Stop Worrying About Interferences With These ICP-OES …...Stop Worrying About Interferences With...

ASTS 2013

Agilent Science & Technology Symposium

Stop Worrying About Interferences With

These ICP-OES Solutions

Steve Wall

Agilent Technologies

Agilent ICP-OES The world's most productive high performance simultaneous ICP-OES

•Continuous wavelength coverage

provides extended dynamic range and

reduced interferences, giving you

maximum confidence in your results

•Robust plasma ensures reliable and

reproducible results—even with the most

complex matrices

•One view, one step measurement of

major, minor, and trace elements, plus the

fastest warm-up, increases throughput

and productivity

•Unique FBC (fitted background correction)

simplifies method development by

eliminating correction point selection

Agilent ICP-OES - Computer-optimized echelle optical and detector design

USP Webinar

Dec. 08, 2010

• Thermostatted to -35oC for low noise

• Adaptive Integration Technology (AIT)

• Provides true simultaneous measurement

• All wavelengths irrespective of signal intensity

• Background signal and internal standards

• Thermostatted to 35oC for stability and fast

start-up

• All wavelengths captured in one reading

• Fewer optical components

• High light throughput

• Excellent signal-to-noise

ICP-OES Long Term Stability Continuing Calibration Verification (CCV)

60

70

80

90

100

110

120

0 1 2 3 4 5 6 7 8 9

Time (Hours)

% R

eco

very

of

CC

V

Ag 328.068

Al 237.312

As 188.980

Ba 585.367

Be 313.042

Ca 315.887

Cd 214.439

Co 228.615

Cr 267.716

Cu 324.754

Fe 238.204

K 769.897

M g 285.213

M n 257.610

Na 568.821

Ni 231.604

Pb 220.353

Sb 217.582

Se 196.026

Tl 190.794

V 292.401

Zn 206.200

Lower limit

Upper limit

Long-term precision (RSD): 0.98% MAX

USP Webinar

Dec. 08, 2010

700-ES Interference Avoidance and Removal Tools

– Wavelength Database

– Confirmation and Qualifier Wavelengths

– Hidden Wavelengths

– Semi Quant

– Echellogram (720 and 725-ES)

– Fitted Background Correction (FBC)

– FACT Spectral Deconvolution

– Optimization Strategy

Wavelength Database

Wavelength database:

- Access to all wavelengths. Potential interferences

have been identified and appear in this database.

- Choose wavelengths based on freedom from

interferences as well as required sensitivity.

- Helps to know what elements are present in your

sample, although this is often not the case!

- Wavelengths are ranked as “most commonly used”

Wavelength Database





– Semi Quant





Confirmation and Qualifier Wavelengths

11


Element Result Element Result

Er 337.275

Er 349.910

0.15

0.16

P 177.434

P 213.618

0.24

0.22

Fe 238.204

Fe 259.940

440

480

Si 251.611

Si 252.851

46.5

46.4

Mn 257.610

Mn 259.372

11.2

12.3

Sn 189.927

Sn 235.485

0.01

388

Ni 216.555

Ni 231.604

1.06

0.97

Sr 407.771

Sr 421.552

1.24

1.35

12


• Table shows likely cause

is Fe overlap

• Make use of interference

free wavelength

• If no alternate line, use

FACT modeling





– Semi Quant





Hidden Wavelengths





– Semi Quant





Method Editor for Semi Quant Method





– Semi Quant





Echellogram Multi Element Solution

Echellogram Blank

Echellogram Multi-Element Solution - Blank





– Semi Quant





Background Correction Options

Off Peak, Manually Selected Correction Points

FBC Fitted Background Correction

FACT (Fast Automated Curve-Fitting Technique)

25

FBC (Fitted Background Correction)

• Improved accuracy

• Requires no user input

• Truly simultaneous correction

Peak shaped functions applied to the analyte

peak

Polynomial Interpolation of background signal

Only Agilent offers Fitted Background Correction!

Pb 220 with 1000ppm Mo





– Semi Quant





27

FACT (Fast Automated Curve-fitting Technique)

Peak modeling approach - Uses spectral data from analyte and interference standards

to de-convolve the analyte peak from nearby interference peaks

• Resolves extremely complex

spectral interferences

• Gives access to extra

wavelengths for improved

validation

• Allows resolution of interferences

as close as 3 pm





– Semi Quant





Condition Set “A”

Low Power, High Neb

Flow, Low viewing height

Condition Set “B”

High Power, Low Neb

Flow, Mid viewing height

Optimization Strategy

Page 22

30

Choice of three different optimization criteria

– Signal to Background Ratio (SBR), Intensity, Signal to Root Background

ratio (SRBR).

Optimize all or sub-set of

Optimization Strategy: AutoMax

Flame AAS

ICP-MS

AAS instruments can be

flame only, furnace only, or

combined (switchable)

4100 MP-AES

ICP-OES

Graphite Furnace AAS

ICP-QQQ

Agilent’s Atomic Spectroscopy Portfolio

Stop Worrying About Interferences With These ICP-OES …...Stop Worrying About Interferences With...

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