Agilent ICP-MS Series 7700 BasicsProduct OverviewApplications

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General scheme for a ICP MS

MS – mass spectrometer• Quadrupole analyzer

– Separates iosn– Information about element isotopes

ICP-MS, inorganic analyzer

ICP – Inductively coupled plasma• Ion source

– Matrix suppresion, ion generation

Be0.08

H

Li0.19

Mg0.27

Na3.3

K1100

Rb0.12

Y0.01

LA

RdFr

Cs0.06

Ba0.22

AC

Ca48

Sr0.04

Sc0.67

Co0.14

Ni1.57

Ru0.11

Fe9.2

Ir0.09

Pt0.09

Au0.17

Rh0.04

Pd0.11

Ag0.08

Zr0.04

Tc0.12

Cr0.99

Mn0.66

Nb0.04

Ti1.9

Hf0.05

Ta0.04

W0.13

Re0.04

Os0.29

Cu0.41

V014

Mo0.12

Al0.71

B2.9

C N O F

Rn

Xe

Kr

Ar

Ne

I2.02

Zn1.02

Ga0.07

Ge1.13

As0.41

Br34.8

Si800

S20*

Cl4.6*

Pb0.16

Po At

In0.03

Sn0.24

Cd0.08

Tl0.08

Sb0.08

Te1.08

Hg0.18

P114

Se6.4

Bi0.03

Lu0.02

LrPa NoEs

Ho0.01

Fm

Er0.04

Md

Tm0.01

Eu0.02

Cm

Gd0.05

Bk

Tb0.01

Cf

Dy0.07

Pm

Np

Sm0.06

Pu Am

Pr0.01

U0.02

Nd0.05

Ce0.02

Th0.03

Yb0.05

ICP-MS Agilent 7700x – Detection Limits en ng/L

La0.01

Ac

He< à 0.1 ng/L

0.10 à 1.0 ng/L

1.0 à 10 ng/L

> à 10 ng/L

Standard nebulizer, Mode He ou NoGasintegration time 3 sec/masse, n = 10 et 3 sigma

* S and Cl : LD en µg/L

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Tokyo Analytical Division (TAD)

300 Employees

Focus on Innovation and highest possible build quality

Accredited ISO 9001, ISO 14001 manufacturing facility

Worldwide R&D and Production of Agilent ICP-MS

Products for worldwide shipment Agilent ICP-MS mainframe Agilent ICP-MS Software Agilent ICP-MS peripherals

Tokyo

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1987 – PMS 100 introduced – First computer-controlled ICP-MS1988 – PMS 200 introduced – Second generation ICP-MS with off-axis Qpole lens1989 – 1st ETV accessory for semicon analysis by ICP-MS1990 – PMS 2000 introduced – Omega off-axis lens. Lowest random background ICP-MS1992 – ShieldTorch interface developed - Ar interferences virtually eliminated in cool

plasma, enabling ppt analysis of K, Ca, Fe by ICP-MS1994 – 4500 Series introduced - World's first benchtop system. Hyperbolic profile quad,

motorized torch XYZ, cool plasma1998 – First real time ICP-MS chromatographic software – PlasmaChrom. T-mode

reaction interface introduced1999 – 4500 Series 100, 200 & 300 introduced: 1st applications-specific ICP-MS.2000 – Agilent 7500 Series introduced - 7500a, 7500i and 7500s - the next generation in

ICP-MS instrumentation. 9 orders detector range2001 – Agilent 7500c launched – 1st generation ORS for high matrix samples. 2002 – New digital generators and LAN control introduced. First commercial GC-ICP-MS

interface. 2003 – Agilent 7500cs launched – 2nd generation ORS for high purity semicon samples. 2004 – Agilent 7500ce launched – 2nd generation ORS for high matrix samples. 2005 – Low flow cell gas MFC’s for Xe NH3, O2, etc added to 7500ce/cs. 2006 – Agilent acquires 100% of Agilent/Yokogawa joint venture 2007 – Agilent 7500cx introduced: He only mode ICP-MS2008 – High Matrix Interface developed – enables 2% TDS samples to be run by ICP-MS2009 – Agilent 7700 Series introduced – replaces 7500 Series. MassHunter Software

introduced - common platform with other Agilent MS. ISIS-DS Discrete sampling system, for ultra high throughput analysis

Agilent 4500 Series

Agilent’s History of Innovation in ICP-MS – 1987 to 2009

ShieldTorch System

Agilent 7700 Series

Octopole Reaction

System

Agilent 7500 Series

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Inorg. Analysis Techniques in a Typical Laboratory ICP-OES – for majors and high matrix samples

Multi-element, ~2 min/ sample

10’s ppb to 1000’s ppm

Few Elements/Samples

ppt

ICP-MS – for trace elements and clean samplesMulti-element, ~4min/ sample

Single ppt to 10’s ppm

GFAASSingle

element, ~6min/ sample

10’s ppt to 100’s ppb

Many Elements/Samples

%

ppm

ppbHydride/AFSFew elements, ~2min/ sample

Single ppt to 10’s ppb

LOD

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Inorganic Analysis Techniques in a Typical Laboratory

ICP-OES

Multi-element, ~2 min/ sample

10’s ppb to 1000’s ppm

Few Elements/Samples

ppt

ICP-MS – for trace elements and clean samplesMulti-element, ~4min/ sample

Single ppt to 10’s ppm

GFAASSingle

element, ~6min/ sample

10’s ppt to 100’s ppb

Many Elements/Samples

%

ppm

ppbHydride/AFSFew elements,

~2min/ sample

Single ppt to 10’s ppb

LOD

7700 ICP-MSMulti-element

Single cell gas mode and productivity tools reduce run timeHMI for samples with % level solids

Single ppt (incl. hydride and Hg) to 100’s ppm (1000’s ppm with HMI)

Uniquely, the Agilent 7700 can replace all these separate techniques, providing high

throughput, matrix tolerance, wide elemental coverage and low LODs in

a single run

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• Enviro is by far the biggest market for ICP-MS (includes everything from contaminated soil to drinking water!)

• Other key application areas for ICP-MS are:– Foods– Pharma– Biomedical– Academic/research

• (academic comprises geo, metallomics, enviro, foods; emphasis on speciation)

• Agilent is leading supplier of coupled systems (HPLC, GC or CE with ICP-MS as detector) for chromatography

Who Uses ICP-MS?

ICP-MS Market by Industry (estimated)

ACADEMIC7.7%

BIOMEDICAL4.6%

CHEMICAL2.8%

CONSUMER PRODS1.0%

ENVIRO47.2%

FOODS7.2%

FORENSIC1.5%

GEOLOGICAL1.0%

METALS0.5%

NUCLEAR3.4%

PETROCHEMICAL2.8%

PHARMACEUTICAL5.4%

PROTEOMICS0.3%

SEMICON14.3%

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Agilent ICP-MS Family - Comparison

7700x with optional ISIS

7700x

• High productivity system• High Matrix Interface • Environmental, food,

clinical, pharmaceutical, speciation and general purpose applications

7700s

• Clean room ready• Cool plasma• Mineral acids, silicon

matrices, organics, DIW, process chemicals

7700e

• Easy operation• He collision• Expandable

7700e

7700s with Integrated Autosampler

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7700x – The Three Key Performance Benefits

1. Matrix Tolerance – Sample Intro/Plasma/HMI

2. Interference Removal – He Mode

3. Dynamic Range – 9 Orders at the Detector

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Matrix Tolerance

7700 Plasma is the Hottest of Any ICP-MS

(even without HMI!)

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Matrix Tolerance - Comparison of Plasma Loading/Cooling

High sample load, narrow central channel poor matrix decomposition

Low sample load, wide central channel good matrix decomposition

Conventional ICP-MS0.5 - 1.0mL/min, 1.8-2.0 mm Injector, no water vapour removal Low central channel temperature

Optimized ICP-MS – 7700x0.10 - 0.25mL/min, 2.5mm Injector, water vapour removed High central channel temperature

ICP-MS plasma produces ions

Needs a high plasma temperature

Sample introduction must be designed to maintain high plasma temperature

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Lower CeO+/Ce+ ratio (from 3.0% to 1.0%, 3x reduction) removes ~70% of many matrix-based interferences (ArCl+, ClO+, CaO+, etc)

Hotter plasma is less affected by a variable matrix (more robust)

Better matrix decomposition reduces interface and lens contamination and therefore reduces maintenance

Hotter plasma improves the ionization of poorly ionized elements, so MUCH lower DLs possible for Be (right), B, As, Se, Cd, Hg (below), etc

Other Benefits of High Plasma Temp.

Sub ppt Be detection

limit!

10ppt

5ppt

30ppt

Hg BEC (ppt) DL (ppt)

201 9.49 1.51Be BEC (ppt) DL (ppt)9 0.465 0.235

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Interference Removal

He mode on the 7700 ORS3 still can’t be

matched by any other ICP-MS

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All New Octopole Reaction System (ORS3)

The 7700 uses a completely new collision/ reaction cell, with:• 18% longer rods• 15% smaller IDand operates at• 16% higher pressure• 20% higher frequency

ORS3 also operates with a much larger energy discrimination step.Result is much more effective removal of interferences in He mode with KED

Major improvement compared to 7500 Series, which already offered by far the best He mode performance of any ICP-MS

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Polyatomic Interferences in Complex Matrices

Some manufacturers claim that ICP-MS has only a few interferences, and that reaction gases can be used to remove them.That’s true in a simple sample, but in a complex sample there are many interferences, and no reaction gas can remove all of them

But He mode on the 7700 can!!

Isotope Principal Interfering Species (mixed matrix)45Sc 13C16O2, 12C16O2H, 44CaH, 32S12CH, 32S13C, 33S12C47Ti 31P16O, 46CaH, 35Cl12C, 32S14NH, 33S14N49Ti 31P18O, 48CaH, 35Cl14N, 37Cl12C, 32S16OH, 33S16O50Ti 34S16O, 32S18O, 35Cl14NH, 37Cl12CH51V 35Cl16O, 37Cl14N, 34S16OH52Cr 36Ar16O, 40Ar12C, 35Cl16OH, 37Cl14NH, 34S18O53Cr 36Ar16OH, 40Ar13C, 37Cl16O, 35Cl18O, 40Ar12CH54Fe 40Ar14N, 40Ca14N, 23Na31P55Mn 37Cl18O, 23Na32S, 23Na31PH56Fe 40Ar16O, 40Ca16O57Fe 40Ar16OH, 40Ca16OH58Ni 40Ar18O, 40Ca18O, 23Na35Cl59Co 40Ar18OH, 43Ca16O, 23Na35ClH60Ni 44Ca16O, 23Na37Cl61Ni 44Ca16OH, 38Ar23Na, 23Na37ClH63Cu 40Ar23Na, 12C16O35Cl, 12C14N37Cl, 31P32S, 31P16O264Zn 32S16O2, 32S2, 36Ar12C16O, 38Ar12C14N, 48Ca16O65Cu 32S16O2H, 32S2H, 14N16O35Cl, 48Ca16OH66Zn 34S16O2, 32S34S, 33S2, 48Ca18O67Zn 32S34SH, 33S2H, 48Ca18OH, 14N16O37Cl, 16O2

35Cl68Zn 32S18O2, 34S269Ga 32S18O2H, 34S2H, 16O2

37Cl70Zn 34S18O2, 35Cl271Ga 34S18O2H, 35Cl2H, 40Ar31P72Ge 40Ar32S, 35Cl37Cl, 40Ar16O273Ge 40Ar32SH, 40Ar33S, 35Cl37ClH, 40Ar16O2H74Ge 40Ar34S, 37Cl275As 40Ar34SH, 40Ar 35Cl, 40Ca 35Cl, 37Cl2H77Se 40Ar 37Cl, 40Ca 37Cl78Se 40Ar 38Ar80Se 40Ar2, 40Ca2, 40Ar40Ca, 32S2

16O, 32S16O3

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Helium interactions in an Octopole Reaction CellCollision: Energy discrimination

He

Collision

Ar

Cl

Ar

Cl

As

As

Electrical potential (Octopole)

Reaction cell

Electrical potential (Q-pole)

Molecular interference(ArCl) has larger cross section than the analyte (As).

↓More frequent interactions with He.

↓A significant reduction in kinetic energy relative to the analyte (As). Energy filtering can be used to ensure only the analyteenters the quadrupole analyzer.

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2E5cps

45 50 55 60 65 70 75 80Mass

Blank Acid Matrices and IPA in No Gas Mode

No Gas Mode

Unspiked 5% HNO3 + 5% HCl + 1% H2SO4 + 1% IPA MatrixUnspiked Matrix – ALL peaks are due to polyatomic interferences

Multiple polyatomic interferences affect almost every mass – Interferences are matrix-dependent

Color of spectrum indicates which matrix gave each interfering peak

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45 50 55 60 65 70 75 80Mass

2E5cps

He Mode

ALL polyatomic interferences are removed in He Mode

Unspiked 5% HNO3 + 5% HCl + 1% H2SO4 + 1% IPA MatrixALL polyatomic interferences are removed in He Mode (same cell conditions)

Blank Acid Matrices and IPA in He Mode

Color of spectrum indicates which matrix gave each interfering peak

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2E5cps

45 50 55 60 65 70 75 80Mass

Blank Acid Matrices and IPA in No Gas Mode

No Gas Mode

Unspiked 5% HNO3 + 5% HCl + 1% H2SO4 + 1% IPA MatrixUnspiked Matrix – ALL peaks are due to polyatomic interferences

What will happen with a reactive gas like Hydrogen?

Color of spectrum indicates which matrix gave each interfering peak

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SO, SOH

S2, SO2, S2H, SO2H

ClO, ClOHCO2H

Cl2

2E5cps

45 50 55 60 65 70 75 80MassH2 Mode

SO, SOH

S2, SO2, S2H, SO2H

ClO, ClOHCO2H

Cl2

Many polyatomic interferences remain (or new ones are created) in Reaction (H2) Mode.Interferences are different in each matrix!

Reaction mode is used on ALL other ICP-MS

Unspiked 5% HNO3 + 5% HCl + 1% H2SO4 + 1% IPA MatrixMany polyatomic interferences can still be seen in H2 Mode

Blank Acid Matrices and IPA in H2 (Reaction) Mode

Color of spectrum indicates which matrix gave each interfering peak

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45 50 55 60 65 70 75 80Mass

2E5cps

He Mode

We go back to He Mode and will add a 10 ppb spike

Unspiked 5% HNO3 + 5% HCl + 1% H2SO4 + 1% IPA MatrixALL polyatomic interferences are removed in He Mode (same cell conditions)

Blank Acid Matrices and IPA in He Mode

Color of spectrum indicates which matrix gave each interfering peak

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2E5cps

45 50 55 60 65 70 75 80Mass

10ppb Spike in 5% HNO3 + 5% HCl + 1% H2SO4 + 1% IPA MatrixConsistent high sensitivity for all isotopes of all elements in He Mode

Matrix Mix with Spike (10ppb) in He Mode

He Mode

Good signal for all spike elements at 10ppb Spike. Perfect template fit for all elements – no residual interferences and no loss of analyte signal by reaction

Consistent sensitivity and perfect template match for all elements

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Dynamic Range

9 orders dynamic range of the 7700 detector is really

available

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Detector range comparison: The entire green-shaded area is within the measurement range of the 7700 Series detector, but 90% of these concentrations would be over-range on other detectors, requiring manual signal attenuation or dilution for these concentrations to be measured on other ICP-MS instruments.

1) 7700 Series detector – 9 orders dynamic range, from 0 to 500ppm

2) Typical ICP-MS detector – 8 orders dynamic range, from 0 to 50ppm

3) Older, pulse-count only detector – 6 orders dynamic range, from 0 to 0.5ppm

7700 – 9 Orders Detector Dynamic Range

Original ICP-MS pulse-count detectors gave 6 ordersdynamic range (up to 2Mcps) Analog mode on other ICP-MS typically gives total of 8 ordersdynamic range (up to 400Mcps), equivalent to about 50ppmHigher than this, need different interface or different tuning

Agilent 7700 Series detector has 9 orders dynamic range in analog mode – up to 4,000Mcps or around 500ppmUpper range is even higher for mineral elements in He mode, as low-mass signal is reduced when cell is pressurized.

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78 Se [ 3 ]

Conc(ppt)

0.0 100.0 200.0 300.0

CP

S

1x10

0

2

4

y = 0.1757 * x + 0.8000R = 0.9993

DL = 5.915 ppt

BEC = 4.553 ppt

7700x – Largest Analytical Range of any ICP-MS

Calibration rangesHg (10 – 200ppt) – NoGas ModeAs (10 – 200 ppt) – He ModeSe (10 – 200 ppt) – He ModeNa (0.05 – 1000 ppm) – He Mode

Overall calibration range 10ppt (Hg, As) to 1000 ppm (Na) in a single method - without manual attenuation of sensitivity to increase range

NaTypically, ICP-MS cannot measure above 200ppm Na without changing interface, quad resolution or ion lens settings

HgHg LOD on 7700x is about 2ppt –7700x can QUANTITATE at 10ppt!

7700x can do both of the above in the same run!

1000ppm Sodium

AsHg

Na

10 ppt Mercury

These 4 plots were obtained under the same analytical conditions on the 7700x – only the gas mode (no gas for Hg) changed

As

10 ppt Arsenic

Se

20 ppt Selenium

Good fit at 0.2ppm

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Application of the 7700 ICP MS to the foodanalysis

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Analysis of “Metals” in Food by ICP-MSWide Range of Food Matrices• Dairy, Meat, Fish, Grain, Vegetables, Fruit, etc• Processed goods

– Canned, frozen, dried and preserved food– Drinks (soda, tea, coffee etc.)– Preservatives, “fillers” and additives such as calcium carbonate

• “Nutraceuticals”

In order to measure all elements, MULTIPLE techniques have been required

• ICP-OES for majors, GFAAS for Cd & Pb; CV/AFS (or HGAAS) for Hg– Other elements such as As, Se, etc. must also be monitored (Hydride AAS)

• Disadvantages of multiple instruments– Lab cost increases– Capital expense on instruments– Staffing costs– Slows turnaround time

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Which Elements are Monitored in Foods?1. Toxic trace elements

As, Cd, Hg, Pb, Tl, Cr(VI) - low level analysis (ppt to ppb)

2. Common elements that are toxic in excessAl, Ni, Cu, Zn, Se, Mo, Sn, etc.

3. Essential minerals at high levels (100ppb to 1000ppm)Na, Mg, P, S, K, Ca, Fe

4. Essential elements at low levels (100ppt to 10ppb)V, Cr(III), Co, Se, I

5. Screening (semi-quant) analysisICP-MS can measure almost every element at ng/L levels and is virtually free from interferences – ideal screening tool

6. For some elements, chemical form may determine toxicity/availabilityChromatographic separation before ICP-MS analysis

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Analysis of Food CRM Digests Using Agilent 7700 with He Mode Only (single mode)Single sample preparation is required•Food CRMs microwave digested with 6ml HNO3 + 2ml H2O2

•Final volume 100 mL

Single analysis by 7700x ICP-MS for all the analytes!

Full mass range scan of food digest (e.g. microwave digestion)

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Putting All Together the advantages of the 7700xsimple, one cell gas, interference-free ICP-MS for real world sample analysis

One Configuration (standard –

robust plasma conditions)

One gas mode* (helium

collision)

One method for waters,

soils, wastes, food…

28 elements in less than 3.5 minutes per

run

* Plus no gas mode for non-interfered elements

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Method Detection Limits - 3σ (n = 10)in Parts Per Billion (in 1% HNO3/0.5% HCl)

•All elements except low mass non-interfered elements were run in helium mode•Low mass, non-interfered elements run in no gas mode

•No correction equations used

Element Mass MDL (ppb) Cell mode Element Mass MDL

(ppb) Cell mode

Be 9 0.005 No gas Zn 66 0.014 HeB 11 0.005 No gas As 75 0.011 He

Na 23 0.058 No gas Se 78 0.017 HeMg 24 0.002 No gas Sr 88 0.002 HeAl 27 0.007 No gas Mo 95 0.006 HeK 39 0.076 He Ag 107 0.002 HeCa 44 0.090 No gas Cd 111 0.002 HeV 51 0.014 He Sb 121 0.006 HeCr 52 0.004 He Ba 137 0.005 HeMn 55 0.008 He Hg 202 0.001 HeFe 56 0.014 He Tl 205 0.002 HeCo 59 0.004 He Pb 208 0.001 HeNi 60 0.014 He Th 232 0.001 HeCu 63 0.002 He U 238 0.001 He

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Excellent Linear Range for 56Fe in He Mode at 50x the Upper Calibration Limit – reduced need for reruns due to over range samples

Fe Calibration on left up to 10 ppm

500 ppm linear range sample

measured against curve on right resulted in 518 ppm (104%

recovery)

104% recovery

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Na, Ca, Mg measured at 50x the Upper Calibration Level (500 ppm each)

97.8% recovery

108% recovery

106.5% recovery

Wide linear dynamic range permits accurate quantification far beyond calibration range

-minimizes need for extremely high calibration levels-reduces need for dilution and re-analysis of over range samples

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Recoveries of Certified Values – Food CRMsin Helium Mode Only

NRC-CNRC DORM3 Fish Protein

NIST SRM 2976Mussel Tissue

NIST RM 8415 Whole Egg Powder

Certified value (mg/kg)

Recovery (%)

Certified value (mg/kg)

Recovery (%)

Certified value (mg/kg)

Recovery (%)

23 Na - - - - 3770 101.0

43 Ca - - - - 2480 109.7

52 Cr - - - - 0.37 93.0

55 Mn - - - - 1.78 91.9

56 Fe 347 93.4 171 92.7 - -

60 Ni 1.28 100.8 - - - -

63 Cu 15.5 92.6 4.02 82.6 2.7 96.5

66 Zn 51.3 89.4 137 88.4 - -

75 As 6.88 89.5 13.3 94.5 - -

78 Se - - 1.8 104.3 1.39 89.7

95 Mo - - - - 0.247 87.2

111 Cd 0.29 95.4 0.82 96.8 - -

202 Hg 0.382 101.4 0.061 112.0 - -

208 Pb 0.395 100.8 1.19 97.8 0.061 91.0

Recoveries include both

extraction efficiency by microwave

digestion and analytical accuracy

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Chromatographic Applications of ICP-MS: Speciation analysis

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Chemical forms of trace elements

Inorganic Organometalliccompounds

Biomolecules Complexed with humic substances

Cr(III) vs Cr(VI)ToxicEssential

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Chromatographic ApplicationsSimple link to Agilent LCDirect sequence control from ICP-MS sample log tableMethod setup for LC/GC from ICP-MS PC

Predefined application packs available, as for 7500Data Analysis software now integrated into main suiteSame service support for all units

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Speciation with LC-ICP-MS and GC-ICP-MSEmerging elements/compounds:

• Pesticide and OP nerve agent residues• PBDEs• Nanoparticles

As Speciation using LC-ICP-MSAgilent Application Note: Routine Analysis of Toxic Arsenic Species in Urine Using HPLC with ICP-MS, 5989-5505EN, by TetsushiSakai and Steven Wilbur,

Agilent Technologies

Conventional “organo-metallic” compounds:• Inorganic vs organic arsenic• Organo-tin• Methyl-mercury, etc

Application Examples

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Agilent Restricted1 : Sn(Ⅳ), 2 : MBT, 3 :TPrT (IS), 4 : DBT,5 : MPhT, 6 : TBT, 7 : DPhT, 8 : TPhT

concentration : 5ug/l (5pg) as metal

Chromatogram of Mixed Organotin Standards (Ethylated)

3 Sigma Detection Limit

MBT 4.4fg

TPrT 5.3fg

DBT 9.4fg

MPhT 44fg

TBT 9.9fg

DPhT 10fg

TPhT 11fg

Injection volume 1uL

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Summary

• The Agilent ICP-MS exceeds the tough sampling demands of the laboratory– The robust sample introduction system handles waters or digested

food samples easily• Without causing cone clogging, loose of sensitivity, matrix effects…

• The Agilent ICP-MS provides multielement measurement with unsurpassed management of interferences– The ORS offers a simple method of eliminating troublesome molecular

species• Without compromising detection limits

• The Agilent ICP-MS has the widest dynamic range of any commercial ICP-MS– 9 linear orders allows measurements at ppt and 100’s ppm in the

same acquisition• Improving productivity

Assessing the effectiveness of ICP-MS in the water and food analysis

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