Finnigan™ TRITONFinnigan™ NEPTUNE

Analyze • Detect • Measure • Control™

High ResolutionMulticollector Mass Spectrometers

m a s s s p e c t r o m e t r y

Finnigan™

TRITON

/ Finnigan™

NEPTU

NE

High Resolution M

ulticollector Mass Spectrom

eters

• High resolution ion opticscorrected for second orderimage aberrations– largest mass dispersion

(812 mm)– angular and energy

focusing image planesare almost coincident

• Zoom optics to enhancedynamic multicollectormeasurements– precise peak overlap

for multi-dynamicmeasurements

• Field proven Faraday cups withlargest aspect ratio– No cup factors

• Multiple Ion Counting (MIC)– Up to 8 moveable

miniaturized SEMs in parallel

• Variable multicollector– Variable in position– Variable in detector type

(Faraday/SEM)– Up to 17 collectors in

parallel– “Plug-in” design of

Faradays and SEMs– 17 % relative mass range

• Virtual Amplifier system– No amplifier calibration

bias– Linear response up to 50 V

(positive ion mode)• 10 kV acceleration voltage

– Highest sensitivity • All metal-sealed vacuum

system– Ultra high vacuum system– High abundance sensitivity– Bakeable at high

temperature• Retardation lens (RPQ option)

– Excellent abundance sensitivity

• Single focusing for thermalionization source– Finnigan TRITON

• Double focusing for inductivelycoupled plasma source– Finnigan NEPTUNE

Based on more than 25 years experience in variable multicollector instrumentation, Thermo ElectronCorporation has developed two instruments based on an innovative multicollector platform.

Finnigan™ TRITONFinnigan™ NEPTUNEHigh Resolution Multicollector Mass Spectrometers

No compromiseis the common philosophy

The Finnigan TRITON sets a new standard in high precision TIMSisotope ratio measurements. The Finnigan TRITON’s uniquecapabilities have earned it the reputation of the “natural choice”in TIMS instrumentation.

• Guaranteed external precision of Nd and Sr is 5 ppm (1 SD),both in static and multi-dynamic acquisition

• 2 ppm external precision has been shown• Improved sensitivity• 21 position sample turret for high throughput• User friendly software for high throughput, with network

capabilities

Finnigan™

TRITON

/ Finnigan™

NEPTU

NE

High Resolution M

ulticollector Mass Spectrom

eters

Finnigan TRITON

Finnigan NEPTUNE

The Finnigan NEPTUNE completes Thermo Electron Corporation’sintegrated product family for elemental and isotopic analysis.It shares the field proven ICP interface with the Finnigan ELEMENT2, the most advanced single collector high mass resolution ICPMS.Finnigan NEPTUNE and Finnigan TRITON are using the same highprecision multicollector platform.

The Finnigan NEPTUNE defines a “third generation” MC-ICPMS,combining, for the first time, the features of high mass resolution,variable multicollection, zoom optics and multiple ion counting (MIC).

• High mass resolving power with flat top peak sections• Excellent short-term and long-term stability

of signal intensity and mass bias• Full sensitivity with standard sample

introduction system• Fully integrated software for unattended

operation and high throughput

Key Technologies

Source

Magnet lens

Faraday cup

Magnification = 1

Secondary particles arereleased close to the cupentrance

Source

Magnet lens

Faraday cupMagnification = 2

Larger effective depth of cups:less emission of scattered particles

Advanced Multicollector IonOpticsLarge mass dispersion using an ion opticalmagnification of 2:The large mass dispersion of 812 mmprovides generous space for the versatilecollector array. The mass dispersion isachieved by an ion optical magnificationof 2, which has the additional advantagesof increased focal depth and improvedcup performance.

High Performance Faraday CupsThe Faraday cups are the largest everproduced for a commercial multicollector.They are laser machined from solid carbonto guarantee uniform response, highlinearity, low noise and long lifetime. The

Faraday cups are designed to completelyeliminate the need for cup factors 1.

The effect of ion optical magnificationon cup performance is depicted in thegraph. With increasing ion opticalmagnification the divergence angles of the

ion beams are reduced and the dispersion isincreased. As a result, cups can be widerand deeper. Scattered particles released atthe cup's side wall by the incoming ionbeams are less likely to escape and do notalter the “true” ion current.

Ions

Inside view of a Faraday Cup

1 Patent No. US 6,452,165 B1

d

d'=2d

Finnigan™

TRITON

/ Finnigan™

NEPTU

NE

High Resolution M

ulticollector Mass Spectrom

eters

The Variable MulticollectorEight moveable collector supports and onefixed center channel are installed on theoptical bench of the new high precisionvariable multicollector module. The centerchannel is equipped with a Faraday cup andoptionally an ion counter with or withoutthe retardation lens (RPQ) to achieve theultimate abundance sensitivity.

The eight detector supports can beprecisely positioned along the focal plane,according to the specific needs of theapplication. The maximum distancebetween the outermost channelscorresponds to a relative mass range of17% sufficient for the simultaneousmeasurement of 6Li and 7Li or 202Hg to 238U.

The variable detector supports aredriven by motors.

Beneath each variable detector platformthere is a position sensor located inside thevacuum chamber. Precise in situ monitoringof the detector position directly at the opticalbench of the variable multicollector ensuresreliable positioning, which is a must for highprecision isotope ratio measurements at highmass resolution.

Multiple Ion Counting (MIC)Each moveable support can carry either aFaraday cup, or a miniature SecondaryElectron Multiplier (SEM) or a combinationof both in a package. All detectors are of‘plug-in’ design2 and can be readilyexchanged. It is possible to equip onedetector platform with a package of ioncounters plus one Faraday cup. The abovecombination is perfect for fixed counterpackages for specific elements in the highmass range e.g. lead and uranium becausethe packages can be built very compact.

The configuration where the ioncounter packages are attached to the outermoveable Faraday cups (H4, L4) keeps thefull flexibility of the Faraday cup array. Theinsertion of the additional ion counters atthese outer positions does not block anyFaraday cup configuration. A fully equippedsystem can be loaded with a maximum of17 channels: 9 Faraday cups plus 8 ioncounters - all of which can be used in asimultaneous multicollector measurement.

2 Patent applied for US 10/618 285

Multi Ion Counting

• 50 V Dynamic Range• Elimination of Amplifier Biases• No Cup Factors• Up to 17 Ion Beams can be detected simultaneously

Key TechnologiesFinnigan™

TRITON

/ Finnigan™

NEPTU

NE

High Resolution M

ulticollector Mass Spectrom

eters

V F

V F

V F

V F

V F

V F

V F

V F

V F

1 2 3 4 5 6 7 8 9

Faraday cups

Relay MatrixAmplifier andV/F converter

relay open relay closed

evacuated and thermostated housing

1

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8

9

Measurem

ent channels

The Virtual AmplifierThe goal of the new multicollectordevelopment was to break through the 5 ppmprecision barrier. Finnigan TRITON andFinnigan NEPTUNE use a patentedmeasurement procedure, which completelyeliminates gain calibration biases: theVirtual Amplifier concept 3. In all previousmulticollector systems the relation

(connection) between individual Faradaycups and amplifiers was fixed. In the VirtualAmplifier concept all Faraday cups involvedin a certain measurement are sequentiallyconnected to all amplifiers. As a result allsignals have been measured with the sameset of amplifiers and for the calculation ofthe isotope ratios all calibration biases ofthe amplifiers are cancelled.

The AmplifierEach Faraday cup is connected to a currentamplifier. The amplifier signal is digitized bya high linearity voltage to frequencyconverter with an equivalent digitalresolution of 22 bits. This ensures sub-ppmdigital resolution of all measured signalsindependent of the actual signal intensity.The amplifiers are mounted in a doublyshielded, evacuated and thermostatedhousing with a temperature stability of± 0.01 °C.

The dynamic range of the currentamplifiers is extended to 50 V in positive iondetection mode. For negative ions it isrestricted to 15 V. The extended dynamicrange supports the measurement of largeisotope ratios, because it directly leads toan improved signal to noise ratio for theminor isotopes.

For classical systems the need for aprecise cross calibration of the currentamplifiers defines a precision barrier in staticmulticollection. Even with perfect Faradaycups giving uniform response, results of staticmeasurements are biased by the accuracyand reproducibility of the gain calibration. Inthe classical method of cross calibration, ahigh precision, constant current source issequentially connected to all amplifiers.However, with this method, amplifiers cannotbe calibrated to better than ~5 ppm perchannel. For instance if one considers anisotope system consisting of three isotopesthe best external precision can be estimatedto be: 5 ppm x √3 = ~9 ppm.

3 Patent No. US 6,472,659 B1

Measuring Large Isotope RatiosThe measurement of large isotope ratios isaffected by scattered ions generated at slitsand apertures, the flight tube walls and mostimportantly the interaction of ions withresidual gas particles. Ions which sufferedone of these interactions have lost kineticenergy and/or have changed their directionof motion. As a result, these ions appear atincorrect mass positions along the focalplane, typically increasing background atneighbouring masses. The Finnigan TRITONand Finnigan NEPTUNE employ an optionalRetarding Potential Quadrupole Lens (RPQ)4

that acts as a high selectivity filter for ionswith disturbed energy or angle.

With the Finnigan TRITON, whosethermal ionization source produces ions witha small energy spread (0.5 eV), the RPQreduces the abundance sensitivity by twoorders of magnitude from typical 2 ppm (238U ± 1 u) to 20 ppb. The dark noise of theion counting system used in the RPQ is lessthan 10 counts per minute. This combinationof low dark noise and high abundancesensitivity allows the determination of largeisotope ratios with the highest accuracy.Combining the RPQ with the FinniganNEPTUNE, whose ICP source generates ionswith an energy spread up to ~5 eV, improvesthe abundance sensitivity by one order ofmagnitude from guaranteed 5 ppm to 500ppb with more than 90 % transmission.

The abundance sensitivity of theFinnigan NEPTUNE can be further improvedby increasing the energy barrier of the RPQfilter: At 50 % transmission, an abundancesensitivity of 150 ppb can be achieved.However, the stability of the system willbe reduced.

4 Patent No. US 5180913

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1

0

-1229.5 Mass (u) 231.5

Coun

ts /

s

Peak tail of 232Th

A < 2 x 10-6

A < 5 x 10-9

232Th / 230Th = 2 900 000 : 1

RPQ

Finnigan TRITON: abundance sensitivity with and without RPQ filter

Finnigan NEPTUNE: abundance sensitivity without RPQ filter

Thermal Ionization SourceThe thermal ionization source is characterizedby a very small (~0.5 eV) kinetic energyspread of the ions. Therefore, a singlefocusing geometry that focuses for angulardivergence only is fully sufficient. Chromaticaberrations due to the initial energy spreadof the ions can be neglected. In thisconfiguration the magnetic sector lensfocuses ions of different mass along aninclined focal plane with 45° angle. Themagnet is laminated for high speed peakjumping and low hysteresis. The inner widthof the flight tube is 14 mm, ensuring minimalscattering. Baffles are present along theflight path to directly catch any diverging ionsand to minimize scattering at the side walls.

The New TI SourceThe new ion source optics of the FinniganTRITON have been optimized for maximumion transmission for both single and doublefilament techniques. It makes the FinniganTRITON about twice as sensitive as theFinnigan MAT 262. The new sample turretholds 21 single or double filaments. Thefilaments can be easily exchanged withoutusing any tools.

Special care has been taken by shapingthe ion source lens elements so that thebuild up of contaminations and memory inthe source are minimized. The lens stack iseasily accessible by the user for inspectionand maintenance.

The ion source is held at an accelerationpotential of 10 kV to achieve optimumsensitivity.

Finnigan™

TRITON

/ Finnigan™

NEPTU

NE

High Resolution M

ulticollector Mass Spectrom

eters

Finnigan TRITON

Blockwise Amplifier Rotation

140Ce 142Nd 143Nd 144Nd 145Nd 146Nd 147Sm 148Nd150Nd

Faraday Faraday Faraday Faraday Faraday Faraday Faraday Faraday Faraday

Cup

L4

Cup

L3

Cup

L2

Cup

L1

Cen

ter

Cup

H1

Cup

H2

Cup

H3

Cup

H4

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9 1 2 3 4 5 6 7 8

8 9 1 2 3 4 5 6 7

7 8 9 1 2 3 4 5 6

6 7 8 9 1 2 3 4 5

5 6 7 8 9 1 2 3 4

4 5 6 7 8 9 1 2 3

3 4 5 6 7 8 9 1 2

2 3 4 5 6 7 8 9 1Amplifier Number

84Sr 85Rb 86Sr 87Sr 88Sr

Faraday Faraday Faraday Faraday Far/IC Faraday Faraday Faraday Faraday

Cup

L4

Cup

L3

Cup

L2

Cup

L1

Cen

ter

Cup

H1

Cup

H2

Cup

H3

Cup

H4

Cup

L2

The Zoom OpticsMulti-dynamic measurements can be usedto eliminate cross calibration biases ofFaraday cup detectors or multiple-ion-counting (MIC) detectors. The philosophy of‘no compromises’ led us also to achieve theultimate performance using this procedure.

Historically, the collectors had to be setto compromise positions in order to fullycatch the ion beams in all different cupconfigurations. The Zoom Optics is a tool tochange mass dispersion. If usedsynchronously with switching the ionbeams, perfect overlap of all peaks in allconfigurations is achieved. This scheme isfully integrated into Finnigan TRITON’sautomatic measurement.

For instance, the Zoom Optics allowsmeasurement of all isotopes of UO in thesame detector configuration as U withoutthe need of mechanical readjustment of thedetector positions.

Multicollector configurations for Nd and Sr,along with the amplifier rotation scheme(Virtual Amplifier)

Double Focusing High ResolutionMC-ICP-MSThe kinetic energy distribution of ionsgenerated in an ICP source is large (~20 eV),compared to ions from a thermal ionizationsource. A double focusing analyzer, focusingboth ion energy and angular divergence, is thebest technical solution for this challenge.

Reduced Energy Spread Using aCD-SystemFinnigan NEPTUNE’s ICP interface reducesthe initial kinetic energy spread from ~20 to~5 eV by capacitively decoupling (CD) theplasma from the load coil using a groundedplatinum guard electrode. This low kineticenergy distribution, together with a wideenergy acceptance of the mass analyzerand 10 kV ion acceleration voltage,eliminates all effects of ionenergy spread on isotoperatios and mass bias.

Plasma interface at groundpotentialThe plasma interface is held at groundpotential, allowing easy access to thenebulizer, spray chamber and torch. Changingfrom solution to laser ablation is as easy asthe connection of an autosampler.

The plasma interface can be isolated fromthe analyzer through an automatic gate valve.

The ion transfer optics focus the ionsfrom the plasma interface onto the entranceslit of the double focusing analyzer. Massbias is mainly generated in the plasmainterface and the ion transfer optics.Finnigan NEPTUNE’s excellent mass biasstability, sensitivity and low backgroundresult from Thermo Electron Corporation’sunique ion transfer optics5.

Finnigan NEPTUNE

Reduced Energy SpreadUsing a CD-System

Finnigan™

TRITON

/ Finnigan™

NEPTU

NE

High Resolution M

ulticollector Mass Spectrom

eters

5 Patent No. US 5625185

Peakscan of all Fe isotopes and molecular interferences at high resolving power. Fe isotopes can be measured free of any interferences inthe first peak plateau at the low mass side. At the multicollector mass position indicated in the figure just the elemental ion beams enter theFaraday cups while the molecular interferences are stopped at one side of the detector slit (see right hand side Figure).

Interference Free Measurementsby High Mass ResolutionMulticollection

High Mass ResolutionThe ion optics of the Finnigan NEPTUNEachieve high mass resolving power on alldetectors along the image plane. Thiscapability is based on its refined ion optics with• Almost coincident angular and energy

image planes• Large focal depth due to large ion optical

magnification (see page 6)

Finnigan NEPTUNE can be operated inthree different resolution settings: Low,medium and high resolution. In highresolution settings the resolving power cango up to m/∆ m = 10.000. The m/∆ m isderived from the peak slope of the risingedge measured at 5% and 95% relativepeak height.

For single collector sector fieldinstruments the mass resolution is changedby switching both the source slit width andthe detector slit width. For high massresolution a small source slit and a smalldetector slit is used. This typically resultsinto very narrow triangular shaped peaks inthe mass spectrum and ensures safe peakseparation of interfering species. However,for high precision isotope ratiomeasurements a wide peak flatness rangeis required and triangular peak shapescannot be used. In order to separatemolecular interferences from elementalpeaks on a multicollector instrument a smallsource slit has to be selected as well,however, the detector slit can be kept atlow resolution setting. The individualdetectors of the variable multicollector canbe positioned such that just the elementalions can enter the detector whereas theinterfering ions are stopped on one side ofthe detector slit. The typical operation modeof a multicollector instrument is a staticoperation mode where the magnetic fieldremains constant and the interferences arestopped at the detector slit.

According to the systematics of thenuclear mass defect all molecularinterferences in the low and medium massrange are heavier than the elementalspecies and all interferences can readily bestopped at the same side of the detectorslit. The use of the wide detector slit for allresolution settings is the best choicebecause it guarantees the widest peakflatness at high resolving power, which is amust for high precision and accurate isotoperatio measurements.

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50.6500.6559.5509.5558.55

sig

nal

[V]

no

rmal

ized

to56

Fe+ secnerefretnI+eF

04 rA 61 O+

04 rA 61 O1H+

04 rA 81 O+

04 rA 41 N+

45 eF +

65 eF +

75 eF +

85 eF +

mul

ticol

lect

or m

ass

mass

Faraday 1

collector slit

56 Fe 40 Ar 16 O

Faraday 2

collector slit

57 Fe 40 Ar 16 O 1 H

Software PackageFinnigan™

TRITON

/ Finnigan™

NEPTU

NE

High Resolution M

ulticollector Mass Spectrom

eters

The Finnigan TRITON andFinnigan NEPTUNE softwarepackageMost of the software modules are commonto both instruments:• Cup configuration editor to define and

select cup configurations• Method editor to set up user-defined

measurement procedures• On-line and off-line data evaluation

packages including statistical capabilitiesand display of the results in spreadsheetor graphical form

• Sequence editor for automatic,unattended acquisition and evaluation ofsamples including sample/standardbracketing and blank substraction.

• Automated report generation of analyticalresults.

Tuning the Source Finnigan TRITON (TI source)

• Fully automated sample turretmanipulation

• Configurable and automated filamentheating

• Pyrometer readout of the filamenttemperature

Finnigan NEPTUNE (ICP source)

• Fully automated plasma start sequence• Easy auto sampler setup

Method Setup

• Selection of cup configuration– Cup position – Faraday or SEM– Assignment of isotope masses to

the detector• Data collection strategy:

– Static measurements– Dynamic measurements– Fast single collector peak jumping

measurements• Integration of sample heating program

(Finnigan TRITON)• Selection of bias/fractionation

corrections• Definition of isotope ratios

– Outlier tests– Interference correction– Equation editor for user-defined

data reduction• Switch key to synchronize start of

data acquisition with Laser ablation(Finnigan NEPTUNE)

Finnigan TRITON Method Editor

Finnigan NEPTUNE Tune Window

Process Control Language (PCL)• Script language based on C programming

language• Modification of existing procedures:

– Baseline determinations– Gain calibration

• Definition of new procedures– Open for user-defined experiments

• Scripts can be:– Run individually– Combined with existing software modules

Evaluation

• On-line and off-line evaluation• User configurable display of results:

– Spreadsheet– Graphical display

• Access to all raw data• On-line monitoring of ratios, intensities,

statistics vs. time

Sequence Editor• Automatic acquisition of samples,

standards and/or blanks• Computer control of autosampler• Online blank subtraction and mass bias

correction using an external standard• Report of delta-values• Online ASCII export• Sequence accepts external trigger for

starting (i.e. from Laser system)

Result Display

Sequence Editor

PCL Script Editor

The software runs under the latest MicrosoftWindows® operating system. The softwarepackage is optimized for stability, performanceand is fully compatible with future operatingsystems. The software combines the strengthof an optimized, Windows-based packagewritten in C++ with the power and flexibility ofa user-friendly open structure, realized in ourunique Process Control Language, PCL. TheMicrosoft Windows® operating system allowsthe data system to be easily connected to anetwork, enabling data transfer and remotecontrol of the instrument.

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