Volume 10 - Materials Characterization Part 6 pot

tertiary p References cited in this section Determination of Organic Compounds: Methods and Procedures, Determination of Organic Compounds: Methods and Procedures, Anal. Chem., Determination of Organic Compounds: Methods and Procedures, J. Biol. Chem., J. Biol. Chem., Mikrochim. Acta, J. Am. Chem. Soc., Anal. Lett., Anal. Chem., Chem. Rev., Analytical Chemistry of Polycyclic Aromatic Hydrocarbons, Anal. Chem., Fuel, The Systematic Identification of Organic Compounds, Ind. Eng. Chem., Anal. Ed., J. Org. Chem., J. Org. Chem., Talanta, J. Chromatography, Note cited in this section Elemental and Functional Group Analysis Walter T. Smith, Jr., Department of Chemistry, University of Kentucky Karl Fischer Method for Water Determination References cited in this section Z. Angew. Chem., Aquametry, Anal. Chem., Fresenius Z. Anal. Chem., Anal. Chem., Elemental and Functional Group Analysis Walter T. Smith, Jr., Department of Chemistry, University of Kentucky Unsaturation (Alkenes) References cited in this section Determination of Organic Compounds: Methods and Procedures, Fatty Acids, Anal. Chem., Elemental and Functional Group Analysis Walter T. Smith, Jr., Department of Chemistry, University of Kentucky References Modern Organic Elemental Analysis, Advances in Analytical Chemistry and Instrumentation, Mikrochim. Acta, Determination of Organic Compounds: Methods and Procedures, Determination of Organic Compounds: Methods and Procedures, Anal. Chem., Determination of Organic Compounds: Methods and Procedures, J. Biol. Chem., J. Biol. Chem., Mikrochim. Acta, J. Am. Chem. Soc., J. Am. Chem. Soc., Anal. Lett., Anal. Chem., Chem. Rev., Analytical Chemistry of Polycyclic Aromatic Hydrocarbons, Anal. Chem., Fuel, The Systematic Identification of Organic Compounds, Ind. Eng. Chem., Anal. Ed., J. Org. Chem., J. Org. Chem., Talanta, J. Chromatography, Z. Angew. Chem., Aquametry, Anal. Chem., Fresenius Z. Anal. Chem., Anal. Chem., Determination of Organic Compounds: Methods and Procedures, Fatty Acids, Anal. Chem., Elemental and Functional Group Analysis Walter T. Smith, Jr., Department of Chemistry, University of Kentucky Selected References Treatise on Analytical Chemistry, Analytical Chemistry of Inorganic and Organic Compounds, Instrumental Methods of Organic Functional Group Analysis, Analytical Chemistry of Nitrogen and its Compounds, Chemical Analysis, Determination of Organic Compounds: Methods and Procedures, Chemical Analysis High-Temperature Combustion R.B. Fricioni and Loren Essig, Leco Corporation General Use • Samples • Form: • Size: • Preparation: Limitations • • • Estimated Analysis Time • Sample preparation: • Analysis time: Capabilities of Related Techniques • Optical emission: • X-ray fluorescence: High-Temperature Combustion R.B. Fricioni and Loren Essig, Leco Corporation Introduction High-Temperature Combustion R.B. Fricioni and Loren Essig, Leco Corporation Combustion Principles Accelerators Table 1 Combustion accelerators Accelerator Good combustion aid for steel, iron, and nonferrous metals and alloys in a high-frequency furnace for determination of percent carbon; may be combined with iron chips for nonferrous alloys; may be combined with tin chips on some systems for sulfur determination Same guidelines as copper chips, but used with resistance furnace systems Good accelerator for combusting steel, iron, or nonferrous metals and alloys for determination of carbon or sulfur; when analyzing for concentrations below 0.05% C and 0.002% S, high-grade iron chips should be used to provide consistent results; iron chips must be used when combusting nonferrous materials in a high-frequency furnace system Fig. 1 Typical high-frequency combustion configuration. Good additive accelerator for combustion of steel, iron, and nonferrous materials; tin chips have relatively low combustion point and assist in the initial stages of combustion by generating a higher temperature at an earlier stage Tungsten Good accelerator for most steels, irons, and nonferrous materials; provides excellent combustion when combined with tin chips; used primarily where very low carbon and sulfur concentrations are being determined High-Temperature Combustion R.B. Fricioni and Loren Essig, Leco Corporation Separation of Interfering Elements [...]... irradiation Element Radioisotope detected, T1/2 Principal γ-rays used, KeV μ 100 0 2700 3200 120 4500 1500 750 8.0 60 350 400 0.2 40 200 Dysprosium 1 56 Dy (2.35 h) 94 .68 , 361 .66 0.9 γ Table 2 Typical nondestructive TNAA detection limits for elements in rock or soil samples five days after irradiation Element Radioisotope detected, T1/2 Principal used, KeV γ-rays μ ... thermal-conductive detector/readout Inert Gas Fusion R.B Fricioni and Loren Essig, Leco Corporation Detection of Fusion Gases Thermal-conductive detection Table 1 Thermal conductivity of gases Gas Molecular weight 150 39 33 10. 4 5.7 5 .6 5.4 5.4 3.8 3.3 Sulfur dioxide 64 1 .6 Fig 6 Typical thermal-conductive detection cell Infrared Detection Fig 7 Typical infrared detection system Inert Gas Fusion R.B Fricioni and...High-Temperature Combustion R.B Fricioni and Loren Essig, Leco Corporation Detection of Combustion Products Infrared detection Thermal-conductive detection Table 2 Thermal conductivity of gases Gas 150 39 33 10. 4 5.7 5 .6 5.4 5.4 3.8 3.3 Sulfur dioxide 1 .6 High-Temperature Combustion R.B Fricioni and Loren Essig, Leco Corporation Total... Helium supply; 2, two-stage pressure regulator; 3, NaOH-impregnated clay; 4, Mg(ClO4)2 desiccant; 5, flow restrictor; 6, flow meter; 7, pressure regulator; 8, needle valve; 9, gas doser (optional); 10, flow manifold; 11, sample holding chamber; 12, electrode (impulse) furnace; 13, dust filter; 14, heated rare earth copper oxide; 15, flow control; 16, infrared detector/readout; 17, thermal-conductive detector/readout... evident from the proximity of the peaks at 1115.5 keV (65 Zn) and 1120.5 keV (46Sc) N N N t N (Eq 1) e σ N T τ t N γ γ T γ γ γ τ Fig 2 -ray spectra of a neutron-irradiated NBS fly ash sample showing the change that occurs as a function of time The upper spectrum was recorded in the time interval 18 to 27 min after irradiation; the lower spectrum is a 2-h count recorded after 20 days of decay None of the... 2, pressure regulator; 3, heated copper; 4, NaOH-impregnated clay; 5, Mg(ClO4)2 desiccant; 6, flow control; 7, flow manifold; 8, gas doser (optional); 9, sample holding chamber; 10, electrode (impulse) furnace; 11, dust filter; 12, heated rare earth copper oxide; 13, Mg(ClO4)2 desiccant; 14, silica gel column; 15, thermal conductive detector/readout; 16, flow rotameter Fig 5 Insert gas fusion system... Limitations • • • • • Estimated Analysis Time • Capabilities of Related Techniques • X-ray fluorescence: Z≥ • Atomic absorption: ≥ • Inductively coupled plasma emission spectroscopy: • Inductively coupled plasma mass spectroscopy: • Isotope dilution mass spectrometry: • Spark source mass spectrometry: • Particle-induced x-ray emission spectroscopy: Neutron Activation Analysis M.E Bunker, M.M Minor, and... References cited in this section Modern Trends in Activation Analysis, 6th Conference on Modern Trends in Activation Analysis (Abstracts), Phys Med Biol., Anal Chem., Neutron Activation Analysis M.E Bunker, M.M Minor, and S.R Garcia, Los Alamos National Laboratory Nondestructive TNAA T T γ γ γ γ Fig 1 γ-ray spectrum of a neutron-irradiated ore sample from the Jemez mountains, New Mexico, recorded using... High-Temperature Combustion R.B Fricioni and Loren Essig, Leco Corporation Total and Selective Combustion v Total combustion w Selective combustion High-Temperature Combustion R.B Fricioni and Loren Essig, Leco Corporation Applications Example 1 Example 2 Example 3 High-Temperature Combustion R.B Fricioni and Loren Essig, Leco Corporation Selected References Catalysis and Inhibition of Chemical Reactions, Chemisorption, . high-grade iron chips should be used to provide consistent results; iron chips must be used when combusting nonferrous materials in a high-frequency furnace system Fig. 1 Typical high-frequency. detection Table 2 Thermal conductivity of gases Gas 150 39 33 10. 4 5.7 5 .6 5.4 5.4 3.8 3.3 Sulfur dioxide 1 .6 High-Temperature Combustion R.B. Fricioni and Loren Essig, Leco Corporation. Related Techniques • Optical emission: • X-ray fluorescence: High-Temperature Combustion R.B. Fricioni and Loren Essig, Leco Corporation Introduction High-Temperature Combustion R.B. Fricioni