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Maura Rury Americas Regional Marketing Manager, Trace Elemental Analysis

Deliver Quality ICP-MS Results with Advanced Simplicity and Unmatched Productivity

Quality ICP-MS Results…

• Trace elemental quantification is used in numerous industries to monitor metal concentrations: • Toxic metals (e.g. As, Cd, Hg, Pb) • Impurities (e.g. S, Al, Ni) • Essential elements (e.g. Fe, Se) • Elemental species or nanoparticles

• Challenges associated with elemental quantification:

• Data must be accurate and free from interferences • Instruments must be stable and deliver high precision results • The system must handle a wide variety of sample matrices • Large volumes of data must be measured and reported

Safe Drinking Water Act (SDWA)/ National Pollutant Discharge Elimination System (NPDES)

• Protect drinking water supplies and sources

• SDWA: National Primary Drinking Water Regs.

A Closer Look at Elemental Analysis for Environmental Monitoring

Resource Conservation and Recovery Act (RCRA)/Office of Solid Waste (OSW)

• Protect public from hazards of waste disposal:

• River/groundwater, industrial waste, soil, sludge, sediments, solid waste

• Goals:

• Determine nature/extent of contamination

• Assess priorities for response

• Determine clean-up actions

Element MCL (mg/L) Potential Health Effects

Antimony 0.006 Inc. in blood cholesterol; dec. in blood sugar Arsenic 0.010 Skin damage/increased risk of cancer

Barium 2 Increase in blood pressure Beryllium 0.004 Intestinal lesions Cadmium 0.005 Kidney damage Chromium 0.1 Allergic dermatitis Copper 1.3 Gastrointestinal distress/Liver or kidney damage

Lead 0.015 Delays in physical or mental development

Mercury 0.002 Kidney damage Selenium 0.05 Hair or fingernail loss; circulatory problems

Thallium 0.002 Hair loss; kidney, intestine, or liver problems

Uranium 0.03 Increased risk of cancer, kidney toxicity

Safe Drinking Water Act (SDWA)/ National Pollutant Discharge Elimination System (NPDES)

• Protect drinking water supplies and sources

• SDWA: National Primary Drinking Water Regs.

A Closer Look at Elemental Analysis for Environmental Monitoring

Resource Conservation and Recovery Act (RCRA)/Office of Solid Waste (OSW)

• Protect public from hazards of waste disposal:

• River/groundwater, industrial waste, soil, sludge, sediments, solid waste

• Goals:

• Determine nature/extent of contamination

• Assess priorities for response

• Determine clean-up actions

Element MCL (mg/L) Potential Health Effects

Antimony 0.006 Inc. in blood cholesterol; dec. in blood sugar Arsenic 0.010 Skin damage/increased risk of cancer

Barium 2 Increase in blood pressure Beryllium 0.004 Intestinal lesions Cadmium 0.005 Kidney damage Chromium 0.1 Allergic dermatitis Copper 1.3 Gastrointestinal distress/Liver or kidney damage

Lead 0.015 Delays in physical or mental development

Mercury 0.002 Kidney damage Selenium 0.05 Hair or fingernail loss; circulatory problems

Thallium 0.002 Hair loss; kidney, intestine, or liver problems

Uranium 0.03 Increased risk of cancer, kidney toxicity

Quality ICP-MS Results…QA/QC

• Typical QA/QC checks for EPA Methods 200.8 and 6020 QC Check QC Assessment Method 200.8 Limit Method 6020 Limit

Short Term RSDs Instrument Performance < 5% on 5 measurements < 5% on 4 measurements

Linear Dynamic Range Instrument Performance Upper LDR < 10% below extrapolated level

-

Quality Control Standard Method Accuracy +/- 10% certified value +/- 20% certified value

Method Detection Limit Instrument Performance - -

Laboratory Reagent Blank/Calibration Blank Laboratory Contamination < 2.2 * MDL < 3 * IDL

Initial/Continuing Calibration Verification Calibration Accuracy +/- 10% or within

acceptance limits +/- 10%

Interference Check Solution

Instrument Performance - -

Lab. Fortified Matrix/Post Digestion Spike Method recovery +/- 30% +/- 25%

Duplicate Sample Analysis Repeatability +/- 20% duplicate +/- 20% duplicate

Internal Standardization Analyte Recovery/Data Quality 60 - 125 70 - 130

How ICP-MS Can Contribute to Delivering Quality Results

• ICP-MS can measure almost the whole periodic table in just about every sample matrix • Matrix tolerance – robust interface and sample handling systems can significantly increase analysis times

between operator intervention • Interference removal – advances in collision/reaction cell technology providing way to analyze more

accurately at lower levels • High sensitivity – higher detection power enables lower limits of detection • > 9 orders dynamic range – enables the analysis of both minors and majors in one analytical run

• Information derived: • Element concentrations • High precision isotope ratios • Species concentrations • Particle number and composition

Thermo Scientific iCAP RQ ICP-MS

Simplified power connections to facilitate

installation further

New robust interface for reliable long-term

analysis of dirty samples

New robust RF generator –

maximum uptime

All new electronics – maximum uptime and

stability

Increased capacity interface pumping for

higher sensitivity

Long life detector

Vertical analyzer and compact footprint

Quick connect sample intro and torch design

for easy handling

Collision/reaction cell; high transmission and low

mass cut off

Handling Interferences – What Are Interferences?

H2O, Ca, Na, K, Mg, Cl, etc

Ar, Air (O, N)

Reaction

Reactants

Handling Interferences – What Are Interferences?

H2O, Ca, Na, K, Mg, Cl, etc

Ar, Air (O, N)

Reaction

Reactants

ArAr, ArO, ArN, ArC, ArH, ArCa, ArNa, ArK, ArMg, ArCl, ClO, NO, CO, CaO, NaO, etc

Products

Interferences

• Some typical interferences in ICP-MS:

Handling Interferences – What Options are Available?

• Alternative Sample Introduction Techniques

• E.g. aerosol desolvation to minimize the population of the precursor (parent) ions in the ICP ion source

• Cold Plasma:

• Reduce plasma power to reduce amount of Ar ionization

• Mathematical Correction Equations:

• Measure the isotope of interest, an un-interfered isotope, a polyatomic isotope and mathematically de-convolute to return an interference free value

Mass Interferences Precursors

51V 35Cl16O, 37Cl14N,

34S16OH H, N, O, S, Cl

56Fe 40Ar16O, 40Ca16O O, Ar, Ca

63Cu 40Ar23Na, 12C16O35Cl,

31P32S C, N, O, Na, P,

S, Cl, Ar

75As 40Ar35Cl, 40Ca35Cl,

40Ar34SH, 37Cl2H H, S, Cl, Ca, Ar

• Some typical interferences in ICP-MS:

Handling Interferences – What Options are Available?

• Alternative Sample Introduction Techniques

• E.g. aerosol desolvation to minimize the population of the precursor (parent) ions in the ICP ion source

• NOT A UNIVERSAL SOLUTION

• Cold Plasma:

• Reduce plasma power to reduce amount of Ar ionization

• NOT A UNIVERSAL SOLUTION

• Mathematical Correction Equations:

• Measure the isotope of interest, an un-interfered isotope, a polyatomic isotope and mathematically de-convolute to return an interference free value

• AMPLIFIES ERRORS, DOESN’T ACCOUNT FOR UNKNOWN INTERFERENCES

Mass Interferences Precursors

51V 35Cl16O, 37Cl14N,

34S16OH H, N, O, S, Cl

56Fe 40Ar16O, 40Ca16O O, Ar, Ca

63Cu 40Ar23Na, 12C16O35Cl,

31P32S C, N, O, Na, P,

S, Cl, Ar

75As 40Ar35Cl, 40Ca35Cl,

40Ar34SH, 37Cl2H H, S, Cl, Ca, Ar

• Thermo Scientific™ iCAP™ QCell Technology • He Kinetic Energy Discrimination (KED)

Target

Analyte 75As+

Quadrupole set to filter out exact mass of target analyte

QCell in collision mode with with pure He uses energy discrimination

ArCl+, Ca(OH)2H+

Quadrupole isolates ions required for

measurement

He KED filters out unwanted polyatomic

interferences, based on difference in cross-sectional size of the

analyte and polyatomic

Complex Sample Matrix

Comprehensive interference removal is achieved

Handling Interferences with Collision Reaction Cell Technology

• …and Low Mass Cut Off Target

Analyte 75As+

Quadrupole set to filter out exact mass of target analyte

QCell flatapole dynamically applies LMCO relative to target analyte

Low mass cut off filters out unwanted

precursor ions; ions are unable to recombine later in the QCell and

backgrounds are reduced further than

He KED alone

Complex Sample Matrix

40Ar+, 40Ca+, 35Cl+, 16O+, 1H+

Handling Interferences with Collision Reaction Cell Technology

Comprehensive interference removal is achieved

Quadrupole isolates ions required for

measurement

• Low Mass Cut Off (LMCO) • Prevents the lower mass ions that contribute to interferences from traveling through the QCell...

Handling Interferences – Low Mass Cut Off

Mass Interferences Precursors 51V 35Cl16O, 37Cl14N,

34S16OH H, N, O, S, Cl

56Fe 40Ar16O, 40Ca16O O, Ar, Ca 63Cu 40Ar23Na,

12C16O35Cl, 31P32S C, N, O, Na, P, S, Cl, Ar

75As 40Ar35Cl, 40Ca35Cl, 40Ar34SH, 37Cl2H

H, S, Cl, Ca, Ar

Mass LMCO Interferences Precursors 51V 35 35Cl16O, 37Cl14N,

34S16OH H, N, O, S, Cl

56Fe 39 40Ar16O, 40Ca16O O, Ar, Ca 63Cu 45 40Ar23Na,

12C16O35Cl, 31P32S C, N, O, Na, P, S, Cl, Ar

75As 47 40Ar35Cl, 40Ca35Cl, 40Ar34SH, 37Cl2H

H, S, Cl, Ca, Ar

• Low Mass Cut Off (LMCO) • Prevents the lower mass ions that contribute to interferences from traveling through the QCell...

• …and reduces BECs even further than He KED alone

Handling Interferences – Low Mass Cut Off

Mass Interferences Precursors 51V 35Cl16O, 37Cl14N,

34S16OH H, N, O, S, Cl

56Fe 40Ar16O, 40Ca16O O, Ar, Ca 63Cu 40Ar23Na,

12C16O35Cl, 31P32S C, N, O, Na, P, S, Cl, Ar

75As 40Ar35Cl, 40Ca35Cl, 40Ar34SH, 37Cl2H

H, S, Cl, Ca, Ar

Mass LMCO Interferences Precursors 51V 35 35Cl16O, 37Cl14N,

34S16OH H, N, O, S, Cl

56Fe 39 40Ar16O, 40Ca16O O, Ar, Ca 63Cu 45 40Ar23Na,

12C16O35Cl, 31P32S C, N, O, Na, P, S, Cl, Ar

75As 47 40Ar35Cl, 40Ca35Cl, 40Ar34SH, 37Cl2H

H, S, Cl, Ca, Ar

National Primary Drinking Water Regulations National Secondary Drinking Water Regulations

Unregulated Contaminant Monitoring Rule 3

Limits of Detection for U.S. EPA Method 200.8 with He KED

Element MCL (mg/L) IDL (mg/L) Antimony 0.006 0.000006 Arsenic 0.010 0.000009 Barium 2 0.000011 Beryllium 0.004 0.000012 Cadmium 0.005 0.000008 Chromium 0.1 0.000017 Copper 1.3 0.000008 Lead 0.015 0.000002 Mercury 0.002 0.000012 Selenium 0.05 0.000430 Thallium 0.002 0.000002 Uranium 0.03 0.000001

Element MCL (mg/L) IDL (mg/L) Aluminum 0.050-0.200 0.000456 Copper 1 0.000008 Iron 0.3 0.000103 Manganese 0.05 0.000008 Silver 0.1 0.000009 Zinc 5 0.000102

Element MRL (mg/L) IDL (mg/L) Chromium 0.0002 0.000017 Cobalt 0.001 0.000004 Molybdenum 0.001 0.000020 Vanadium 0.0002 0.000009

Matrix Handling – Customized Interfaces for Maximum Flexibility

Matrix Handling – Customized Interfaces for Maximum Flexibility

Unique interface designed for maximum sensitivity and dynamic range:

Robust 4.5 mm

High Matrix

3.5 mm

High Sensitivity

2.8 mm

• Easy execution via software • Dedicated grouping and autotunes

• U.S. EPA Method 200.8

• Blank & Calibration of 28 Analytes • Initial QC checks: ICV, ICB, LFB, QCS • Ongoing QC checks: CCB, CCV • IS monitoring across mass range with 6Li, 45Sc, 71Ga, 89Y, 115In and 159Tb • Drinking water (faucet) spiked with 100 ppm Ca (hard water)

Matrix Handling – U.S. EPA 200.8 for Drinking Water Analysis

0 1 2 3 4 5 6 7 8 9 10 11 12

Time/hours

3.5 mm insert

Matrix Handling – New Robust Interface for Improved Long-term Stability

0 1 2 3 4 5 6 7 8 9 10 11 12

Time/hours

3.5 mm insert

4.5 mm insert

• U.S. EPA Method 200.8

• Drinking water (faucet) spiked with 100 ppm Ca (hard water) • He KED used to comprehensively remove interferences

Matrix Handling – U.S. EPA Method 200.8 for Drinking Water

0 1 2 3 4 5 6 7 8 9 10 11 12

Time/hours

4.5 mm insert

• U.S. EPA Method 6020

• Blank & Calibration of 23 Analytes • Initial QC checks: ICV, ICB, ICSA, ICSAB • Ongoing QC checks: CCB, CCV • IS monitoring across mass range with 6Li, 45Sc, 71Ga, 89Y, 115In and 159Tb • Drinking water (faucet) spiked with 500 ppm Ca (waste water/digested solid waste)

Matrix Handling – U.S. EPA 6020 for Waste Water/Solid Waste

Time/hours 0 1 2 4 6 7 8 5 3

4.5 mm insert

• ICP-MS software provides complete control of the ESI prepFAST:

• Automated prescriptive dilution for preparing: • Samples • Standards

• Automated intelligent dilution: • Internal standard range auto-dilution • Over calibration range auto-dilution

• Discrete sampling valves coupled closely to the instrument

• Minimize uptake and washout

• Increase throughput

Matrix Handling – Prescriptive, Intelligent Auto-dilution

• Calibration Over-Range • User defines:

• The maximum calibration limit as a percentage of the top calibration standard, e.g. 110%

• The target concentration of the analyte after auto-dilution

Matrix Handling – Intelligent Auto-dilution

• Internal Standard Recovery • User defines:

• The range of acceptable Internal Standard Recovery, e.g. 60 - 125%

• The autodilution factor step and # of possible dilutions

• Without auto-dilution • Samples with very high matrix, analyzed w/o dilution

Auto-dilution for Highly Varied Semi-Saline Waste Water Samples

Calibration Samples

Internal standard recovery outside of method defined criteria (60 to 120 %)

• With auto-dilution • Samples diluted prescriptively and progressively

• Without auto-dilution • Samples with very high matrix, analyzed w/o dilution

Auto-dilution for Highly Varied Semi-Saline Waste Water Samples

Calibration Samples Calibration Samples Method validation, QC

Internal standard recovery significantly more stable and outliers now in acceptable range

Internal standard recovery outside of method defined criteria (60 to 120 %)

• Simple workflows to quality results

Thermo Scientific Qtegra Intelligent Scientific Data Solution Software

• Export: • “What You See is What You Get” • Various formats supported

• Reporting:

• Series of default reports provided • Support of company logos • Fully configurable report editor provided • Exportable as PDF or XML

• Automated data export and/or report per analysis

Qtegra ISDS Software – Handling the Data

Qtegra ISDS Software – Advanced Applications

• Nanoparticle characterization with spICP-MS

• Fast, easy data acquisition with npQuant plug-in for Qtegra ISDS

• High sensitivity interface for small NP size

• Integrated set of parameters for statistical data evaluation of spICP-MS

• Speciation with fully integrated IC-ICP-MS

• Thermo Scientific™ Dionex™ Chromeleon™ Chromatography Data System plug-in enables fully integrated control

• Dedicated tQuant software plug-in for full chromatographic data processing

• Accurate trace element quantification enabled through comprehensive interference removal • Simple method development – only one measurement mode for all analytes • Higher productivity – no overhead required to change measurement mode

• Reliable and consistent data with new robust interface • More uptime – less cleaning and longer periods of uninterrupted analysis • Fewer re-runs – increased confidence when running high matrix samples

• Automated solutions, with integrated software control and features • Accelerate the trace element workflow with intelligent dilution • Unattended operation - leave personnel free to do more important tasks in the lab

• Qtegra ISDS software provides intuitive workflows to streamline efficiency • Default QC checks, customized reports, intuitive data management and LIMS integration • Common platform with iCAP 7000 Series ICP-OES for reduced training and increased operator flexibility • Plug-in based platform enables easy implementation of advanced applications

Thermo Scientific iCAP RQ ICP-MS: Delivering Quality ICP-MS Results

Complete Your Analytical Workflow

• High Purity Reagents and Chemicals • High purity acids:

• HCl, HNO3, HF, H2SO4 • High concentration, single-element standards • Multi-element organometallic standards

• Multi-element, Method-Compliant Standards • USP <232>,<233> • EPA Methods:

• 200.7, 200.8, 6010

• Instrument Accessories • Atomic absorption hollow cathode lamps • Peristaltic pump tubing

• Laboratory Equipment • Gloves and safety glasses • Pipettes (fixed or adjustable volume) • Pipette tips • Class A volumetric flasks

Thank You

Now please join me in the iCAP RQ ICP-MS section of our booth and I will address any further comments and questions.