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M. Tiepolo M. Tiepolo C.N.R. C.N.R. - - Istituto di Geoscienze e Georisorse Istituto di Geoscienze e Georisorse Sezione di Pavia Sezione di Pavia Laser Ablation Inductively Laser Ablation Inductively Coupled Plasma Mass Coupled Plasma Mass Spectrometry Spectrometry ( ( LA LA - - ICPMS) ICPMS)
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Page 1: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

M. TiepoloM. TiepoloC.N.R.C.N.R.--Istituto di Geoscienze e Georisorse Istituto di Geoscienze e Georisorse –– Sezione di PaviaSezione di Pavia

Laser Ablation Inductively Laser Ablation Inductively Coupled Plasma Mass Coupled Plasma Mass

Spectrometry Spectrometry ((LALA--ICPMS)ICPMS)

Page 2: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Bulk vs. Microanalysis

Page 3: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):
Page 4: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

LALA--ICPICP--MSMS(Laser (Laser AblationAblation -- InductivelyInductively CoupledCoupled Plasma Plasma -- Mass Mass SpectrometrySpectrometry))

ICP mass spectrometer+Laser microprobe

• Elevata risoluzione spaziale• Capacità di campionare solidi

naturali e sintetici

• Alta efficienza di ionizzazione del plasma

• Alta sensibilità

Determinazioni elementari ed isotopiche

Scienze geologiche, ambientali, biologiche, forensi, semiconduttori

Page 5: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Elementi costituenti un LAElementi costituenti un LA--ICPICP--MSMS

1. Sorgente laser (Ablazione)

2. Cella di Ablazione + linea di trasferimento (Trasporto del particolato)

3. Spettrometro di Massa ICP (Ionizzazione + discriminazione delle masse)

Page 6: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):
Page 7: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Il processo di ablazione laserL’interazione fra solido e laser produce:

• Eccitazione elettronica all’interno del solido con espulsione di elettroni

• Trasferimento di energia al lattice del solido

• Fusione e vaporizzazione del campione

• Ionizzazione e formazione di un microplasma costituito dagli elementi del campione

• Interazione con il gas circostante ed espulsione del particolato

Da Borisov et al., 2000

Page 8: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Efficienza di ablazioneEfficienza di ablazione266 nm - Quarzo266 nm - Calcite

213 nm - CalciteFunzione del coefficiente di assorbimento & lunghezza

d’onda

Page 9: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

NdNd:YAG (266 :YAG (266 nmnm) vs. ) vs. ExcimerExcimer ArFArF (193 (193 nmnm))

Nd:YAG-Laser266 nm

Excimer-Laser ArF193 nm

Page 10: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

266nm laser microprobe configuration266nm laser microprobe configurationBrilliant - Quantel pulsed Nd:YAG laser source

Nd:YAG 2ω 4ω

1064 532 266 attenuatore

IR Vis UV

Frequency 10 Hz – Max output energy 35.5 mJ/pulseSpot size 10-150 µm

Page 11: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

213nm laser microprobe 213nm laser microprobe configurationconfiguration

Frequency 10 Hz Max output energy : 0.8 mJ/pulseSpot size: 10-50 µm

Page 12: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

213 nm generator

Page 13: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Excimer Laser ArF 193 nm

Page 14: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

ArF 193 nmHomogenizer

Page 15: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):
Page 16: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):
Page 17: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

QuickTime™ e undecompressore

sono necessari per visualizzare quest'immagine.

Il processo di ablazione

BCR-2Vetro basaltico

100 µm

266 nm5.0 mW20Hz

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Dimensioni dello spotDimensioni dello spot

variando la posizione del campione rispetto al punto di fuoco del laser

variando l’apertura del diaframma sul percorso ottico

Obiettivo

100 µm

10 µm

40 µm

Page 19: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):
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Cella di Ablazione + linea di trasferimentoCella di Ablazione + linea di trasferimentoHe

He + particolato

Ar

ICP-MS

He

He He

He + particolato

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Segnale transienteSegnale transienteDiminuzione dell’intensità del segnale nel tempo

100

1000

10000

100000

1000000

10000000

0 50 100 150 200scans

cps

44Ca

93Nb

208Pb

Page 25: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Frazionamento elementareFrazionamento elementare(ablazione non stechiometrica)(ablazione non stechiometrica)

Cambiamento dell’intensità dei segnali nel tempo indipendente dal campione

0.1

1

10

0 100 200 300 400 500

scans

206Pb238U

206Pb/238U

Page 26: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

100

1000

10000

100000

1000000

10000000

0 50 100 150 200scans

cps

44Ca

93Nb

208Pb

FRACTIONATION INDEX =

MEAN SIGNAL M+ (min 2-4)/MEAN SIGNAL Ca+ (min 2-4)

MEAN SIGNAL M+ (min 0-2)/MEAN SIGNAL Ca+ (min 0-2)

Da Fryer et al., 1995

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Spettrometro di Massa

Page 29: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):
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Sorgente ICP (1) - ionizzazione

Page 31: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Sorgente ICP (2) - ionizzazione

Page 32: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Mean Free PathPressione

(torr)“Mean Free

Path”760 (1atm) 0.1 µm

1 0.05 mm

0.05 1 mm

10-5 5 m

10-6 50 m

10-7 500 m

10-8 5000 m

Affinché gli ioni si possano muovere èrichiesto un determinato grado di vuoto all’interno dello strumento

Page 33: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Ingresso nello spettrometro

Page 34: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Analizzatore

• Ha la funzione di discriminare le masse

• I principali tipi di analizzatori sono:– Quadrupolo– Settore magnetico (+ESA)– TOF (Tempo di volo)

Page 35: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Quadrupole analyser

The key result is that for an ion with a particular m/z ratio to pass through the quadrupole (and on to the detector), certain combinations of U and V must be obtained.

Thus, if U and V are scanned such that U/V = const. then successive detection of ions of different mass will be achieved. The following figure illustrates the principle graphically. The three stability curves represent values of U and V for which the three masses m1, m2 and m3 have stable trajectories through the quadrupole. Only those values which lie within the black shaded regions allow ion transmission.

Notice that resolution of the mass analyser can be increased by increasing the slope of the curve U/V = const., and that if U = 0 then ions of all m/z are transmitted.

The quadrupole analyser consists of four parallel rods to which a varying voltage is applied, resulting in a fluctuating electric field. The potential applied to the rods is made up of a DC (U) and RF (Vcos wt) component:

Page 36: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):
Page 37: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Settore magnetico a doppia focalizzazione

Reversed Nier-Johnson geometry

Page 38: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Lenti di trasferimento

Page 39: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Magnetic sector

Settling time ∝ ∆(m/z) VrH

em

2

22

=

H = campo magneticor = raggio del magneteV = accelerazione

Page 40: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

“High power magnet field regulator”

0.000

0.200

0.400

0.600

0.800

1.000

1.200

0 50 100 150 200 250

mass (a.m.u.)

Sett

ling

Tim

e / a

.m.u

. (m

s)

da ThermoFinnigan

m/z 7-238 230 msm/z 7-238 75 ms

Old field regulator

New field regulator

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Page 43: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Settore elettrostaticoElectrostatic sectorScan speed: 1 ms/jump

0,1

0,2

0,3

0,4

0,5

0,6

0,7

0,8

0,9

1

1,1

Hg202 Pb 204 Pb 206 Pb 207 Pb 208 Th 232 U 235 U 238

sens

itivi

tyE

S/se

nsiti

vity

BS

magnet mass

VrH

em

2

22

=

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MSA + ESA(doppia focalizzazione)

H2r2

2Vm/e =

Page 45: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Fenditure ingresso/uscita

Fenditura d’ingresso

Fenditura d’uscita

Page 46: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Peak shapequad vs. sector field

Page 47: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

“Flat top” peaks

207Pb

208Pb

Page 48: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Risoluzione

MRP (Mass Resolving Power) = m/∆m

LR = bassa risoluzione (300)MR = media risoluzione (3000)HR = alta risoluzione (6000)

m

∆m5% dell’altezza del picco

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Interferenze

m1 m2

HR

Page 50: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Detector (contatore)Responsabile del conteggio degli ioni

counting

analog

Page 51: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Acquisizione simultanea vs. Acquisizione sequenziale

Multi-collettore

∆t Singolo-collettore

(44Ca/208Pb)m = f [∆t ; (44Ca/208Pb)S]

Page 52: Laser Ablation Inductively Coupled Plasma Mass ... · PDF fileLaser Ablation Inductively ... I RSF C I STD i SAMP i STD i ... Inductively Coupled Plasma – Mass Spectrometry (LA–ICP–MS):

Response curveResponse curveIsotopic abundance normalizedIsotopic abundance normalizedC

ps/p

pm

1.E+03

1.E+04

1.E+05

Mg25

Si29

Ca43

Ca44

Sc45

Ti49

V51

Cr53

Rb85

Sr88

Y89

Zr90

Nb93

Cs133

Ba137

La139

Ce140

Pr141

Nd146

Sm149

Eu151

Gd157

Tb159

Dy163

Ho165

Er167

Tm169

Yb173

Lu175

Hf177

Ta181

Pb208

Th232

U238

Conventional torch

Capacitive Decoupling torch

In He ablationLaser frequency: 10HzLaser Power 2.2 mW 40 µm spot size

NIST 612NIST 612

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Determinazioni elementari

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Analisi quantitativaAnalisi quantitativa

RSFIIC

STDi

SAMPi

STDi

⋅⋅

=C SAMPi

RSF è uguale per tutti gli elementi in una singola analisi

Elemento maggiore (livello %)

Elemento presente sia nello standard che nel campione

Elemento multi-isotopo che permetta la scelta di quello a minore abbondanza (segnale meno intenso)43Ca, 29Si, 25Mg, 49Ti

SAMPis

STDis

SAMPis

STDis

CIICRSF ⋅

=

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Limits of detection (Limits of detection (3σRnet/S)1 ppm

0,00001

0,0001

0,001

0,01

0,1

1

Li Sc Ti V CrCoRb Sr Y ZrNbCs Ba LaCe Pr NdSmEuGdTbDyHo ErTmYbLu Hf Ta Pb Th U

1 ppb

NIST 61250 µm - 2.8 mW

In He ablationLaser frequency: 10Hz

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-40%

-30%

-20%

-10%

0%

10%

20%

30%

40%

Sc V Cr Rb Sr Y Zr Nb Ba La Ce Pr NdSmEu Gd Tb DyHo Er TmYb Lu Hf Ta Pb Th U

In He ablationLaser frequency: 10HzLaser Power 1.0 mW NIST 612 external standard44Ca internal standard

Precision and accuracy at 40 Precision and accuracy at 40 µµm spot sizem spot size

USGS standard BCR-2 (basalt glass)40 analyses in one day

Precision 1 x R.S.D.Accuracy

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0,1

1

10

100

La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu

Calcite/C1CaCO3

Determinazioni elementari su fasi mineralogiche

Anfibolo – Clinopirosseno –Ortopirosseno – Titanite – Calcite –Ossidi – Plagioclasio…..

100

1000

10000

La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er TmYb Lu

Titanite/C1CaTiOSiO4

0,01

0,1

1

10

100

1000

10000

100000

RbSr Y Zr NbCsBaLa Ce Pr NdSmEuGdTbDyHoEr TmYbLuHfTa PbTh U

Zircone/C1

ZrSiO4

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Reperti ossei di età romana

0,01

0,1

1

10

100

1000

Li Sc Ti V Cr Co Rb Sr Y Zr Nb Cs Ba La Ce Pr NdSmPb Th U

ppm

Osso UmanoOsso di CavalloOsso di Cane

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Quercia centenaria del Parco del Ticino abbattuta nel 2001Quercia centenaria del Parco del Ticino abbattuta nel 2001

Determinazioni elementari su matrici di Determinazioni elementari su matrici di interesse ambientaleinteresse ambientale

1 spot di 60 µm a cerchio di crescita 18802000

Assenza di standard interno – tutti elementi rapportati al Mg

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Pb

0,0100

0,1000

1,0000

1880

1890

1900

1910

1920

1930

1940

1950

1960

1970

1980

1990

2000

norm

aliz

zato

a 25

Mg

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V

0,0001

0,0010

0,0100

0,1000

1,0000

norm

aliz

zato

a 25

Mg

1970

1920

1930

1940

1950

1960

1990

2000

1880

1890

1900

1910

1980

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Rb

0,0010

0,0100

0,1000

1,0000

10,0000

norm

aliz

zato

a 25

Mg

1880

1890

1900

1910

1920

1930

1940

1950

1960

1970

1980

1990

2000


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