb) DL Off-Peak (ppb)

Zn 213.857 1.7 5.5
Mn 403.076 0.2 0.3
Mn 257.610 0.6 2.8
Cu 324.754 0.2 0.2
K 766.491 1.1 1.2
As 193.759 55 125
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Fast Linear Interference Correction (FLIC)
FLIC adds an extra model to correct for spectral interferences
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FLIC Performance Example – Ni Interference on Co
Same result for both Co lines in high Ni sample
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FLIC Performance Example – Fe Interference on As
As concentration in the presence of 1000 ppm Fe is <IDL when

using FLIC
Using Auto Using FLIC
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OneNeb Nebulizer
• Robust PFA and PEEK construction

– Inert - resistant to strong acids such as HF
– Resistant to breakage
– Moulded plastic design provides improved nebulizer
to nebulizer reproducibility
• Constant diameter narrow bore tubing through to

nebulizer tip
– Ideal for high solids/particulates
– Improved tolerance to high TDS samples
• Narrow aerosol size distribution provides

improved precision
• Handles a wide flow range from 0.1 to 2 mL/min.

– No sensitivity loss at low flow rates
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Principle of Operation – Inert OneNeb Nebulizer
Tip geometry dimensioned to

allow carrier gas to mix with the
sample
Turbulent mixing of liquid and
gas occurs
– Produces aerosol with a narrow
size distribution range
Droplets mixed into gas flow
No area of low pressure
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Comparison of Droplet Size Distribution
Unique Flow Blurring action increases nebulization efficiency
• 3x greater efficiency than conventional concentric nebulizer
• Improved sensitivity
14
12
Inert OneNeb nebulizer
10
Conventional concentric nebulizer
Proportion
8
of Total
0
0 10 20 30 40 50 60 70 80 90 100
Droplet Size (um)
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Cyanide Leach Solutions – Conventional setup
• CN Leach solution is 0.3% CN, 0.8% NaOH

• Run with Standard Sample intro system
• Blocked concentric nebulizer within 4 hours
• Blocked torch injector within 4 hours
Glass Concentric Nebulizer After < 4hrs of CN/NaOH.

Blocked!
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OneNeb setup
• Orange/green sample tubing

• Double pass spray chamber
• 3 rpm pump rate
• 30s uptake (fast pump on)
• 30s rinse with DI Water (fast pump on)
• Target was 12 hours – a shift in a high throughput lab.
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OneNeb
After ~37 hours of operation
Tip of the OneNeb nebulizer after 37 hours of operation!

Still working perfectly!
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Geochemical, Metals and Mining Ordering Review
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Dusty Environment Ordering Review
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Applications for the
Agilent 4100 MP-AES
Geochemical, Metals and
Mining Applications
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Instrument Parameters
Parameter Setting
Nebulizer Glass concentric
Spray chamber Single-pass glass cyclonic
Read Time 3s
Replicates 3
Sample uptake delay 10 s
Stabilization time 5s
Fast Pump On (80 rpm)
Background correction Auto
Nebulizer Pressure 140 to 240 kPa (auto optimized)
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4100 MP-AES Method Setup
Sample introduction kit

• Glass concentric Nebulizer – May use OneNeb Nebulizer
• Single pass cyclonic spray chamber
• Orange/Green pump tubing
Easy to use MP Expert software

• Auto background correction
• Auto Optimization for Neb and Viewing position
Improved productivity
• Automate analysis using SPS 3 autosampler
• Fast pump during uptake and rinse
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Traditional Off-Peak Correction for Ag in Digest
Limitations with Off-Peak Correction
• Correction points must be set manually
• Susceptible to spectral interferences
Is this the best correction

point for this matrix?
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Better Alternative - Use “Auto” Correction
Auto background correction uses the spectrum around

the peak of interest to create:
1. Models of the background (the blank) and the analyte (the
standards) – these are created during calibration
2. For every sample the amount of blank model and the
amount of analyte model in the spectrum is calculated
3. Once the amount of analyte is known, the corrected
concentration can be determined
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Auto Correction for Ag in Digest…
… improves detection limits,
is easier to use, Accurate model of the
no method development and no correction sloping background from
points to select the partial peak overlap
Blank Spectrum Standard Spectrum
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Accuracy – Gold in Custom CRMs*
CRM Certified value (mg/L) MP-AES result (mg/L)

1 19.8 19.3
2 7.9 7.4
3 23.1 22.7
4 5.6 5.7
5 57.8 55.3
6 3.1 3.3
7 35.9 35.4
8 8.4 8.9
* These custom CRMs were professionally prepared from solid ore

samples and certified through a round robin test process
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Results for Au in Unknown Samples
MP-AES is the Ideal FAAS Alternative
Sample MP-AES Flame AA Agreement

Result Result with AA Result (%)
(mg/L) (mg/L)
1 0.09 0.09 100
2 0.85 0.84 100
3 5.3 5.1 104
4 13.7 14.4 95
5 20.8 21.8 95
6 4.3 4.1 105
7 1.0 1.0 100
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Comparison of Au values measured with Agilent
4100 MP-AES compared to AAS and ICP-OES
6
MP - AAS correlation
y = 0.9918x - 0.0009
5
MP - ICP correlation
y = 0.974x + 0.0027
Au MP-AES (ppm)
4
MP - AAS
MP - ICP
Correl=1
3 Linear (Correl=1)
Linear (MP - ICP)
Linear (MP - AA)
2
0
0 1 2 3 4 5 6
Au ICP/AAS (ppm)
Very good correlation of Agilent MP-AES Au values in aqua regia

digests compared to ICP-AAS values
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Superior Performance – Detection Limits
Analyte Wavelength (nm) Method Flame AA

DL (ug/L) IDL (ug/L)
Au 267.595 4 11
Pt 265.945 13 76
Pd 363.469 0.7 15
MDL = 3σ, 3s read time, 20 blanks
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4100 MP-AES at Newmont Mining Automated Lab
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Standards ~ 0 to 1.0 ppm 267 nm Au Line
0.025 / 0.050 / 0.10 / 0.25 / 0.50 / 1.0
Low Detection Limit
Blank 10% 0.001
Blank 10% -0.001
Blank 10% -0.002
4 blanks before and
Blank 10% 0 after
0.025 0.0235
0.025 0.024 10 consecutive
0.025 0.0241
0.025 0.0242 readings of 0.025
0.025 0.0241 and 0.050 ppm
0.025 0.0238 respectively
0.025 0.0246
0.025 0.0235
0.025 0.0236 25 ppb DL = 1.3 ppb
0.025 0.023
0.050 0.0492
50 ppb DL = 1.9 ppb
0.050 0.0481
0.050 0.0493
0.050 0.0487 AVG DL = 1.6 ppb
0.050 0.049
0.050 0.0498
0.050 0.0486
0.050 0.0484
0.050 0.0477
0.050 0.0491
Blank 10% -0.002
Blank 10% -0.003
Blank 10% -0.003
Blank 10% -0.004
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Typical Detection Limits
Au – 10% aqua regia 1.6 ppb

Au – 0.03% NaCN + 0.08% NaOH 3.0 ppb
Ag – 33% aqua regia 0.6 ppb
Cu – 33% aqua regia 6.0 ppb
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Au – Extended Calibration Range
MP - normal AA range
MP - Extended Range
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Au – Fire Assay Results
Excellent correlation with AA results
FA QC
FA Q
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Au – Fire Assay Results
Excellent correlation with AA results – FA Q
6
3 MP ~ 267 Rational
AA ~ 242 Rational
0
0 1 2 3 4 5 6
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Cu / Ag - 33% Aqua Regia
Excellent correlation with AA results – Batch 3413
100
80
60
MP ~ Cu 324.754 Rational
MP ~ Ag 328.068 Rational
40 MP ~ Ag 338.289 Rational
AA ~ Cu 327.395 Rational
AA ~ Ag 328.068 Rational
20
0
1 3 5 7 9 11 13 15 17 19 21 23 25 27 29 31 33 35 37 39 41 43 45 47 49
-20
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Cu – 0.3% NaCN + 0.8% NaOH
Correlation with AA results – a bit more work to do
40
35
30
25
20
AA ~ Cu 327.395 Rational
15
10
0
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23
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Comments from Newmont Mining
“With the MP-AES instrument Agilent seems to have hit a homerun for both gold analysis and base metal
analysis. It provides superior detection limits and vastly expanded calibration range – this enables quick easy
analysis at trace levels as well as eliminates the need for time consuming dilutions of higher grade samples. All
of this at an affordable price of well below that of ICP and only slightly higher than top of the line AA units. ”
- Bobby Joe Reichel
Newmont Mining Corporation
Other Comments –
Very low detection limits for gold compared to AA and graphite furnace
Greatly extended calibration range for gold (0 to 400 ppm)
Extended calibration range for Cu & Ag (Cu-MP up to 125 ppm vs. Cu-AA up to 35 ppm; Ag-MP up to 50 ppm vs. Ag-AA up to 10
ppm.
Ease of operation and training superior to AA
Diagnostic software excellent and easy to use
Would not recommend for of high-cyanide / high-caustic samples at this time
Excellent within-run and between-run stability
Excellent accuracy at all points on the calibration curve
Improved efficiency because of higher linear range
Excellent calibrations without the need for numerous standards
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EGCM Overview
Examples in Chemical and Petrochemical

Applications
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External Gas Control Module (EGCM)
Purge
• O2 in the atmosphere absorbs low UV (<185nm)
• Purge with N2 to remove O2 from the Mono
• Purge takes ~3 hours

• Enables analysis of Sulfur
Add Air to Plasma
• Prevents carbon build up on the injector when running organics
• Reduces the background emissions from the plasma
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Why Add Air?
1. Prevents carbon build up on the injector when running

organics
2. Reduces the background emissions from the plasma
3. Air is added to the Intermediate flow
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Solvent background can be minimized with EGCM
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Solvent background can be minimized with EGCM
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Mono Purge enables analysis of S in the low UV
• O2 in the atmosphere absorbs low UV (<185nm)

• Purge with N2 to remove O2 from the Mono
• Purge takes ~3 hours
• Enables analysis of Sulfur
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Chemical and Petrochemical Ordering Review
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Purging Ordering Review
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Agilent 4100 MP-AES
Chemical and Petrochemical
Applications
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Challenges with Wear Metal Determinations
Reduce plasma solvent loading

• OneNeb nebulizer + Double Pass spray chamber
• Orange/Green solvent resistant tubing
• 5 rpm
Control the background

• Medium setting for Phosphorus at 213.618 nm
• High setting for all others
Improve Throughput and Ease of use

• SPS 3 with fast pump during sample uptake and rinse
• Auto-optimization of nebulizer pressure and viewing position
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4100 MP-AES Solves the Challenges
High vapour • OneNeb nebulizer

pressure from • Reduced sample flow
solvents • Cooled spray chamber
• EGCM
Carbon build up in
injector
• OneNeb nebulizer
Nebulizer
blockage
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Parameter Setting
Nebulizer Inert OneNeb
Spray chamber Double-pass glass cyclonic
Sample tubing Orange/green solvent resistant
Waste tubing Blue/blue solvent resistant
Read Time 3s
Replicates 3
Stabilization time 15 s
Rinse time 45 s
Fast Pump (80 rpm) On
Pump speed 5 rpm
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Measured Results for SRM 1085b Wear Metals
Great
recoveries
for all key
elements
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Measured Recoveries on 10 ppm Spike of Gear Oil
Great recoveries
for all key
elements
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Measured Results for Additive Elements
Measured Results vs Certified Values

Element Measured (mg/kg) Certified (mg/kg) Recovery %
P 213.618 301.5 ± 0.1 299.9 ± 7.2 101
Zn 481.053 314.9 ± 0.3 296.8 ± 6.8 106
Mg 285.213 300.6 ± 0.2 297.3 ± 4.1 101
Ca 422.673 279.6 ± 0.1 298 94
Ba 614.171 281.2 ± 0.1 300.1 ± 2.4 94
Measured Recoveries on 10 ppm Spike of Gear Oil
Element Mixed Gear (ppm) Spike (ppm) Recovery %
P 213.618 17.16 26.71 95
Zn 481.053 6.99 17.17 101
Mg 285.213 1.53 11.32 97
Ca 422.673 8.89 19.69 107
Ba 614.171 0.00 9.16 91
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Organics – Long Term Stability
1.5
1.4
1.3
1.2
1.1
1
Normalized Conc
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0:00 1:00 2:00 3:00 4:00 5:00 6:00 7:00 8:00
Time (h:mm)
Zn 213.857 nm Si 251.611 nm Fe 259.940 nm Ni 305.081 nm Ag 328.068 nm

Pb 283.305 nm Cu 327.395 nm Mg 285.213 nm Ti 334.941 nm Al 396.152 nm
10 ppm S21. All lines show precision of <1% RSD
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Limits on Target Elements in Diesel Fuel - EN14538
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Parameter Setting
Spray chamber Double-pass glass cyclonic
Read Time 3s
Replicates 3
Pump speed 5 rpm
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Method Detection Limits
3σ, 3s read time, 10 blanks
Element Wavelength (nm) MDL (ppb)

Mg 285.213 2.7
Ca 422.673 8.2
Na 588.995 18.7
K 766.491 2.7
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Direct Measurement of Impurities in Gasoline
Same ASTM D6751 limits

•Ca, Mg combined 5 ppm
•Na, K combined 5 ppm
High volatility of the gasoline is a challenge

•Cooled spray chamber -10 oC
•Standard Additions calibration
•Direct measurement of samples
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Parameter Setting
Spray chamber IsoMist cooled spray chamber (-10 oC)
Read Time 3s
Replicates 3
Background correction Off-peak
Pump speed 5 rpm
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Calibrations and Detection Limits
Element Wavelength (nm) Correlation Coeff MDL (ppb)

Mg 285.213 0.99993 2.7
Ca 422.673 0.99934 4.3
Na 588.995 0.99939 5.3
K 766.491 0.99975 29.4
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Spike Recoveries on Gasoline
Gasoline fuel sample spiked with 1.1 ppm S21+K
Element Sample (ppm) Spike (ppm) Recovery %

Mg 285.213 nm < MDL 1.11 100
Ca 422.673 nm < MDL 1.06 95
Na 588.995 nm < MDL 1.11 100
K 766.491 nm 0.05 1.12 96
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MSIS Overview
Examples of Food and Agriculture Applications
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MSIS
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Multimode Sample Introduction System (MSIS)
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Nebulization mode
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Vapour generation mode
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Dual mode
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Typical DL’s (ppb)
Analyte Neb Mode Dual Mode

As 90 1.0
Se 126 2.0
Hg 14 0.5
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MSIS Hg single mode
Calibration 10 points from 0.5 to 5 µg/l
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MSIS Ordering Review
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High TDS Ordering Review
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Agilent 4100 MP-AES
Food and Agricultural
Applications
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Sample Types
Wide Range of Matrices

• Dairy, Meat, Fish, Grain, Vegetables, Fruit, etc
• Processed goods
• Canned, frozen, dried and preserved food
• Drinks (soda, tea, coffee, alcoholic beverages etc.)
• Preservatives, “fillers” and additives such as calcium carbonate
• “Nutraceuticals”
Other Important Samples

• Water (used for irrigation)
• Soil
• Fertilizer
• Food additives / flavors / colors
• Packaging material
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Which Elements are Monitored in Foods?
Toxic trace elements
• Low level analysis – typically ppb levels

• As, Cd, Hg, Pb, Tl, Cr
Common elements that are toxic in excess
• Typically range from ppb to ppm level

• Al, Ni, Cu, Zn, Se, Mo, Sn
Essential minerals
• Can cover a wide range from ppm to % levels

• Na, Mg, P, S, K, Ca, Fe
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Food Applications – Solving the Challenges
• Standard Sample Introduction

Robust Sample • Concentric nebulizer
Introduction • Single pass spray chamber
• Improved throughput compared to Flame

Many Elements AA
Per Sample • CsCl buffer
• Over 14,000 wavelengths to chose from for

Wide Dynamic low and high concentration
• Lower detection limits for P compared to
Range Flame AA
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Parameter Setting
Nebulizer Glass concentric
Spray chamber Single pass glass cyclonic
Sample tubing White/white
Waste tubing Blue/blue
Read Time 10 s
Replicates 3
Fast Pump On (80 rpm)
Pump speed 12 rpm
Nebulizer pressure 160 – 180 kpa (auto optimized)
Background Correction Auto
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Method Detection Limits
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Measured Results for CRM Food Samples
NIES No. 10c Rice Flour High Purity Stds CRM Wheat Flour
* Reference values only
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Measured Results for CRM Food Samples
NIST 1577 Bovine Liver High Purity Stds CRM Oyster Tissue
* Reference values only
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Feedback from Sachsenforst, Germany (soil lab):
“The results for our aqua regia soil extract samples are convincing,
and those results are in very good agreement with the round robin,
which was performed Europe wide on those samples.”
- Frank Symossek
Sachsenforst
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Feedback from CERA Laboratory. India
“We are using MP-AES instrument for last couple of months, and we
found instrument is best to detect trace metals compare to AAS. In
AAS sensitivity for B and P is very poor and fuel cost is very high,
whereas using the MP-AES, sensitivity is very, very good and fuel cost
is very low. In AAS, with elements like Al, Ca, Mo,Ti, V, Si etc, it
consumes high quantities of Acetylene and Nitrous Oxide gas, and is
very tricky - whereas using the MP-AES, it is very easy to detect.
There is also no need to change Hollow Cathode Lamps which is time
consuming and costly.”
- S.S. Mhatre
CERA Laboratory
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THANK YOU!
QUESTIONS?
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Geochemistry, Mining

Chemical and Petrochemical

Agilent 4100 MP-AES

S1 CAG EMEAI FY13 |

•Auto & FLIC Background Correction Overview

S1 CAG EMEAI FY13 |

• Fast sequential measurement

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S1 CAG EMEAI FY13 |

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Auto uses the spectrum around the peak of interest to create

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Measured spectrum Blank substracted spectrum

Variation is below 20 counts/sec

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Measured spectrum Blank substracted spectrum

1ppm Pb is 3200 counts/sec

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Measured spectrum Blank substracted spectrum

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Measured spectrum Blank substracted spectrum

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Element Wavelength (nm) DL Auto (ppb) DL Off-Peak (ppb)

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FLIC adds an extra model to correct for spectral interferences

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Same result for both Co lines in high Ni sample

S1 CAG EMEAI FY13 |

As concentration in the presence of 1000 ppm Fe is <IDL when

S1 CAG EMEAI FY13 |

• Robust PFA and PEEK construction

• Constant diameter narrow bore tubing through to

• Narrow aerosol size distribution provides

• Handles a wide flow range from 0.1 to 2 mL/min.

S1 CAG EMEAI FY13 |

Tip geometry dimensioned to

S1 CAG EMEAI FY13 |

Droplet Size (um)

S1 CAG EMEAI FY13 |

• CN Leach solution is 0.3% CN, 0.8% NaOH

Glass Concentric Nebulizer After < 4hrs of CN/NaOH.

S1 CAG EMEAI FY13 |

• Orange/green sample tubing

S1 CAG EMEAI FY13 |

Tip of the OneNeb nebulizer after 37 hours of operation!

S1 CAG EMEAI FY13 |

S1 CAG EMEAI FY13 |

S1 CAG EMEAI FY13 |

S1 CAG EMEAI FY13 |

S1 CAG EMEAI FY13 |

Sample introduction kit

Easy to use MP Expert software

S1 CAG EMEAI FY13 |

Is this the best correction

S1 CAG EMEAI FY13 |

Auto background correction uses the spectrum around

S1 CAG EMEAI FY13 |

Blank Spectrum Standard Spectrum

S1 CAG EMEAI FY13 |

CRM Certified value (mg/L) MP-AES result (mg/L)

* These custom CRMs were professionally prepared from solid ore

S1 CAG EMEAI FY13 |

Sample MP-AES Flame AA Agreement

S1 CAG EMEAI FY13 |