1. Methanol, hexane, water, dioxane and isopropyl alcohol are some of the solvents used in HPLC.

The decreasing order of their polarity is: Ans. Water> methanol > isopropyl alcohol> dioxane> hexane 2. The concentration of a sample is 1.5 mg/mL. If an impurity at a level of 0.02% is present, what would be its concentration in ppm units? Ans. 300 ppm. 3. The viscosity of water is 1.00 and that of methanol is 0.60. Explain whether the viscosity of a mixture of water and methanol in a ratio of 50:50 (v/v) would be greater than 1.00, lesser than 1.00 or greater than 0.60. Ans. Greater than 1.0 due to intermolecular hydrogen bonding. 4. Distinguish between accuracy and precision of a method. Which statistical function is used to measure the precision of a method? Ans. Accuracy is the closeness of an experimental measurement or result to the true or accepted value. Precision is the closeness of agreement between replicated measurements or results obtained under the same prescribed conditions. Standard deviation (SD) is used as a measure of precision. 5. Distinguish between determinate errors and indeterminate errors. Ans. Determinate errors also known as systematic errors, or bias, arise from determinate or identifiable sources causing measured values to differ from a true or accepted value. Indeterminate errors also known as random errors arise from a variety of uncontrolled sources and cause small random variations in a measured quantity when the measurement is repeated a number of times. 6. What is meant by buffer solution. Give one example of buffers used in preparation of buffer solutions. Ans. Any solution which has the capability to resist small changes in its pH is known as a buffer solution. Any example. 7. Expand the term ANOVA. Ans. Analysis of variance. 8. Mention at least two detectors that are commonly used with Gas chromatography. Ans. thermal conductivity detector, electron capture detector, flame ionization detector, thermionic detector. 9. Which chromatographic technique can be used to separate a mixture of proteins? Ans. Size exclusion chromatography.

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The specific gravity of commercial HCl is 1.18 and its purity is 35.5%. What would be the volume of commercial HCl required to prepare 600 ml of 0.1 N HCl solution. (Mol. Wt of HCl = 36.5). Ans. 5.228 mL. Which indicator is used during the determination of water by Karl-Fischer titration? Ans. None. The titration is performed either potentiometrically or using the Karl-Fischer reagent as a self indicator. Mention two elements/ions that can be estimated with a precipitation titration. Ans. Chloride, bromide, iodide etc. Expand the terms (a). SE and (b). SPE (these techniques are used for separating of mixture of substances). Ans. (a). Solvent Extraction (b). Solid phase extraction. A compound is subjected to a flame test and gives intense yellow orange color. Which metal could be present in that compound? Ans. Sodium. What is the range of chemical shift (ppm) of protons for a carboxylic acid group? Ans. 9-12. A C-13 spectrum of a compound shows chemical shifts in the range of 180-220 (ppm). What functional groups could be present in the compound? Ans. Aldehyde and ketone. An IR spectrum of a compound containing a carbonyl group (>C=O) should nearly always have a very strong absorption peak at: Ans. 1700 cm-1. What is the characteristic absorption band for a cyano compound in an IR spectrum? With which analytical technique is the Time Of Flight (TOF) detector used? Ans. Mass spectrometry. Carboxylic acids exist as dimers in liquid or solid state and in CCl4 solution when at a concentration of over 0.01 M. In which region of the IR spectrum, is the O-H stretching absorption of carboxylic acid dimers seen? Ans. 3300-2500 cm-1. Band usually centers near 3000 cm-1. Predict the fragmentation pattern of Cyclohexene. A 0.53 g sample of primary-standard grade Na2CO3 requires 20.0 ml of a H2SO4 solution to reach the end point in a reaction: CO32- + 2H+ H2O + CO2 (g) What is the Normality of H2SO4 solution? (Mol. Wt. of Na2CO3 = 106, Mol. Wt. of H2SO4 = 98). Ans. 0.5 N.

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Distinguish between fluorescence and phosphorescence. Ans. In fluorescence the molecules are first excited from the ground state (So) to higher energy states. These exited molecules drop to the S1 excited singlet electronic level losing their energy through a radiationless process, from which they return directly to the ground state through the emission of photons known as fluorescence. Its a fast process, with a delay time of about 10-9 to 10-7 s. In phosphorescence the exited molecules first shift to a meta stable triplet level from S1 and then to the ground state emitting photons. This is a delayed process compared to fluorescence with a decay time of about 10-1 to 10 s.

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What is turbidimetric titration? Give one example. Ans. Titrations which result in the formation of insoluble product (precipitate) are called as turbidimetric titrations. Example: Titration of halides (Cl, Br, I etc with Silver nitrate (AgNO3) solution. Name at least four different types of titrations. Ans. Acid-base neutralization, Redox, precipitation (turbidimetric or nephelometric), complexometric and surfactant titrations. 26. What is meant by finger print region in the IR spectrum? Mention its range in cm-1 units. The region from about 1500 to 500 cm-1 usually contains a very complicated series of absorptions. These are mainly due to all manner of bending vibrations within the molecule. This is called the fingerprint region. It is much more difficult to pick out individual bonds in this region than it is in the "cleaner" region at higher wavenumbers. The importance of the fingerprint region is that each different compound produces a different pattern of troughs in this part of the spectrum.

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Mention at least four detectors used with HPLC. Ans. UV/PDA, Refractive Index, Mass detector, Evaporative light scattering detector, Conductivity detector, NPD detector. 28. Give two examples of solvents used as mobile phase in normal phase chromatography. Ans. Hexane, dioxane, Isopropyl alcohol, ethanol. What is preparative HPLC used for? What is meant by Rf. Give the expression used for calculating Rf values. How many significant figures are present in

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(a) 1.0062 g 32.

(b) 0.0025 kg

Ans. (a) 5 (b) 2

What is pyrolysis gas chromatography? Ans. Pyrolysis GC is a technique in which a non-volatile sample is pyrolysed (broken down) under rigidly controlled conditions, usually in the absence of oxygen and the decomposition products separated in the gas chromatography column. Its main application is for polymer analysis. Expand the term EDTA. Under which category do EDTA titrations fall? Ans. Ethylenediaminetetraacetic acid. Complexometric titrations. How can barium be estimated quantatively? By gravimetric titration. Barium when titrated with sulfuric acid forms water insoluble barium sulfate. This can be dried in an oven at 800 C and then weighed as barium sulfate. A glass electrode is made up of a combination of indicator electrode and a reference electrode. Which electrode is used as the reference electrode? Ans. Silver-Silver chloride electrode. In polarographic analysis what is the charge of the dropping mercury electrode? Ans. Negative (used as cathode). What are the X-axis and Y-axis in a polarograph? Ans. Voltage (volts) on X-Axis and Current (microamperes) on Y-Axis. What type of compounds can be analyzed by Atomic Absorption Spectroscopy? Ans. Metallic salts or compounds having metals as a constituent. Inductively coupled plasma spectrometry is a technique used for determining trace levels of elements. Which gas is used for creating a plasma? Ans. Argon. A high-voltage discharge into argon flow creates a plasma, which is sustained by induction heating due to the field of radiofrequency coil. Which is a superior technique of purification, HPLC or TLC? Ans. HPLC

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