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Analytical Applications

Materials   Analysis

Thermogravimetric Analysis

Thermogravimetric analysis is the quantitative measurement of any change in weight of a substance under investigation or examination with the increase in temperature.

Summary Analysis

Thermogravimetric analysis is the quantitative measurement of any change in weight of a substance under investigation or examination with the increase in temperature.

Thermogravimetry (TG) can directly record the loss in weight with time or temperature due to dehydration or decomposition on heating the sample. Thermograms are characteric for a given compound or system because of hte unique sequence of physiochemical reactions which occur over definite temperature ranges and at rates that are a function of the molecular structure. the change in weight of the compound or system occurs as a result of the rupture and/or formation of various bonds at elevated temperature.

Reference & Additional Information
  • Ambasta, B.K., Chemistry for Engineers

Simultaneous Thermal Analysis

A popular and useful device is a combined DTA/TG (simultaneous thermal analysis: STA) system in which both thermal and mass change effects are measured concurrently on the same sample.

Summary Analysis

A popular and useful device is a combined DTA/TG (simultaneous thermal analysis: STA) system in which both thermal and mass change effects are measured concurrently on the same sample. STA can be used to follow the course of chemical reactions, thermal decompositions or phase changes as a function of temperature. The sensitive balance associated with the TG capability of teh system allows the mass change of a specimen to be measured as a function of temperature. Simultaneous DTA, TG and mass spectrometer measurements provide information about the cause of the mass changes.

Reference & Additional Information
  • Speyer, R.F., Thermal Analysis of Materials
  • Khandpur, R.S., Handbook of Analytical Instruments

Dynamic Mechanical Analysis

DMA supplies an oscillatory force, causing a sinusoidal stress to be applied to the sample, which generates a sinusoidal strain. By measuring both the amplitude of the deformation at the peak of the sine wave and the lag between the stress and strain sine waves, quantities like the modulus, the viscosity, and the damping can be calculated.

Summary Analysis

DMA supplies an oscillatory force, causing a sinusoidal stress to be applied to the sample, which generates a sinusoidal strain. By measuring both the amplitude of the deformation at the peak of the sine wave and the lag between the stresss and strain sine waves, quantities like the modulus, the viscosity, and the damping can be calculated. One can calculate properties like the tendency to flow from the phase lag and the stiffness form the sample recovery. These properties are often described as the ability to lose energy as heat and the ability to recover from deformation.

Reference & Additional Information
  • Menard, K.P., Dynamic mechanical Analysis - A Practical Introduction

Dilatometric Analysis

The dilatometric method utilises either transformation strains or thermal strains; the basic data generated are in the form of curves of dimension against time and temperature.

Summary Analysis

The dilatometric method utilises either transformation strains or thermal strains; the basic data generated are in the form of curves of dimension against time and temperature. Used to fabricate metallic alloys, compressed adn sintered refractor compounds, glasses, ceramic products, composite materials, and plastics.

Reference & Additional Information
  • Bhadeshia, H.K.D.H, University of Cambridge, Materials Science & Metallurgy
  • Hans Lehmann, refuge Gatzke Dilatometrie and differential thermal analysis for the evaluation of processes

Multi-Modular Adiabatic

Calorimetric Analysis Adiabatic calorimetry is becoming increasingly important in many areas of modern materials research and safety engineering. Instrumentation allows for the analysis of relatively large sample volumes consisting of several milliliters.

Summary Analysis

Adiabatic calorimetry is becoming increasingly important in many areas of modern materials research and safety engineering.Instrumentation allows for the analysis of relatively large sample volumes consisting of several milliliters. During the measurements, additional substances can be injected and/or mixing of heterogeneous substances can be secured. Changes in pressure resulting from the reaction are also recorded. Furthermore, in addition to purely adiabatic or purely isothermal measurements, the investigations can be carried out in Scanning mode. Properties such as heat capacities can thus be quickly and precisely analyzed. Also, exothermic and endothermic effects can be quantitatively characterized with instrumentation. This offers the user nearly unlimited application possibilities.

Reference & Additional Information
  • Netzche - Article

Porisometric Analysis

Mercury intrusion porosimetry is one of only a few analytical techniques that permits an analyst to acquire data over such a broad dynamic range using a single theoretical model.

Summary Analysis

Mercury intrusion porosimetry is one of only a few analytical techniques that permits an analyst to acquire data over such a broad dynamic range using a single theoretical model. Mercury porosimetry routinely is applied over a capillary diameter range from 0.003 µm to 360 µm— five orders of magnitude! This is equivalent to using the same tool to measure with accuracy and precision the diameter of a grain of sand and the height of a 30-story building. Not only is mercury porosimetry applicable over a wide range of pore sizes, but also the fundamental data it produces (the volume of mercury intruded into the sample as a function of applied pressure) is indicative of various characteristics of the pore space and is used to reveal a variety of physical properties of the solid material itself.

Reference & Additional Information

Scanning Electron Microscopy

The scanning electron microscope (SEM) permits the observation and characterization of hetrerogeneous organic and inorganic materials on a nanometer to micrometer scale. The popularity of the SEM stems from its capability of obtaining three-dimensional-like images of the surfaces of a very wide range of materials.

Summary Analysis

The scanning electron microscope (SEM) permits the observation and characterization of hererogeneous organic and inorganic materials on a nanometer to micrometer scale. the popularity of the SEM stems from its capability of obtaining three-dimensional-like images of the surfaces of a very wide range of materials.

In the SEM, the area to be examined or the microvolume to be analyzed is irradiated with a finely focused electron beam, which may be swept in a rasster across the surface of the specimen to form images or may be static to obtain an analysis at one position. The types of signals produced from teh interaction of the electron beam with the sample include secondary electrons, backscattered electrons, characteristic x-rays, and other photons of various energies. These signals are obtained from specific emission volumes within the sample and can be used to examine many characteristics of the sample.

The imaging signals of greatest interest are the secondary and backscattered electrons because these vary primarily as a result of differences in surface topography. The secondary electron emission, confined to a very small volume near the beam impact area for certain choicces of the beam energy, permits images to be obtained at a resolution approximately the size of the focused electron beam. the three-dimensional appearance of the images is due to the large depth of the field of the scanning electron microscope as well as to the shadow relief effect of the secondary and backscattered electron contrast.

Characteristic x-rays are also emitted as a result of electron bombardment. The analysis of hte characteristic x-radiation emitted from samples can yield both qualitative identification and quantitative elemental information from regions of a specimen nominally 1 micron in diameter and 1 micron in depth under normal operating conditions. the evolution of the SEM and the specific capabilities of modern commercial instruments are discussed below.

Reference & Additional Information
  • Goldsten et al, Scanning Electron Microscopy and X-Ray Microanalysis - 3rd edition

Digital Optical Microscopy

Metallic materials are usually opaque; therefore investigations of plane cross-sections by incident light prevail in metallography. However, the transparency of some metals and silicon to infrared light in thin sections has been effectively exploited.

Summary Analysis

Metallic materials are usually opaque; therefore investigations of plane cross-sections by incident light prevail in metallography. Hoever, the transparency of some metals and silicon to infrared light in thin sections has been effectively exploited. Optically, the individual components of a metallic alloy differ in their amplitude and phase characteristics. WHile amplitude objects become visible owing to differences in light absorption and thus appear in different grey shades or even colours, phase objects only differ in the refractive indices which cannot be recognized without additional provision. The preparation of cross-sections, the enhancement of contrast by etching and other methods, as well as the miscroscopic setup mus be carefully optimized for the material under investigation and adjusted to the purpose of investigation in order to get maximum information from a mocroscopic study.

Reference & Additional Information

Metallographic Analysis

Metallography may be defined as the study of the internal structure of metals and alloys, and of its relation to their composition, and to their physical and mechanical properties.

Summary Analysis

Metallography may be defined as the study of the internal structure of metals and alloys, and of its relation to their composition, and to their physical and mechanical properties. The needs of practical metallurgy, especially in the iron and steel industries, have been the motive of the earliest, and of many of the most important metallographic investigations. Teh study of structure has proved itself an indispensable auxilary to chemical analysis in the scientific control of the metallurgical industries, an auxiliary of which the applications become more extensive and more important every year. The characterization of materials by metallographic techniques has been paralleled by a remarkable improvement in material capabilities. The ability to measure and characterize those material parameters that provid improved mechanical and physical properties has led directly the development of new and better materials. The successful correlation of the structure and properties of materials, whether on a theoretical or empirical level, has been one of the primary forces in the current materials revolution.

Reference & Additional Information
  • Metallography - A practical tool for correlating the structure and properties of materials, American Society for Testing and Materials
  • Desch, C.H., Metallography

Gas Chromatography

Chromatography encompasses a series of techniques that have in common the separation of components of a mixutre by a series of equilibrium operations that result in separation of the entities as a result of their partitioning (differential sorption) between two different phases, one stationary with a large surface and the other a moving phase in contact with the first.

Summary Analysis

Chromatography encompasses a series of techniques that have in common the separation of components of a mixutre by a series of equilibrium operations that result in separation of the entities as a result of their partitioning (differential sorption) between two different phases, one stationary with a large surface and the other a moving phase in contact with the first. Chromatography is not restricted to analyrical separations. It may be used in the preparation of pure substances, the study of the kinetics of reactions, structural investigations on the molecular scale, and the determination of physiochemical constants, including stability constants of complexes, enthalpy, entropy, and free energy.

The mixture to be separated and analyzed may be either a gas, a liquid, or a solid in some instances. All that is required is that the sample components be stable, have a vapour pressure of approximately 0.1 Torr at teh operating temperature, and interact with the column material (either a solid adsorbent or a liquid stationary phase) and the mobile phase (carrier gas). The result of this interaction is the differing distribution of the sample components between the two phases, resulting in the separation of hte sample component into zones or bands. The principle that governs the chromatographic separation is the foundation of most physical methods of separation, for example, distillation and liquid-liquid extraction.

Reference & Additional Information
  • Grob, R.L. and Barry, E.F., Modern Practice of Gas Chromatography - Fourth Edition

Fuel Cell Analysis

Fuel Cell Analysis Testing features of our system include: Advanced and Flexible Software is designed specifically for fuel cell testing Wide Dynamic Range allows testing of different sized fuel cells with the same system Stoichiometric Flow Control allows users to control flowrates based on proper stoichiometric ratio.

Summary Analysis

Testing features of our system include:

  • Advanced and Flexible Software is designed specifically for fuel cell testing
  • Wide Dynamic Range allows testing of different sized fuel cells with the same system
  • Stoichiometric Flow Control allows users to control flowrates based on proper stoichiometric ratio
Cyclic Voltammetry

Cyclic Voltammetry provides insight into the fuel cell reaction kinetics. It is used to characterize the fuel cell catalyst activity in greater detail. Capacitive charging current flows in response to the linearly changing voltage. The second current response is nonlinear and corresponds to a hydrogen adsorption increase. Following, the reaction current reaches a peak and then falls off as the entire catalyst surface becomes fully saturated with hydrogen. Performing CV experiments is easy with the Arbin FCTS equipped with a potentiostat load and charging power supply option.

Lifetime Testing

Apply a constant current discharge on the fuel cell until the voltage drops by 10% or out of the acceptable range.

Internal Resistance Measurement

Internal Resistance Measurement Using current interrupt method, all Arbin FCTS systems can measure the DC Internal Resistance and use the collected value to control the test.

Polarization Curves

Polarization curves provide useful information about the optimal operating point and performance characteristics for a fuel cell. Generating the polarization curve is an easy process with the FCTS system and this can be done with a variety of fuel cell operating conditions.

Input Gas Handling

The Input Gas Handling module controls flowrate at 1% of full-scale accuracy with a turn down ratio of 50:1 using standard analog mass flow controllers. Digital mass flow controllers with improved accuracy and turndown are also available as an option. The flow rate change can be ramped at adjustable rates during the test procedure. Unlimited gas inlets can be added for reformate gas simulation. Programmable mass flow controllers are used for reactant gases. These controllers can be automatically adjusted according to the load. The Input Gas Handling module also includes a gas mixing facility and stoichiometric flow control as standard features.

Liquid Reactant Handling

The liquid reactant handling module accommodates liquid reactants such as methanol or bio-fuels. The desired temperature, pressure, and flow rate of the solution is controlled and programmed in the software. The user also has the ability to select "single pass" or "recirculation" mode for the liquid fuel. This module also includes the capability to separate and release the gaseous products, such as CO2, from the liquid solution.

Gas Humidification and Heating

This module is composed of gas humidification and gas heating. It employs Arbin's proprietary dew point humidification technology which has been proven to provide precise dew point temperature control and very short response time. The dew point humidifier (DPH) accurately, quickly, and automatically provides the supplied gas to the fuel cell at the desired programmed dew point and temperature. Additionally, the water level in the DPH is automatically monitored and maintained with the included fill pump. External boilers, condensers, and chillers are not necessary for the humidification process.

Exhaust Treatment and Pressure Regulation

The exhaust gas from the fuel cell is first cooled through a heat exchanger. Condensed water is separated from the gas and purged automatically and smoothly without pressure interruption to the system. Back pressure control is completely automatic and programmable in all FCTS systems.

Stack/Cell Temperature Control

Arbin Instruments’ FCTS systems incorporate either Stack Cooling/Heating, which allows the user to accurately control the temperature of the fuel cell stack using a liquid coolant, or electronic heater cartridge control. Liquid coolant loops are typically used for systems above 500W and are used to keep a higher power stacks at the appropriate temperature. Electronic heater cartridges are typically used for stacks and single cells below 500W and are used to warm the cell to the proper operating temperature.

Electronic Load

The electronic load module in all Arbin FCTS systems uses our proprietary circuitry which is shared from our extensive background in battery and supercapacitor testing areas. All Arbin Instruments loads provide the ability to program simple or complex testing schedules or profiles. The electronic load can perform constant current or voltage discharge, constant load or power discharge, current and voltage ramps, pulses, and staircases. Control types also included are the use of variables instead of concrete values and formula control. Arbin also offers potentiostatic loads with charging capability which allow the user to perform cyclic voltammetry and other more extensive electrochemical experiments.

Reference & Additional Information
  • Arbin Instruments

Fourier Transform Infrared Spectroscopy

In infrared spectroscopy, IR radiation is passed through a sample. Some of the infrared radiation is absorbed by the sample and some of it is passed through (transmitted).

Summary Analysis

In infrared spectroscopy, IR radiation is passed through a sample. Some of the infrared radiation is absorbed by the sample and some of it is passed through (transmitted). The resulting spectrum represents the molecular absorption and transmission, creating a molecular fingerprint of the sample. Like a fingerprint no two unique molecular structures produce the same infrared spectrum. This makes infrared spectroscopy useful for several types of analysis.

So, what information can FT-IR provide?

  • It can identify unknown materials
  • It can determine the quality or consistency of a sample
  • It can determine the amount of components in a mixture

Infrared spectroscopy has been a workhorse technique for materials analysis in the laboratory for over seventy years. An infrared spectrum represents a fingerprint of a sample with absorption peaks which correspond to the frequencies of vibrations between the bonds of the atoms making up the material. Because each different material is a unique combination of atoms, no two compounds produce the exact same infrared spectrum. Therefore, infrared spectroscopy can result in a positive identification (qualitative analysis) of every different kind of material. In addition, the size of the peaks in the spectrum is a direct indication of the amount of material present. With modern software algorithms, infrared is an excellent tool for quantitative analysis.

Reference & Additional Information

Raman Spectroscopy

Raman spectroscopy involves the measurement of the difference in energy between the incident light and the Raman scattered photons, which corresponds to the energy of the vibrational transitions.

Summary Analysis

Infrared (IR) absorption and Raman scattering are both commonly used to study and identify substances using the compound's characteristic internal vibrations.

Infrared spectroscopy is an absorption process, measuring the fraction of the light absorbed as the wavelength of the light is varied. The incident light is absorbed when the energy of the light closely matches the energy of a vibrational transition in the sample.

A tiny proportion (approximately 1 in 109) of the photons incident on a sample interacts with vibrations in the sample and is scattered at higher or lower energy (Raman scattered).

Raman spectroscopy involves the measurement of the difference in energy between the incident light and the Raman scattered photons, which corresponds to the energy of the vibrational transitions.

  • Forensics
  • Pharmaceuticals
  • Art restoration and archaeology
  • Catalysts
  • Polymers
Reference & Additional Information
  • Reinshaw Raman FT-IR

Sintering Analysis

Sintering is essentially a removal of the pores between the starting particles, combined with growth together and strong bonding between adjacent particles.

Summary Analysis

Sintering is essentially a removal of the pores between teh starting particles, combined with growth together and strong bonding between adjacent particles. Sintering is studied by plotting density or shrinkage data as a function of time and by actual examination of the microstructure at various stages of sintering using scanning electron microscopy, transmission microscopy, and lattice imaging.

Reference & Additional Information
  • Richerson, D.W., Modern Ceramic Engineering - Properties, Processing, and Use in Design

Fatigue Analysis

To finalize the choice of materials, he needs to know how they behave under various loadings in various environments, and then, knowing these properties, he must be able to correlate them with the load-carrying capacity of his proposed component or structure.

Summary Analysis

Materials, whether they be matallic or non-metallic, are of no practical use to mankind intul they are turned into working components or structures. One link in the process chain by which this happens is called engineering design.

A major problem facing the designer is hte selection of hte right materials from which to manufacture a particular design of component or structure; the material properties must ensure that it carries out the duties for which it was designed without breaking within a guaranteed life nad yet enable it to be sold at a price which the customer is prepared to pay. To enable hum to do this, the designer needs to know the loads to which his component or structure will b esubjected in service, the environment in which it will work, the owrking life expected, and what it will cost to make. This information now sets boundaries on the range of materials from which to select those to use for his specific design. To finalize the choice of materials, he needs to know how they behave under various loadings in various environments, and then, knowing these properties, he must be able to correlate them with the load-carrying capacity of his proposed component or structure. The subjcts of stress analysis and fracture mechanics have been developed exclusively for this purpose. A major part of those testing areas is what is known as fatigue analysis.

Reference & Additional Information
  • Frost, N.E., Marsh, K.J., and Pook, L.P., Metal Fatigue

Nano-Indentation Analysis

It is not only hardness that is of interest to materials scientists. Indentation techniques can also be used to calculate elastic modulus, strain-hardened exponent, fracture toughness, and viscoelastic properties. The goal of nano-indentation tests is to extract elastic modulus and hardness of the specimen from load-displacement measurements.

Summary Analysis

It is not only hardness that is of interest to materials scientists. Indentation techniques can also be used to calculate elastic modulus, strain-hardenint exponent, fracture toughness, and viscoelastic properties. The goal of nanoindentation tests is to extract elastic modulus and hardness of the specimen from load-displacement measurements. Conventional indentation hardness tests involve the measurement of the size of a residual plastic impression in the specimen as a function of the indenter load. This provides a measure of the area of contact for a given indenter load. In a nanoindentation test, the size of teh residual impression is often only a few microns and this makes it very difficult to obtain a direct measure using optical techniques. In nano-indentation testing, the depth of penetration beneath hte specimen surface is measures as hte load is applied to the indenter. The known geometry of the indenter then allows the size of the area of contact to be determined. the procedure also allows for the modulus of the speciment material to be obtained from a measurement of the stiffness of the contact, that is, the rate of change of load and depth. The principal goal being to extract elastic modulus and harndess of the specimen material from these experimental readings.

Reference & Additional Information
  • Fischer-Cripps, A.C., Nanoindentation - 2nd Edition

Tension Analysis

A tensile test, also known as tension test, is probably the most fundamental type of mechanical test you can perform on material. Tensile tests are simple, relatively inexpensive, and fully standardized. By pulling on something, you will very quickly determine how the material will react to forces being applied in tension.

Summary Analysis

A tensile test, also known as tension test, is probably the most fundamental type of mechanical test you can perform on material. Tensile tests are simple, relatively inexpensive, and fully standardized. By pulling on something, you will very quickly determine how the material will react to forces being applied in tension. As the material is being pulled, you will find its strength along with how much it will elongate.

You can learn a lot about a substance from tensile testing. As you continue to pull on the material until it breaks, you will obtain a good, complete tensile profile. A curve will result showing how it reacted to the forces being applied. The point of failure is of much interest and is typically called its "Ultimate Strength" or UTS on the chart.

Reference & Additional Information

Compression Analysis

A compression test determines behavior of materials under crushing loads. The specimen is compressed and deformation at various loads is recorded. Compressive stress and strain are calculated and plotted as a stress-strain diagram which is used to determine elastic limit, proportional limit, yield point, yield strength and, for some materials, compressive strength.


Tension Analysis

A compression test determines behavior of materials under crushing loads. The specimen is compressed and deformation at various loads is recorded. Compressive stress and strain are calculated and plotted as a stress-strain diagram which is used to determine elastic limit, proportional limit, yield point, yield strength and, for some materials, compressive strength.

Reference & Additional Information

Hardness Analysis

Hardness may be defined as the resistance of a material to permanent penetration by another material. A hardness test is generally conducted to determine the suitability of a material to fulfill a certain purpose or application.

Hardness may be defined as the resistance of a material to permanent penetration by another material. A hardness test is generally conducted to determine teh suitability of a material to fulfill a certain purpose or application. COnventional types of static indentation hardness tests, such as the Brinell, Vickers, Rockwell, and Knoop hardness, provide a single hardness number as the result, which is the most useful as it correlates to other properties of the material, such as strength, wear resistance, and ductility. the correlation of hardness to other physical properties has made it a common tool for industrial quality control, acceptance testing, and selection of materials.

With the rising interest in the testing of thin coatings and in order to obtain more information from an indentation test, the instrumented indentation tests have been developed and standardized. In addition to obtaining conventional hardness values, the instrumented indentation tests can also determine other material parameters such as Martens hardness, indentation hardness, indentation modulus, indentation creep and indentation relaxation.

Hardness testing is one of the longest used and well known test methods not only for metallic materials, but for other tpes of material as well. It has special importance in the field of mechanical test methods, because it is a relative inexpensive, eassy to use and ndarly nondestructive method for the characterization of materials and products.

Hardness data are test-system dependent and not fundamental metrological values. For htis reason, harness testing needs a combination of certified reference materials and vertified calibration machines to establish and maintain national and world-wide uniform hardness scales.

Reference & Additional Information
  • Montaser, A., Inductively Coupled Plasma Mass Spectrometry

Impact Analysis

Impact testing is performed to evaluate the toughness of materials. There are several loading methods, including tension, compression, bending and torsion. The typical test is the Charpy impact test in which three-point bending is employed.

Summary Analysis

Impact testing is performed to evaluate the toughness of materials. There are several loading methods, including tension, compression, bending, and torsion. The typical test is the Charpy impact test in which three-point bending is employed. A hammer is dropped to hit a rectangular speciment. A V- or U-type notch is introduced to allow easy fracture due to stress concentration for ductile materials. In the case of brittle materials such as ceramics, cast iron etc., a notch is not introduced. Parts of the hammer before and after hitting (breaking) a specimen are compared. The balance is considered to show the resistance to fracture, and the energy needed to bend and fracture the specimen.

Reference & Additional Information
  • Czichos, Saito, Smith, Springer Handbook of Materials Measurement Methods