X Series ICP-MS Training Course Introduction to ICP-MS theory and X Series ICP-MS PlasmaLab...

X Series ICP-MS Training Course

• Introduction to ICP-MS theory and X Series ICP-MS

• PlasmaLab• Analytical Method

Development• Dealing with

interferences

Application areas

Metals / Industrial

Analysis of major, minor and trace elements

Purity of fine metals

Solution Analysis via nebulisation

Solids Analysis via Laser Ablation

Reagents required:

40% v/v/ Primar Nitric acid and deionised water

No sample preparation required. Bulk or feature analysis can be performed on metals.

Nuclear

Fuel quality certification

Environmental and bioassay monitoring of low level actinides

Precise and accurate isotope ratio measurementSignal to noise ratio needs

to be maximized for ppq & sub ppq LOD’s. Use of high efficiency nebulisers.

For waste minimization use of low flow nebulisers, e.g. PFA-50

Semiconductor

Determination of low levels of impurities in ultra-pure process reagents

Impurity analysis of wafers

Transition metals suffer from Argon oxide and Argon nitride interferences, which are greatly reduced with the PlasmaScreen Plus and CCT options.

Use ultra-clean glassware, cones etc.

Recommended Accessories: USN and PFA-50, if low sample volume

Biological & Clinical

Speciation of metals

Elemental uptake and excretion studies

Stable isotope tracer studies

Analysis of salvia, serum, blood and urine

CCT technique recommended to overcome interferences on key elements such as Cr, Fe, As, Se in heavy biological matrices

Geological

Rocks, sediments and soils

Direct solid analysis using Laser Ablation on:

Individual minerals, thin section, isotope ratios, zonation studies, depth profiling.

Oxide interferences within REE

e.g. BaO on 151Eu and 153Eu, NdO on 150Tb, 160Gd and 162Dy.

Residual HClO4 or saline matrices will interfere with Cr,V and As(ClO & ArCl interferences).

Environmental

Analysis of drinking and waste water

Seawater and marine life (shellfish, corals etc.)

Analysis of industrial effluents

Soil/sediment studiesTransition metals suffer from Argon oxide and Argon nitride interferences, which are greatly reduced with the CCT option.

Reagents required

40% v/v Primar Nitric acid and deionised water

Sample dried into a digest ‘bomb’, if required.

Minimising contamination

• Laboratory environment• Water quality• Ultrapure reagents

Handling of ultrapure reagents

• Selection of material for containers & cleaning procedures

• Sample and standard preparation

Tracing sources of contamination

The Step-by-Step Approach

• Instrument blank

• Water blank

• Dilute acid blank

• Analysis blank

Causes of interferences

Interferences – mass spectroscopic

Interferences – non mass spectroscopic

ELEMENTI ISOTOPI in ICP-MS

Isotopi : Atomi dello stesso elemento con differenti masse (stesso numero di protoni & elettroni ma diverso numero di neutroni)

50 4.34552 83.78953 9.50154 2.365

Mass : 55,9116

Mass : 52,0554

Isobaric Interference

Mass 54

Isotope for FeIsotope for Cr

Mass Abundance 54 5.80056 91.72057 2.2058 0.280

Isotopes for Iron

Isotopes for Chromium

Cr

Fe

INTERFERENZE

Le interferenze Molecolari e Isobariche vengono classificate come interferenze spettroscopiche

- Interferenze Molecolari (poliatomiche): sono Ossidi ed Idruri, Specie poliatomiche

Gli ossidi possono essere minimizzati attraverso il tuning, gli idruri mediante sistemi per l’abbattimento delle interferenze (CCT)

-Interferenze Isobariche: questo tipo di interferenze sono dovute alla sovrapposizione di diversi isotopi

Interferences

SpectrometerLenses(CCT)

Ar +, N +, O +, N 2+, O 2

+, Ar 2+, etc.

ArO + ,ClO + ,ArNa + etc.

Ar Ar + (0.1%)

Ar

diss .“metal”,H 20, HNO 3,HCI, etc.

dry “metal” or

metal-oxide, decomposing

anions

MetalAtoms

MetalIons (M +)

Conventional “Front-End” approaches toreduce interferences

“Analyzer approach” to reduce or resolve interferences

Mo > M + + e -

“Ionization potential”

ESEMPI DI INTERFERENZE SPETTROSCOPICHE

Interferenze poliatomiche Interferenzeda Ossidi, Idrossidi,

Idruri e doppie cariche

• Polyatomic peak overlaps Causes/sources : solvent

– Anions in sample– Cations in sample– Ar gas– Entrained air

• Signal suppression • Ionisation suppression or enhancement

Causes/sources : Overloading plasma– Overloading nebuliser– Cone orifice issues– Unintended plasma cooling effects

• Elemental peak (isobaric) overlaps Generally precludes the use of some

isotopes if overlap exists

Interferences

Analyte portion of total measured signal

Illustration of overlapping peaks

Total measured signal = analyte + polyatomic

Correction equations

Monoisotopic As in a Cl matrix

76 77 78 79 80 81 8275

Se(82)

ArAr40,40

ArAr38,40

ArAr36,40

ArCl40,37

Se77

ArCl40,35

As75

Therefore we can calculatethe contribution of ArCl at 77

Correction equations

76 77 78 79 80 81 8275

Se(82)

ArAr40,40

ArAr38,40

ArAr36,40

ArCl40,37

Se77

ArCl40,35

As75

Se(77) = Se(82) x AbSe(77)

AbSe(82)

ArCl(77) = Int(77) - Se(77)

ArCl(75) = ArCl(77) x Ab(ArCl(77)) Ab(ArCl(75))

As(75) = Int(75) - ArCl(75)

Monoisotopic As in a Cl matrix

Calculate 77Se contribution at mass 77 from 82Se

Calculate 77ArCl contribution at mass 77 from 77Se

Calculate ArCl contribution at mass 75 from 77ArCl

Calculate 75As contribution from 75ArCl

Instrument performance options

But the X Series ICP-MS, does supply a few ‘hardware’ remedies for these problems…..

• PlasmaScreenPlus - a)‘cool’ screen operation - analysis of Li, Na, K, Ca, Feb) ‘hot’ screen operation – enhances sensitivity while maintaining low background

• CCT - removal of polyatomics

• Xi – improves matrix tolerance and reduces polyatomics

Instrument performance options

Isotope Interferant Technique 6,7 Li Background CP 23Na Background CP 24Mg C 2 CCT 28Si N2 CCT 31P NOH CCT

56Fe ArO CP,CCT 39,40 K ArH, Ar CP,CCT 40Ca Ar CP,CCT 75As ArCl CCT 51V ClO CCT

52Cr ArC CCT 60Ni CaO Xi80Se Ar 2 CCT

PlasmaScreen Plus

• PlasmaScreenTM Torch

- Grounded metal screen inserted between torch and load coil

- Reliable automatic switching between ‘hot’ and ‘cool’ plasma conditions

• Cool screen conditions (~600 Watts)

- Minimizes argon-based interferences i.e. 38Ar1H+, 40Ar16O+, 40Ar2

+

- Minimizes high backgrounds associated with easily ionizable elements i.e. Li, Na

- ng/L LODs for Li, Na, Ca, K, Fe, Cr

• Hot screen operation

- Enhanced sensitivity

- Low background maintained

- Improved detection limits

COOL PLASMA

Caratteristiche

• RF a bassa potenza: 500-650w con nebulizzatore a flusso alto

• Temperatura del Plasma prossima a 2500-3000K

Vantaggi

• Permette di determinare in ICP-MS elementi come Ca, Mg, Fe, Na, K, Cr, V

Limitazioni

• Plasma non robusto: è necessario analizzare campioni nella medesima matrice

• Impossilità di analizzare elementi con alto potenziale di eccitazione/ionizazione ( As, Hg, Se)

CCT

HEXAPOLE RODS

SKIMMER CONE

EXTRACTION LENSSAMPLE CONE

• Operating the ion guide with a suitable collision/reaction gas (in CCT mode) Selective attenuation of polyatomic

interference ions

– 40Ar35Cl, 40Ar12C, 40Ar22+, 40Ar2H, 38Ar1H+,

40Ar16O+, 40Ar2+

• Innovative, user selectable CCT

• Plasma operated at normal power- Transmission of the analyte ions

remains largely unaffected

• Ability to switch to CCT mode within sample

CCT - ArAr

59Co+

ArAr+H2

He

He

59Co+

ArAr(neutral) + H2+

CCT – analysis of iron

10ppb Fe - CCT

Blank - CCT

• Based on a multipole ion guide contained in a cell into which the collision cell gases flow; cell is located between the interface and the quadrupole analyser

• Hexapole or octopole ion guides are used

Collision cell

Split-flow high-compression turbo pump

Cell Gas

1

Cell Gas

2

MFC 1MFC 2

Detector

COLLISION CELL

Rotary Pump

Plasma

Slide Valve

Quadrupole

Principi della tecnologia a cella di collisione

• Il fascio ionico viene iniettato in una cella pressurizzata

- Tradizionalmente vengono impiegate miscele He, H2 or a He/H2

• Gli ioni poliatomici collidono con il gas della celle e vengono dissociati nei loro componenti atomici, ioni etc.

- 38Ar1H+/39K, 40Ar+/40Ca, 40Ar12C+/52Cr, 40Ar23Na+/63Cu, 40Ar16O+/56Fe, 40Ar35Cl+/75As, 40Ar2+/80Se

• La trasmissione degli ioni analiti attraverso la cella non viene praticamante influenzata

• Le condizioni di plasma ad alta temperartura vengono mantenute

Ferro

ArgonOssigenoIdrogeno

ArO+ ArH2

H2O+

H2

H2

Fe+ Fe+

CCTED – Meccanismi possibili

• Meccanismi possibili Dissociazione collisionale?

–e.g. ArAr+ + He = Ar + Ar+ + He

Reazione chimica?–e.g. ArAr+ + H2 = ArH + ArH+

Trasferimento di carica?–e.g. ArAr+ + H = ArAr + H+

Ritardo collisioneale e successiva flitrazione in termini di energia delle specie?

–e.g. ArAr+* + He = ArAr+ + He*

Solving the problem of cell generated interferences

• Subsequent collisions of cell-generated ions cause them to lose kinetic energy

• These ions (and also plasma derived polyatomic ions), with their larger

collision cross section, lose more energy than the smaller analyte ions

• Can prevent these lower energy interfering ions from being detected by

using an energy barrier between the cell and the quadrupole analyser –

this is called (kinetic) energy discrimination (ED or KED)

+++

+

+

+

+

++

+

How is energy discrimination set up?

• Changing collision cell and quadrupole bias voltages provides a simple way to set up the required energy barrier

Polyatomic ions from plasma or cell reaction products have insufficient energy to pass through the energy discrimination barrier

Po

ten

tial

Position

Without ED

With ED

Potential Barrier

Collision CellLensesQuadrupole

-2V-9V

-18V-14V

Analyte Ion

Isobaric Polyatomic ion

Key

The power of energy discrimination (1)

• In environmental and clinical samples, containing Cl and Ca, 75As is interfered by 40Ar35Cl+ and to a lesser extent, 40Ca35Cl+

• Collision cells are effective for removing these interferences, however, if ED is not used, a large signal is still observed on 75As

• This signal does not match the 3:1 m/z 75 to m/z 77 ratio expected if the interference is Cl - related, so it must be another species

• If Ca is not present, the interference is not observed, so it must be related to Ca

Mass 75 = 17,000 cps

(Mass 77 = 2,000cps)

Scan of 100ppm Ca, collision cell without ED


• The interference is believed to be CaOH(H2O)+ or CaO(H3O)+, formed from collision, then reaction, between CaOH+ and H2O in the cell

• As the Ca-species forms in the cell it’s energy is immediately reduced relative to the As+ analyte ion; further collisions as it passes through the cell reduce the energy further

• Applying a few volts of ED results in elimination of the species

• As+ is still transmitted to the quadrupole and can be determined to low ppt levels

Mass 75 = 6 cps

Scan of 100ppm Ca, collision cell with 2V ED


1ppb 75As = 300 cps

Scan of 100ppm Ca + 1ppb As, collision cell with 2V ED

• The interference is believed to be CaOH(H2O)+ or CaO(H3O)+, formed from collision, then reaction, between CaOH+ and H2O in the cell

• As the Ca-species forms in the cell it’s energy is immediately reduced relative to the As+ analyte ion; further collisions as it passes through the cell reduce the energy further

• Applying a few volts of ED results in elimination of the species

• As+ is still transmitted to the quadrupole and can be determined to low ppt levels

1% HNO3 Blank

1ppb Fe

1ppb Fe

1% HNO3 Blank

Quadrupole – Standard Mode

Quadrupole – CCT Mode (H2/He)

Reduction of 40Ar16O+ and Ar2+ using the collision

cell

Quadrupole – Standard Mode

Quadrupole – CCT Mode (H2/He)

10ppb Se1% HNO3 Blank

10ppb Se

Collision cell ICP-MS Fe / Se calibration performance

80Se (40Ar2+ attenuated)

0.99994

4.0

14.2

3607

56Fe

1.0 Detection limit (3σ, n = 5) (ppt)

4.3 BEC (ppt)

0.99997Correlation coefficient

1648 Sensitivity (cps/ppb)

80SeParameter

56Fe (40Ar16O+ attenuated)

Sample matrix = 2% HNO3, 8% H2 in He collision gas used

Why use oxygen as a collision / reaction gas?

• Some interferences cannot be efficiently removed using 'standard' cell gases (e.g. He, H2, NH3)

• Some interfered analytes react (along with their

interferences), with certain cell gases (e.g. NH3)

– Lose analyte sensitivity; degrade detection limit

• Kinetic energy discrimination (KED) or bandpass

application sometimes not sufficiently effective

– Interference suppression results in too much sensitivity loss

– BEC's and detection limits not low enough for the analytical

requirement

XSeriesII – New Proof Data - 1

Fast Cd and Pb in whole blood analysis

• Blood reference materials measured; diluted 1:50 for analysis

• Standard addition calibration on one sample used to quantify other samples Unique ability for Thermo! Ideal approach for biomedical samples!

• Autosampler probe-to-wash-early function used to maximise throughput Unique for Thermo!

• Sample throughput = 51 per hour, or more than 400 per 8 hour day!

430 - 650499 ± 126 - 3933.3 ± 0.5Bio Rad 3

230 - 340

353 - 443

Reference 208Pb (ppb)

10.4 - 15.6

5.4 - 7.2

Reference 111Cd (ppb)

254 ± 212.5 ± 0.4Bio Rad 2

412 ± 136.2 ± 0.5Seronorm blood 2

Measured

208Pb (ppb)Measured

111Cd (ppb)Sample identity

111Cd

208Pb

XSeriesII – New Proof Data - 2

• Urine reference material diluted 1:20 with 1% (v/v) HNO3 for analysis; spike recovery (0.50 ppb Cd) performed on sample doped with Mo (5 ppm)

• Standard addition calibration on the sample used to quantify other

samples

• Samples run in standard and collision cell mode with O2 in the cell

O2 promotes MoO+ to higher Mo oxides; Cd does not react

Cd in urine in the presence of Mo (removing the MoO interference)

96Mo16O+

95Mo16O+

Mo interference

0.02

0.04

Detection limit3σ (ppb)

5.26

7.98

Conc. (ppb)

Standard mode Collision cell mode (O2)

Spiked Cd value (ppb)Isotope

0.05

0.03

Detection limit 3σ (ppb)

0.490.50113Cd

0.500.50111Cd

Conc. (ppb)

O2 in the cell completely removes the MoO interference!

Without O2 the interference is large

Detection of Pt in 10 ppm Hf solutions

• The problems: HfO+ and HfOH+ interferences on all Pt

isotopes (m/z 190 to 198)

m/z 190 and 198 interferences low

abundance but 190Pt very low abundance

(0.01%) and 198Pt also low (7.2%)

Must suppress HfO+ / HfOH+ interferences

on most abundant remaining Pt isotopes

(194Pt, 195Pt and 196Pt)

• The proposed solution: Use O2 as the collision gas, to promote

formation of higher Hf oxides / hydroxides

Pt less reactive with O2

HfO+, HfOH+ interferences, 10ppm Hf

179Hf16O+ = 3 Mcps

Pt isotopes, 12ppb Pt195Pt+ = 250 Kcps

Pt in 10 ppm Hf, standard mode and O2 data

9

5

7


467*

154*

281*

BEC (ppb)*

Standard mode Standard BEC / collision cell BEC

Collision cell mode (O2)#Hf interference

Isotope

0.054

0.006

0.003


122890.04180Hf16O+196Pt

171110.01179Hf16O+195Pt

165290.02178Hf16O+194Pt

BEC (ppb)

* estimated using the 198Pt (linear) calibration sensitivity # O2 flow rate = 2.7 mL/min, non-KED

195Pt standard mode 195Pt collision cell mode (O2)

Detection of Hg in 10 ppm W solutions

• The problems: WO+ and WOH+ interferences on all Hg

isotopes (m/z 196 to 204)

m/z 196 and 204 interferences low abundance, but 196Hg very low abundance (0.14%) and 204Hg also low (6.8%)

Also have 204Pb interference on 204Hg

Must suppress WO+ / WOH+ interferences on most abundant remaining Hg isotopes (198Hg, 199Hg, 200Hg, 201Hg and 202Hg)

• The proposed solution: Use O2 as the collision gas, to promote

formation of higher W oxides / hydroxides

Hg less reactive with O2

WO+, WOH+ interferences, 10ppm W

184W16O+ = 2.4 Mcps

Hg isotopes, 20ppb Hg200Hg+ = 140 Kcps

Hg in 10 ppm W, standard mode and O2 data

16700.020.24.2334*184W16O+200Hg

8130.030.31.0244*183W16O+199Hg

4.2

0.4

13


247*

12

640*

BEC (ppb)*


Collision cell mode (O2)#

W interference

Isotope

0.02

0.05

0.02


12350.2186W16O+202Hg

400.3184W16O1H+201Hg

32000.2182W16O+198Hg

BEC (ppb)

* estimated using the 201Hg (linear) calibration sensitivity # O2 flow rate = 3.4 mL/min, non-KED

200Hg standard mode 200Hg collision cell mode (O2)

Detection of Cu and Zn in 10 ppm Ti solutions

• The problems: TiO+ (and TiOH+) interferences on all Cu and

Zn isotopes (m/z 63 to 70)

m/z 68 and 70 interferences low abundance

but 70Zn also low (0.6%)

68Zn most useful in absence of collision cell

Must suppress TiO+ / TiOH+ interferences on

Cu and most abundant Zn isotopes

• The proposed solutions: Use O2 as the collision gas to try to promote

formation of higher Ti oxides / hydroxides

Compare with kinetic energy discrimination

(KED) approach, using H2/He collision gas

TiO+ interferences, 10ppm Ti

Cu / Zn isotopes, 10ppb Cu / Zn

47Ti16O+ = 13 Kcps 48Ti16O+ = 130 Kcps49Ti16O+ = 11 Kcps

63Cu+ = 85 Kcps64Zn+ = 68 Kcps65Cu+ = 42 Kcps

Cu, Zn in 10 ppm Ti, standard mode and O2 data

64Zn standard mode 64Zn collision cell mode (O2)

10.150.170.030.250Ti18O+68Zn

90.050.340.042.950Ti16O+66Zn

0.38

0.06

0.20


20.3

3.1

2.1

BEC (ppb)


Collision cell mode (O2)#Ti interference

Isotope

0.23

0.11

0.05


151.3548Ti16O+64Zn

170.1849Ti16O+65Cu

130.1647Ti16O+63Cu

BEC (ppb)

# O2 flow rate = 7.0 mL/min, non-KED

Cu, Zn in 10 ppm Ti, standard mode and H2/He KED data

64Zn standard mode 64Zn collision cell mode H2/He KED

10.130.250.030.250Ti18O+68Zn

120.020.250.042.950Ti16O+66Zn

0.38

0.06

0.20


20.3

3.1

2.1

BEC (ppb)

Standard mode Standard BEC / collision cell

BEC

Collision cell (KED) modeTi interference

Isotope

0.05

0.07

0.02


620.3348Ti16O+64Zn

220.1449Ti16O+65Cu

150.1447Ti16O+63Cu

BEC (ppb)

Data obtained using a 8% H2/He gas flow of 5.5 ml/min and a KED barrier of 3.5V

• 4 Standard Reference Waters were analyzed as ‘unknown’ samples over a 10-hour period

• Wide range of typical environmental analytes were measured - 30 analytes, 55 isotopes

• Several analytes had associated interference problems….

CCTED – Evaluation of Performance

Uptake

25s

Experimental - analytical profileA

naly

tes

Settle

Delay

30s

Settle

Delay

30s

Standard

Mode

3x18s reps

Wash

25s

Total Time Per Sample = 3 minutes, 45 seconds

Tim

e

Pro

file

V

Cr

NH3/He

3x1.6s reps

Li

Be

Na

Rb

Sr

Rb

Mo

Ag

Cd

Sn

Cs

Ba

Tl

Pb

U

Mg

Al

K

Ca

Cr

Fe

Mn

Ni

Cu

Zn

Ga

As

Se

H2/He

3x18s reps

Experimental - procedure

• Calibration: Blank 1ppb multi-element solution 10ppb multi-element solution

• 4 reference water samples analysed as QC checks 12 times over a period of 10 hours against 12 different calibrations

NIST 1640 diluted 1+9 and spiked to 2% HCl CNRC SLRS-2 spiked to 2% HCl CNRC SLRS-3 spiked to 2% HCl CNRC SLRS-4 diluted 1+1 and spiked to 2% HCl

• Detection limits calculated by running 10-replicate blank samples 12 times against 12 different calibrations

Results: stability in different measurement modes -10ppb standard

Long-Term Stability - 12 Hours

0.9

0.95

1

1.05

1.1

0 2 4 6 8 10 12

Time / Hours

No

rma

lise

d S

ign

al I

nte

ns

ity

206Pb NH3 Mode (0.6%)

207Pb H2 Mode (0.6%)

208Pb Std Mode (0.6%)

10ppb Solution

No internal

standard

correction

Each isotope measured in a different mode, switching from NH3 to H2 to Std mode in-sample

Stability of NIST 1640x10 - 10 Hours, 12 Different Calibrations

0

0.5

1

1.5

2

2.5

0 2 4 6 8 10

Time (Hours)

Co

nce

ntr

atio

n (

ug

/L)

51V NH3 Mode (1.5%)

80Se H2 Mode (1.7%)

111Cd Std Mode (0.3%)

Results: stability of real sample in different modes

Sample diluted 1+9 and spiked to 2% HCl

7Li 0.01 55Mn 0.01 77Se 0.1 114Cd 0.0039Be 0.003 56Fe 0.06 78Se 0.03 118Sn 0.0123Na 2 58Ni 0.02 80Se 0.03 120Sn 0.00924Mg 0.1 59Co 0.005 82Se 0.1 133Cs <0.00125Mg 0.3 60Ni 0.03 85Rb 0.004 138Ba 0.00727Al 0.2 63Cu 0.02 87Rb 0.008 140Ce <0.00140Ca 3 64Zn 0.05 88Sr 0.005 203Tl 0.00244Ca 1 65Cu 0.02 95Mo 0.007 205Tl 0.00151V 0.01 66Zn 0.05 98Mo 0.005 206Pb 0.0152Cr 0.2 69Ga 0.02 107Ag 0.009 207Pb 0.0153Cr 0.05 71Ga 0.005 109Ag 0.009 208Pb 0.00954Fe 1 75As 0.01 111Cd 0.002 238U <0.001

H2/He ModeNH3/He ModeStandard Mode

Results – Method detection limits (g/L)

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

1640x10 7Li 9Be 24Mg 51V 52Cr 55Mn 59Co 60Ni 65CuMeasured 4.96±0.03 3.40±0.02 579±4 1.30±0.02 3.58±0.05 11.89±0.09 2.02±0.02 2.67±0.02 8.39±0.07Reference 5.07 3.49 582 1.3 3.86 12.19 2.03 2.74 8.52

Recovery % 98 97 100 100 93 98 99 97 99

1640x10 66Zn 75As 80Se 85Rb 88Sr 107Ag 111Cd 138Ba 208PbMeasured 5.11±0.05 2.61±0.02 2.12±0.04 0.192±0.004 12.0±0.1 0.75±0.03 2.21±0.02 14.2±0.1 2.65±0.03Reference 5.32 2.66 2.2 0.200 12.4 0.762 2.28 14.8 2.79

Recovery % 96 98 97 96 97 98 97 96 95

Results – accuracy of reference samples

SLRS-2 27Al 40Ca 51V 55Mn 56Fe 60NiMeasured 87±3 5500±300 0.248±0.007 10.1±0.2 127±2 1.01±0.03Reference 84 5700 0.25 10.1 129 1.03

Recovery % 104 97 99 100 98 98

SLRS-2 65Cu 66Zn 75As 88Sr 138Ba 238UMeasured 2.96±0.05 3.42±0.06 0.78±0.03 28.1±0.4 13.5±0.1 0.0464±0.0005Reference 2.76 3.33 0.77 27 13.80 0.049

Recovery % 107 103 101 103 98 95

NH3/He ModeH2/He ModeStd Mode

All concentrations in g/L

n=12

Results – accuracy of reference samples

Accuracy of Analysis Summary Plot

y = 0.9664x

R2 = 1

0.001

0.01

0.1

1

10

100

1000

10000

0.001 0.01 0.1 1 10 100 1000 10000

Reference Values (ug/L)

Measu

red

Valu

es (

ug

/L)

Analysis of Seawater Reference Materials

• Direct analysis of seawater is challenging: Extreme matrix Severe interferences Ultra trace analyte concentrations

• Analysed against a matched external calibration

• H2/He KED CCT mode used for ALL analytes

• Rapid method (~3 min/sample)

• No gas switching required

• No instrument settings switching required

• Easy set-up

XSeriesII – New Proof Data (ppt)

Analyte Measured Known Rec% 100ppt Spike Rec% 51V 146.2 120 122 9452Cr 13.43 11 122 9855Mn 93.72 91.9 102 10256Fe 60.88 20.7 294 9859Co 1.923 1.1 175 10060Ni 25.09 25.3 99 10365Cu 33.03 29.7 111 9366Zn 9.898 10.2 97 11075As 162.2 127 128 9778Se 1.927 1.8 108 84

111Cd 1.686 2.3 73 107114Cd 2.55 2.3 111 99208Pb 1.291 0.8 161 99

NASS-5 1:10


Analyte Measured Known Rec% 100ppt Spike Rec%51V 139.5 118 118 10652Cr 14.36 14.4 100 9455Mn 282.1 278 101 10256Fe 119.7 71.3 168 10759Co 3.008 2.6 116 10960Ni 31.02 31.4 99 10865Cu 62.43 59.2 105 10466Zn 42.69 38.1 112 11075As 146.9 111 132 10478Se 8.874 - - 113

111Cd 2.318 2.6 89 98114Cd 2.186 2.6 84 99208Pb 1.69 0.98 172 91

CASS-4 1:10


Analyte Measured Known Rec% 500ppt Spike Rec%51V 581.5 514 113 9652Cr 39.61 36.6 108 10055Mn 323.5 322 100 10156Fe 161.8 113.6 142 10359Co 9.048 8.4 108 11160Ni 257.9 246 105 9865Cu 325.9 310 105 10166Zn 35.36 40.2 88 10375As 361.9 272 133 8978Se 23.91 - - 96

111Cd 9.736 9.6 101 100114Cd 9.642 9.6 100 101208Pb 2.275 1.8 126 96

SLEW-3 1:5

CCTED Evaluation of Performance - Summary

• Provides Ease of Set-up– Auto-tune, performance reports allow fully automated set-up and analysis

• Ultimate Flexibility– Single mode runs ( e.g.. Seawater example)

• Fast analysis

– Mode Switching runs • Ultimate Detection Limits

• Handles the most extreme matrices (seawater) to give interference free measurements on difficult analytes

• Retains excellent stability and accuracy

X Series ICP-MS Training Course Introduction to ICP-MS theory and X Series ICP-MS PlasmaLab...

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Transcript of X Series ICP-MS Training Course Introduction to ICP-MS theory and X Series ICP-MS PlasmaLab...