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    phrarm d 6th semester labs

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    © All Rights Reserved
    Download as PDF or read online from Scribd
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    35 views24 pages

    Analytical Lab Semester 6

    Uploaded by

    2K20PHA92 Qamar
    phrarm d 6th semester labs

    Copyright:

    © All Rights Reserved
    Download as PDF or read online from Scribd
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    af ; le Axt Se faci t oh webe Se Object: Estimate As tisha , a Reyuirements: ° phen by Acid basvstitration. / a - Chemicals: Aspirin 50% *? bye roxide 0.1N SOml or absolute alcoho! 20ml, Phenolphthalein (in ss ware: Measurin ee : Measu i j Ba nel bance suring cylinder 25/50 and 100ml, conic flask 250 and 500m beaker 250/500ml, glass rod, 4) paratus / | ie or er had gee et Analytical blancs, ron ail aluminium foil, filter hice: . face mask and marker pen ‘Y tration / Titrimetri 2} eaton Titimerie analysis / Titrimetry: Refers t0 ae syoline of a solution or amount of reagent / stan ‘act quantitatively witl i meninete Weer ly with a measured volume of solution of on fone / Reference / Titrant The solution of accurately known stré cate BS Soe Eien 1 ana substance being determined or estim; Eealvalence /tieoreGes! point: wine the reaction of titer and tier is cor fea ed The point where the equivalence point is observed physicall toichiometric polat: The mio ot which titer and titrant requirgd to physically observation of equivalence point. Titration error: difference of volume or amount Indicator: a chemical which shows observable physical Piimary standard: A chemical with high chemical purit Secondary standard: the purity of a chemical we chemical reaction to make it as primary standard. Standard solutions: the concentration is a general term’ ed to refer the quantity of a substance in a defined ared in which the / known volume of solution. In quantitative es analysis, base unit is mole. Mole: As per IUPAC “The mole i = 3 substance which contains as many as elementary units as there are atoms in 0.012 kilogram of carBy . The elementary unit must be specified and may be an atom, ae cule fon, radical, electron other partifes or specified group of such particles? Molarity-— number of moles{vplagegf solution in lies. it Equivalent wae of solution in litres. hy metry / Acid base titratio ds by hydrolysis with a standard acid ak bases by hydrolysis with a standard iven samph \dicator), Sodium sb, tissue : Me the reaction. end point: :gen eqhiyalence and end point of titrant be the end or completion of reaction. ings, standard solution is preps fimetry and alkali hose formed from salts of weak aci free acid or those formed from salts of we Neutralisation rea{jon / Titration of free bi (acidimetry tkitragan base (alkalimet i Wve the combination of hydrogen and hydroxide ions to form water. standard solution: 1% available in pure state, prepared simply by weighing ov sntial to weigh out exactly an required and the a solution of definite molar strength is definite fraction or dissolving it an appropriate solvent Tt is not esse ent to prepare the solution a little more concentrated thi ed molarity by using MiVi=M2V2. ‘a be obtained in a state of high purity and are suitable prepare standard solutions: sodium carbonate, sodium hydrogen phthalate, benzoic acid, sodium tetra bora eilphamic acid, potassium hydrogen fodate,soditum oxalate silver, silver nitrate, sodium chloride, potassi chloride, iodine, potassium bromate, potassium iodate, potassium dichromate, lead nitrate etc. a mol mole in practice it is more convenie to dilute it with solvent to obtain requir Following is a list of some substances which cat Eye } t é When the reagent is not available in pure foem as in the ¢qse of andy alka potassium hydroxide, barium hydroxide, potassium permanganate, ammonium sodium thiosulphate). Some inorganic acids and various deliquescent chemicals tl prepared and then standardised by titrations against a solution of a pure substance of known conce! The titration error and other errors are considerably reduced. Deseripti : Aspirin is known as acetyl salicylic acid and used non-steroidal anti- drug. It is white color powder has molecular weight 180.57 and mostly soluble in absolute alco neutral acetone, chloroform ether and dimethyl sulphoxide. It is less soluble in water because hy’ nonpolar nature due to presence of carboxylic acid and ester group. When aspirin reacts bicarbonate (NaHCOs) it forms H2COs (H20 + CO:) which acts like explosive. Aspirin is treated with strong base sodium hydroxide (NaOH) it released H” to combine with OH’ of/Na roduce water while sodium salt of acetyl salicylic acid (weak acidic salt). Procedure: Dissolve equivalent weight of 500mg aspirin from given sample in absolute et acetone 20ml. Filter the sample solution and titrate with 0.1N sodium hy solution as indicator. Each ml of 0.1 N sodium hydroxide is equivalent to Preparation of phenolphthalein indicator: Dissolve 0.5g of phenolphthalein in 50 ml ethanol and add 5Oml precipitate forms. droxide 7 at equivalence point) Reaction of weak acid with strong base reacts in one-to-one ratio. At the equivalence point of a weak acid and strong base titration , the PH is larger than 7. Strong acid-strong weak base: 2B * (PH&7 at equivalence point) + Here acid and base react to give an acidic solution 4- Weak acid- weak base: «(PH varies) The acid and base react to give a slightly basic solution. PH mete ‘APH meter is a precise instrument that weighs the hydrogen-ion movement in water based suspension , showing it a acidity or alkalinity expressed as PH. Itis also called a potentiometric PH meter between a PH electrode and a reference because it measure the variation in electrical potent electrode. This meter us used for experimentation, quality control etc. Basically PH is a unit of measure that express level of acidity or alkalinity of a suspension itis graded on a range of 0-14 PH=-log{+H]. Calibration of PH meter:- : Calibration required because the glass electrode does not provide reproducible electrostatic potentials, across longer period of time. First make sure the correct measurement mode is selected in PH meter, Then wash the electrode with distilled water and don’t wipe electrodes otherwise it will generate an electrostatic charge on electrodes. All standards and samples are brought to 25 degree centigrade before use. Now immerse the electrodes with in the standard buffer solution or calibration solution make sure end point of electrodes are fully immersed within the buffer solution. To create homogenous sample stare the electrodes with in the buffer. © Wait until the PH value get stabilized. After stabilization confirm the calibration by pressing the hold/ enter key. Now PH meter is calibrated to current buffer solution, Finally wash electrodes with distilled water and place it into buffer solution. ADVANTAGES OF PH meter: ‘© PH calibration is low priced and robust. ‘* Pocket size PH meter are use. ‘* Accounts are reliable and specific. DISADVANTAGES OF PH meter: «Heat affects output readings ‘© PH calibration utilizing glass electrodes need to be clean as deposition on the electrodes influences the readings. Potentiometer:- Potentiometer is one of the methods of electro analytical chemistry. It is usually employed to find the concentration of a solute in a solution. Potentiometric titration:- In potentiometric titration the end point of titration is determined by following the variation of potential differences between 2 electrode ( either one as indicator electrode and other one is reference electrode or 2 indicator electrode) immersed in a solution to be examined as a function of quality of titrant added. * For acid-Base titrations and unless otherwise prescribed a glass-calomel or glass-silver, silver chloride electrode combination is used. PROCEDURE 1. First need to clean and dry the conical flask, burette, and funnel required to perform the experiment. 2. Then fill the burette with a standard solution or titrant of known concentration using funnel. S- Then caref lly titrate th 6- Stare th 'e Sample in the flask by —— potentiometer unt the speci re naming sine drops to faltinto a note down the end point. will not be show. Prepared by Shah Nawaz jakhrani 2k20/PHAE/85 @ Analytical chemistry lab 3" year 6 semester. Experiment no” 4 ‘Object:- Observe refractive index of a solution by using Abbie's refractometer. Requirements: Abbie's refractometer , distilled watery Dharma © prprcton : Theory:- Refractive index:~ ‘The refractive index is the ratio of the speed of light in a medium relative to it’s speed in vacum, This change in speed from one medium to another is what causes light rays to bend. This is because as light travels through another medium other than a vacur the atoms of that medium constantly absorb and reemit the particle of light slowing down the speed of light travels at the refractive index can be calculated by using equation below: speed of light in vacuum speed of light in the medium Factors that affect the refractive index:- The two factors which affect the value of refractive index are: 1- Temperature:: © Refractive index values are usually determined at standard temperature. A higher temperature means the less dense and less viscous causing light travel faster in medium. This results in a smaller value for the refractive index due to similar ratio. ‘A lower temperature means the liquid becomes dense and has a higher viscosity causing light to travel slower in medium. This results in a larger values for the refractive index due to large ratio. Refractometer have a means of temperature regulation 2+ Wavelength of light: «The refractive index varies with the wavelength linearly because different wavelengths interfere to different extent with atoms of medium. It is important to use monochromatic lights to prevent dispersion of light into different colors. The chosen wavelength should not be absorb by the medium The sodium wavelength of light at 598 nm is mot frequently use wavelength of light for a refractometer. Applications of refractive index:- Refractive index has a large no of applications. 1. It is mostly applied for identify a particular substance, confirm it's purity or m concentration. jeasure it’s 2. itis used to calculate the focusing power of lenses and the dispersive power of Prism, 3. it can also be used to determine drug concentration in pharmaceutical industry Snell’s law: Snell's la in optics a relationship between the path taken by 2 vary of lights in crossing the boundary or surface of separation between tow contacting substances and the refractive index of each oR Snell's law states that the ratio of the singor the angles of incidence and refraction when referring to light or other waves passing through a boundary between two different isotropic media. Therefore another method is use to calculate the refractive index of a medium is to apply Snell’s law. ‘e= the angle of refraction 7 4.8" gx the refractive indices of the two mediums ne How refractive index measured:- There are many different A refractometer is used to measure the refractive index of medium. refractometer using Abbie’s refractometer. Basically a refractometer works based on the principle that when light when it enter into a different medium This instrument measure the angle refraction of light rays passing through and unknown sample PROCEDURE::- 1. Open prism assembly and remove lens tissue inspect the prism for cleanliness. If necessary clean with water, methanol or acetone. Place liquid sample on depression in the lower prism using pipette and close the prism. 2 Experience will show how much sample is messy while too little give poor contrast for reading. 3- Move the illuminator arm upward. Turn the adjustment control until the lower field dark and upper field light. Turn the mode selection ND. Focus on cross hair by moving eye piece Turn the dispersion correction where minimum color is seen adjust the lamp for maximum contrast if necessary. Turn the adjustment controls to adjust the sharp line to precisely intersect with cross hairs. 8- Depress read button and record reading. 9- Depress temperature button and record reading. 10- Clean the prism by blotting off the bulk samples with a lens tissue followed by cleaning with water. Methanol or acetone 11- Make sure the prism are clean or close them. Turn the instrument off Fluia Refractive Sound Index (ro) velocity (ms Carbon tetrachloride 1.46 926 Ether 1.35 985 Chloroform 1.44 995 Heptanes 1.38 1138 Alcohol, ethyl (ethanol) 1.36 1144 Hexane 1.37 1203 Carbon disulfide 1.63 1149 ‘Turpentine (wood) 1.47 1240 Benzene 1.50 1298 Water 1.33 1493 Acetic Acid 1.37 1584 Ethylene glycol 1.43 1644 Abbie's refractometer Shah Nawaz jakhrani 2k20/PHAE/85 == exPERIMENT NO 4 OBSERVATION OF REFRECTIVE INDEX OF DIF FERENT PI HAS ay USING ABBE’S REFERECTROMETER RMACEUTICAL PREPERATIONS efractive Index, measure of the bending of a ray of lish: another. 18 of a ray of light when passing from one medium into Ifis the angle of incidence of a ray in vacuum (angle between the incomi to the surface of a medium, called the normal) and r is the angle of the medium and the normal), the refractive i incidence to the sine of the angle of refraction; ie..n= sin / sin Refractive index is also equal to the velocity of light c of a gi i ivi F ve ind given wavelength in empty space divided its velocity v in a substance, aaeianreaneene i. Refractive index c= speed of light y=velocity in a substance ‘Snell's law is a formula used to describe the relationship between the angles of incidence and angle of refraction, when referring to light or other waves passing through a boundary between two

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