Today s Agilent Solutions for Determining Heavy Metals in Food using Atomic Spectroscopy Evrim Kilicgedik Product Specialist, Atomic Spectroscopy Agilent Technologies 04.11.2011
2011 The Atomic Spectroscopy Revolution With the 2011 launching of the Atomic Spectroscopy Revolution, Agilent now offers the most comprehensive and innovative range of inorganic (atomic) spectroscopy instruments for liquid sample analysis: Flame Atomic Absorption (AA); Graphite Furnace AA; Vapor Generation AA; Microwave Plasma-Atomic Emission (MP-AES); ICP-Optical Emission; as well as The 7700 Series ICP-MS Page 2
Agilent Atomic Absorption The world s fastest flame AA; the world s most sensitive furnace AA Superior flame, graphite furnace, and vapor generation or a combination of techniques let you exactly match your analytical needs and your budget Patented Fast Sequential capability lets you measure multiple elements in each sample doubling productivity and lowering the cost per analysis Easy-to-use software and rugged, reliable hardware simplify operation and maximize uptime
Agilent ICP-OES The world's most productive high performance simultaneous ICP-OES Continuous wavelength coverage provides extended dynamic range and reduced interferences, giving you maximum confidence in your results Robust plasma ensures reliable and reproducible results even with the most complex matrices One view, one step measurement of major, minor, and trace elements, plus the fastest warm-up, increases throughput and productivity Page 4
Agilent ICP-MS Unmatched matrix tolerance and unparalleled interference removal Patented High Matrix Introduction (HMI) technology increases matrix tolerance up to 10x to handle the toughest samples with ease! Third generation collision cell design with helium collision mode effectively removes polyatomic interferences, ensuring more accurate results in unknown or complex sample matrices Delivers the highest productivity in the most demanding lab environments
2011 Start of the Atomic Spectroscopy Revolution! Agilent has launched a revolutionary new Atomic Spectroscopy instrument This instrument doesn t just redefine a category it creates a new one! No other instrument like it exists! This technique delivers: Improved performance compared with conventional flame AA Improved ease of use Lower running costs Allows unattended multi-element analysis Improved laboratory safety If you re a flame AA user, be prepared to save thousands of dollars per year Does that sound appealing??? Page 6
Common Challenges facing Laboratories doing Elemental Analysis Today Increased need for multi-element determination over a wide dynamic range Desire to reduce the overall cost of analysis due to rising costs (instrument supplies and consumables; power; labour etc) Difficulty in sourcing some gases esp. in remote areas and emerging geographies Availability of suitably trained personnel to develop methods, perform sample measurement and interpret results Some laboratories under pressure to improve safety by removing flammable gases Page 7
Agilent 4100 Microwave Plasma-Atomic Emission Spectrometer (MP-AES) New technique for elemental determination using atomic emission Microwave excited plasma source Nitrogen based plasma - runs on air (using a N 2 generator) Improved performance compared with flame AA: Higher sample throughput with fast sequential measurement More than 2x faster than conventional flame AA Superior detection limits and improved dynamic range Easy to use: New generation software featuring automated optimization and software applets that load a preset method One piece torch with easy torch removal and replacement no alignment Reduced operating costs: Runs on air eliminates need for Acetylene, Argon, etc. Eliminates need for source/hollow cathode lamps Simple installation no chiller, 10 A supply Improved Safety: Eliminates need for flammable gases and cylinder handling Safe, reliable unattended multi-element overnight operation Page 8
Accessory Options for the 4100 MP-AES Automate and simplify analysis with the SPS3 autosampler (required for unattended overnight operation) For organic applications, use the EGCM to bleed air into the plasma minimizing C build-up and reducing background also requires the OneNeb inert nebulizer (incl. with the Organics kit) To enable low ppb level detection of As, Se or Hg, use the Multimode Sample Introduction System (MSIS) also requires the 5 channel peristaltic pump option Page 9
Applications the MP-AES can do by Market Still the leader in Xenon flash lamp technology after 12 years! Page 10
Food Applications Types of Measurement Product Labeling Nutrient Levels Food Quality Contamination Pollutants Food Production QA/QC Research Developing Better Products Page 11
Which Elements are Monitored in Foods? Toxic trace elements Low level analysis typically ppb levels As, Cd, Hg, Pb, Tl, Cr Common elements that are toxic in excess Typically range from ppb to ppm level Al, Ni, Cu, Zn, Se, Mo, Sn Essential minerals Can cover a wide range from ppm to % levels Na, Mg, P, S, K, Ca, Fe Page 12
Food and Agriculture Applications The Challenge Robust Sample Introduction Large number of samples Wide range of matrices High total dissolved solids (TDS) Many Elements Per Sample Potential for spectral interferences Labs. need high sample throughput Labs. also want low cost of analysis Wide Dynamic Range Trace (ppb) level to % level Avoid sample dilution (if possible) Page 13
Major, Minor and Trace Analysis in Foodstuffs A range of samples 1.NIES CRM No.7 Tea Leaves 2.NIES CRM No.10c Rice Flour 3.NIST SRM 1577 Bovine Liver: Plus pre-prepared sample solutions in 4 % HNO 3 (High Purity Standards) 4.CRM-Wheat Flour 5.CRM-Milk Powder 6.CRM-Oyster Tissue Page 14
Preparation of Food Samples Samples Various Certified Reference Materials Digestion Add 10 ml HN0 3 acid Heat until dissolved Cool & dilute to 100 ml Analysis Using the 4100 MP-AES Page 15
Food Applications Solving the Challenges Robust Sample Introduction Standard Sample Introduction Concentric nebulizer Single pass spray chamber Many Elements Per Sample Improved throughput compared to Flame AA Auto background correction CsCl buffer Wide Dynamic Range Over 14,000 wavelengths to chose from for low and high concentration Lower detection limits for P compared to Flame AA Page 16
Improving Detection Limits for As, Se, Hg with MSIS Analyte Conventional Nebulization ug/l MSIS in Simultaneous Mode ug/l As 90 1.0 Se 126 2.0 Hg 14 0.5 Page 17
Fast Linear Interference Correction (FLIC) FLIC uses models of the blank, standard and potential interferent elements to correct for spectral interferences Page 18
Instrument Parameters Parameter Setting Nebulizer Glass concentric Spray chamber Single pass glass cyclonic Sample tubing White/white Waste tubing Blue/blue Read Time 10 s Replicates 3 Stabilization time 10 s Fast Pump On (80 rpm) Pump speed 12 rpm Nebulizer pressure 160 180 kpa (auto optimized) Background Correction Auto Page 19
Method Detection Limits Page 20
Measured Results for CRM Food Samples NIES No. 7 Tea Leaves High Purity Stds CRM Milk Powder * Reference values only Page 21
Measured Results for CRM Food Samples NIES No. 10c Rice Flour High Purity Stds CRM Wheat Flour * Reference values only Page 22
Measured Results for CRM Food Samples NIST 1577 Bovine Liver High Purity Stds CRM Oyster Tissue * Reference values only Page 23
Certified (mg/kg) Certified (mg/kg) Certified (mg/kg) Certified (mg/kg) Wide Dynamic Range Magnesium (r=0.9997) Phosphorus (r=1.0000) 10000 10000 1000 1000 100 100 10 10 1 1 10 100 1000 10000 1 1 10 100 1000 10000 Measured (mg/kg) Measured (mg/kg) Calcium (r=1.0000) Potassium (r=0.9999) 10000 100000 1000 10000 100 1000 100 10 10 1 1 10 100 1000 10000 1 1 10 100 1000 10000 100000 Measured (mg/kg) Measured (mg/kg) Page 24
Agilent 4100 MP-AES Runs on air the most significant advance in atomic spectroscopy o Lowest running cost of any atomic spectroscopy technique due to capability to run on air ideal for remote and at site operation o Improved safety capability to run on air means no flammable gases and no manual handling of cylinders o Easy-to-use software with MP applets and plug and play torch which simplify operation and maximize uptime o Superior performance to flame AA, with capability to run unattended overnight Page 25
Agilent s Atomic Spectroscopy Portfolio ICP-OES ICP-MS 4100 MP-AES Flame AAS Graphite Furnace AAS AAS instruments can be flame only, furnace only, or combined (switchable) Page 26
Dedicated MP-AES Microsite: www.agilent.com/chem/runsonair Page 27
Questions? Poster session this afternoon G51 ICP-OES for wine analysis G58 LC-ICP-MS for Hg speciation Agilent MP-AES The Market Leaders in Atomic Spectroscopy Page 28