Atomic Absorption Techniques & Applications

Atomic Absorption Techniques & Applications

1. AA Techniques & Applications

2. Thanks To everyone who has helped us with support, new books, hard/soft ware And over the internet Special thanks for THERMO

3. Contents Introduction Theory AAS Setup Validity Accessories Techniques and facilities Software Application Air Water & Soil Foods Clinical Petrochemicals Pharmaceutical

4. Introduction

5. Metals Metals account for about two thirds of all the elements and about 24% of the mass of the planet. Metals have useful properties including strength, ductility, high melting points, thermal and electrical conductivity, and toughness. From the periodic table, it can be seen that a large number of the elements are classified as being a metal.

6. Abundance of Metals in Earth’s crust 3. Aluminum (7.5%) 4. Iron (4.71%) 5. Calcium (3.39%) 6. Sodium (2.63%) 7. Potassium (2.4%) 8. Magnesium (1.93%) 10. Titanium (0.58%) 13. Manganese (0.09%)

7. Abundance of Metals in the Human Body Calcium (1.4%) Magnesium (0.50%) Potassium (0.34%) Sodium (0.14%) Iron (0.004%) Zinc (0.003%)

8. Toxic and nutrition elements Toxic metals Pb, Cd, As, Hg, Al, Cr, Cu Low PPM levels in original material Recent interest in radio-nuclides Pu, Am and Np. Cs-137, Cs-134, Sr-90 and K-40 Nutrition elements Ca, Mg, Na, K, P %age to high PPM levels in original material Micro-nutrients Zn , Se, Mo, etc… high PPM to PPB levels in original material

9. Heavy metals Heavy metals are natural components of the Earth's crust. They cannot be degraded or destroyed. To a small extent they enter our bodies via food, drinking water and air. As trace elements, some heavy metals (e.g. copper, selenium, zinc) are essential to maintain the metabolism of the human body. However, at higher concentrations they can be toxic.

10. Theory

11. Absorption The process whereby the intensity of a beam of electromagnetic radiation is attenuated in passing through a material medium by conversion of the energy of the radiation to an equivalent amount of energy appearing within the medium; the radiant energy is converted into heat or some other form of molecular energy.

12. The beer – Lambert Law The absorption that takes place in an atomic absorption system follows beer law. A beam of light with intensity I is aimed at the tested solution placed in a cuvette. The intensities of the entering beam I and the emerging beam I 1 are measured, and the absorbance A - is calculated from the ratio of the two A = - log (I 1 /I ) Different molecules absorb radiation of different wavelengths. An absorption spectrum will show a number of absorption bands corresponding to structural groups within the molecule

13. Atomic Absorption Atomic absorption spectrometry (AAS) is an analytical technique used to measure a wide range of elements concentration in samples.

14. Atomic Absorption Atomic absorption Mean “The free atoms ( Atomic )of the sprayed element solution Absorbed ( Absorption )the radiation of the Hollow cathode lamp”

15. Periodic table 70 elements can be analyze using AA About 80 of the 106 elements are metals

16. Calibration Optical absorption spectrometry is a comparative technique in which the signals by solutions of known concentrations used to generate a calibration curve is compared to the signals of unknown samples to generate results.

17. AA Setup

18. AA Steps The sample is weighed and then dissolved. The resulting solution is sprayed into the flame and atomized. Light of a suitable wavelength for a particular element is shone through the flame, Some of this light is absorbed by the atoms of the sample. The amount of light absorbed is proportional to the concentration of the element .

19. AA main parts Lamp Atomizer Monochromator Photomultiplier tube Optical system Automatic gas control

20. 1. Lamps Hollow Cathode Lamps (HCLs) are high intensity, stable light sources that emit the element specific spectral lines required for Atomic Absorption spectrometry. Provide a constant intense beam of analytical light. There are Coded or uncoded lamps.

21. Deuterium Lamp The deuterium lamp emits radiation extending from 112 nm to 900 nm, although its continuous spectrum is only from 180 nm to 300 nm. The Deuterium lamp emits a blue-white light. However, these lamps are used to produce Ultra-Violet (UV) emissions which we can't see.  The outer lamp envelope is made form quartz rather than glass. because glass does not transmit short wave UV light. What makes Deuterium lamps so special, as a UV source, is its continuous spectrum in the range from 180nm - 300 nm.

22. Background Background interference is caused by either, non-specific absorption arising from light scattering caused by solid particles or liquid droplets in the atomizing cell or, by light absorption caused by molecules or radicals originating in the sample matrix. It is usually measured by separate experiment and subtracted from the absorption of the sample solution.

23. Background Correction The cathode lamp and the deuterium lamp are sequentially pulsed with a chopper or electronically with delay of about 2ms . When hollow cathode lamp is on and deuterium lamp off total absorbance (AA + BG) is measured. When the HCL is off and the deuterium lamp on the continuum energy recorded is (BG). The atomic signal is automatically calculated by subtracting background from total absorbance.

24. Zeeman Background Zeeman Background Correction is used mainly in graphite furnace atomic absorption systems. When an atom is placed in a magnetic field and its absorption of observed in polarised light, the normal single line is split into three components – б-, π and б +displaced symmetrically about the normal position

25. Zeeman Background Correction Free atoms show Zeeman splitting in a magnetic field but molecules, liquid droplets or solid particles show no Zeeman splitting and so advantage can be taken of polarized light. The π component is linearly polarized parallel to the magnetic field while the б components are circularly polarized perpendicular to the magnetic field. A polarizer is positioned in the optical system to remove the π components of the transmitted radiation. This affords background measurement at the exact analyte wavelength when magnetic field is applied. Since the background is measured at the analyte wavelength and not averaged as in D2 system structural molecular background and spectral interferences are easily corrected.

26. 2. Atomizers Metal in the sample must undergo desolation and vaporization in a high-temperature source such as a flame or graphite furnace to be free atoms. Destroy any analyte ions and breakdown complexes Create atoms (the elemental form) of the element of interest

27. Types of Atomizers The main function is generate a free atoms Flame Graphite Hydride System

28. 3. Monochromator A monochromator is an optical device that transmits a mechanically selectable narrow band of wavelengths of light or other radiation chosen from a wider range of wavelengths available at the input. Echelle monochromator provides automatic wavelength and band pass set-up. The high energy Quad Line background correction system corrects for up to 2A of background with less than 2 % error, and is fitted as standard to all instruments.

29. The Grating Grating An optical device within the spectrometer used to separate the emitted light into its component wavelengths. The grating has a dual feature: it diffracts the light and focuses it on the slits. The grating is the main optic part of the spectrometer; It separates the light into all the wavelength that composes it. It Has 1800 grooves/mm.

30. 4. Photo multiplier tube The PMT change the incidence photons into electrical signal As the detector the PMT determines the intensity of photons of the analytical line exiting the monochromator

31. 5. Optical System Furnace Toroid Mirror Flame Toroid Mirror Plane Mirror Rear Beam Selector Furnace Plane Mirror Flame HCL Carousel D 2 Lamp

32. Auto-aligning Optics Perfect setup every time Auto-alignment and memory Lamp carousel for 6 lamps Dedicated power supply for each position Data coding of both element and lamp current High optical modulation frequency

33. 6. Automatic Gas Control Full safety monitoring facilities and safe shutdown. Completely enclosed “kitchen” area. Automatic binary flow gas control system for superb reliability and reproducibility.

34. System Techniques

35. AA Analytical methods A- Flame Atomic Absorption. B- Furnace Atomic Absorption. C- Vapor Atomic Absorption.

36. A- Flame Atomic Absorption Atomization through flame (1) Air- Acetylene (9 psi) . (2) Air- Acetylene -Nitrous oxide Nitrous oxide (N2O) needs to be used instead of air (78% N2 + 21% O2) The level of measuring is about mg/l (ppm) Support gases 1. Air 2.07 bar (30psi) 2. Nitrous oxide 2.75 bar (40psi)

37. Flame System Universal Finned Titanium 50mm burner suitable for air/acetylene and nitrous oxide/acetylene flame types. An inert fluoroplastic spray chamber incorporating an externally adjustable inert impact bead and flow spoiler. An inert over-pressure membrane should be housed in the rear of the spray chamber for maximum operator safety. Automatic gas system using binary flow control and programmable array state logic for reliability Full safety interlocks, including pressure sensors on both lines, power failure protection, burner interlock and flame sensor Fuel and oxidant flow rates software controllable Automatic flame ignition and optimization

38. Flame Control Burner type recognition Gas pressure sensors Auto-ignition of flame Fully automatic gas control Software change over of flame type Auto flame shut down Power failure protection Spray chamber over pressure protection

39. Flame Safety If carbon deposits appear, the flame must be extinguished immediately and the deposits removed. Aspiration of solutions of perchloric acid and metal per chlorates into a nitrous oxide supported flame can increase the risk of explosion or flashback Certain elements, notably Ag, Au and Cu, can form unstable acetylides, increasing the risk of explosion or flashback. The use of organic solvents in flame AAS is an inherently hazardous procedure. The door must be closed when lighting a flame, and during normal operation. All flames produce large quantities of heat and toxic combustion products. These must be removed by a suitable fume extraction system.

40. Burners Two types of burner are available for spectrometer: 5cm slot Universal Titanium Burner suitable for general purpose use with all flame types 10cm slot Titanium Burner suitable for air/acetylene flames only. Sensitivity for elements measured with this flame will be improved compared to the Universal Burner.

41. B- Furnace atomic Absorption Electrothermal atomization (ETA) is a technique for improving the sensitivity and limit-of-detection (1000 times) for atomic absorption measurements. A small amount of sample or standard solution is placed inside a hollow graphite tube. This is resistively-heated in a temperature program to remove liquid, burn off organics, atomize the residuals to form a plume of free metal vapour, detect the metals and finally clean the tube.

42. Furnace main parts The furnace main Technique parts Electrical Thermal heating "power supply”. Furnace head. Auto sampler. Shield and cleaning gas. Cooling system.

43. Furnace System Choice of Deuterium or Zeeman background correction furnaces Mount directly in dedicated compartment Binary flow controlled internal gas system Choice of alternate or inert gases Furnace cycle to allow up to 20 phases to be programmed Cuvette firings counter Furnace auto-sampler to be included with furnace head and power supply Slow injection and uptake options ‘Wash and waste vessels to be part of the auto-sampler system and not occupy extra space on the floor or bench of the laboratory

44. Furnace Program The main four Furnace programs 1. Drying phase, where the sample is warmed to remove the solvent 2. Ashing phase, where as much of the sample matrix as possible is removed 3. Atomization or measurement phase 4. Cleaning phase, where the cuvette is heated to a high temperature to remove any previous sample

45. 1. Furnace power supply Power 200/220/240V at 50/60 Hz, 30A Single phase. Power consumption 7.2kVA. GF95Z - additional 1.5kVA Description All cuvettes mount directly in an all-graphite containment with end loaded contacts. Cuvettes are self aligning, and can be rapidly exchanged with a single lever movement. The binary flow controlled internal gas system, with gas stop, offers a choice of the inert gas or an alternate gas, and the fixed external inert gas flow protects the cuvette and purges the optical temperature sensor.

46. 2. Furnace Head Dynamic, optical cuvette temperature control, pre-heated cuvette injection and coolant water temperature compensation optimize analyses All graphite containment reduces contamination risk Very wide range of alternative cuvettes: Extended Lifetime Cuvettes (ELC) provide uninterrupted overnight analysis and lower cost of ownership Ash/Atomize self-optimization with SOLAAR software Maximum furnace sensitivity and the widest furnace dynamic working range Correction up to 2A of background, with <2% residual error for even the fastest transient signals The optional Zeeman Background Correction is performed at the exact analyte wavelength

47. The Zeeman Background The Zeeman background is the splitting of spectral lines into several polarized components as a result of the effect of an applied magnetic field. On the application of the magnetic field a central line appears at the same wavelength as the original line (the π line) having half the intensity of the original line. On either side of the π line appears two other lines (the σ ± lines) having one quarter of the intensity of the original line. The π line is linearly polarized with the electric vector parallel to the magnetic field and the σ ± lines are circularly polarized at right angles to the direction of the magnetic field. the π line is absorbed by both sample and back ground whereas the σ ± components are only absorbed by the background.

48. Zeeman Background The magnet fitted to the GF95Z Zeeman Furnace Head produces a variable magnetic field up to 0.85 Tesla at mains frequency during the atomization and auto zero phases. This can affect other electronic systems in the vicinity.

49. Cuvettes Normal Cuvettes (Electro graphite) Volatile elements Coated Electro graphite (Pyrolytically coated) Carbide forming elements Medium volatile Refractory elements Extended Life-time Cuvettes (ELC’s) More stable Omega Platform ELC’s Volatile elements in ‘heavy’ matrices

50. 3. Autosampler Features of the Furnace Autosampler 1- Automatic matrix modification - wet and dry mixing options . 2- Automatic standard preparation - fixed and variable volume may be used 3- Automatic re-concentration of samples, using multiple injections . 4- Automatic, intelligent dilution of samples 5- Automatic standards addition preparation 6- Automatic re-scale and re-calibration

51. 4. Argon Gas This protects the hot cuvette from atmospheric oxygen, and flushes sample vapours from the cuvette interior. Argon is recommended; nitrogen can be used with some loss of performance for some elements. Connect the inert gas supply to the inlet port labeled ARGON 2 at the rear of the Furnace Power Supply unit. The inert gas supply must be regulated to 1.1±0.14 bar (15±2 psi).

52. 5. Cooling System A supply of reasonably clean (e.g. drinking) water, at a temperature of less than 30ºC and a pressure of 1.4 to 6.9 bar (20 - 100psi), capable of providing a minimum flow rate of 0.7l/min is required. Do not allow the pressure to exceed 6.9 bar (100 psi). Connect the cooling water inlet and outlet hoses to the water inlet and outlet connections on the Furnace Power Supply unit. Recirculators The Furnace can be cooled by a temperature controlled Recirculators/chiller unit instead of mains water. Set the recirculating water temperature to about 5ºC above ambient temperature, providing that this is less than 30ºC.

53. Chiller An air-cooled re-circulating water chiller shall be provided to cool. suitable for operation with an ambient temperature range +15 C to + 35 C Highly efficient cooling Accurate temperature control Environmental friendly (CFC - free) Quiet operation

54. C- Vapor Atomic Absorption Parts per billion sensitivities for a number of environmentally important elements are not attainable by conventional flame atomic absorption spectrometry and alternative techniques have to be used. Hydride generation AAS is applicable to mercury and the arsenic group elements, and provides cost effective analysis with sub-ppb detection limits. The elements that can be determined with the VP100 are those that can form gaseous hydrides, or in the case of mercury, a mono-atomic vapour. These include As, Se, Bi, Te, Sb, Sn, and Hg.

55. Vapor AA Detection limits typically 1000x better than those achieved by conventional flame analysis Hydrochloric acid + sodium borohydride unstable hydride of 8 elements give free atoms Hg - As - Se – Sb Ge - Bi - Sn – Te For a volatile elements in the range of ug /l (ppb)

56. Vapor Reaction As 3 + NaBH 4 AsH 3 (gas) + B 2 H 6 AsH 3 (gas) As + 3/2 H 2 The arsenic ions are reduced by the strong reducing agent sodium borohydride (NaBH4) and the arsenic hydride is formed.

57. 4 Channel peristaltic pump Full automation All functions controlled through software Simple Installation and Plumbing 4 Colour coded channels Single RS232C connection to spectrometer Compatible with all SOLAAR supported auto-samplers Channel 1 – Reductant Channel 2 – Acid Reagent Channel 3 – Sample Channel 4 – Drain

58. Peristaltic pump Stepper motor driven Precise and accurate Software controlled Pump speed is now a Method parameter Flexible operation Optimise reagent consumption/sensitivity trade off Repeatable results

59. Sophisticated new design Gas Liquid Separator new design Mixing manifold Reaction zone Phase separation zone Semi-permeable membrane Pumped drain

60. AA Facilities

61. Secondary Wavelength Using secondary wavelength we can decrease the amount of light inter the detector so increase the concentration of the metal measured e.g. Zinc secondary wave length give 4000 X Measure high conc. Of metals

62. Atomic Emission Spectroscopy Higher wavelength higher stability of emission. uses quantitative measurement of the optical emission from excited atoms to determine analyte concentration

63. Environmental

64. Lab Requirements Ensure avoidance of: Direct sunlight. Proximity to heat sources. Draughts, particularly from such items as air conditioning vents and fans. Excessive vibration. temperature is maintained between +5oC and +40oC with a maximum temperature variation of less than 2oC per hour. Relative humidity should be maintained between 20% and 80%. These instruments are designed for operation in clean air conditions. The laboratory must be free of all contaminants that could have a degrading effect on the instrument components. Dust, acid and organic vapours must be excluded from the work area..

65. Fume Extraction All flames produce large quantities of heat and toxic combustion products. These must be removed by a suitable fume extraction system. Specifications of a suitable extraction system are provided in the Pre-Installation Manual. The fume extraction hood must not be attached to the chimney, and an air-gap of between 150 and 230mm must be made.

66. Accessories

67. Slotted Tube Trap This accessory enhances the flame sensitivity for certain elements by 2-5 times. It consists of a slotted tube held in the flame . NEVER ATTEMPT TO LIGHT OR EXTINGUISH A FLAME WITH The stat in the operational position.

68. ID 100 Auto-dilutor This is an accessory that will provide automatic sample dilution and standard preparation for flame AAS ID 100 is not compatible with VP90 AND VP 100. The ID100 Auto dilutor System can automatically prepare working calibration standards from a single master standard as they are needed, so that no manual dilution steps are required. It also simplifies the task of handling over-range samples by intelligently diluting them into the calibration range, thus extending the effective working range. Full automation is possible by combining the ID100 with any of the Thermo Elemental range of AA Flame autosampler .

69. Auto-sampler ASX520-ASXR8 ASX520 Auto sampler A workhorse auto sampler for unattended analysis with a maximum load of 360 samples for busier laboratories EXR8 Auto sampler A large sample load of up to 720 samples with automatic, unattended analysis for high throughput laboratories

70. EC 90 Electric heating It replaces the Flame Heated Measurement Cell with an Electrically Heated Atomization Cell, so that Vapor measurements can be made without a flame. The accessory consists of two parts: 1- the EC90 Furnace Head. 2- the EC90 Power Supply

71. Aliquot Micro-sampling Simple accessory to allow you to use manual Aliquot Micro sampling to measure your samples when 1- The available volume of sample is limited 2- The sample is too viscous, 3- Contains too high concentration of dissolved solids

72. Furnace Vision System GF TV CCD camera provides high definition images Uses spectrometer optical path for a clear, direct, on-axis view of the cuvet Simplified method development Accurate adjustment of capillary possible Perfect sample injection depth Drying and ashing phases can be easily optimised High quality and reproducible results Images can be captured and stored

73. HG90 Mercury Concentration System In the SOLAAR HG90 Mercury Concentration System, the mercury vapor from the HS90 is passed over a gold/platinum gauze for a defined length of time to collect it as an amalgam. It is then released by heating the gauze and a flow of argon transports it into the measurement cell. Collection for up to 120 seconds will give a detection limit of about 20 ng/L (or ppt ).

74. Segmented Flow Injection Flow Injection Operation A peristaltic pump is used to generate continuously flowing streams of reagents. A 6 port valve and sampling loop are used to inject discrete portions of the sample into one of the reagent streams. The reagent streams are mixed, and the volatile hydrides are separated in a gas liquid separator and transported to the spectrometer for measurement. The signal is measured as a peak.

75. ISQ – Intelligent Spectrometer Qualification ISQ is an automatic, software driven process to demonstrate that your spectrometer hardware is performing consistently to specification over the intended operating ranges. Intelligent Identifies instrument in use Selects appropriate tests Software automatically controls tests Clear result display Spectrometer Tests the hardware of the spectrometer Helps to diagnose the source of any hardware problems at an early stage Qualification Verifies that the instrument is operating entirely within the designed specifications Confirms instrument is capable of producing sound analytical data.

76. Software

77. Easy to learn SOLAAR Software Software design is essential to make the instrument easy to learn, easy to use and the full capabilities of the hardware. SOLAAR software was the first AA software designed to run under Microsoft Windows. Evolutionary software development strategy now on Version 10 We incorporate Customer feedback Result – Stable, refined full functionality.

78. AA Software Compatible with Windows 2000, XP Professional and VISTA Ultimate Wizard based interface Complete user help facility to provide a comprehensive AA Cookbook for all elements. Context sensitive help Automatic programming of up to 16 elements Facility to record lamp usage Capable of automatically switching lamps on and off in an intelligent manner to preserve lamp life but also ensure lamps are warmed up sufficiently at time of use Normal, standard addition and standard curve calibration methods supported Flexible and comprehensive results database filters to select and display the required data Export of data to other applications possible Integrated Quality Control protocols

79. Validation

80. 3M Validation According to ISO/IEC 17025 “General requirements for the competence of testing and calibration laboratories” Machine Method Man

81. 1. Validation of the Machine Validation kit helps 1- Monitor the regulatory compliance status of spectrometer. 2- Determine the conformity of an AA spectrometer to internally established standards. 3-Provide confidence for managerial and regulatory personnel that the system is under control provide all the documentation, hardware and standard solutions necessary for the validation process.

82. Validation Packages Package contain Log book Ca/Mg lamp Ni/Cr/Mn lamp Pyro coated cuvettes Ni, Cr, & Mn standard solutions ASTM type 1 water Optical filters Certificates

83. Validation Unit Tests performed Wavelength Accuracy Monochromator Resolution Photometric Accuracy Photometric Stability D2 Background Correction Polariser Orientation Polariser Repeatability

84. Calibration Automatically peaks wavelength Automatically sets band pass Automatically adjusts lamp current Automatically recalls flame conditions Automatically balances D 2 intensity Automatically sets baseline

85. 2. Validity of the method Contaminant Methodolgy 13 Antimony ICP-Mass Spectrometry Hydride-Atomic Absorption Atomic Absorption; Platform Atomic Absorption; Furnace Arsenic 14 Inductively Coupled Plasma 15 ICP-Mass Spectrometry Atomic Absorption; Platform Atomic Absorption; Furnace Hydride Atomic Absorption Barium Inductively Coupled Plasma Atomic Absorption Furnace According to EPA

86. According to EPA Contaminant Methodolgy 13 Cadmium ICP-Mass Spectrometry Hydride-Atomic Absorption Atomic Absorption; Platform Atomic Absorption; Furnace Calcium Inductively Coupled Plasma 15 ICP-Mass Spectrometry Atomic Absorption; Platform Atomic Absorption; Furnace Chromium Inductively Coupled Plasma Atomic Absorption Furnace

87. 3. Man Validation Thermo Training Courses. Thermo Technical support. Meslo Training Courses. Meslo Technical support. Service after sell. Service center. Application Consultations.

88. Applications

89. Applications Environmental Clinical Pharmaceutical Foods Agriculture Petrochemicals

90. 1. Environmental Applications Waters – sea, fresh, waste Plant materials Soils, Sludges and sediments Airborne particulates Biological samples

91. Essential and Toxic elements Essential major elements C N O P S Cl Na K Ca Mg Essential trace elements F I Se V Cr Mn Fe Co Ni Cu Zn Mo Si Sn As Toxic elements Li Be Ba F Cl Br As Sb Bi Pb Sn Tl V Cr Mn Fe Co Ni Cu Zn Cd Hg

92. 2. Clinical Applications The majority of samples analysed are taken from the main group of biological fluids, such as whole blood, plasma, serum and urine. hard and soft tissues, such as bone, finger nails and hair flame based analysis for the major and minor essential elements, graphite furnace analysis for the trace elements and vapour analysis for the group of toxic

93. Essential elements Essential major elements Ca Mg Na K Essential minor elements Zn Cu Fe Essential trace elements Cr Mn Mo Co V Se Ni

94. Toxic elements Toxic elements are often defined as those that interfere with metabolic processes. The elements usually included in this group are as follows: Lead, Mercury, Arsenic, Thallium, Cadmium, Aluminum, Boron, Antimony.

95. 3. Pharmaceutical Applications Samples of diclofenac sodium for Na, K, Ca and Al analysis Magnesium Stearate sample to be analysed for Cd, Ni and Pb.  Samples of vitamin tablets Se analysis

96. Drug discovery and testing Most Pharmaceutical Companies these days develop drugs which are targeted at specific cells in the body. These drugs must be tested for correct activity but more importantly for the absence of any adverse side reactions.

97. 4. Food and Drink Applications No. Raw materials Intermediates Food Products 1 Cereals Flour Bread 2 Vegetables Sugars, Milk 3 Fruit syrups Butter 4 Meat Processed meat and fish candy 5 Dairy Processed dairy products Sweets 6 Fish Flavourings Juice 7 Water Additives Etc

98. Toxic and nutrition elements Toxic metals Pb, Cd, As, Hg, Al, Cr, Cu Low PPM levels in original material Recent interest in radio-nuclides Pu, Am and Np. Cs-137, Cs-134, Sr-90 and K-40 Nutrition elements Ca, Mg, Na, K, P %age to high PPM levels in original material Micro-nutrients Zn , Se, Mo, etc… high PPM to PPB levels in original material Process monitoring and control Fe, other transition elements in frying oil Ni in fat hydrogenation Levels vary with process, typically 1000 – 10PPM

99. 5. Agriculture Applications soil analysis provides a measure of a soil‘s potential to supply the necessary nutrients to plants. Plants may be sampled to monitor nutrient uptake efficiency and also to check for toxic metal accumulation for health reasons.

100. Soil nutrient elements P, K, Ca, Mg Macro nutrients at % level Cu, Fe, Mn, Zn Micro nutrients at ppm level Al, B, Na, Mo, Se Other nutrient elements As, Cd, Co, Cr, Ni, Pb Elements of toxic interest

101. 6. Petrochemical Applications Measure refinery contaminant elements Na, V, Fe, Ni by Flame-PPM Measure fuel elements Pb, Mn, usually low ppm-typically flame or furnace Measure lube oil elements Fresh - Ca, Ba, Mg, Zn, Mo, Na (flame) Used - Ag, Al, Cr, Fe, Mn, Ni, Pb, Sn, Ti, Zn (often furnace)

102. lubricating oils Every rotating mechanism in machinery of all types depends on their use for smooth operation. Like engines and gearboxes used in modern transportation, such as aircraft, ships, cars and lorries and heavy construction equipment. Oils in use so that oil changes can be carried out in time to prevent excessive wear occurring in the components concerned.

103. Wear Metals Wear metal Indicated condition 1 Silicon Indicates dust intrusion, usually from improper air cleaner service. Causes rapid engine wear and early failure. 2 Iron Indicates wear originating from engine block, cylinder, gears, wrist pins, rings (case iron), camshaft, oil pump, or crankshaft. 3 Copper Usually indicates wear in bushings, injector shields, valve guides ,connecting rods, or piston pins. 4 Nickel l Wear of plating on gears and certain types of bearings. 5 Tin Wear of certain types of bearings and coatings of connecting rods and iron pistons

104. Wear Metals Wear metal Indicated condition 6 Lead In diesel engines indicates wear of bearings. In petrol engines fuel blow by is indicated. 7 Chromium Indicates ring wear or cooling system leakage if chromates are used as inhibitors. 8 Aluminum Indicates wear of pistons and certain types of bearings. 9 Molybdenum Indicates wear in certain types of bearing alloys and in oil coolers.

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