Materials Characterization Lab
                                                    www.mri.psu.edu/mcl



Elemental Analys...
Materials Characterization Lab
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Materials Characterization Lab
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Materials Characterization Lab
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          Outline...
Materials Characterization Lab
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Emission of the 590 n...
Materials Characterization Lab
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Materials Characterization Lab
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                ...
Materials Characterization Lab
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Plasma Torch
Materials Characterization Lab
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Optical Path in Leeman PS3000UV
Materials Characterization Lab
                                              www.mri.psu.edu/mcl



Spectrum as dispersed ...
Materials Characterization Lab
                          www.mri.psu.edu/mcl


Elements by ICP-AES




core
electrons
Materials Characterization Lab
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        Common Problems in...
Materials Characterization Lab
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      ...
Materials Characterization Lab
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Materials Characterization Lab
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           ...
Materials Characterization Lab
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Materials Characterization Lab
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            ...
Materials Characterization Lab
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       ...
Materials Characterization Lab
          www.mri.psu.edu/mcl




Basic Analytical
    Scheme



  Concepts, Instrumentatio...
Materials Characterization Lab
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        ...
Materials Characterization Lab
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          ...
Materials Characterization Lab
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Graphite crucibl...
Materials Characterization Lab
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         ...
Materials Characterization Lab
          www.mri.psu.edu/mcl




Acid digestion in a Pt
        dish
Materials Characterization Lab
                                                            www.mri.psu.edu/mcl


         ...
Materials Characterization Lab
      www.mri.psu.edu/mcl




    MARS 5
   Microwave
Digestion System
Materials Characterization Lab
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Materials Characterization Lab
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        ...
Materials Characterization Lab
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Typical An...
Materials Characterization Lab
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Typical applications o...
Materials Characterization Lab
           www.mri.psu.edu/mcl




Natural Waters


•Leaching from mine sites
•Geochemical ...
Materials Characterization Lab
                                              www.mri.psu.edu/mcl




              More Sa...
Materials Characterization Lab
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Strengt...
Materials Characterization Lab
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Weakne...
Materials Characterization Lab
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MCL capab...
Materials Characterization Lab
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H...
Materials Characterization Lab
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Acceptable...
Materials Characterization Lab
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www.mri.psu.edu/mcl


     Henry Gong
  ...
Materials Characterization Lab
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Elemental Analyses by
High Resolutio...
Materials Characterization Lab
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Materials Characterization Lab
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Materials Characterization Lab
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                      Out...
Materials Characterization Lab
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         ...
Materials Characterization Lab
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Finnigan HR-ICP-MS Element ...
Materials Characterization Lab
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 Sampler Cone, ~1mm o...
Materials Characterization Lab
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          Plasma Inte...
Materials Characterization Lab
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Nebulizer and spray cha...
Materials Characterization Lab
               www.mri.psu.edu/mcl




Spectrum
Materials Characterization Lab
           www.mri.psu.edu/mcl




Ni60
Materials Characterization Lab
             www.mri.psu.edu/mcl




ICP-MS
 IDLs
Materials Characterization Lab
                                  www.mri.psu.edu/mcl




          ICP-MS Challenges



― ...
Materials Characterization Lab
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Spectral Interferences
     Fe56...
Materials Characterization Lab
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Spectral Interferences
      ...
Materials Characterization Lab
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Spectral Interferences
     As75...
Materials Characterization Lab
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Spectral Interferences
     As7...
Materials Characterization Lab
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       Spectral Inte...
Materials Characterization Lab
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          ...
Materials Characterization Lab
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Strengt...
Materials Characterization Lab
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Some A...
Materials Characterization Lab
                                     www.mri.psu.edu/mcl



Wear Metals in Lubricating Oil
Materials Characterization Lab
                            www.mri.psu.edu/mcl




Laser Ablation ICP-MS
Materials Characterization Lab
                                www.mri.psu.edu/mcl




New-Wave Research LUV266X
Materials Characterization Lab
                                     www.mri.psu.edu/mcl




Raster pattern on NIST SRM 495...
Materials Characterization Lab
                                                www.mri.psu.edu/mcl




         Laser Abla...
Materials Characterization Lab
                                          www.mri.psu.edu/mcl




How to get started

1) Co...
Materials Characterization Lab
                                                        www.mri.psu.edu/mcl




Acceptable ...
Materials Characterization Lab
                                                             www.mri.psu.edu/mcl



ICP-MS ...
Materials Characterization Lab
                           www.mri.psu.edu/mcl




www.mri.psu.edu/mcl


     John Kittleso...
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Chem Analysis

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Chem Analysis

  1. 1. Materials Characterization Lab www.mri.psu.edu/mcl Elemental Analyses by ICP-AES/ICP-MS Henry Gong, Senior Analytical Chemist John Kittleson, ICP Mass Spectroscopist July 27, 2005
  2. 2. Materials Characterization Lab www.mri.psu.edu/mcl Summer Characterization Open Houses Technique Time Date Location Thermal analysis (TGA, DTA, DSC) 9:45 AM June 8 250 MRL Bldg. Transmission Electron Microscopy (TEM/STEM) 9:45 AM June 15 114 MRI Bldg Scanning electron microscopy (SEM) 9:45 AM June 22 541 Deike Bldg. Analytical SEM 11:00 AM June 22 541 Deike Bldg. X-ray Diffraction (XRD) 9:45 AM June 29 250 MRL Bldg. Dielectric Characterization (25 min lecture only) 9:45 AM July 6 250 MRL bldg. High temperature sintering lab (20 min lecture only) 10:15 AM July 6 250 MRL Bldg. Focused Ion Beam (FIB) 9:45 AM July 13 114 MRI Bldg TEM sample preparation 11:00 AM July 13 114 MRI Bldg Orientation imaging microscopy (OIM/EBSD) 9:45 AM July 20 250 MRL Bldg. Chemical analysis (ICP, ICP-MS) 9:45 AM July 27 541 Deike Bldg. Atomic Force Microscopy (AFM) 9:45 AM August 3 114 MRI Bldg Small angle x-ray scattering (SAXS) 9:45 AM August 10 541 Deike Bldg. Particle Characterization 9:45 AM August 17 250 MRL X-ray photoelectron spectroscopy (XPS/ESCA) 9:45 AM August 24 114 MRI Bldg Auger Electron Spectroscopy (AES) 11:00 AM August 24 114 MRI Bldg NOTE LOCATIONS: The MRI Bldg is in the Innovation Park near the Penn Stater Hotel; MRL Bldg. is on Hastings Road. More information: www.mri.psu.edu/mcl
  3. 3. Materials Characterization Lab www.mri.psu.edu/mcl Materials Characterization Lab Locations Bldg Telephone MRL 863-7844 MRI 865-0337 MRI Bldg: Hosler 865-1981 XPS/ESCA, SIMS, E&ES 863-4225 TEM, HR-TEM, FE- Auger, AFM, XRD MRL Bldg: Hosler Bldg: SEM, XRD, OIM, DTA, SEM, ESEM, FE- DSC, TGA, FTIR, Penn Stater SEM, EPMA, ICP, Hotel Raman, AFM, Powder, E&ES Bldg: ICP-MS,BET, SAXS dielectric, prep, shop, SEM IC, UV-Vis Route 322 Steidle Bldg: Atherton Street Nanoindenter (322 Business) I-99 Park Ave. 0 0 0 0 0 0 0 Ave. 0 0 0 0 0 Park 0 Beaver 0 0 Stadium 0 0 0 Centre 0 0 Porter Road Community Univ Shortlidg Hospital 0 0 Burrowes Road ersi ty D e Pollock Road Road rive North Hastin Deike Bldg: gs Ro ad College Ave.
  4. 4. Materials Characterization Lab www.mri.psu.edu/mcl Outline of ICP-AES segment ― a discussion of ICP-AES principles ― various problems encountered in ICP-AES ― sample dissolutions ― data reduction ― some applications ― ICP-MS ― a brief lab tour after ICP-MS talk
  5. 5. Materials Characterization Lab www.mri.psu.edu/mcl Emission of the 590 nm wavelength (aka yellow) Water High Na solution
  6. 6. Materials Characterization Lab www.mri.psu.edu/mcl ICP-AES – inductively coupled plasma atomic emission spectrophotometry Electrons of an atom absorb energy and jump to higher energy levels When they return to normal states, they emit characteristic photons of energy By isolating these photon wavelengths, we can determine the types and concentrations of the elements present. Concepts, Instrumentation, and Techniques in Inductively Coupled Plasma Optical Emission Spectrometry, Boss and Freeden, Perkin Elmer
  7. 7. Materials Characterization Lab www.mri.psu.edu/mcl Sample Introduction • Solution is drawn up by means of a peristaltic pump • Solution is turned into a fine aerosol by a nebulizer • Aerosol is introduced into a plasma which excites the atomic species in the aerosol
  8. 8. Materials Characterization Lab www.mri.psu.edu/mcl Plasma Torch
  9. 9. Materials Characterization Lab www.mri.psu.edu/mcl Optical Path in Leeman PS3000UV
  10. 10. Materials Characterization Lab www.mri.psu.edu/mcl Spectrum as dispersed by diffraction grating
  11. 11. Materials Characterization Lab www.mri.psu.edu/mcl Elements by ICP-AES core electrons
  12. 12. Materials Characterization Lab www.mri.psu.edu/mcl Common Problems in ICP-AES Sampling and Sample Preparation Spectral Interference Matrix Effects Instrumental Drift
  13. 13. Materials Characterization Lab www.mri.psu.edu/mcl Sampling and Sample Preparation Are the samples representative of what you are trying to measure? What steps should MCL take to make your samples representative? Will any elements volatilize during sample preparation? How much contamination can the sample tolerate during preparation?
  14. 14. Materials Characterization Lab www.mri.psu.edu/mcl Spectral Interference Some elemental lines may interfere with others. Best solution is to find another spectral line. Samples should be scanned for possible problems Concepts, Instrumentation, and Techniques in Inductively Coupled Plasma Optical Emission Spectrometry, Boss and Freeden, Perkin Elmer
  15. 15. Materials Characterization Lab www.mri.psu.edu/mcl Matrix Effects Differing viscosities can affect amount of sample uptake Matrices can change nature of plasma Certain matrices (HF) can attack torch Matrices can contain interfering spectral components
  16. 16. Materials Characterization Lab www.mri.psu.edu/mcl Combined Effects Concepts, Instrumentation, and Techniques in Inductively Coupled Plasma Optical Emission Spectrometry, Boss and Freeden, Perkin Elmer
  17. 17. Materials Characterization Lab www.mri.psu.edu/mcl Instrumental Drift Instrument reading can drift over a period of time due to physical changes in the optical system, or the configuration of the plasma. Standards need to be run at the beginning and end of each run in order to estimate and correct for this drift.
  18. 18. Materials Characterization Lab www.mri.psu.edu/mcl Compensation Standards run with every sample run Drift Correction taken with every sample run Matrix of standards should be closely matched with that of the samples Preliminary scans are taken to see if any spectral overlaps occur
  19. 19. Materials Characterization Lab www.mri.psu.edu/mcl Basic Analytical Scheme Concepts, Instrumentation, and Techniques in Inductively Coupled Plasma Optical Emission Spectrometry, Boss and Freeden, Perkin Elmer
  20. 20. Materials Characterization Lab www.mri.psu.edu/mcl Sample Dissolution for Solid Samples Salt Fusions – typically lithium metaborate and sodium peroxide Acid Digestions – nitric, hydrochloric, perchloric and hydrofluoric Microwave Digestion – basically acid digestion in controlled temperature and pressure vessels. Samples are typically dried, ashed if necessary, and ground to <74 microns prior to dissolution procedures
  21. 21. Materials Characterization Lab www.mri.psu.edu/mcl Salt Fusion Sample is mixed with lithium metaborate in a 1:9 ratio Mix is melted at 900C and dissolved in a nitric acid solution Pros: Attacks geologicals and most ceramics Provides a high concentration salt environment which dampens any intersample matrix differences. Cons: Easily volatilized elements cannot be determined High metal contents may prove difficult
  22. 22. Materials Characterization Lab www.mri.psu.edu/mcl Graphite crucible with lithium metaborate in furnace
  23. 23. Materials Characterization Lab www.mri.psu.edu/mcl Acid Digestion Sample is allowed to dissolve in an acid mix. Sample is typically heated to speed dissolution. Pros: Most direct dissolution, minimizing possible introduction of contaminants Usually best for metals Cons: Ineffective against geologicals and ceramics, especially if Si is to be determined Can be time consuming
  24. 24. Materials Characterization Lab www.mri.psu.edu/mcl Acid digestion in a Pt dish
  25. 25. Materials Characterization Lab www.mri.psu.edu/mcl Microwave Digestion Sample is allowed under controlled temperature and pressure conditions in a pressure vessel. Pros: Effective for a wide range of materials, especially those containing organics Direct method of dissolution, minimizing introduction of contaminants Cons: Time consuming method development Labor intensive
  26. 26. Materials Characterization Lab www.mri.psu.edu/mcl MARS 5 Microwave Digestion System
  27. 27. Materials Characterization Lab www.mri.psu.edu/mcl Data Reduction Concepts, Instrumentation, and Techniques in Inductively Coupled Plasma Optical Emission Spectrometry, Boss and Freeden, Perkin Elmer
  28. 28. Materials Characterization Lab www.mri.psu.edu/mcl What do the data mean? Precision and accuracy •Precision is how well the instrument replicates data over time •Accuracy is how close to the true value the observed results will be •Precision is generally on the order of 2 to 5 relative weight percent •Precision will vary from sample type to sample type depending on a number of factors
  29. 29. Materials Characterization Lab www.mri.psu.edu/mcl Typical Analytical Data Sample 1st 2nd 3rd Mean Extrapolated 04-1141 2.788 2.728 2.739 2.743 2.76 04-1152 .279 .269 .268 .272 .27 04-1160 1.112 1.112 1.118 1.114 1.12 blank -.0005 -.0004 -.0003 -.0004 -.01
  30. 30. Materials Characterization Lab www.mri.psu.edu/mcl Typical applications of ICP-AES/ICP-MS • Natural Waters • Saline Brines • Geological Materials • Ceramics and glasses • Coals and Paper Products
  31. 31. Materials Characterization Lab www.mri.psu.edu/mcl Natural Waters •Leaching from mine sites •Geochemical prospecting •Sediment analyses
  32. 32. Materials Characterization Lab www.mri.psu.edu/mcl More Sample Types Discarded candy wrappers Glass and geologicals
  33. 33. Materials Characterization Lab www.mri.psu.edu/mcl Strengths of ICP-AES • Can detect most cations and some anions • Detection Limits down to parts per trillion for some elements • Rapid simultaneous determination of selected elements • Selective determination of other elements in sequential mode • Good linear range – up to hundreds of ppms for alkalis • Suitable for routine analyses of multiple samples • Effective screening tool for ICP-MS samples
  34. 34. Materials Characterization Lab www.mri.psu.edu/mcl Weaknesses of ICP-AES • Not effective for low levels of alkalis (less than 1-5 ppm) • subject to matrix problems • suitable standards required on every run • Only elemental data is provided - no direct structural information • Does not provide, in most cases, parts per billion or parts per trillion data
  35. 35. Materials Characterization Lab www.mri.psu.edu/mcl MCL capabilities: Leeman Laboratories PS3000UV for ICP-AES Lithium Metaborate and Sodium Peroxide Fusion capabilities. Acid Digestion Facilities MARS Microwave Digestion Capabilities
  36. 36. Materials Characterization Lab www.mri.psu.edu/mcl How to get started 1) contact myself, or John Kittleson to discuss your needs 2a) attend regular training session OR 2b) have one of us perform analysis and data interpretation 3) provide budget and fund number to keep us from getting yelled at.
  37. 37. Materials Characterization Lab www.mri.psu.edu/mcl Acceptable sample forms: Solutions, preferably aqueous based with minimal or no HF Minimal solution volume is 3-4 ml or more depending on analyses Solids, can usually be dissolved using various techniques
  38. 38. Materials Characterization Lab www.mri.psu.edu/mcl www.mri.psu.edu/mcl Henry Gong 312 Hosler Bldg 865-1981 hxg3@psu.edu
  39. 39. Materials Characterization Lab www.mri.psu.edu/mcl Elemental Analyses by High Resolution ICP-MS John Kittleson 317 Holser Building 865-3385 jlk38@psu.edu July 27, 2005
  40. 40. Materials Characterization Lab www.mri.psu.edu/mcl Summer Characterization Open Houses Technique Time Date Location Thermal analysis (TGA, DTA, DSC) 9:45 AM June 8 250 MRL Bldg. Transmission Electron Microscopy (TEM/STEM) 9:45 AM June 15 114 MRI Bldg Scanning electron microscopy (SEM) 9:45 AM June 22 541 Deike Bldg. Analytical SEM 11:00 AM June 22 541 Deike Bldg. X-ray Diffraction (XRD) 9:45 AM June 29 250 MRL Bldg. Dielectric Characterization (25 min lecture only) 9:45 AM July 6 250 MRL bldg. High temperature sintering lab (20 min lecture only) 10:15 AM July 6 250 MRL Bldg. Focused Ion Beam (FIB) 9:45 AM July 13 114 MRI Bldg TEM sample preparation 11:00 AM July 13 114 MRI Bldg Orientation imaging microscopy (OIM/EBSD) 9:45 AM July 20 250 MRL Bldg. Chemical analysis (ICP, ICP-MS) 9:45 AM July 27 541 Deike Bldg. Atomic Force Microscopy (AFM) 9:45 AM August 3 114 MRI Bldg Small angle x-ray scattering (SAXS) 9:45 AM August 10 541 Deike Bldg. Particle Characterization 9:45 AM August 17 250 MRL X-ray photoelectron spectroscopy (XPS/ESCA) 9:45 AM August 24 114 MRI Bldg Auger Electron Spectroscopy (AES) 11:00 AM August 24 114 MRI Bldg NOTE LOCATIONS: The MRI Bldg is in the Innovation Park near the Penn Stater Hotel; MRL Bldg. is on Hastings Road. More information: www.mri.psu.edu/mcl
  41. 41. Materials Characterization Lab www.mri.psu.edu/mcl Materials Characterization Lab Locations Bldg Telephone MRL 863-7844 MRI 865-0337 MRI Bldg: Hosler 865-1981 XPS/ESCA, SIMS, E&ES 863-4225 TEM, HR-TEM, FE- Auger, AFM, XRD MRL Bldg: Hosler Bldg: SEM, XRD, OIM, DTA, SEM, ESEM, FE- DSC, TGA, FTIR, Penn Stater SEM, EPMA, ICP, Hotel Raman, AFM, Powder, E&ES Bldg: ICP-MS,BET, SAXS dielectric, prep, shop, SEM IC, UV-Vis Route 322 Steidle Bldg: Atherton Street Nanoindenter (322 Business) I-99 Park Ave. 0 0 0 0 0 0 0 Ave. 0 0 0 0 0 Park 0 Beaver 0 0 Stadium 0 0 0 Centre 0 0 Porter Road Community Univ Shortlidg Hospital 0 0 Burrowes Road ersi ty D e Pollock Road Road rive North Hastin Deike Bldg: gs Ro ad College Ave.
  42. 42. Materials Characterization Lab www.mri.psu.edu/mcl Outline ― High Resolution ICP-MS Overview ― Challenges ― Applications ― Laser Ablation
  43. 43. Materials Characterization Lab www.mri.psu.edu/mcl HR-ICP-MS The Promise • Bulk elemental analysis: Everything in Everything (almost) • Low detection limits • Accurate and precise quantification • Precise isotopic analysis
  44. 44. Materials Characterization Lab www.mri.psu.edu/mcl Finnigan HR-ICP-MS Element Layout
  45. 45. Materials Characterization Lab www.mri.psu.edu/mcl Sampler Cone, ~1mm orifice Plasma side at 1 atm, back side at ~10-4 mbar
  46. 46. Materials Characterization Lab www.mri.psu.edu/mcl Plasma Interface Ions produced by plasma are sampled directly!
  47. 47. Materials Characterization Lab www.mri.psu.edu/mcl Nebulizer and spray chamber attached to torch
  48. 48. Materials Characterization Lab www.mri.psu.edu/mcl Spectrum
  49. 49. Materials Characterization Lab www.mri.psu.edu/mcl Ni60
  50. 50. Materials Characterization Lab www.mri.psu.edu/mcl ICP-MS IDLs
  51. 51. Materials Characterization Lab www.mri.psu.edu/mcl ICP-MS Challenges ― Spectral Interferences ― Matrix Effects
  52. 52. Materials Characterization Lab www.mri.psu.edu/mcl Spectral Interferences Fe56 @ 55.93494 Ar40O16 @ 55.95729 Required resolution = ~2,500
  53. 53. Materials Characterization Lab www.mri.psu.edu/mcl Spectral Interferences Fe56 @ 55.93494 Ar40O16 @ 55.95729 Element using medium resolution
  54. 54. Materials Characterization Lab www.mri.psu.edu/mcl Spectral Interferences As75 @ 74.92160 Ar40Cl35 @ 74.93123 Required resolution = ~7,800
  55. 55. Materials Characterization Lab www.mri.psu.edu/mcl Spectral Interferences As75 @ 74.92160 Ar40Cl35 @ 74.93123 Element using high resolution
  56. 56. Materials Characterization Lab www.mri.psu.edu/mcl Spectral Interferences Other methods: -Mathematical interference corrections, based on isotopic ratios, e.g. Rb87 corrected for Sr87 using Sr88 and natural isotopic abundances. -Matrix removal, eg hydride generation (for As, Se, Ge) and chromatographic separations. -Collision/Reaction cells (on quadrupole instruments)
  57. 57. Materials Characterization Lab www.mri.psu.edu/mcl Matrix effects ― Viscosity effects sample uptake rate. Use internal standard. ― Matrix can effect rate of ionization in plasma. Use good internal standard ― Matrix can contain interfering spectral components. Remove matrix. ― Calibration standards must be matrix matched, or calibration performed by standard addition.
  58. 58. Materials Characterization Lab www.mri.psu.edu/mcl Strengths of High Resolution ICP-MS • Relatively free from spectral interferences • Detection Limits down to parts per quadrillion for some elements • Good linear range (over 9 orders of magnitude) • Rapid determination of many elements • Solid sampling possible via laser ablation Weaknesses of High Resolution ICP-MS • Expensive, fragile detector (cannot handle concentrations >1ppm) • Cannot handle high total dissolved solids • Somewhat tedious mass calibrations
  59. 59. Materials Characterization Lab www.mri.psu.edu/mcl Some Applications • Trace metals in biological media (after dilution) • Trace metals in drinking water (direct aspiration) • Wear metals in lubricating oil (via microwave wet ashing) • Trace metals in soil samples (via microwave wet ashing) • Trace elements in glass via laser ablation • Trace metals in native copper fragments via laser ablation
  60. 60. Materials Characterization Lab www.mri.psu.edu/mcl Wear Metals in Lubricating Oil
  61. 61. Materials Characterization Lab www.mri.psu.edu/mcl Laser Ablation ICP-MS
  62. 62. Materials Characterization Lab www.mri.psu.edu/mcl New-Wave Research LUV266X
  63. 63. Materials Characterization Lab www.mri.psu.edu/mcl Raster pattern on NIST SRM 495 Unalloyed Copper
  64. 64. Materials Characterization Lab www.mri.psu.edu/mcl Laser Ablation Highlights • Simplified matrix (reduced spectral interferences) • Minimal sample preparation • Very fast (rinse out times ~ seconds) saves $ • Good calibration standards hard to find • Elemental fractionation • Qualitative analysis (no standards) is easy
  65. 65. Materials Characterization Lab www.mri.psu.edu/mcl How to get started 1) Contact me to discuss your needs 2) Bring me your samples 3) Provide budget and fund number!
  66. 66. Materials Characterization Lab www.mri.psu.edu/mcl Acceptable sample forms: Aqueous Solutions, dilute HCl, HNO3, HF Minimal solution volume depends on concentration Solids and slurries, minimum 100mg, depending on digestion method Some solids may be suitable for laser ablation Rock sections Metal fragments Pressed pellets Anything that can be glued to a petrographic slide!
  67. 67. Materials Characterization Lab www.mri.psu.edu/mcl ICP-MS Fees Instrument time (includes operator) = $90/hr Staff time (sample prep, data workup, digestions, etc) = $30/hr Consultation time to discuss your samples, data, etc is free. Typical ‘Easy’ analysis – low resolution multielement determination of dilute nitric acid solutions as received ~$15/sample) Typical ‘Difficult’ analysis – medium or high resolution scans on complex matrices, or refractory samples requiring digestion ~$50/sample Method development and instrument setup are the most time consuming. Cost per sample goes down with larger sample sets.
  68. 68. Materials Characterization Lab www.mri.psu.edu/mcl www.mri.psu.edu/mcl John Kittleson 317 Hosler Bldg 865-3385 jlk38@psu.edu

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