USER TRAINING

OPERATION AND MAINTENANCE

Agilent 240FS-240Z DUO

Atomic Absorption Spectrometer

Manila Water Co., Inc.

August 30-31, 2017

AISAH D. PEÑARUBIA
Application Chemist

Agilent AA 55B
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Objectives

Identify the use and advantages

Understand the functions of the hardware and software
Recognize the applications and evidences of the good
performance
Operate and maintain the system with ease and confidence

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Agenda

Schedule Activities

August 30-31, 2017 Presentation and Discussion

- Company Overview, Goals and Expectation in the Training
- Overview, Principles, Functions and Benefits of Agilent 240FS AA
- Methods and Applications
Hands-On Training
- Operation of SpectrAA software
- Maintenance of the hardware of Agilent 240FS AA and 240Z
- Optimization of Lamp, Burner and Nebulizer Flow (Flame 240FS)
- Alignment of Graphite Tube and Sample Probe (Graphite 240Z)
- Method Development and Analysis of standard calibration
- Analysis using Actual sample
- Evaluation of Results
- Preparation of Report

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Company Overview
Molave Trading Inc.
Established in 1973.
ISO 9001:2008 certified since year 2011
One of the leading suppliers of scientific and analytical instruments in the country
Dedicated and highly trained application specialists and technical service
engineers
Continues to bring quality products from the best known manufacturers around the
world

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Spectroscopy Products

2010

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The Atomic Absorption History and Principle

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Atomic absorption remained an interesting phenomenon
in physics until 1952 when Dr. Alan Walsh, an Australia
physicist, considered the father of atomic absorption,
started his work on the development of the first atomic
absorption instrument.

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1955, Walsh demonstrated successfully the AA-1 now on
display in Australia

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Walsh’s first atomic absorption eventually lead to commercial
production of the AA-2 in 1962 by Techtron, an Australian manufacturer,
that merged with Varian in 1967

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History - Agilent AA Development Timeline
1952-53 Sir Alan Walsh Develop & Patent AAS & CSIRO

1962 Techtron First commercially available AAS under

license from CSIRO
1966 John Willis Nitrous Oxide/Acetylene flame AAS
& Phil Thomas
1967 Varian-Techtron Varian Associates acquires Techtron
1971 Varian-Techtron Zeeman Patents, GFAAS developed
1987 Varian-Techtron Zeeman furnace introduced
1991-92 Varian-OSI ISO-9001 certified factory
1997 Varian – OSI Fast Sequential AA patents
1999 Varian, Inc. Varian Associates splits into 3 cos.
Varian – OSI part of Varian, Inc.
2010 Agilent Technologies Final Acquisition of Varian, Inc.

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Characteristics of AAS as an Analytical Technique

• Analyze concentration of metals in solution (67

elements)
• PPB to % levels
• Typically better than 1% RSD
• Sample preparation is simple
• instrument is easy to tune and operate

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Basic Principles of AA
• All atoms can absorb light
• Wavelength of light absorbed is specific for
each element
• Amount of light absorbed at analyte
wavelength
• Amount of light absorbed by sample can be
compared to amount of light absorbed by
standards.

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Atomic absorption is the process that occurs when a
ground state atom absorbs light of a specific wavelength
and is elevated to a higher energy level (i.e. the process
of moving electrons from the ground state to an excited
state.

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Diagram

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Schematic of Typical AA Flame System

Light-sensitive detector
Electronic readout system
Resonance Line
0.723
Hollow cathode
lamp ( light source)

Atomizer Monochromator
(flame, furnace
or hydride)
Resonance Solution
Non-resonance (blank, standards
Fill Gas or sample)

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Atomic Absorption: Technology
Principal:
Samples are volatized by heat. Elements in a sample are measured by
light absorption. Each atom has a unique light absorption signature.

Ground State Excited State

Lamp
Monochromator Quantitation
 Hollow Cathode
Lamp (HCL) &Detector
 Electrode-Less
Discharge Lamp
(EDL) Sample is heated to produce atoms
Atoms are excited by light
Or Different lamp for each element
(some multi-element lamps)
Flame Graphite Furnace
Energy absorbed by atom excitation is
measured
Sample Quantitation is done by standard curve

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Elemental Coverage with AAS

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Flame Type and Measurement Technique

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Light Source

A light source is used to generate light at the wavelength

which is characteristic of the analyte element. This is most
often a hollow cathode lamp, which is an intense narrow
line source.
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Atomization

Atomization is the process by

which atoms are made available for
absorbance measurement.

Consists of Burner, Spraychamber and

Nebulizer.

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Three Major Classification of Atomizers

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Agilent AA 55B
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Burner

• Constructed from Incoloy

alloy with Teflon base
corrosion resistance
• Choice of air-acetylene or
N2O-acetylene burner
• Manual adjustment of
burner height and burner
rotation

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Nebulizer

• Externally adjustable glass

impact bead (tuneable
performance for optimum
sensitivity and best precision)
• With adjustable flow, inert
platinum/iridium capillary and
PEEK venturi for corrosion
resistance
• Integral liquid trap with magnetic
float liquid level interlock

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The aerosol exiting the nebulizer, strikes the impact bead at extremely high
speed. During this impact some of the larger droplets are shattered and
others cling to the bead and are removed from the system.
This shattering of some of the large droplets accomplishes two important
functions..
.
1. The number of small droplets in the aerosol increases increasing the
sensitivity of the measurement.

2. The size distribution of the droplets in the aerosol is made more

uniform by about an order of magnitude. This makes the flame quieter,
reducing the noise of the measurement, allowing lower detection
limits.

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Spraychamber
• Fluorinated HDPE
(compatible with acidic and
organic solutions)
• Twist and lock assembly
• With pressure relief bung at
the rear and twin-headed
mixing paddle
• Integral liquid trap with
magnetic float liquid level
interlock

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Agilent’s Mark 7 Flame Atomization System
Design is proprietary to Agilent/Varian
Incoloy Burner instruments
Burner Rotation Handle
Spray
Chamber

Nebulizer Impact
Bead
Capillary

Mixer
Paddles
Spray
Chamber
Bung

Float

Drain Trap

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Satisfying Flame Analysis Challenges
Mark 7 atomization system benefits:
•Easy to use
• “Twist and Lock” assembly
• Externally adjustable impact bead
•“Tunable” performance
• Achieve high sensitivity — typically
> 0.9 Abs. from 5 mg/L Cu
• Optimize precision — typically < 0.5%
RSD from ten 5 second integrations
•Reduce interferences with complex
samples:
• Twin headed mixing paddles ensure
thorough mixing and produce a fine
aerosol
•Reduced memory - efficient drainage
•Extended operation with difficult samples
• Contoured burner cross section provides
outstanding resistance to blockage
•Increased durability - corrosion-resistant
components

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Optical System

An optical system to direct light from the source

through the atom population and into the
monochromator
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Monochromator

A monochromator is used to isolate the specific analytical

wavelength of light emitted by the hollow cathode lamp
from the non-analytical lines including those of the fill gas

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Detector

A light-sensitive detector (usually a photomultiplier

tube) to measure the light accurately and convert
the light energy into electrical energy
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Portfolio Overview - AAS
Entry level - 55 AA Series
• Stand alone system
• Keyboard control with LCD screen
• Optional PC control

Mid range – 240 AA Series

• External PC control
• Automatic lamps
• Optional “Fast Sequential” capability (4 lamps)

Top end – 280 AA Series

• External PC control
• Premium positioning
• Highest performance
• Greatest automation
• “Fast Sequential” capability std (8 lamps)

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High End 240 FS Series AA – Key Features
• Fully automated AA with PC control
• 4 lamp capacity with automatic lamp
selection
• Fast Sequential capability is standard
• Built-in D2 background corrector
• High performance Mk 7 atomization
system
• Better optics specification
- Supports 4 lamps in FS operation
- Support for 4 UltrAA lamps with 2
positions loomed as standard
- Larger 330 mm focal length
monochromator (1800 l/mm grating with
0.1 nm resolution)
• Option to add the GTA120 graphite furnace
• Positioned at premium end of market
• Offers highest performance/productivity
available

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 Conventional AA Operation
• Measures 1 element at a time

• Multi-element capability by
measuring elements sequentially
1 at a time

• Samples aspirated time and time

again during multi-element
determination
- Increases delays
- Increases analysis time
- Consumes more sample

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Fast Sequential AA Operation
• Measures ALL elements in rapid sequence

• Samples aspirated once

• Improves productivity by up to 50%

• Reduces sample delays

• Conserves valuable sample volume

• Saves labor and reduces running costs

Only Agilent has FS Operation

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How Fast Sequential AA Works?

1. All lamps operated simultaneously

2. Fast lamp selection using motor driven

mirror

3. Instantaneous changes to gas flows

4. High speed wavelength drive

5. Software Wizard optimizes measurement

time

Agilent AA 280 FS

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Fast Sequential Operation
Conventional AA spectrometers
• Analyze all samples for one element
• Then repeat all samples again for subsequent elements
• Increases sample consumption and analysis time

Fast Sequential AA
• Analyze each sample one at a time for several elements
• To change from one element to another
–All lamps operated simultaneously
–Fast rotating mirror to switch lamps
–Change wavelengths at fast slew speed of 2,000 nm/min
–Rapidly change gas flows to the programmed flows

Provides dramatic reduction in sample analysis time from reduced

sample delay
Agilent AA 280 FS

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Fast Sequential Lamp Selection
High Speed
High
High
HighSpeed
Speed
Speed
Monochromator
Monochromator
Monochromator
Monochromator

HC Lamps
D2 HC
HC
HCLamps
Lamps
Lamps
D2
D2
D2
Lamp
Reference Beam Lamp
Lamp
Lamp
Reference
Reference
ReferenceBeam
Beam
Beam

Burner
Burner
Burner
Burner
Motorised
Motorised
Motorised
Motorised
Mirror
Mirror
Mirror
Mirror

Agilent AA 280 FS

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Portfolio Overview – AA Accessories
SPS 4 for SIPS 10/20
automated for on-line
sample dilution &
presentation Calib. from
with flame AA 1 Std with
flame AA

High intensity UltrAA

lamps for lower GTA 120 for graphite VGA 77 for hydride
detection limits furnace determinations determinations of As, Se &
(with GFAAS) (ppb levels) Hg (ppb levels)

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Agilent GFAA for Superior Furnace Performance
Agilent GFAA systems provide:
•Superior furnace performance
• 25 mm length tube for high sensitivity
• Separate internal and external gas flows with
2 stage flows for extended tube life
• Optional high intensity UltrAA lamp support
(plug & play using integrated supply)

•Accurate background correction

• Can handle high background
• < 2 % error at 2 Abs.

•Ease of use features

• Furnace viewing camera
• Automated furnace optimization wizard

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Furnace Thermal Stages

Clean
Out
Atomize

Ash Cool
Down T
E
M
Dry P

T I M E

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GTA120 Constant Temperature Zone Design

• Power supply matched to low

thermal mass tubes

• Ensures rapid, controlled and

even heating

• Creates a Constant
Temperature Zone around the
injection hole

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Benefits of the Constant Temperature Zone Design
• Extremely fast atomization,
even with difficult sample
matrices
• Best signal-to-noise
characteristics
• Best detection limits
• Reduced memory effects
• Accurate temperature
0.50 5.0

0.45 4.5

control without inaccurate 0.40 4.0

optical sensors 0.35 3.5

Replicate Precision (% RSD)

• Greater reproducibility
0.30 3.0
Absorbance

0.25 2.5

• Extended tube lifetime and 0.20 2.0

lower inert gas consumption 0.15 1.5

0.10 1.0

0.05 0.5

0.00 0.0
0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000
No. of Tube Firings

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Sophisticated PSD120 Furnace Autosampler
• Provides extended capacity for up to 135
solutions

• Automates calibration using 1 standard

• Prepares standard additions spikes

• Performs automatic over range volume

reduction

• Provides flexible dispensing options, such

as:
- Hot Inject
- Multiple inject

• Reduces analytical cycle times

- Solutions collected while furnace operates

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GTA120 Furnace Viewing Camera

Option for the GTA120 which

allows:
• Real time viewing of the
injection zone
• Capture still images or video
analysis
• Simplify method development
- Optimize dispensing height
- Confirm furnace conditions
e.g. optimum drying conditions
- Monitor analysis

Capture a still picture to

include with the results

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Furnace Viewing Camera Option

Record a movie while checking drying conditions – good!

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Automated Furnace Method Optimization

• SRM “Wizard” automates furnace

optimization

• Optimizes absorbance as a function of

ashing and atomization temperature

• Automatically creates a method using

recommended conditions

• Reduces training requirements for new

users

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World’s Best Zeeman GFAA
Agilent’s Zeeman AA systems
provide:

• Outstanding performance at
ppb levels from the CTZ
furnace design

• Easy alignment – only a

single light source is required

• Most accurate correction

using Agilent’s Zeeman
correction
• Polynomial interpolation of
the background signal
• Zeeman magnet modulated
at twice the mains frequency

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Advantages of Agilent Zeeman GFAA
Less than 2 % error with > 2 Abs.
Good For difficult samples Background from NaCl
• High background
2.14 ABS
• Unknown interferences

Good when spectral interferences

occur
• Se in the presence of high Fe
2% Error
• As in the presence of high Al or
phosphate

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Agilent’s Duo Systems Double AA Productivity
• Simultaneous flame and GFAA operation
improves productivity
• Customize the system to your needs
• Centralize method and data storage
• Save time – eliminate change-over and
alignment
• Simplify set-up – each atomizer is
permanently aligned
• Ideal for busy environmental, chemical or
industrial laboratories

Page 50
Background Absorption & Correction
Background absorption can be caused by:
• Molecular absorption in the gas phase
• Light scattering or absorption by particles in the light path
• Absorption of light by the flame

Why Correction ?
* Radiation from hollow cathode lamp is attenuated by NON-ATOMIC source
• Molecular species
• Solid particles
• Flame absorption
• Signal is added to the atomic signal
• Results in falsely high signal

Types of BG correctors:
• Deuterium
• Zeeman

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Why Graphite Furnace Atomization?

Entire sample is atomized at

one time

100 mg/L Pb @ 217.0 nm

Free atoms remain in the
optical path longer 0.936
Furnace Signal
for 10 mL
Absorbance
Enhanced sensitivity Flame Signal

0.004
Reduced sample volume

Page 27
 Detection Limit Comparison (mg/L)

Element Flame Furnace

Ag 1.7 0.020
Al 20.0 0.10
As 42.0 0.22
Cd 1.5 0.010
Cr 5.0 0.04
Ni 5.8 0.40
Pb 14.0 0.20
Tl 15.0 0.25

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Cross Section Views of Furnace Workhead
Water Cooling Gas Out Sealed
Quartz
Window
Optical
Path

Gas Inlet Flexible Seal

Internal Gas Internal Gas

flow flow

External Gas flow

Page 54
Flow Chart
Sample Preparation Standard Preparation
(Direct, Extraction or Acid (Dilution of Calibration
Digestion) Standard)

Method Development System Check

(Element, Wavelength, Flame (Gases, Power Supply, Waste,
Type and Other Parameters) Exhaust)

AA Analysis Evaluation of Results

(Calibration Curve Creation and (Acceptable or Subject to Re-
Analysis of Samples) analysis)

Preparation of Report
“For every minute spent organizing,
an hour is earned”
- Benjamin Franklin

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Summary - Agilent Atomic Absorption
The world’s fastest flame AA; the world’s most sensitive AA

•Superior flame, graphite

furnace, and vapor generation—
or a combination of
techniques—let you exactly
match your analytical needs

•Easy-to-use software and

rugged, reliable hardware
simplify operation and maximize
uptime

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Agilent AA 55B
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