A Thermo Electron Corporation új XSeries
1 / 60

- PowerPoint PPT Presentation

  • Uploaded on

A Thermo Electron Corporation új XSeries II ICP-MS készülékének és környezetvédelmi alkalmazásainak bemutatása. Száraz Sándor Unicam Magyarország Kft. 1144 Budapest, Kőszeg u. 29. unicam@unicam.hu. XSeries II ICP-MS. Brief introduction to ICP-MS. Characteristics of ICP-MS.

I am the owner, or an agent authorized to act on behalf of the owner, of the copyrighted work described.
Download Presentation

PowerPoint Slideshow about '' - ekram

An Image/Link below is provided (as is) to download presentation

Download Policy: Content on the Website is provided to you AS IS for your information and personal use and may not be sold / licensed / shared on other websites without getting consent from its author.While downloading, if for some reason you are not able to download a presentation, the publisher may have deleted the file from their server.

- - - - - - - - - - - - - - - - - - - - - - - - - - E N D - - - - - - - - - - - - - - - - - - - - - - - - - -
Presentation Transcript
Sz raz s ndor unicam magyarorsz g kft 1144 budapest k szeg u 29 unicam unicam hu

A Thermo Electron Corporation új XSeriesII ICP-MS készülékének és környezetvédelmi alkalmazásainak bemutatása

Száraz Sándor

Unicam Magyarország Kft.

1144 Budapest, Kőszeg u. 29.


Xseries ii icp ms


Brief introduction to ICP-MS

Characteristics of icp ms
Characteristics of ICP-MS

  • Wide element coverage

  • Low limits of detection

  • Elemental and isotopic information

  • Wide dynamic range

  • Wide variety of samples

Icp ms process


Ion Analysis Separation by m/z ratio


Ion Focusing / Optional Collision Cell


M+ Species Generated in the Plasma


Ion Detection by electron multiplier







Ar Plasma



ICP-MS Process

  • 4 Basic Stages

    1. Sample Introduction and Ion Generation

    2. Ion Focusing

3. Separation of Analyte Ions in Quadrupole Mass Filter

4. Ion Detection

Icp ms sample introduction
ICP-MS - Sample Introduction

  • Samples are normally analyzed as solutions

  • Sample is introduced into an argon plasma as a fine aerosol, via a peristaltic pump, nebulizer and spray chamber

  • Within the plasma (< 6000K) the solvent is evaporated and the sample species are decomposed into their constituent atoms and ionised

    - Ionisation process is extremely efficient in the plasma, and contributes to the high sensitivity of ICP-MS

As the solution passes through

the Ar plasma, 4 main processes

will occur

Icp ms sample introduction1
ICP-MS - Sample Introduction

  • Normally via concentric nebulizer ~1ml/min uptake

  • Typical sample volume - 20 elements using 3 x 2 secs. integrations - 4 - 5ml sample required

  • Optional low flow nebulizer for μl. sample analysis

  • Optional laser ablation for direct solids analysis

Icp ms sample introduction2






ICP-MS - Sample Introduction

  • Maximize M+

    • - Minimize MO+

    • - Minimize M++

  • Sample Uptake

    - Nebulizer dependent

  • Plasma Gases

    - Cool

    • Auxiliary

    • Nebulizer dependent

  • Torch Position

    - x, y, z control

Ion sampling and focusing
Ion Sampling and Focusing

  • Ions formed in the plasma are extracted through a sample and skimmer cone arrangement

  • Ion Lenses focus & optimize ion transmission to quadrupoleanalyser

  • Sample treatment is important to minimize deposition on cones:-

    - Dissolve and dilute to ~ 0.2% w/v

    - up to ~ 5% nitric acid preferred

    - up to ~ 5% hydrochloric acid

    - ~ 1% hydrofluoric acid (using an Inert Sample Introduction Kit), phosphoric acid or sulfuric acid

Slide Valve

Skimmer Cone

Ion Lens

Sample Cone


Extraction Lens

Increasing vacuum

Ion focusing mechanism
Ion Focusing Mechanism

  • Optimizes ion transmission to quadrupole analyser

  • Conventional ion focusing devices

    - Complex lens configuration and often incorporate a photon stop

    - Backgrounds typically 10-20 cps

  • XSeriesII: New high efficiency ion guide

    - Simple design with reduced number of lenses

    - Incorporate an innovative chicane deflector and off-axis quadrupole

    - Backgrounds of <0.5 cps

    - Upgradeable to collision cell technology (CCT)

Ion analysis quadrupole ms
Ion Analysis – Quadrupole MS

  • Quadrupole consists of 4 rods mounted equidistant to each other around the circumference of a circle

  • Separates Ions according to their mass to charge (m/z) ratio

  • Principles of operation

    - Alternating RF / DC potentials are applied to the quadrupole rod pairs

    - Ions move in a spiral motion down the quadrupole axis

    - Majority of masses are put into an unstable trajectory and are rejected

    - However under a given condition, ions of a specific m/z will pass through the analyser and reach the detector

Ion detection
Ion Detection

  • Ion detection is made with an electron multiplier

  • Measures the number of Ions arriving at the detector - proportional to the concentration of that isotope in the original solution

  • Detector operates in pulse counting (ion counting) and analogue (ion current) modes

  • With automatic cross calibration measures major, minor and trace analytes in a single acquisition



Data acquisition modes
Data Acquisition Modes

  • Scanning

    - Qualitative analysis and Quantitative analysis

    - SemiQuantitative analysis: Post run data retrieval on un-calibrated elements

  • Peak Jumping

    - Selected isotopes

    - Optimized dwell times

    - Improved detection limits

  • Time Resolved Analysis

    - Transient signal analysis

    - Applicable to laser ablation ICP-MS and chromatographic studies

Icp ms full mass spectrum
ICP-MS Full Mass Spectrum

  • Simple spectra (primary M+ ions)

    - Facilitates simple interpretation

  • Very high signal to background

    - Low detection limit capabilities

V ICP-MS Spectra - Vanadium 10mg/L

V ICP-AES Spectra - Vanadium 10mg/L

Calibration techniques
Calibration Techniques

  • Semi Quantitative

    - Analyte sensitivity can be determined from the instrument response built from the response to other known analytes.

    • Relative Sensitivity Factors (RSF) apply corrections for ionization and sample processing effects, these can be pre-determined for a given matrix to improve accuracy

  • Full Quantitative

    - Multi element external calibration standards

    - Standard additions calibration

    - Isotope ratio determination (for isotope dilution measurement)

Semi quantitative analysis
Semi-Quantitative Analysis

  • External standards not required for each analyte

  • Calibration via RSFs from Response Curve

  • Full elemental and isotopic information

  • Major to trace concentration determined

  • No prior knowledge of sample required

Semi Quantitative Calibration Plot

Fully quantitative analysis
Fully Quantitative Analysis

External Calibration

  • External calibration standards measured prior to unknown samples

  • Element or isotope responses are plotted against concentration

  • Concentration of unknown samples calculated from the calibration graph

Standard Additions

  • Known sample is spiked with known concentrations of analytes

  • Standard addition calibration plot provides accurate low level concentration data from the x-axis intercept

  • Eliminates need for matrix matched calibration standards

Time resolved analysis



AsC +








Time (min)

Time Resolved Analysis

  • Enables time resolved data to be acquired both qualitatively and quantitatively from transient signals

  • Wide applicability including Laser Ablation ICP-MS and chromatographic studies

Xseries ii icp ms1


Routine Environmental Applications

Environmental applications sample types
Environmental Applications – Sample types

  • Wide variety of environmental sample types

    • Drinking water

    • Ground water

    • Waste water / effluent

    • Leachates

    • Soil / contaminated land digests

    • Sediment digests

    • Plant / animal tissue digests

  • Generally high sample numbers (>100 per day in many laboratories)

Enviromental applications myths and misconceptions in icp ms
Enviromental applications:Myths and misconceptions in ICP-MS

  • Considered in the flame AA, furnace AA and ICP-OES communities that:

    • Not possible to measure high ppm concentrations (>100ppm) by ICP-MS

    • Interferences are a significant problem

    • Instrumentation is complex and difficult to use

    • Very high cost

Memory effects vs wide dynamic range monitored sample uptake and wash
Memory effects vs wide dynamic range: Monitored Sample Uptake and Wash

  • Intelligent sample monitoring to ensure stability prior to data acquisition.

  • Monitored washout eliminates sample carry over.

Xseries ii xt interface
XSeriesII - Xt Interface

  • Optimized response for Environmental Analysis

  • Maximum productivity through long-term matrix tolerance and excellent signal stability

  • Minimum recalibrations between samples

  • Extended dynamicrange

    • EnablesLinear determination of Na,Mg,K,Ca to 200 mg/L

    • >> 1000mg/L when used in conjunction with high resolution measurement

Reaching high ppm concentrations variable resolution what does it mean in practice






Reaching high ppm concentrations:Variable resolution – what does it mean in practice?

  • Allows the user to extend the dynamic range even further

    • The dynamic range limitation then becomes the 0.2% total dissolved solids upper level imposed by the interface cones

  • Can be adjusted down to peak widths lower than 0.3 amu

  • Can be adjusted on-the-fly to allow standard and ‘high’ resolution measurements to be made analyte by analyte

Na ca calibration x t interface standard resolution
Na, Ca, calibration – Xt interface, standard resolution

Na: blank to 300 ppm

Cr: blank to 100 ppb

Sensitivity = 0.9 Mcps/ppm

BEC = 107 ppb

Sensitivity = 1.3 Mcps/ppm

BEC = 0.2 ppb

Standard XSeriesII configuration (no CCT), using In as the internal standard

Peak width (at 10% peak height) = 0.75 amu

Reaching even higher ppm concentrations na calibration x t interface increased resolution
Reaching even higher ppm concentrations:Na calibration – Xt interface, increased resolution

Na: blank to 2000 ppm

2000 ppm

Sensitivity = 0.5 Mcps/ppm

BEC = 38 ppb

Standard XSeriesII configuration (no CCT), using Ga as the internal standard

Peak width (at 10% peak height) = 0.2 amu

Long term drift of x series with x t interface borehole water matrix
Long Term Drift of X Series with Xt Interface (Borehole Water Matrix)

Li = 21 µg l-1 RSD = 1.6 %

In = 10 µg l-1 RSD = 1.1 %

U = 4 µg l-1 RSD = 1.5 %

Comparison with icp o es
Comparison with ICP-OES

R2 = 0.984

R2 = 0.997

n = 188

Conclusions for x series ii standard with environmental work
Conclusions for XSeriesII standard with environmental work

  • Hardware and software advancements of the XSeriesII ICP-MS allow rapid, accurate analyses of environmental samples with turnkey operation.

  • Great improvement in sample throughput.

  • Linear range extended and matrix tolerance improved with Xt interface.

  • Protocol compliance even without CCT.

Xseries ii icp ms2


Performance Options


Environmental Research Applications

Peltier controller option do we need it
Peltier Controller option – do we need it?

  • Rapid, precise temperature control of spray chamber for optimum performance

    - constant aerosol formation independent of the laboratory temperature control

  • Typical operation at 2oC

    - reduced solvent loading into the plasma

    - lower oxides and other interferences

    - improved MDLs

  • Can be used with the standard quartz or inert spray chamber

  • Rapid changeover between aqueous and organic matrices using the organics kit

Variable temperature Peltier (thermo-electric) block

C ct ed when do we need it
CCTED – When do we need it?

  • Research Applications

  • Ultimate Detection Limits - well below regulatory levels

  • Analysis of some complex or pristine environmental matrices such as seawater or snow / ice.

    • Common interferences can not be eliminated using conventional quadrupole ICP-MS technology

    • Interference correction equations

    • Matrix removal

  • CCTED enables direct analysis without the need for matrix removal leading to improved DLs and enhanced productivity

Introduction to the use of cct with enviro nmental analysis principles of collision cell technology
Introduction to the use of CCT with environmental analysis:Principles of Collision Cell Technology





Introduction to the use of cct with enviro nmental analysis
Introduction to the use of CCT with environmental analysis

  • Some analytes have few interference problems and perform best with the cell unpressurised, i.e. standard ICP-MS mode, e.g. Pb

  • The ideal multi-element analysis would result in several analyses under different conditions, e.g.

    • Standard mode

    • H2 mode

    • NH3 mode

  • A more efficient method is to switch modes “in-sample”

    • is this viable in terms of speed, stability and accuracy?

Spectra for upw water 35 65 amu



Spectra for UPW Water (35-65 amu)

Cct for environmental applications instrument
CCT for environmental applications: Instrument

  • XSeriesII ICP-MS with CCTED and Xt interface

  • CCT connected to two gases:

    • 8% H2 in He

    • 1% NH3 in He

  • 2 computer controlled MFCs allow gases to be changed “in-sample”

Cct for environmental applications experimental considerations
CCT for environmental applications: Experimental - considerations

Wide range of typical environmental analytes were measured:

- 30 analytes, 55 isotopes

Many analytes have associated interference problems….

Cct for environmental applications experimental timing
CCT for environmental applications:Experimental - Timing



































3x1.6s reps





3x18s reps






3x18s reps



Time Profile

Total Time Per Sample (3 repeats) = 3 minutes, 45 seconds

Cct for environmental applications results detection limits m g l
CCT for environmental applications:Results - detection limits (mg/L)

Based on 3s on 12x10replicates of blank, each from a new calibration

Cct for environmental applications results stability of real sample in different modes
CCT for environmental applications:Results – stability of real sample in different modes

Sample diluted 1+9 and spiked to 2% HCl

Cct for environmental applications conclusions
CCT for environmental applications:Conclusions

  • The XSeriesII allows rapid settings changes, allowing two different cell gases and normal ICP-MS mode to be used in a single sample analysis

    • 3¾ minutes per sample, 55 isotopes, 3 measurements/isotope,

  • Excellent stability is retained in each mode

    • RSDs of typically <1% over a 12 hour duration for a signal of ~50,000cps

  • Mode switching allows the optimum conditions for each analyte to be utilised, resulting in ultimate performance:

    • DLs in the ppt or sub-ppt range for almost all elements

  • The technique results in freedom from many interferences

    • Accuracy of within ±5% for the vast majority of analytes, even after spiking to 700ppm chloride

Xs interface option do we need it
Xs Interface option – do we need it?

  • Xs- extraction provides enhanced sensitivity whilst retaining the extremely low background characteristics of the XSeriesII

  • For research and ultra trace applications

    • Actinides

    • Isotope ratios

    • Small spot laser applications

  • Interchangeable with the Xi interface

    - User interchangeable ~ 2 minutes

  • Typical sensitivity >200Mcps/ppm for mid –high mass elements (In – U)

X series e nvironmental methods icp ms productivity pack
X Series Environmental Methods ICP-MS Productivity Pack

  • Supplied to customers on instrument delivery:

    • PlasmaLab Productivity Method Template

    • Detailed instructions on instrument set-up, solution preparation and sample analysis

    • A Productivity Method Template that can be modified to a laboratory’s own working method

    • All calibration and quality control solutions required to run each protocol

    • A printed file containing the Productivity Method Template

Environmental protocols
Environmental Protocols

  • US EPA has developed a series of methods for the analysis of drinking water, waste water and other environmental samples: -

    • OW 200.8 drinking water 1991

    • OSW 6020 waters, wastes, soils, etc 1994

    • OSW 6020A waters, wastes, soils, etc 1998

    • CLP ILM05.2D waters, wastes, soils, etc 2001

      These are challenging, QC intensive, multiple analyte, multiple concentration methods with tough specifications for accuracy, precision and DLs

Environmental protocols typical requirements
Environmental Protocols - Typical Requirements

  • Methods are ‘Prescriptive’ with specific rules on various analytical practices that must be followed e.g.

  • Specified Elements:

    • Up to 23 elements, 7-orders of magnitude range (ppt to high ppm)

  • QC Checks – post calibration:

    • Separate source calibration verification

    • Interference check - High Matrix

    • Interference check - High Matrix + Spike

  • QCChecks – every 10 samples:

    • Continuing calibration verification

    • Reference material

    • Detection limit check standard

  • Sample QCs - every 20 samples:

    • Duplicate

    • Serial Dilution and Spike Recovery

Xseries ii interference correction equations
XSeriesII - Interference Correction Equations

X Series interference correction equations derived for use with EPA protocols

Xseries ii mdls vs ilm05 3 crqls epa ilm 05 3 environmental water and waste water
XSeriesII MDLs vs. ILM05.3 CRQLs- EPA ILM 05.3 Environmental water and waste water

Xseries ii environmental productivity pack
XSeriesII Environmental Productivity Pack

Supplied to customers on instrument delivery:

  • PlasmaLab Productivity Method Template on CD

  • Detailed instructions on instrument set-up, solution preparation and sample analysis

  • Productivity Method Template can be modified to a laboratory’s own SOP

  • All calibration and quality control solutions required to run each protocol

  • A printed file containing full instructions of the operating procedure

Environmental Productivity Pack - Contents

Xseries ii icp ms environmental analysis summary
XSeriesIIICP-MS – Environmental Analysis Summary

  • Routine

    • MDLs - XSeriesIIICP-MS easily provides protocol compliant detection limits

    • QC checks: XSeriesII consistently produces accurate results on QCs and samples

    • Interference checks : XSeriesII design offers excellent freedom from interference and stable correction where necessary

    • Fastest sample throughput with protocol compliance

  • Productivity Pack uniquely offers:

    • Proven, reliable off-the-shelf EPA methods for the - XSeriesII ICP-MS

    • Unbeatable rapidity of start-up after installation

  • Research

    • Peltier cooled spray chamber for improved long term stability and MDLs

    • CCTED for interference removal / improved accuracy and detection limits in complex matrices

    • Xs interface for special applications requiring the ultimate signal/background

    • LC / GC packages for speciation studies

Xseries ii icp ms3


Speciation analysis

Why speciation analysis
Why Speciation Analysis?

e.g. Arsenic Toxicity

  • Elemental speciation data can reveal valuable information in addition to total element concentrations: -

    bioavailability, mobility, metabolic

    processes, bio transformations and

    toxicity implications

  • Elemental speciation is receiving increasing interest in both academic & commercial laboratory environments

    • Applications often use HPLC-ICP-MS and GC-ICP-MS techniques

    • Growing number of publications for elemental speciation analyses

    • Elemental speciation increasingly recognised in EPA protocols

Inorganic As3+ arsenite (AsO3)3-

Inorganic As5+ arsenate (AsO4)3-

Monomethylarsonate (MMA)

Dimethylarsinate (DMA)

Arsenobetaine ((CH3)3As+CH2COOH)-

Arsenocholine ((CH3)3As+(CH2)2OH)

Increasing Toxicity

Topical species in environmental life science and food samples
Topical Species in Environmental, Life Science and Food Samples

  • Arsenic – (As5+, As3+, DMA, MMA, AB)

    • urine, biological tissues, foods, waters

  • Chromium – (CrVI and CrIII)

    • biological fluids, waters

  • Selenium – (SeIV, SeVI, SeMet, SeEth, SeMC)

    • urine, biological tissues, foods & supplements,

  • Mercury – (Hg2+, MeHg)

    • biological tissues, foods, waters

  • Tin – (MBT, DBT, TBT)

    • biological tissues, foods, waters

Flexible hplc icp ms product packages
Flexible HPLC-ICP-MS product packages Samples

  • XSeriesII ICP-MS with Finnigan Surveyor HPLC

  • XSeriesII ICP-MS with SpectraSYSTEM HPLC

  • ‘HPLC Coupling Packs’ for X Series ICP-MS

    • Simple analytical and electrical connections to ‘any’ HPLC

    • External Trigger Board for 2-way communications between the LC and the ICP-MS

X series icp ms for hplc applications
X Series ICP-MS for HPLC applications Samples

  • Simple to interchange between standard ICP-MS & HPLC sample introduction

  • XSeriesII ICP-MS organics kit for reverse/normal phase HPLC

  • Burgener AriMist nebulizer for mobile phases with high TDS & 50–2000 μL/min flow rates

  • Sensitive multi-element capability

  • Field upgradeable XSeriesII ICP-MS

Flexible gc icp ms product packages
Flexible GC-ICP-MS product packages Samples

  • XSeriesII ICP-MS with Finnigan Focus GC

  • XSeriesII ICP-MS with Finnigan Trace GC

  • ‘GC Coupling Packs’ for XSeriesII ICP-MS

    • Simple analytical and electrical connection to ‘any’ GC

Xseries ii icp ms for gc applications
XSeries SamplesII ICP-MS for GC applications

  • Unique DUAL MODE sample introduction

    • Gas or solution analyses without reconfiguring the interface

    • Three legged GC-ICP-MS torch

    • Flexible tuning & performance testing with aqueous solution

    • On-line addition of aqueous internal standards

    • Robust plasma conditions for GC-ICP-MS analysis

Speciation with lc icp ms arseno sugars in kelp

Arsenosugar II Samples

Arsenosugar IV

Arsenosugar III

Arsenosugar I

Speciation with LC-ICP-MS: Arseno sugars in kelp

  • SpectraSYSTEM HPLC

    • mobile phase: 5 mM TBAH at pH 6.0 (0.7 ml/min)

    • HPLC column: Discovery C18 (150mm x 2.1mm i.d)

    • 0.2 g kelp extracted in 5ml MeOH/water (50:50 v/v)

    • Injection volume: 1 micro-litre

    • Dimethylarsinoylriboside standards (deionised water)

    • Fast separation, baseline separationof all peaks in just over 2 mins.

  • LC-ICP-MS Coupling Pack

  • XSeriesII ICP-MS

    • Xt interface

    • PlasmaScreen Plus

    • Peltier Cooled Spray Chamber

Speciation with gc icp ms organo sn speciation in sediments
Speciation with GC-ICP-MS SamplesOrgano-Sn speciation in Sediments

  • Finnigan Focus GC

    • GC column: 30 m Restek MXT-1

    • Mobile phase: He at 25 ml/min

    • Make-up gas: Ar 350 ml/min

    • Injection volume: 1 μL

    • Oven program: 70-250ºC (50ºC/min plus 1 minute hold)

  • GC-ICP-MS Coupling Kit

  • XSeriesII ICP-MS

    • Xt interface

    • PlasmaScreen Plus

    • Timeslice internal standard: (5 ng/ml Sb)

Plasmalab for chromatographic applications
PlasmaLab for chromatographic applications Samples

  • Transient TRA data acquisition

  • External Triggers for controlling ‘any’ HPLC or GC accessory

  • Intelligent bi-directional communication for failsafe, high throughput analysis

  • Unique ‘Timeslice’ & ‘Transient’ internal standard modes for improved data quality

  • In-house peak integration for quantitative analysis

The new xseries ii icp ms
The New XSeries SamplesII ICP-MS

More Practicality, More Productivity, More Performance for every application