FM Lab Assignment 1 Osama Hasan CHE-01-A 2008-NUST-BE-CHEM-27 NUST School of Chemical and Materials Engineering (NUST-SCME) FT-IR:

How would you identify the metal or alloy of the pipe you are working on in your workshop? How will you check the quality of metal used in its manufacture? Suppose if it is an alloy; how are you suppose to determine the composition of the alloy components?
A Human Thumb Impression

As all the humans are identified by distinct fingerprints or thumb impressions, similarly all molecules produce discrete spectrum (molecular fingerprint of the sample) when it exposed to an infrared radiation. We can say that similar to a thumb impression, no two unique molecular structures produce the same infrared spectrum. On exposure of infrared radiations to the sample, absorption and transmission phenomenon takes place. The characteristic molecular structure absorbs the uniform wavelength infrared radiation and transmits a varied wavelength characteristic infrared spectrum which no two unique molecular structures can produce. This is observed because infrared spectrum is the representation of the absorption peaks which correspond to the frequencies of vibrations between the bonds of the atoms that the material is made up of. The bonds between the atoms are different with the parameters of bond length, bond energy, bonding orbital and bond angles etc; therefore no two compounds can produce the same infrared spectrum. This characteristic infrared spectrum can answer the above laid questions via a much practiced spectroscopic method of Fourier Transform InfraRed (FT-IR). FT-IR, as the name suggests used Fourier Transformations for converting the characteristic infrared spectrum to a human understandable plot of intensity vs. frequency which can be FT-IR Equipment deciphered to reply the above questions.
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The Sample Analysis Process

The normal instrumental process is as follows: 1. The Source: Infrared energy is emitted from a glowing black-body source. This beam passes through an aperture which controls the amount of energy presented to the sample (and, ultimately, to the detector). 2. The Interferometer: The beam enters the interferometer where the spectral encoding takes place. The resulting interferogram signal then exits the interferometer. 3. The Sample: The beam enters the sample compartment where it is transmitted through or reflected off of the surface of the sample, depending on the type of analysis being accomplished. This is where specific frequencies of energy, which are uniquely characteristic of the sample, are absorbed. 4. The Detector: The beam finally passes to the detector for final measurement. The detectors used are specially designed to measure the special interferogram signal. 5. The Computer: The measured signal is digitized and sent to the computer where the Fourier transformation takes place. The final infrared spectrum is then presented to the user for interpretation and any further manipulation. FT-IR has become a much pratcised technique than the conventional (dispersive) infrared spectroscopy because of the following advantages: Felgett Advantage: Most FT-IR measurements are done in few seconds because all of the frequencies are measured simultaneously. It can also increase speed, collecting a scan every second. Interferograms Jacquinot Advantage: The detectors are much more sensitive and of low noise levels. It can also increase sensitivity one second scans can be co-added together to ratio out random noise Connes Advantage: FT-IR are self calibirating instruments because of presence of a HeNe laser as an internal wavelength calibration standard. Non-destructive technique: The sample destruction doesnot take place. Mechanical Simplicity: It is mechanically simple with only one moving part
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Bomb Calorimeter:
Which apparatus would you use to determine the heat of a chemical reaction or a physical change? Or what instrument would be your choice for measuring the heat capacity of water? Your answer would most probably be a Calorimeter. But what if you are assigned to determine the heat of combustion of diesel or kerosene oil? What will you opt for? To your surprise, the answer is still a Calorimeter, but a modified constant-volume calorimeter technically named Bomb Calorimeter. A Bomb Calorimeter consists primarily of the sample, oxygen, the stainless steel bomb, and water. The dewar (insulated container) prevents heat flow from the calorimeter to the rest of the universe. Since the bomb (reaction) is made from stainless steel, the combustion reaction occurs at constant volume and there is no work. Thus, the change in internal energy for the calorimeter is zero. The thermodynamic interpretation of this equation is that the calorimeter is isolated from the rest of the universe. Bomb calorimeters are such designed that they can withstand high pressures while a reaction is being measured within it. Electrical energy is used to ignite the fuel, as the fuel is burning, it will heat up the surrounding air, which expands and escapes An inside view of Bomb Calorimeter through a tube that leads the air out of the calorimeter. When the air is escaping through the copper tube it will also heat up the water outside the tube. The temperature of the water allows for calculating calorie content of the fuel. The whole bomb pressurized with excess pure oxygen and contains a known mass of sample and a small fixed amount of water (to absorb produced acid gases). It is submerged under a known volume of water before the charge is ignited. The bomb, with sample and oxygen, forms a closed system - no air escapes during the reaction. The energy released by the combustion raises the temperature of the steel bomb, its contents, and the surrounding water jacket. The temperature change in the water is then accurately measured. This temperature rise, along with a bomb factor (which is dependent on the heat capacity of the metal bomb parts) is used to calculate the energy given out by the A Bomb Calorimeter sample burn

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GC-MS:
How can the analysis of fire debris containing very complex matrices and results be carried out most accurately? How are the drugs or poisons in biological specimens of suspects, victims, or deceased traced these days? Which analytical technique has made its way to US airports after the 9/11 attacks? What can act as an effective tracker of organic pollutant in the environment? What is used to control the ratios of aromatic compounds such as esters, GC-MS Apparatus; Left segment has a Gas Chromatograph column; Right fatty acids, alcohols, aldehydes, terpenes etc in segment has a Mass Spectrometer. foods and beverages? The answer to all above questions is easy and inexpensive: Gas Chromatography-Mass Spectrometry (GC-MS). The GC-MS apparatus is composed of two major building blocks: the gas chromatograph and the mass spectrometer. The gas chromatograph utilizes a capillary column which depends on the column's dimensions (length, diameter, film thickness) as well as the phase properties. The difference in the chemical properties between different molecules in a mixture will separate the molecules as the sample travels the length of the column. The molecules take different amounts of time (called the retention time) to come out of (elute from) the gas chromatograph. This difference in time allows the mass spectrometer to capture, ionize, accelerate, deflect, and detect the ionized molecules separately. The mass spectrometer does this by breaking each molecule into ionized fragments and detecting these fragments using their mass to charge ratio. It is not possible to make an accurate identification of a particular molecule by gas chromatography or mass spectrometry alone. These two components, used together, allow a much finer degree of substance identification than either unit used separately. Combining the two processes makes it extremely unlikely that two different molecules will behave in the same way in both a gas chromatograph and a GC-MS Scheme mass spectrometer. Therefore when an identifying mass spectrum appears at a characteristic retention time in a GC-MS analysis, it typically lends to increased certainty that the analyte of interest is in the sample. The GC-MS has been widely heralded as a "gold standard" for forensic substance identification because it is used to perform a specific test which positively identifies the actual presence of a particular substance in a given sample.

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HPLC:
How can you separate two non-volatile substances while working in your chemistry lab? How are two polymeric materials expected to be discriminated via separation? Which separation technique is much employed in a crime or forensic lab? Which is the most versatile and widely used type of elution chromatography by the chemists to separate and determine species in a variety of organic, inorganic A HPLC apparatus and biological materials? The answer is HPLC. High-Performance Liquid Chromatography or High Pressure Liquid Chromatography (HPLC) is a form of column chromatography used frequently in biochemistry and analytical chemistry to separate, identify, and quantify compounds. HPLC utilizes a column that holds chromatographic packing material (stationary phase), a pump that moves the mobile phase(s) through the column, and a detector that shows the retention times of the molecules. Retention time varies depending on the interactions between the stationary phase, the molecules being analyzed, and the solvent(s) used. The separation of mixtures in microgram to gram quantities is made by the passage of the sample through a column containing a stationary solid by means of a pressurized flow of a liquid mobile phase. Components migrate through the column at different rates due to different relative affinities for the stationary and mobile phases based on adsorption, size or charge. HPLC is an efficient, highly selective and widely applicable technique these days. It requires only a small sample and the sample remains nondestructive. It is generally applicable to inorganic ions but can also accommodate nonvolatile and thermally unstable compounds. HPLC Scheme The types of HPLC are classified by separation mechanism or the stationary phase. These include: Liquid-liquid or Partition Chromatography Liquid-solid or Adsorption Chromatography Ion-exchange or Ion Chromatography Size-exclusion Chromatography Affinity Chromatography Chiral Chromatography
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