By Dhanush P R WDS

11 June 2013

Its very important to identify an Unknown material. Finding the chemical composition of the material is very important in many of the mineral ore and manufacturing companies.

Qualitative an analysis gives an indication of the identity of the chemical species in the sample

Quantitative analysis determines the amount of one or more of these components.

Chemical Analysis methods can be separated into Classical and Instrumental

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1.Galvimetric 2.Titration 3.Flame Test 4.Acid test

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Instrument Method-Uses Scientific Instruments

1. Optical Emission Spectroscopy

a. Atomic Absorption Spectroscopy b. Atomic Emission Spectroscopy

c. X-ray Fluorescence
d. Spark Emission Spectroscopy

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Optical Emission Spectroscopy

General Uses Quantitative determination of major and trace elemental constituents in various sample types. Qualitative elemental analysis Examples of Applications Rapid determination of concentrations of alloying elements in steels and

other alloys
Determination of trace impurity concentrations in semiconductor materials Determination of alkali and alkaline earth concentrations in aqueous samples Determination of calcium in cement
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Samples Form: Conducting solids, powders, and solutions Size: Depends on specific technique; from approximately 10-6 g to several grams Preparation: Machining or grinding (metals), dissolution (for flames), and

digestion.
Limitations Some elements are difficult to determine, such as nitrogen, oxygen, hydrogen, halogens, and noble gases Sample form must be compatible with specific technique. Estimated Analysis Time 30 s to several hours, depending on sample preparation requirements

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The atom is made up of a nucleus surrounded by electrons. Ground state most stable configuration of an atom with lowest energy.

If energy of the right magnitude is applied to an atom,

the energy will be absorbed by the atom.

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AES Principle Contd.

Electron will be promoted to a less stable configuration, excited state configuration. This state is unstable, the atom will immediately and spontaneously return to its ground state configuration. Radiant energy equivalent to the amount of energy initially absorbed in the excitation process will be emitted.

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Advantages

Simultaneous multielement analysis

Quantitative and qualitative analysis for over 70 Determination of major, minor, and trace elemental components

Examples of Applications

Composition of metal alloys Trace impurities in alloys, metals, reagents, and solvents

Limitations

Cannot analyze for noble gas Halogens and some nonmetals require vacuum.

Estimated Analysis Time

Dissolution of solids in sample preparation may require up to 16 h Analysis may require minutes to several hours
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ATOMIC ABSORPTION SPECTROSCOPY (AAS) is an analytical technique that measures the concentrations of elements.

Atomic absorption is a very common technique for detecting metals and metalloids in environmental samples.

It makes use of the absorption of light by these elements in

order to measure their concentration .

The analyte concentration is determined from the amount of absorption.

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ATOMIC ABSORPTION SPECTROSCOPY(AAS) Basic Principle

The ability of an atom to absorb very specific wavelengths of light. By measuring the amount of light absorbed, a quantitative determination of

the amount of analyte element present can be made.

The use of special light sources and careful selection of wavelength allow the specific quantitative determination of individual elements in the presence of others.

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The Atomic Absorption Spectrometer

Atomic absorption spectrometers have 4 principal components

1 - A light source ( usually a hollow cathode lamp )

2 An atom cell ( atomizer )

3 - A monochromator 4 - A detector , and read out device .

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Quantitative analyses of approximately 70 elements

Examples of Applications

Trace impurities in alloys and process reagents

Direct solids analysis of ores and finished metals.

Samples

Form: Solids, solutions, and gaseous Size: Depends on technique used from a milligram grams.

Preparation: Depends on the type of atomizer used;

usually a solution must be prepared.
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Estimated Analysis Time

Highly variable, depending on the type of atomizer and technique used.

Sample dissolution may take 4 to 8 h or as little as 5

min Typical analysis times range from approximately 1 min (flames) to several minutes (furnaces) Using the graphite-tube furnace atomizer usually

used for ultra-trace-level analysis.

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Limitations
Detection limits range from subparts per billion to parts per million Cannot analyze directly for noble gases, halogens, sulfur, carbon, or nitrogen

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Elements detectable by atomic absorption are highlighted in pink in this periodic table
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x-ray source from an x-ray tube or a radioactive source strikes a

sample.

The x-ray can either be absorbed by the atom or scattered through the material.

if the x-ray had sufficient energy, electrons are ejected from the inner shells, creating vacancies.

Vacancies

an unstable condition for the atom.

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XRF-Contd..

For stable condition, electrons from the outer shells are

transferred to the inner shells. Giving off a characteristic x-ray whose energy is the

difference between the two binding energies of the

corresponding shells.

The emitted x-rays produced from this process are called X-ray Fluorescence. Fast and non-destructive to the sample. Better choice for insitu appilcations. Reductions in cost and time Material is inexpensive Applications to materials and thin films and for solids and liquids
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Detection limits for bulk determinations are normally a few ppm to a

few tens of ppm,

Not suitable for elements of atomic number less than 11

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Sample is placed in an OES instrument and flooded with argon gas

the sample is made as an anode and connected to a cathode.

High energy sparks are produced between cathode and anode across the argon filled gap. The spark first ionize argon and create a plasma. At the spark point of impact, spark melt , evaporate and excite the sample elements. The atoms goes to the higher energy unstable state.

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As higher energy state is unstable the atoms suddenly comes to the

stable lower energy state.

They emit light with characteristic wave length for each element. The intensities of these emissions are detected measured and compared to known standards

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Quick, reliable and reproducible analysis technique Good limit of detection for most materials - generally less then 50 ppm although 10ppm detection limits are typical.

Detection O and N possible

Applications
Usually used for metals\alloy analysis, such as :Steel, cast iron and high alloyed steels Non-ferrous metals and their alloys Cu: bronze, brass, cupronickel, etc. Mg, Zn alloys, Nitrogen in steel P in aluminium, Elments such as Se, La, Te, etc. Ultra low carbon analysis

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Quantitative determination of an analyte based on the mass of a

solid. By measuring the mass of the precipitates which precipitated by

adding a precipitation reagent in the solution.

Dissolve sample Add ppting reagent Filter Dry Weigh

sample

dissolved components

precipitating agent

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Gravimetric analysis precise analysis. Provides very little-instrumental error Does not require a series of standards for calculation of an unknown. Expensive equipment not required Due to its high degree of accuracy-can also be used to calibrate other instruments.

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Time Consuming process Gravimetric analysis usually only provides for the analysis of a

single element, or a limited group of elements, at a time.

Not that efficient compared spectroscopy A slight mis-step in a procedure can often mean disaster for the

analysis.

Difficult for insitu analysis. Estimated Analysis Time 2 to 8 h per element

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Aluminium, by the 8-Quinolinol Gravimetric Method.

Molybdenum by 8-Hydroxyquinoline Gravimetric Method in Ni

based and Co based alloys. Nickel by the Dimethylglyoxime Gravimetric Method,Carbon steel,

Low-alloy steel, Ni-Mo Steel

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Common laboratory method for quantitative chemical analysis.

To determine the unknown concentration of an analyte.

It is also known as volumetric analysis. A reagent called the titrant is prepared as a standard solution.

A known concentration and volume of titrant reacts with a

solution of analyte to determine concentration.

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Titration Contd.
Beaker contains solution of the analyte Small amount of indicator placed underneath a calibrated Burette containing the titrant.

Small volumes of the titrant are then added to the analyte and
Colour of the analyte changes Reflects arrival at the endpoint of the titration. When the endpoint of the reaction is reached, the volume of reactant consumed is measured and used to calculate the concentration of analyte by where Ca is the concentration of the analyte Ct is the concentration of the titrant, Vt is the volume of the titrant used, M is the mole ratio of the analyte and reactant Va is the volume of the analyte used.
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Chromium by the Peroxydisulfate method Manganese by the Peroxydisulfate-Arsenite

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Spark testing is a method of determining

the general classification of ferrous materials

Characteristic features of spark streams Include carrier lines, forks, bursts, and arrowheads.

Length of Spark - the longer the spark, the lower the amount of carbon. Color of Spark - the lighter the spark, the lower the amount of carbon Spark volume - More alloy results in a larger spark volume. Forks or Bursts - Indicate alloys present in the material. Forks are where one spark splits into two or three. Bursts are where one spark splits off into many, as shown below.
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Advantage of Spark testing is quick, easy, and inexpensive.

Test samples do not have to be prepared, a piece of scrap can be used.

The main disadvantage is its inability to identify a material positively; if positive identification is required, chemical analysis must be used.

The spark comparison method also damages the material being tested, at least slightly.

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