Sources of Errors in Trace Element and Speciation Analysis

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1 Sources of Errors in Trace Element and Speciation Analysis Zoltan Mester, National Research Council of Canada, Institute for National Measurement Standards Outline Definitions Sources of errors in the analytical process Detection methods in trace element analysis Trace element measurement methods and the associated errors Summary TAQC-WFD, Budapest, November 2-4, Expression of an analytical result Value 1 ± Value 2 Expression of an analytical result Value 1 ± Value 2 Free of systematic error (bias) Uncertainty Free of systematic error (bias) Uncertainty Verification of traceability of the results: CRMs Primary methods (or reference methods) Consideration of all sources of error of the analytical process: 1. Random errors: Method precision 2. Correction of systematic errors Verification of traceability of the results: CRMs Primary methods (or reference methods) Consideration of all sources of error of the analytical process: 1. Random errors: Method precision 2. Correction of systematic errors 3 4 1

2 Measurand Particular quantity subject to measurement Measurement Set of operations having the object of determining a value of a quantity Result of a measurement Value attributed to a measurand, obtained by measurement Uncertainty (of measurement) Parameter associated with the result of a measurement, that characterises the dispersion of the values that could reasonably be attributed to the Measurand Conventional true value (assigned value, best estimate of the value, conventional value or reference value) Value attributed to a particular quantity and accepted, sometimes by convention, as having an uncertainty appropriate for a given purpose. Error (of measurement) The result of a measurement minus a true value of the measurand Systematic error Mean that would result from an infinite number of measurements of the same measurand carried out under repeatability conditions minus a true value of the measurand 5 6 Arithmetic mean x Arithmetic mean value of a sample of n results Sources of Errors in Trace Element and Speciation Analyses Sample Standard Deviation s An estimate of the population standard deviation σ from a sample of n results

3 Sources of Errors in Trace Element and Speciation Analyses Sources of Errors in Trace Element and Speciation Analyses Perhaps Perhaps it should be Sources of Errors and Uncertainities in Trace Element and Speciation Analyses 9 10 (i) (ii) (iii) (iv) It is easy to recognize that increasing the complexity of an analytical protocol (i.e.: more steps during the analytical process) increases the chance of errors. In an ideal situation, analytical measurements would be done: in-situ, removing the issues related to sampling and sample integrity. Directly in the matrix even for solids, without extensive sample preparation such as leaching, decomposition, etc. Using highly selective, absolute measurements, with the dynamic range of the measurement method extending from percentage to ppt levels, thus removing potential sources of error due to interferences, calibration etc. without human intervention, i.e., automated, removing the human variable from the system. (i) (ii) (iii) (iv) It is easy to recognize that increasing the complexity of an analytical protocol (i.e.: more steps during the analytical process) increases the chance of errors. In an ideal situation, analytical measurements would be done: in-situ, removing the issues related to sampling and sample integrity. Directly in the matrix even for solids, without extensive sample preparation such as leaching, decomposition, etc. Using highly selective, absolute measurements, with the dynamic range of the measurement method extending from percentage to ppt levels, thus removing potential sources of error due to interferences, calibration etc. without human intervention, i.e., automated, removing the human variable from the system

4 Overview of the analytical process Overview of the analytical process Sampling Sample preparation Instrumental analysis Data evaluation Sampling Sample preparation Instrumental analysis Data evaluation Sampling and sample preparation are by far the largest contributors to measurement errors and uncertainty!!!! Contamination, sample loss -Sample Container Material -Container Transpiration -Stability of Metals at ppb Concentration Levels -Environmental Contamination -Contamination From Reagents -Contamination From the Analyst and Apparatus Overview of the analytical process Sampling Sample preparation Instrumental analysis Data evaluation

5 Detection Technologies Optical Absorption, AA, GF-AA Emission, ICP, Flame Fluorescent, Mass spectrometry ICP GD MIP Atomic Absorption spectrometry (AA) Discovered in the late fifties Shine light specific for an element through an atom reservoir (flame or furnace) Light is absorbed by the ground state atoms of given element The absorption rate is proportional with the number of analyte atoms in the atom source AA FAST, (seconds per determination) Low cost per analysis Low capital investment and low operating cost Single element determination Easy to use Well understood interferences (mature technique) Versatile Requires separate lamp for each element to be determined Hollow Cathode (HCL) or Electrodeless Discharge Lamp (EDL) Interferences Technique Type of Interference Compensation Method Flame AA Ionization Ionization buffer Chemical Releasing agent or nitrous - oxide-acetylene flame Physical Dilution, matrix matching or method of additions

6 Graphite Furnace Atomic Absorption (GF-AAS) Low detection limits for most elements parts per billion (μg/l) Slower then flame analysis Min per determination Single element determination Small sample volume (μl) Interferences Cost per analysis higher than Flame AA More technical experience needed Interferences Technique Type of Interference Compensation Method GFAA Molecular absorption background correction Matrix interferences modifiers Special case of AA or AFS Dedicated system for cold vapor Hg analysis Detects ppt levels of Hg High intensity Hg lamp Long path length cell Solid state detector Extremely sensitive but prone to matrix interferences Inductively Coupled Plasma Optical Emission Spectrometry ICP is an argon gas discharge (~6-9000K) Excites atoms in sample and Light being emitted. The emitted light is separated and measured. Wavelengths are characteristic of element Intensity of light emitted is proportional to amount of element in the sample

7 ICP-OES Fast or very fast analysis time Many elements in a few minutes Low detection limits Parts per billion in axial view mode Wider dynamic range Over 3 times better than flame AA (Two viewing options) Cost per analysis Comparable to flame AA Lower than GF AA Some technical experience needed Interferences Technique Type of Interference Compensation Method ICP-OES Spectral Background correction or use of alternate analytical wavelengths Physical Internal standardization Spectrum of a high Ca containing matrix (red line) causing a sloping background for the Cu or Ge lines are used. Background correction is difficult at best in these situations. 27 Spectrum of a high concentration of Fe (red line) showing a direct spectral overlap upon the B line and a wing overlap on a B

8 Wing overlap interference of Fe (red line) upon the Ba nm line Overview of ICP-OES Detection limits not as good as GFAA or ICP-MS Some specific applications require lower detection limits Some elements in line-rich area of spectrum Thousands of wavelengths for Fe Rare earths (Dy, Eu, La, Ce) Interferences for particular elements Transuranics (U, Am, Pu, Tc) Sensitivity for some elements not sufficient Halogens Higher initial investment than AA More gas consumption than AA Requires ~16 L/min of argon gas Advantages of ICP-OES Multielement technique Speed samples can be analyzed in seconds to minutes Excellent linear dynamic range up to mg/l Detection limits moderate to excellent ug/l Interferences spectral interferences controlled through instrument design / software Plasma view: axial or radial axial view has lower DLs radial view has wider linear range and less interferences Lower cost per (similar to AA)

9 Nebulizers ICP-MS Same type of plasma source as in ICP-OES Ions are generated by intense ICP ion source, separated and detected by a mass spectrometer Nebulizers The main function of the sample introduction system is to generate a fine aerosol of the sample. It achieves this purpose with a nebulizer and a spray chamber Nebulizers generate an aerosol from the aqueous sample and spray chambers filter out heavy droplets and dampen noise. In general, nebulizers designed for use with ICP-OES are not recommended for ICP-MS 1-2% total dissolved solids (TDS) for OES and only % for MS Nebulizers Concentric design. In the concentric nebulizer,the solution is introduced through a capillary tube to a low-pressure region created by a gas flowing rapidly past the end of the capillary. Concentric pneumatic nebulizers can provide excellent sensitivity and stability, particularly with clean solutions. However, the small orifices can be plagued by blockage problems, especially if large numbers of heavy matrix samples are aspirated

10 Nebulizers Crossflow design. For samples that contain a heavier matrix or small amounts of undissolved matter, the crossflow design is probably the best option. With this design the argon gas is directed at right angles to the tip of a capillary tube, in contrast to the concentric design, where the gas flow is parallel to the capillary. Spray chambers Crossflow nebulizers are generally not as efficient as concentric nebulizers at creating the very small droplets needed for ICP-MS analyses. 37 Schematic of a cyclonic spray chamber (shown with concentric nebulizer). 38 Spray chambers Ion source Schematic of a Scott double-pass spray chamber (shown with crossflow nebulizer

11 Plasma Plasma Mass analyzer is the region of the ICP mass spectrometer that separates the ions according to their mass to charge ratio (m/z)

12 Mass analyzers Quadrupole Quadrupole TOF (Iinerar, ortogonal) Sector instruments Schematic of a quadrupole mass analyzer Sensitivity comparison of a quadrupole operated at 3.0, 1.0, and 0.3 amu resolution (measured at 10% of its peak height) Quads are low res analyzers 47 Ions entering the quadrupole are slowed down by the filtering process and produce peaks with a pronounced tail or shoulder at the low-mass end. The abundance sensitivity for quadrupoles is always worse on the low mass side than on the high mass side and is typically 1 x 10-6 at M - 1 and 1 x 10-7 at M

13 Sector instruments Schematic of a double-focusing magnetic-sector ICP mass spectrometer Why we need high mass resolution? Resolution required to resolve some common polyatomic interferences from a selected group of isotopes

14 Q Ion transmission with a magneticsector instrument decreases as the resolution increases. HR TOF (on-axis, ortogonal design) Schematic of an orthogonal acceleration TOF analyzer

15 m/z = 2Ut 2 /D 2 Where (U) is the accelerating voltage, mass-to-charge ratios (m/z), time (t), length of the flight path (D) Schematic of an on-axis acceleration TOF analyzer Mass analyzer Resolution Quad TOF Sector 10,000 Reflectron TOF MS design

16 Resolution required to resolve some common polyatomic interferences from a selected group of isotopes. ICP-Mass Spectroscopy Overview Very fast analysis Comparable to simultaneous ICP-OES Superior detection limits Parts per trillion Semi-Quant analysis Isotope analysis Cost per analysis Same as ICP-OES Some technical experience required Technique Type of Interference Compensation Method ICP-MS Mass Overlap Interelement correction, use of alternate mass values or higher mass Resolution Dynamic Reaction Cell Physical Internal Standardization

17 ICP MS Very fast analysis Comparable to simultaneous ICP-OES and standard ICP-MS Superior detection limits Up to parts per quadrillion Removes isobaric and argon interferences Cost per analysis Slightly more than standard ICP-MS Some technical expertise required

18 Flame AA A few elements per sample to analyze 5 ml/min sample consumption Detection levels needed are in the sub-mg/l region GFAA Detection levels of μg/l to sub- μg/l levels ul sample consumption ICP-OES Several elements per sample (5+) 1-5 ml/min sample consumption Detection levels are in the sub-mg/l and μg/l region ICP-MS Detection levels of sub- μg/l to sub-ng/l levels Typical 1-2 ml/min sample consumption Can use low consumption nebulizers 69 Interferences in ICP MS Isobaric Interferences Polyatomic (Molecular) Interferences Doubly Charged Ion Interferences 70 Isobaric Interferences: Isobaric interference is a result of equal mass isotopes of different elements present in the sample solution. Low-resolution instruments (quad, TOF) cannot distinguish between the isotopes. There are many examples in the intermediate mass regions where the second and third row transitions and the rare earths appear. There are no elemental singly charged isotopes that overlap with monoisotopic elements (9Be, 23Na, 27Al, 45Sc, 55Mn, 75As, 89Y, 103Rh, 127I, 133Cs, 141Pr, 159Tb, 165Ho, 169Tm, 197Au, and 232Th). For elements having more than one isotope, the quickest fix may be to use another isotope of that element. Isobaric Interferences: If the interference is from an isotope with roughly the same or lower peak intensity, it is possible to perform a correction by measuring the intensity of another isotope of the interfering element and subtracting the appropriate correction factor from the intensity of the interfered isotope. If you are working with an unknown sample composition, a semi-quantitative analysis is suggested with low-resolution instruments using a quick scan of the sample and the rather sophisticated semi-quantitative programs available on current instrumentation

19 Polyatomic (Molecular) Interferences: Molecular interferences are due to the recombination of sample and matrix ions with Ar and other matrix components such as O, N, H, C, Cl, S, F, etc. The light elements (Li, Be, B) are not affected due to their small masses. Starting with 39K, this type of interference becomes a significant issue. For example, 39K is interfered with by 38ArH and 23Na16O. Some polyatomic interferences can be avoided by eliminating certain matrix elements such as the classic 40Ar35Cl interference upon the monoisotopic element 75As, where the use of HCl in the sample preparation is to be avoided. The isotopes 56Fe, 39K, and 44Ca or 40Ca are all interfered with by combinations of the Ar, O, and N isotopes. 73 Polyatomic (Molecular) Interferences: As we go to the heavier elements the major polyatomic interferences come from isotopes that are 16 atomic mass units lower than the analyte isotope through molecular oxide (MO) interference. The lanthanide element isotopes are especially prone to molecular oxide formation. The use of cool plasma techniques, reaction / collision cells, desolvation, and chromatographic separations -- to name a few approaches -- have resulted in reduction and, in some cases, complete elimination of many polyatomic interferences. 74 Polyatomic (Molecular) Interferences: The severity of the MO interference can be reduced through reduction of the sample argon gas flow rate. Mass corrections may be an option in cases where the use of an alternate isotope is not an option. Polyatomic interferences are particularly troublesome in the determination of first row periodic table elements (K thru Se) due to the vast number of combinations of Ar with matrix components. Doubly Charged Ion Interferences: Doubly charged ion interference is due to doubly charged element isotopes with twice the mass of the analyte isotope. For example, interference from 206Pb++ (m/e = 103) upon 103Rh is likely at high Pb concentration levels. Reduction in the sample Ar will minimize this interference. Fortunately, this type of interference is not as prominent in Ar plasmas, but care should be exercised in matrices containing high levels of mid to heavy mass element isotopes. The alkaline and rare earth elements form doubly charged ions to a extent that is greater, relative to the other elements

20 ICP MS background mass spectrum of high-purity water. 77 Common polyatomic spectral interferences in ICP-MS. 78 Space Charge Effects: These effects are thought to occur at the MS interface, the region between the skimmer tip and ion optics and in the ion optics region. The net result is a suppression of the signal in high concentrations of a matrix element. The kinetic energy of the ion element matrix affects the degree of suppression with larger masses (higher kinetic energy) causing more depression than lower masses. Due to differences between instruments in interface and ion optic designs it is difficult to predict the conditions under which the effect is minimal. Under 'cool plasma' conditions, this suppression effect is more pronounced. Keep the matrix element concentration at or below the 100 µg/g! 79 How to eliminate spectral interferences? isobaric interferences from isobaric element ions cannot be eliminated easily solution: use an other isotope if you can Front end solutions (chromatography, hydride generation etc) polyatomic interferences could be eliminated by solution: cool plasma conditions increased mass resolution gas phase chemistry 80 20

21 How to eliminate spectral interferences? Collision/Reaction Cell Technology isobaric interferences from isobaric element ions cannot be eliminated easily solution: use an other isotope if you can Front end solutions (chromatography, hydride generation etc) polyatomic interferences could be eliminated by solution: cool plasma conditions increased mass resolution gas phase chemistry Examples of polyatomic interferences: 40Ar16O on the determination of 56Fe 38ArH on the determination of 39K 40Ar on the determination of 40Ca 40Ar40Ar on the determination of 80Se 40Ar35Cl on the determination of 75As 40Ar12C on the determination of 52Cr 35Cl16O on the determination of 51V. Elimination of the ArO interference with a dynamic reaction cell

22 Calibration Collision/reaction cells have given a new lease on life to quadrupole mass analyzers used in ICP-MS External Calibration: Use this approach for matrices that are known and can be matched. The use of internal standards is helpful in accounting for drift. Must know your sample composition! A semi-quantitative analysis using a scanning approach for the entire mass range allows the analyst to predict interferences and select internal standards and analyte isotopic masses. Perform interference check analysis. Prepare for the variations in the matrix and analyte composition and determine if corrections that have been built into the procedure are capable of providing the required accuracy. External Calibration: Use this approach for matrices that are known and can be matched. The use of internal standards is helpful in accounting for drift. Must know your sample composition! A semi-quantitative analysis using a scanning approach for the entire mass range allows the analyst to predict interferences and select internal standards and analyte isotopic masses. Perform interference check analysis. Prepare for the variations in the matrix and analyte composition and determine if corrections that have been built into the procedure are capable of providing the required accuracy. Simple and cheap BUT prone to interferences

23 Standard Additions: This approach is common with ICP-OES & ICP-MS. Could correct interferences but not for instrument drift Isotope Dilution: Isotope dilution in mass spectrometry is a type of internal standardization. ID is a primary (definitive) analytical method for the determination of metals in a variety of sample types. (other primary analytical methods are gravimetry, titrimetry, coulometry, differential scanning calorimetry) and nuclear magnetic resonance spectroscopy. Only applicable for multi isotope elements. (not for: 9Be, 23Na, 27Al, 45Sc, 55Mn, 75As, 89Y, 103Rh, 127I, 133Cs, 141Pr, 159Tb, 165Ho, 169Tm, 197Au, and 232Th) ID could correct both for systematic and random errors in the analysis. But it is expensive and involves complicated mathematics Expression of an analytical result Value 1 ± Value 2 Free of systematic error (bias) Verification of traceability of the results: CRMs Primary methods (or reference methods) Uncertainty Consideration of all sources of error of the analytical process: 1. Random errors: Method precision 2. Correction of systematic errors Thank you for your attention!

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