Agilent ICP-MS Series 7700

Basics Product Overview Applications

ICP-MS, inorganic analyzer

General scheme for a ICP MS

ICP Inductively coupled plasma

Ion source
Matrix suppresion, ion generation

MS mass spectrometer
Quadrupole analyzer
Separates iosn
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Information about element isotopes

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

H
Li
0.19

< 0.1 ng/L 0.10 1.0 ng/L

He
B
2.9

Be
0.08

1.0 10 ng/L > 10 ng/L

Standard nebulizer, Mode He ou NoGas integration time 3 sec/masse, n = 10 et 3 sigma * S and Cl : LD en g/L

C
Si
800

N
P
114

O
S
20*

F
Cl
4.6*

Ne Ar Kr Xe

Na Mg
3.3 0.27

Al
0.71

K
1100

Ca
48

Sc
0.67

Ti
1.9

V
014

Cr
0.99

Mn
0.66

Fe
9.2

Co
0.14

Ni
1.57

Cu
0.41

Zn
1.02

Ga Ge
0.07 1.13

As
0.41

Se
6.4

Br
34.8

Rb
0.12

Sr
0.04

Y
0.01

Zr
0.04

Nb Mo
0.04 0.12

Tc
0.12

Ru
0.11

Rh
0.04

Pd
0.11

Ag
0.08

Cd
0.08

In
0.03

Sn
0.24

Sb
0.08

Te
1.08

I
2.02

Cs
0.06

Ba
0.22

LA AC

Hf
0.05

Ta
0.04

W
0.13

Re
0.04

Os
0.29

Ir
0.09

Pt
0.09

Au
0.17

Hg
0.18

Tl
0.08

Pb
0.16

Bi
0.03

Po At Rn
Er Tm Yb Lu
0.02

Fr Rd

La
0.01

Ce
0.02

Pr
0.01

Nd Pm Sm Eu Gd Tb
0.05 0.06 0.02 0.05 0.01

Dy
0.07

Ho
0.01

0.04

0.01

0.05

Ac Th Pa
0.03

U
0.02

Np Pu Am Cm Bk Cf Es Fm Md No Lr

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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Agilents History of Innovation in ICP-MS 1987 to 2009

1987 PMS 100 introduced First computer-controlled ICP-MS 1988 PMS 200 introduced Second generation ICP-MS with off-axis Qpole lens 1989 1st ETV accessory for semicon analysis by ICP-MS 1990 PMS 2000 introduced Omega off-axis lens. Lowest random background ICP-MS 1992 ShieldTorch interface developed - Ar interferences virtually eliminated in cool plasma, enabling ppt analysis of K, Ca, Fe by ICP-MS 1994 4500 Series introduced - World's first benchtop system. Hyperbolic profile quad, motorized torch XYZ, cool plasma 1998 First real time ICP-MS chromatographic software PlasmaChrom. T-mode reaction interface introduced 1999 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 range 2001 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 MFCs 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-MS 2008 High Matrix Interface developed enables 2% TDS samples to be run by ICP-MS 2009 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 ShieldTorch System

Octopole Reaction System

Agilent 7500 Series

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Agilent 7700 Series

Inorg. Analysis Techniques in a Typical Laboratory

% ppm
ICP-OES for majors and high matrix samples
Multi-element, ~2 min/ sample 10s ppb to 1000s ppm

ICP-MS for trace elements and clean samples

Multi-element, ~4min/ sample Single ppt to 10s ppm

LOD ppb

GFAAS
Single element, ~6min/ sample 10s ppt to 100s ppb

Hydride/AFS
Few elements, ~2min/ sample Single ppt to 10s ppb

ppt Few Elements/Samples

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Many Elements/Samples

Inorganic Analysis Techniques in a Typical Laboratory

%
ICP-OES

7700 ICP-MS
Multi-element, Multi-element ~2 min/ sample 10s ppb to 1000s ppm ICP-MS for trace elements and clean samples Single cell gas mode and productivity tools reduce run time

ppm LOD ppb

Multi-element, ~4min/ sample HMI for samples with % level solids

Single ppt (incl. hydride and Hg) to 100s ppm (1000s ppm with HMI) GFAAS
Single element, ~6min/ sample 10s ppt to 100s ppb

Single ppt to 10s ppm

Hydride/AFS
Few elements, ~2min/ sample Single ppt to 10s ppb

ppt Few Elements/Samples

Uniquely, the Agilent 7700 can replace all these separate techniques, providing high throughput, matrix tolerance, wide elemental coverage and low LODs in a singleAgilent Restricted run Many Elements/Samples

Who Uses ICP-MS?

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
PROTEOMICS 0.3% PHARMACEUTICAL 5.4% PETROCHEMICAL 2.8% NUCLEAR 3.4% METALS 0.5% GEOLOGICAL 1.0% FORENSIC 1.5% FOODS 7.2% ENVIRO 47.2%

SEMICON 14.3%

ACADEMIC 7.7%

BIOMEDICAL 4.6% CHEMICAL 2.8% CONSUMER PRODS 1.0%

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ICP-MS Market by Industry (estimated)

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Agilent ICP-MS Family - Comparison

7700e
Easy operation He collision Expandable

7700e

7700x High productivity system High Matrix Interface Environmental, food, clinical, pharmaceutical, speciation and general purpose applications
7700x with optional ISIS

7700s
Clean room ready Cool plasma Mineral acids, silicon matrices, organics, DIW, process chemicals

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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

ICP-MS plasma produces ions Needs a high plasma temperature Sample introduction must be designed to maintain high plasma temperature

Conventional ICP-MS
0.5 - 1.0mL/min, 1.8-2.0 mm Injector, no water vapour removal Low central channel temperature

Optimized ICP-MS 7700x

0.10 - 0.25mL/min, 2.5mm Injector, water vapour removed High central channel temperature

Agilent Restricted High sample load, narrow central channel poor matrix decomposition
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Low sample load, wide central channel good matrix decomposition

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Other Benefits of High Plasma Temp.

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
Sub ppt Be detection limit!

30ppt

10ppt

Hg 201

BEC (ppt) 9.49

DL (ppt) 1.51

5ppt

Be 9

BEC (ppt) 0.465

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DL (ppt) 0.235

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Interference Removal

He mode on the 7700 ORS3 still cant 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 ID and 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 Agilent Restricted 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. Thats 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 45 Sc
47 49 13 31

Principal Interfering Species (mixed matrix) C16O2, 12C16O2H, 44CaH, 32S12CH, 32S13C, 33S12C

Ti Ti 50 Ti 51 V 52 Cr 53 Cr 54 Fe 55 Mn 56 Fe 57 Fe 58 Ni 59 Co 60 Ni 61 Ni 63 Cu
64 65 66 67 68 69 70 71 72 73 74 75 77

P16O, 46CaH, 35Cl12C, 32S14NH, 33S14N P18O, 48CaH, 35Cl14N, 37Cl12C, 32S16OH, 33S16O 34 16 S O, 32S18O, 35Cl14NH, 37Cl12CH 35 Cl16O, 37Cl14N, 34S16OH 36 Ar16O, 40Ar12C, 35Cl16OH, 37Cl14NH, 34S18O 36 Ar16OH, 40Ar13C, 37Cl16O, 35Cl18O, 40Ar12CH 40 Ar14N, 40Ca14N, 23Na31P 37 Cl18O, 23Na32S, 23Na31PH 40 Ar16O, 40Ca16O 40 Ar16OH, 40Ca16OH 40 Ar18O, 40Ca18O, 23Na35Cl 40 Ar18OH, 43Ca16O, 23Na35ClH 44 Ca16O, 23Na37Cl 44 Ca16OH, 38Ar23Na, 23Na37ClH 40 Ar23Na, 12C16O35Cl, 12C14N37Cl, 31P32S, 31P16O2
31 32 32 34 32

Zn Cu Zn Zn Zn Ga Zn Ga Ge Ge Ge As

S16O2, S O2, S SH, S O2,

18 18 18 18 34 16

32

S2, 36Ar12C16O, 38Ar12C14N, S2H,

34 14 33 48

48

Ca16O

S16O2H,

32

N16O35Cl,
48 18 18 14

48

Ca16OH

32

S S, S2H,

S2,

Ca O N16O37Cl, 16O235Cl

33 34

Ca OH, O237Cl Ar31P

32 32 34 34 40 40 40 40 40

S O2H, S O2,
32

S2 34

S2H, Cl2H,
37

16

35

Cl2
40 40

S O2H, Ar S, Ar S,
34 34 35

35

Cl Cl, Cl2

Ar16O2 Cl37ClH,
40

Ar32SH, 40Ar33S,
37

35

Ar16O2H Cl2H

Ar SH,

40

Ar 35Cl,

40

Ca 35Cl,

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Se 78 Se 80 Se

Ar 37Cl, 40Ca 37Cl 40 Ar 38Ar 40 Ar2, 40Ca2, 40Ar40Ca,

32

S2 16O,

32

S16O3

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Helium interactions in an Octopole Reaction Cell Collision: Energy discrimination

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 analyte enters the quadrupole analyzer.

As Ar
Cl

He Collision

As Electrical potential (Q-pole) Ar

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Reaction cell

Cl

Electrical potential (Octopole)

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Blank Acid Matrices and IPA in No Gas Mode

Color of spectrum indicates which matrix gave each interfering peak
2E5 cps Unspiked 5% HNO3 + 5% HCl + 1% H2SO4 + 1% IPA Matrix
Unspiked Matrix ALL peaks are due to polyatomic interferences

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

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45 No Gas Mode
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50

55

60 Mass 65

70

75

80

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Blank Acid Matrices and IPA in He Mode

Color of spectrum indicates which matrix gave each interfering peak
2E5 cps Unspiked 5% HNO3 + 5% HCl + 1% H2SO4 + 1% IPA Matrix
ALL polyatomic interferences are removed in He Mode (same cell conditions)

ALL polyatomic interferences are removed in He Mode

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45 He Mode
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50

55

60 Mass 65

70

75

80

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Blank Acid Matrices and IPA in No Gas Mode

Color of spectrum indicates which matrix gave each interfering peak
2E5 cps Unspiked 5% HNO3 + 5% HCl + 1% H2SO4 + 1% IPA Matrix
Unspiked Matrix ALL peaks are due to polyatomic interferences

What will happen with a reactive gas like Hydrogen?

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45 No Gas Mode
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50

55

60 Mass 65

70

75

80

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Blank Acid Matrices and IPA in H2 (Reaction) Mode

Color of spectrum indicates which matrix gave each interfering peak
2E5 cps Unspiked 5% HNO3 + 5% HCl + 1% H2SO4 + 1% IPA Matrix
Many polyatomic interferences can still be seen in H2 Mode 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

SO, SOH

CO2H

ClO, ClOH

S2, SO2, S2H, SO2H

Cl2
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45 H2 Mode
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50

55

60 Mass 65

70

75

80

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Blank Acid Matrices and IPA in He Mode

Color of spectrum indicates which matrix gave each interfering peak
2E5 cps Unspiked 5% HNO3 + 5% HCl + 1% H2SO4 + 1% IPA Matrix
ALL polyatomic interferences are removed in He Mode (same cell conditions)

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

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45 He Mode
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50

55

60 Mass 65

70

75

80

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Matrix Mix with Spike (10ppb) in He Mode

Consistent sensitivity and perfect template match for all elements
2E5 cps 10ppb Spike in 5% HNO3 + 5% HCl + 1% H2SO4 + 1% IPA Matrix
Consistent high sensitivity for all isotopes of all elements in 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

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45 He Mode
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50

55

60 Mass 65

70

75

80

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Dynamic Range

9 orders dynamic range of the 7700 detector is really available

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7700 9 Orders Detector Dynamic Range

Original ICP-MS pulse-count detectors gave 6 orders dynamic range (up to 2Mcps) Analog mode on other ICP-MS typically gives total of 8 orders dynamic range (up to 400Mcps), equivalent to about 50ppm Higher 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 500ppm Upper range is even higher for mineral elements in He mode, as low-mass signal is reduced when cell is pressurized.
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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

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7700x Largest Analytical Range of any ICP-MS

Calibration ranges Hg (10 200ppt) NoGas Mode As (10 200 ppt) He Mode Se (10 200 ppt) He Mode Na (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 Na Typically, ICP-MS cannot measure above 200ppm Na without changing interface, quad resolution or ion lens settings Hg Hg LOD on 7700x is about 2ppt 7700x can QUANTITATE at 10ppt! 7700x can do both of the above in the same run!
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CPS

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

Hg

As

As

10 ppt Mercury

10 ppt Arsenic

78 Se [ 3 ] x10 1 y = 0.1757 * x + 0.8000 R = 0.9993 DL = 5.915 ppt BEC = 4.553 ppt

Se

Na
1000ppm Sodium Good fit at 0.2ppm

20 ppt Selenium

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0.0 Conc(ppt)

100.0

200.0

300.0

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Application of the 7700 ICP MS to the food analysis

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Analysis of Metals in Food by ICP-MS

Wide 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 excess

Al, 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) analysis

ICP-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/availability

Chromatographic separation before ICP-MS analysis
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May 13, 2011

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!

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

Page 30 May 13, 2011

Putting All Together the advantages of the 7700x

simple, 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

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* Plus no gas mode for non-interfered elements

Page 31 May 13, 2011

Method Detection Limits - 3 (n = 10) in Parts Per Billion

(in 1% HNO3/0.5% HCl)
Element Be B Na Mg Al K Ca V Cr Mn Fe Co Ni Cu Mass 9 11 23 24 27 39 44 51 52 55 56 59 60 63 MDL (ppb) 0.005 0.005 0.058 0.002 0.007 0.076 0.090 0.014 0.004 0.008 0.014 0.004 0.014 0.002 Cell mode No gas No gas No gas No gas No gas He No gas He He He He He He He Element Zn As Se Sr Mo Ag Cd Sb Ba Hg Tl Pb Th U Mass 66 75 78 88 95 107 111 121 137 202 205 208 232 238 MDL (ppb) 0.014 0.011 0.017 0.002 0.006 0.002 0.002 0.006 0.005 0.001 0.002 0.001 0.001 0.001 Cell mode He He He He He He He He He He He He He He Agilent Restricted

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
Page 32 May 13, 2011

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 Agilent Restricted 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 CRMs in Helium Mode Only

NRC-CNRC DORM3 Fish Protein NIST SRM 2976 Mussel Tissue NIST RM 8415 Whole Egg Powder

Recoveries include both extraction efficiency by microwave digestion and analytical accuracy

Certified value Recovery (mg/kg) (%) 23 Na 43 Ca 52 Cr 55 Mn 56 Fe 60 Ni 63 Cu 66 Zn 75 As 78 Se 95 Mo 111 Cd 202 Hg 208 Pb 347 1.28 15.5 51.3 6.88 0.29 0.382 0.395 93.4 100.8 92.6 89.4 89.5 95.4 101.4 100.8

Certified value Recovery (mg/kg) (%) 171 4.02 137 13.3 1.8 0.82 0.061 1.19 92.7 82.6 88.4 94.5 104.3 96.8 112.0 97.8

Certified value (mg/kg) 3770 2480 0.37 1.78 2.7 1.39 0.247 -

Recovery (%) 101.0 109.7 93.0 91.9 96.5 89.7 87.2 -

Agilent -Restricted 0.061 91.0

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Chromatographic Applications of ICP-MS: Speciation analysis

Chemical forms of trace elements

Inorganic

Organometallic compounds

Biomolecules

Complexed with humic substances

Cr(III) vs Cr(VI)
Essential Toxic
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Chromatographic Applications
Simple link to Agilent LC Direct sequence control from ICPMS sample log table Method setup for LC/GC from ICPMS PC

Predefined application packs available, as for 7500

Data Analysis software now integrated into main suite Agilent Restricted Same service support for all units

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Speciation with LC-ICP-MS and GC-ICP-MS

Conventional organo-metallic compounds: Inorganic vs organic arsenic Organo-tin Methyl-mercury, etc Emerging elements/compounds: Pesticide and OP nerve agent residues PBDEs Nanoparticles

Application Examples

As Speciation using LC-ICP-MS

Agilent Application Note: Routine Analysis of Toxic Arsenic Species in Urine Using HPLC with ICP-MS, 5989-5505EN, by Tetsushi Sakai and Steven Wilbur, Agilent Technologies

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Chromatogram of Mixed Organotin Standards (Ethylated)

3 Sigma Detection Limit
MBT TPrT DBT MPhT TBT DPhT TPhT 4.4fg 5.3fg 9.4fg 44fg 9.9fg 10fg 11fg

Injection volume 1uL

1 : Sn(), 2 : MBT, 3 :TPrT (IS), 4 : DBT, 5 : MPhT, 6 : TBT, 7 : DPhT, 8 : TPhT concentration : 5ug/l (5pg) as metal

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

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
Agilent Restricted 9 linear orders allows measurements at ppt and 100s ppm in the same acquisition

Improving productivity
Page 41 May 13, 2011

Agilent Restricted