Volume 10 - Materials Characterization Part 6 pot

References cited in this section Determination of Organic Compounds: Methods and Procedures, Determination of Organic Compounds: Methods and Procedures, Anal.. Smith, Jr., Department of

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tertiary

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References cited in this section

Determination of Organic Compounds: Methods and Procedures,

Anal Chem., Determination of Organic Compounds: Methods and Procedures,

J Biol Chem.,

Mikrochim Acta,

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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.,

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

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Z Angew Chem.,

Aquametry, Anal Chem., Fresenius Z Anal Chem.,

Anal Chem.,

Unsaturation (Alkenes)

Determination of Organic Compounds: Methods and Procedures,

Fatty Acids,

Anal Chem.,

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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,

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.,

Fatty Acids,

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Anal Chem.,

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

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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

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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

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High-Temperature Combustion

Detection of Combustion Products

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Total and Selective Combustion

Total combustion

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Selective combustion

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Coal Testing Conference Proceedings,

Inert Gas Fusion

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Introduction

Principles of Operation

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Fig 1 Graphite crucibles used in inert gas fusion analysis

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Fig 2 Simplified impulse inert gas fusion furnace The graphite crucible acts as a resistor, completing a

high-current circuit and reaching 3000 °C (5430 °F)

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Fig 3 Simplified inductive inert gas fusion furnace The graphite crucible acts as an inductor in a

high-frequency induction furnace, reaching 2500 °C (4530 °F)

Separation of Fusion Gases

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Fig 4 Inert gas fusion system for detecting nitrogen and oxygen 1, Helium supply; 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 for detecting nitrogen and oxygen 1, Helium supply; 2, two-stage pressure

regulator; 3, NaOH-impregnated clay; 4, Mg(ClO4)2 desiccant; 5, flow restrictor; 6, flow meter; 7, pressure

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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

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Detection of Fusion Gases

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Samples

Selective Fusion

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Examples

Tensile and yield strength problems

Structural problems

Cracking

Selected References

Catalysis and Inhibition of Chemical Reactions,

Chemisorption, Adsorption,

Determination of Gaseous Elements in Metals,

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Hydrogen in Steel,

Analytical Chemistry,

Neutron Activation Analysis

M.E Bunker, M.M Minor, and S.R Garcia, Los Alamos National Laboratory

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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:

Reference cited in this section

Nondestructive Activation Analysis,

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Neutron Activation Tables, Activation Analysis in Geochemistry and Cosmochemistry,

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Activation Analysis with Neutron Generators,

Neutron Sources

α α

Modern Trends in Activation Analysis,

6th Conference on Modern Trends in Activation Analysis (Abstracts),

Phys Med Biol., Anal Chem.,

Nondestructive TNAA

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γ γ

γ

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Fig 1 γ-ray spectrum of a neutron-irradiated ore sample from the Jemez mountains, New Mexico, recorded using a Ge(Li) detector five days after irradiation The lower figure is an expanded view of Detail A in the upper figure The necessity of high resolution is evident from the proximity of the peaks at 1115.5 keV (65Zn) and

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1120.5 keV (46Sc)

N N

T

γ

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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 peaks in the lower spectrum is visible in the upper spectrum Peaks denoted by (b) represent background lines

Sample Handling.

γ

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Table 1 Typical nondestructive TNAA detection limits for elements in rock or soil samples 20 min after irradiation

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detected, T1/2 used, keV μ

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Ar, V, Co, I, Cs, Yb, Ir, Sm, Ho, Lu, Au

F, Na, Mg, Al, Sc, Ti, Ga, Br, Ge, As, Sr, Pd, Ag, Sb, Te, Ba, La, Nd, Er, W, Re

Cl, Cr, Ni, Cu, Zn, Se, Ru, Cd, Sn, Ce, Pr, Gd, Tb, Tm, Hf, Pt, Th, U

K, Ca, Co, Rb, Y, Mo, Ta, Os, Hg

Zr, Nb

10 6 -10 7 Si, S, Fe

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Automated Systems.

Anal Chem.,

Nucl Instrum Meth.,

J Radioanal Chem.,

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Uranium Assay by Delayed-Neutron Counting (DNC)

β

T

μ

γ γ

Nucl Instrum Meth.,

Health Phys.,

Radiochemical (Destructive) TNAA

σ

γ

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Modern Trends in Activation Analysis,

Proceedings of the Apollo 11 Lunar Science Conference, Chemical and Isotopic Analyses,

Activation Analysis: A Bibliography Through 1971,

Epithermal Neutron Activation Analysis (ENAA)

Activation Analysis in Geochemistry and Cosmochemistry, Modern Trends in Activation Analysis,

Anal Chem.,

14-MeV Fast Neutron Activation Analysis (FNAA)

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Measured element concentration (a) , μg/g unless

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Prompt Gamma Activation Analysis (PGAA)

γ γ

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Applications

Example 1: Impurities in Nickel Metal

σ

γ

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Fig 3 -ray spectrum of a neutron-irradiated high-purity nickel sample The spectrum, recorded in the time

interval 3 to 8 min after a 20-s irradiation, shows the presence of titanium, manganese, and vanadium in the sample

Example 2: The Iridium Anomaly at the Cretaceous-Tertiary Boundary

Fig 4 Iridium concentration found as a function of depth in strata The peak at approximately 256 m (840 ft)

corresponds to the Cretaceous-Tertiary boundary Source: Ref 39

γ

γ γ

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Fig 5 Comparison of γ-ray spectrums Upper spectrum shows a neutron-irradiated rock sample that contains 3 ppb iridium (26 days decay) Lower spectrum shows the chemically isolated iridium fraction (pure 74.2-d 192Ir)

Science,

Nature, Science,

References

Nondestructive Activation Analysis, Neutron Activation Tables,

Activation Analysis in Geochemistry and Cosmochemistry,

J Radioanal Chem., Modern Trends in Activation Analysis,

6th Conference on Modern Trends

in Activation Analysis (Abstracts),

Phys Med Biol., Anal Chem.,

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Proceedings of the Apollo 11 Lunar Science Conference, Chemical and Isotopic Analyses,

Activation Analysis: A Bibliography Through 1971,

Science,

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Capabilities of Related Techniques

• Isotope dilution mass spectrometry:

• X-ray spectrometry:

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The specific activity

George M Matlack, Los Alamos National Laboratory

Radioactive Decay Modes

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γ

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Detection and Measurement of Radioactivity

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Radioactive Decay Spectrometry.

Reference cited in this section

General Catalog,

Radioanalysis

Sensitivity, Accuracy, and Precision

Detection Limits.

α

γ

σ

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Radiation Protection Needs.

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Laboratory Equipment.

μ

Fig 1 Schematic of apparatus for radioanalysis All components except the detector obtain their power from a

common supply that furnishes ±6 V dc and ±12 V dc

Fig 2 Thermal control plate Approximately 0.1 mL of liquid is being evaporated on a glass plate

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γ β

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β β β

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β γ

Nuclear and Radiochemistry,

Applications of Scintillation Counting,

Rapid Radiochemical Separations,

Table of Isotopes, Radiation Detection,

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Electron Spin Resonance

Charles P Poole, Jr and Horatio A Farach, Department of Physics and Astronomy, University of South Carolina

Capabilities of Related Techniques

• Nuclear magnetic resonance:

• Mössbauer resonance:

• Quadrupole resonance:

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• Microwave spectroscopy:

hν

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n n

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Instrumentation

Fig 1 Typical ESR spectrometer

Microwave Frequency.

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Sample Cavity.

Fig 2 Microwave-resonant cavity modes (a) Cylindrical TE012 cavity (b) Rectangular TE102 cavity (c) Position

of sample in rectangular TE102 cavity RF magnetic field lines (dashed) and electric field orientation (dots and

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Xs) are shown The dots denote vectors directed up from within the cavity; Xs denote vectors aimed down into the cavity

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Fig 3 Power reflected from a microwave-resonant cavity as a function of frequency The resonant frequency is

ω0 the full width at half amplitude is ∆ω

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Supplementary Experimental Techniques

Relaxation.

T

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Saturation Method of Measuring Relaxation Times.

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Electron-electron double resonance (ELDOR)

Acoustic Electron Spin Resonance.

Optical double magnetic resonance (ODMR)

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Fig 4 ESR spectrum of DPPH Y1 is the amplitude of the first peak of the spectrum; the amplitude of the peak

in the hypothetical spectrum in the absence of hyperfine structure is Y1 multiplied by the multiplicity factor D

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Fig 5 Lorentzian and Gaussian absorption curves (a) Curves with the same half amplitude line width (b)

First-derivative curves with the same peak linewidth (c) Second-First-derivative curves with the same peak linewidth

peak-to-N

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ESR Spectra

∆ω

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Fig 6 Energy-level diagrams for an unpaired electron (a) In the absence of hyperfine structure (b) With two

unequal hyperfine coupling constants A1 and A2 (c) With two equal coupling constants Corresponding ESR spectra are shown in Fig 7 and 8

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