An Agilent Technologies’

Presentation at VinaLab 2013

22 March 2013

VinaLab 2013 1

Innovative

Breakthroughs in

Atomic Spectrochemical

Analysis

Contents

1. Introduction

2. Breakthrough #1

Running on Air - Myth or Reality?

3. Breakthrough #2

World’s First Functional ICP-QQQ

featuring Tandem MS/MS

Technology

4. Conclusions

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Introduction Plasma Spectrochemical Analysis

• Chemical analysis of a mixture of

substances or a complex of substance

by a study of spectra (plasma based

atomic spectroscopy)

• Ions (atomic) generated can be

extracted and quantified using a

suitable mass spectrometer (plasma

based mass spectrometry)

• With properly prepared reference

standards, allows for accurate

quantitation from ultratrace to % levels

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Ref: http://www.merriam-webster.com/dictionary/spectrochemical%20analysis, viewed 21 May 2012.

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Agilent Atomic Spectroscopy Portfolio

(from Jan 2012 onwards…)

4

AAS

7700 Series

ICP-MS

Instrument Price

P

erf

orm

an

ce

700 Series

ICP-OES

4100 MP-AES

Agilent 8800

ICP-QQQ

• Academic

• Difficult samples in

Semicon.

Life Science

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Breathrough #1

Running on Air – Myth or Reality?

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Ground State Excited State Relaxation

Sample

Microwave excited Plasma

Monochromator

& Detector

Quantitation

Atom Formation

EXCITATION

Emission

Microwave Plasma-Based Spectrochemical Analysis Fundamentals

Analysis is based upon Well-Proven Atomic

Emission Spectroscochemical Principles!

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Agilent 4100 Microwave Plasma-Atomic Emission

Spectrometer (MP-AES)

New technique for elemental determination using atomic emission

• Microwave excited plasma source

• Nitrogen based plasma - runs on air (using a N2 generator)

Improved performance compared with flame AA:

• Higher sample throughput with fast sequential measurement

– More than 2x faster than conventional flame AA

• Superior detection limits and improved dynamic range

Easy to use: • New generation software featuring automated

optimization and software applets that load a preset method

• One piece torch with easy torch removal and replacement – no alignment

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Agilent 4100 Microwave Plasma-Atomic Emission

Spectrometer (MP-AES)

Reduced operating costs: • Runs on air – eliminates need for

Acetylene, Argon, etc.

• Eliminates need for source/hollow

cathode lamps

• Simple installation – no chiller, 10 A

supply

Improved Safety: • Eliminates need for flammable gases and

cylinder handling

• Safe, reliable unattended multi-element

overnight operation

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Accessory Options for the 4100 MP-AES

• Automate and simplify analysis with the SPS-3 Autosampler (for unattended overnight operation)

Page 9

• To enable low ppb level detection of As, Se or

Hg, use the Multimode Sample Introduction

System (MSIS). Can be used to analyse hydride

and non-hydride forming elements at the same

run!

• For organic applications, the External Gas

Control Module (EGCM) bleeds air into the

plasma minimizing Carbon build-up and reducing

background

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Page 10

IDL’s in ppb, clean water samples

**3 sigma IDLs using a 10 second integration time with dewar nitrogen

*30 second integration time used for these elements

Performance Comparison Typical Instrument Detection Limits**

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Application Notes Available

(downloadable from the Agilent website)

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Geochemical

• New methodology for analysis of gold and precious metals

• Analysis of base metals in geochemical samples

Chemical & Petrochemical

• Analysis of wear metals and contaminants in engine oils

• Analysis of lubricating oil additives

• Analysis of trace elements in petroleum and diesel fuels

Food & Agriculture

• Analysis of soil extracts

• Cost-effective analysis of major, minor, and trace elements in foodstuffs

Environmental

• Determination of metals in industrial wastewaters

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Cost savings based on reductions in gas expenses ONLY!.

Assumes measuring 9 elements (4 nitrous-oxide elements) in batches of 100 samples,

3 days/week using the N2 generator. For a detailed cost comparison, consult your local Agilent representative

Reduced Cost of Ownership

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The Agilent 4100 MP-AES

Key Features

o Runs on air – the most significant advance in Atomic Spectroscopy

o Lowest running cost of any atomic spectroscopy technique due to capability to run on air – ideal for remote and at site operation

o Improved safety – capability to run on air means no flammable gases and no manual handling of cylinders

o Easy-to-use software with MP applets and plug and play torch which simplify operation and maximize uptime

o Superior performance to flame AA, with capability to run unattended overnight

o An even greener technology, displacement of fuel gas (acetylene) reduces carbon footprint, aids CSR initiatives of many organisations (People, Planet, Profit)

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Breathrough #2

World’s First Functional ICP-QQQ featuring

Tandem MS/MS Technology

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Agilent 8800 ICP-QQQ

Agilent 7700

Single-Quad ICP-MS

Agilent 8800

ICP-QQQ

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World’s first Triple Quadrupole ICP-MS (ICP-QQQ)

New modes of operation and performance not possible with quadrupole ICP-MS

The highest performing quadrupole ICP-MS system

Unique capabilities, based on proven technology of world’s best selling ICP-MS

(7700)

8800 ICP-QQQ Key Product Hardware

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Low flow

sample

introduction

system

High matrix

introduction

(HMI)

technology

Fast, frequency-

matching 27MHz

RF generator Efficient twin-turbo

vacuum system

Dual conical Extraction and

Omega lens focuses ions

across the mass range

9 orders

dynamic range

electron

multiplier (EM)

detector

Analyzer quad Q2:

High frequency

hyperbolic quadrupole

– selects ions that

pass to detector

High-transmission,

matrix tolerant interface

First quad Q1: High frequency

hyperbolic quadrupole mass filter –

selects ions that enter the cell

3rd generation collision/

reaction cell (ORS3)

with 4 cell gas lines

Peltier-

cooled

spray

chamber

Robust, high-temperature

plasma ion source

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ICP-QQQ: How Does it Work?

ICP (plasma) and Interface:

Forms and extracts ions from

the sample (just like the 7700)

EM (detector): Measures the

ions that are scanned by Q2

(just like the 7700)

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Q1 – controls ions

that enter the cell

• Consistent reactions

even if sample

composition changes.

ORS3 – collision/

reaction gas added

• Ions react and are

neutralized or moved.

• Product ions are formed.

Q2 – selects the

target analyte mass

• Interference-free analyte

ions passed to EM

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Q1 – controls ions

that enter the cell

• Consistent reactions

even if sample

composition changes

ORS3 – collision/

reaction gas added

• Ions react and are

neutralized or moved

• Product ions are formed

Q2 – selects the

target analyte mass

• Interference-free analyte

ions passed to EM

ICP-QQQ: How Does it Work?

ICP (plasma) and Interface:

Forms and extracts ions from

the sample (just like the 7700)

EM (detector): Measures the

ions that are scanned by Q2

(just like the 7700)

Unique aspect of ICP-QQQ is Q1.

• Controls the ions that enter the cell

Reaction processes in the cell are

consistent and predictable, even if

sample composition is complex or

variable.

• Consistent cell conditions means

reaction mode method development

is easier than on single quad (same

method can be used for different

samples).

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Scan Type on ICP-QQQ

• Single Quad mode

• MS/MS mode

– On-Mass mode

– Mass-Shift mode

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Q2 cell Q1

Cell gas

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ICP-QQQ can function in Single-Quad Mode.

Q1 operates like an ion guide (just like single quad ICP-MS).

ICP-QQQ has typically 2x higher sensitivity and >5x lower background

than 7700, so DLs are better even in single-quad mode.

Single Quad Mode

Q2 (scanned) cell Q1 (ion guide)

Cell gas

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Parameters 7700x ICP-MS 8800 ICP-QQQ #100

Low mass (7Li) > 50 Mcps/ppm > 100 Mcps/ppm

Mid mass (89Y) > 160 Mcps/ppm > 350 Mcps/ppm

High mass (205Tl) > 80 Mcps/ppm > 200 Mcps/ppm

No Gas Background < 2 cps (m = 9) < 0.3 cps (m = 9)

Mass-Shift Measurement: Reactive analyte reacts with chosen cell

gas, is moved to a new product ion mass and can be separated from

unreactive interferences. No existing ions can overlap new analyte

product ion, as all non-target masses are rejected by Q1

With ICP-MS/MS, Q1 rejects all non-target masses, ensuring no existing

ions (analyte, matrix, or polyatomic) can overlap new analyte product ion

How Reaction Mode Works in ICP-MS/MS Mode

Original

interfering ion

On-mass

interference

Analyte

Off-mass

interference

Reaction

gas

Analyte

M+ MR+

Q2 set to analyte product

ion mass – rejects original

interfering ions

Analyte

product ion

Analyte reacts to

form product ion Q1 set to analyte

mass – rejects all

non-target masses

All non-target

masses

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• Q1 is set to precursor ion mass, controlling the ions that enter ORS.

• Q2 is set to mass of reaction product ion (Q1+16amu in O2 mode):

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Example: S with O2 Cell Gas

Q2 (Q1+16)

(scanned) cell Q1 (m/z= 32)

(scanned)

O2

32S+

48Ca+, 48Ti+

36Ar12C +

48SO+ 32S+ 48SO+

48Ca+, 48Ti+

36Ar12C +

Single-quad reaction cell ICP-MS can also do SO mass-

shift to move S (as SO+) away from the O2+ interference.

BUT single quad reaction cell ICP-MS cannot remove

the 48Ca/48Ti and 36Ar12C overlaps on 48SO+.

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Other Benefits of Tandem MS/MS - Greatly Improved Abundance Sensitivity

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8800 Abundance Sensitivity in Single-Quad Mode

- Trace 55Mn is overlapped by 56Fe in 1000ppm Fe

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Abundance Sensitivity (AS) is

the degree of peak “tailing” – the

contribution a peak makes to the

adjacent (-1 and +1amu) masses

7700 specification is 5 x 10-7 on the

low mass side

Note: log intensity scale 55Mn

56Fe

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QQQ Abundance Sensitivity is

the product of Q1 AS x Q2 AS,

so overlaps to adjacent peaks

are virtually eliminated.

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8800 Abundance Sensitivity in MS/MS Mode - 55Mn is free from overlap by 56Fe in 1000ppm Fe

55Mn

56Fe

8800 QQQ AS is almost too

good to measure (<10-10).

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Agilent 8800 ICP-QQQ – Key Features

• World’s first functional ICP-QQQ with Tandem MS/MS capability

• Outperforms single quadrupole ICP-MS for conventional applications

• Provides unique, high-performance MS/MS mode

• ICP-QQQ ensures control of ions that enter the cell; controlled reaction

processes deliver reliable results

• Offers ultimate flexibility for problem solving and advanced research

• Utilizes proven 7700 hardware and same MassHunter software platform

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Factory in Tokyo

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