Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-OES)

Craig Seeley, Elemental Product Specialist

The world leader in serving science

Core Technologies

Optical EMT torch &

design Duo viewing

Clip-in
sample intro
systems

Drain sensor
CID detector
d

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CID versus CCD

Benefits of Charge Injection Device (CID) over Charge Coupled

Device (CCD)
• High sensitivity
• TRUE random access integration
• Extended dynamic range in a single exposure
• Non destructive read allows optimum signal / noise for each pixel
• Full frame capability
• No Pixel Blooming
• Full Wavelength Coverage from 166.25 – 847.00nm
• Reduced dependence on IEC corrections via alternate lines
• Reduced validation tests
• Fullframe analysis capability

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Available Plasma View Configurations

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Sample Introduction Kits for iCAP 7000 Series ICP-OES

• Liquid
Li id hhandling
dli kit
kits ffor D
Duo & R
Radial
di l ICP
ICP-OES
OES
• Aqueous Kits
• Organics Kits
• Volatile
V l til OOrganics
i Kit
Kits
• High Solids Kits
• HF Resistant Kits
• All kits
kit iinclude
l d EMT ttorches
h
• User selectable injectors tubes
• 1.0, 1.5, 2.0 mm quartz tube
• 2.0
2 0 mm ceramic
i ttubes
b
• Pump tubing is not included

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Ceramic D-Torch Accessories – Key Features

• Fully demountable design for cost effective replacement of

parts

• Identical geometry to EMT (parallel tube design for optimized

gas flows and sample
g p channel stability)
y)

• Interchangeable with EMT design in any iCAP 7000 Series ICP

• Silicon nitride (Sialon) ceramic outer tube – highly durable
material

• Alumina intermediate (auxiliary) tube – excellent chemical and

temperature resistance

• Compatible with EMT centre tubes to enable maximum

application flexibility

Ceramic Torch EMT Torch

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Element Finder – Automated Method Development

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Fullframe Capabilities on iCAP7000

• A Fullframe is a graphical depiction of the CID chip. All wavelengths are displayed and can be
identified and semi quantitatively analyzed.
• The bright spots are elements in your sample….the brighter the spot, the higher the
concentration!
• Semiquant determinations can be done at any time

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Typical Method Development Process for ICP-OES – Wavelength Selection

St 1 – Determine
Step D t i which
hi h elements
l t you need
d tto analyze
l

Step 2 – Set wavelengths for analysis

Step
p 3 – Perform initial analysis
y

Step 4 – Review data for interferences

Step 5 – Repeat steps 2-5 as needed

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Application Example – Determination of B in a High Fe Matrix

• Example – asymmetric peak for boron at 249.773 nm

• Clear interference on boron peak (visible at 249.780 nm and 249.790 nm)

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Manual Identification

• First – identify the interference

• Over 55,000 wavelengths in the library
• A number of possible elements could cause this interference
• Aluminum, iron, germanium

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Manual Identification – Confirmation

• Analyze three solutions:

1. The sample
2. A single element solution of the analyte at the concentration in the sample
3. A single element solution of the suspected interference at the concentration in the sample
• If this is not the interfering analyte,
analyte further analysis might be needed to determine this

• Suggested workflow for the

proposed USP chapters on
elemental impurities

• Select an alternative wavelength

that is interference free

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Automated Method Development and Plasma Optimization!

• Element Finder plug-in for Thermo Scientific™ Qtegra™ Intelligent Scientific Data Solution™ (ISDS) Software
• Simplifies method development
• Automatically selects appropriate wavelengths and eliminates interferences before you know they exist
• Automatically sets plasma conditions to optimize the instrument’s performance

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Interference-Free Wavelength Selection – Overview
Number of wavelengths
• User selects the elements of interest

• Each element displays the number of wavelengths that will be used for analysis

• As more elements are added, the list of suggested wavelengths for each element
is refined and reduced

• Wavelength selection is based on known interferences

• The same process happens when matrix elements are selected and added to the
instrument method

• No wavelength selection by the user is taking place

The user only needs to select the elements of interest!

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Element Finder Workflow – Wavelength Selection in Unknown Samples

• Collect a full frame image using Element Finder

• All elements in the sample will be identified and marked as analyte or matrix elements

• Completes in less
than 5 minutes!

• Uses 8 mL of sample!

Elements Scanned

Elements Found

Additional Matrix Elements

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Element Finder Workflow – Processing Full Frame Images
• All user-defined and software-selected elements are displayed in the results
• Analyte
A l t elements
l t are marked
k d with
ith green llabels,
b l matrix
t i elements
l t are marked
k d with
ith bl
blue llabels
b l
• Elements found using Element Finder are selected as matrix elements by default (unless previously defined as analytes by the user)
• User can toggle all element selections between “Analyte” and “Matrix”
• The highest sensitivity interference fee wavelength is automatically selected for analysis

User defined Elements Found Elements

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Element Finder Workflow – Analysis of an Unknown Sample

No user defined Elements

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Element Finder Workflow – Analysis of an Unknown Sample

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Element Finder Workflow – Analysis of an Unknown Sample

• The wavelength that has the highest intensity and no spectral interferences will be selected for analysis
• Additional wavelengths can be selected

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Plasma Optimization

• Plasma conditions can be optimized automatically, following wavelength selection

• Different elements require different optimal conditions
• A range of elements require a set of comprised conditions

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Plasma Optimization

• Customer selects the wavelengths

g to optimize
p
• Can use the wavelengths selected by Element Finder
• Use a sub set of critical performance elements
• Select sample matrix: aqueous or organic
• Select
S l t the
th parametert you are optimizing
ti i i ffor: iintensity,
t it signal-to-background
i lt b k d ratio,
ti detection
d t ti limits
li it
• A set of optimized values will automatically be returned

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Plasma Optimization

• The optimization will take place based on a multi-component analysis

• Complete optimization process takes approximately ten minutes

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Intelligent Autodilution: ESI prepFast

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 prepFAST Inline Syringe Dilution System

• Integrated software control

• Autocalibration
– Autodilution of multi-element stock
standard
• Sample dilution
– Inline autodilution
• QC-Based Autodilution
– High Concentration Samples
– High Matrix sample
• Up to 200x
00 Dilution
ut o Factor
acto

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Modes of On-Line Dilution

Dilution Mode Initiation Action

Prescriptive Sample List Dilute by prescribed factor

Over-range QC Failure Insert new sample, auto dilute, rerun

IS Out-of-range QC Failure Insert new sample, auto dilute, rerun

Pre-emptive Pre-scan measures Qtegra calculates dilution factor to defined

concentration of defined maximum solids level and run
elements as too high

Standards Prep Sample List Automatically dilute multielement standard

solution to prepare calibration curve

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prepFAST iCAP Integrated Valve Module

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Prescriptive Sample Autodilution

Manual vs. Inline Sample

p Dilution

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Intelligent Autodilution

QC Intelligent Dilution

Internal Standard

Calibration Range
g

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Intelligent Autodilution

Intelligent Dilution

Qtegra inserts lines and dilution factors,

factors 40.499
40 499

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iCAP 7600 Sprint Valve

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Switching Valve – How Does it Work?

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Switching Valve – How Does it Work?

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 Why a Segmented Stream?

Uptake / Washout Profile with Contiguous Flow

R i d baseline
Raised b li

Long transients

Uptake / Washout Profile with Segmented Stream

Discrete washout steps

True baseline
Sharpp transients
S s s

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Increasing Through-put: Sprint Valve

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Ultra-Fast Agricultural Soil Analysis with Sprint Valve

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Case-Study – Wear Oil Analysis

T i l Oil Method
Typical M th d Switching
S it hi Valve
V l
(already speed-optimized) Oil Method
Anal sis Step
Analysis Step Time Req ired
Time Required
Analysis Step Time Required

1. Autosampler Movement 5 sec.

2. Sample Uptake 15 sec. 1. Autosampler  Movement, 

Sample Uptake, Stabilization,  17 sec.
3. Stabilization 20 sec. and Rinse

4 Measurement
4. M 10
10 sec.
2. Measurement 10 sec.
5. Rinse 30 sec.

Total Time
Total Time 80 sec
80 sec. Total Time
Total Time 27 sec.

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iCAP 7000 Series Application Examples

The world leader in serving science

ICP-OES Technology to Tackle Any Application

• Agricultural Screening
• Unattended, high throughput for trend analysis

• Use
U off hi
high
h speed
d switching
it hi valve
l ((added
dd d or iintegrated)
t t d) eliminates
li i t uptake,
t k wash
h and
d
minimizes carryover

• Robust sample introduction minimizes maintenance requirements and maximizes uptime

for high matrix sample analysis

• Samples can be screened for both nutritive and toxic elements

• AN43156: Ultra-Fast Agricultural Soil Analysis using the Thermo Scientific iCAP
7600
• AN40756: Environmental Series – Determination of Trace Elements in Soils and
Sediments

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ICP-OES Technology to Tackle Any Application

• Environmental Analysis
• Sensitive, accurate analysis to confidently report trace elements in a wide range of
environmental samples

• High efficiency RF generator and robust sample introduction for reliable analyses of high
solid samples such as sludges

• High sensitivity for quantification of ppb-level contaminants in water samples

• Data collection and reporting in full compliance with applicable state and federal
regulations

• AN43152: U.S. EPA SW-846 Method 6010c using the Thermo Scientific iCAP
7400
• AN43157: U.S.
U S EPA Method 200
200.7
7 using the Thermo Scientific iCAP 7600

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Environmental Applications

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ICP-OES Technology to Tackle Any Application

• Food Safety
• Monitor trace elements during food production to ensure consumer safety

• Quantify key elements for accurate product labeling

• Large dynamic working range and robust sample introduction to quantify a wide range of
concentrations in many sample types

• Data collection and reporting in full compliance with applicable FDA, WHO, FAO
regulations

• AN43151: Analysis of Elemental Contaminants in Beverages using the Thermo

Scientific iCAP 7200
• AN40858: Food Series – Ensuring Regulatory Compliance of Foodstuffs

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Food Safety Applications

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ICP-OES Technology to Tackle Any Application

• Pharmaceuticals/Neutraceuticals
Ph ti l /N t ti l
• Qualified instrumentation and IQ/OQ services to ensure compliance with new and future
legislation

• User-selectable method templates for minimized method development and maximum

ease-of-use

• High
Hi h sensitivity
iti it and
d matrix
t i ttolerance
l ffor quantifying
tif i elemental
l t l iimpurities
iti iin d
drug products
d t
at ppb-level concentrations

• Data collection with full traceability in agreement with 21 CFR Part 11 requirements

• AN43149: Analysis of Elemental Impurities in Drug Products using the Thermo

Scientific iCAP 7600
• AN43086: Analysis of Elemental Impurities in Liquid Pharmaceutical Products

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Key Requirements for Pharmaceutical Analysis (USP Chapters 232 & 233)

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Pharmaceutical Applications

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ICP-OES Technology to Tackle Any Application

• Chemicals
Ch i l
• Perform QA/QC analysis in samples such as brines, caustic solutions, plating baths, and
consumer products

• Superior stability and maximum uptime with sample introduction setups dedicated for
different sample types

• Minimal
Mi i l matrix
ti ddeposition
iti and
d itits affiliated
ffili t d signal
i lddrift,
ift even with
ith th
the mostt challenging
h ll i
sample matrices

• Flexible wavelength and background selection for data collection with optimal sensitivity
and reduced spectral interference effects
• AN40986: Trace Contaminant Analysis in Brines
• AN43150: Analysis of Plating Baths
• AN43178: Analysis of Elemental Impurities in Electronic Grade Copper Sulfate

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ICP-OES Technology to Tackle Any Application

• Petrochemicals
• Monitor trends and quantify elemental contaminants in a high-throughput laboratory
environment

• High efficiency RF generator allows samples from crude oil to gasoline to be analyzed
with minimal sample preparation

• Use of a switching valve further enhances sample throughput by reducing carryover, while
minimizing uptake and wash

• Minimal
Mi i l ddrift
ift nearly
l eliminates
li i t QC ffailures
il and
d sample
l re-runs

• AN43161: Sprint Analysis of Lubricating Oils using the Thermo Scientific iCAP
7600
• AN40787: Analysis of Wear Metals

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Petrochemical Applications

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iCAP 7000 Instrument Configuration

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Volatile Organics

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ICP-OES Technology to Tackle Any Application

• Metals
M t l and
d Materials
M t i l
• High resolution provides consistent and accurate analyses in complex matrices

• Superior reliability and minimal drift virtually eliminates the need to re-run
re run expensive
samples

• Intelligent uptake, wash and dilution reduces carryover between samples

• Ergonomic design and low gas consumption requirements significantly reduces

operating costs

• AN43084: Analysis of Precious Metals

• AN43146: Determination of Trace Elements in Steels and Alloys

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ICP-OES Technology to Tackle Any Application

• Mining
• Robust instrument design allows for data collection in rugged laboratory environments

• Minimal user maintenance for maximum uptime

p and sample
p throughput
g p

• Simple method templates and simple intelligent workflows for rapid setup and data
collection

• Intuitive hardware and software operation for accurate and consistent data collection by
analysts with all levels of experience

• AN40759: Analysis of Geological Samples

• AN43184: Determination of Elemental Components of Fracking Flowback
Solutions from Marcellus Shale

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Mining and Metallurgical Applications

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Chemicals in Fracking solutions

• Hundreds of chemicals in fracking

g solutions
• 50,000 mg/L salt (10-20x seawater)
• The EPA has narrowed the list of compounds down to less than 20.
• The EPA is in the process of developing analytical methods for these target compounds.

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Thank You For Your Attention

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