Field Report

Data record as observed in Kalyani University Lab

Submitted By: Utpal Kumar(09MS070) Date of Field Work: 29/11/2012 Date of Submission: 7/12/2012 1. Measuring pH of different solutions including buffer solution at 22.5 0C Sl. No. Sample pH 1. Acetate Solution 4.1 2. Phosphate solution 7.0 3. Distilled Water 5.42 2. Measuring fluoride in water using ion selective fluoride electrode Ion Selective Electrode: An ion selective electrode is sensitive to a particular ion. The fluoride ion selective electrode consists of a single crystal of europium (II) doped, lanthanum fluoride, LaF3. The response mechanism in this electrode is similar to the ion exchange mechanism of glass electrode. Conduction in the crystal phase occurs by a lattice defect mechanism. Mobile fluoride ions move into a vacant crystal positions. The size and charge of the mobile ions are important in this conduction mechanism. With the LaF3-Eu(II) defect crystal, the fluoride ions are best suited for vacancy filling and thus the electrode becomes ion selective. When this electrode along with reference electrode (Calomel) is immersed in a fluoride solution, the potential difference is developed which is proportional to the logarithm of the activity of the fluoride ion in solution. E = 0.058 log[F-] + constant A calibration curve is drawn plotting measurement of potentials versus fluoride concentration. Then the potential for the sample water is measured and the concentration of F- ion in the sample can be deduced from the calibration curve. Reagents: TISAB (Total Ionic Strength Adjustment Buffer) (i) (ii) (iii) (iv) Cresol: C21H18O55 CDTA: C14H22N2O8.H20 Deionized water NH4Cl and NH4OAc

Caution: OH- may interfere causing larger values. For fluoride electrode, experiment was not shown to us, only principle was told. 3. Conductivity of different Solutions Instrument: Conductivity meter Temperature = 22.80C Sl. Sample No 1. Conductivity/TDS standard solution containing 47ppm as NaCl 2. Distilled Water 3. 4. 5. 6. Kent purified water Cu dissolved in CH3OH Cu dissolved in acetonitride CH3OH dissolved in distilled water

Conductivity(s/cm) 100.2

Temperature(0C) 22.80C 22.80C 24.40C 23.30C 23.20C 23.20C

7.64 60.1 0 0.2 0.29

Inference: There are no dissolved ions, when Cu is dissolved in CH3OH. Therefore conductometer shows zero reading. 4. Estimation of percentage carbon present in soil sample using Walkley and Black method Procedure: i) ii) iii) iv) v) 0.5 gm of dry soil sample was taken and mixed and shaken with 1N K2Cr2O7. Add 20ml conc H2SO4 and 10 ml phosphoric acid with constant stirring and leave for 10-15 minutes . Add 200ml of distilled water Add 0.1N Ferrous Ammonium Sulphate in presence of diphenylamine as indicator A blank reaction is carried out in exactly the same procedure as above but without the soil sample.

Observation Table S.No 1 2 Sample Blank ( without soil) Sample with soil Titrated Volume ( ml) 33.8 20.2

Calculation: i) Percentage of Carbon

Organic Carbon(%)=(3.951*(1-(ml of FAS for soil sample/ml of FAS for blank)))/dry weight of soil = (3.951* (1-(20.2/33.8)))/0.5 = 3.179 Note: FAS = Ferrous ammonium sulfate ii) Organic Matter(%) = Organic Carbon(%)*1.724 = 3.178*1.724 =5.4815 Result: The soil analyzed had 3.179% organic carbon and 5.4815% organic matter

5. Phosphate of water estimation

Procedure: 1. 50ml of sample was taken and 2ml of ammonium molybdate was added to the solution 2. 3-5 drops of SnCl2 solution was added. 3. A blue color appears. 4. Take the absorbance at 690 nm using spectrophotometer against blank. 5. Plot the calibration curve and concentration was known from the graph of absorbance Vs Concentration of phosphate for unknown sample.

Reaction Involved: Po43- + 12 (NH4)2MOO4 + 24 H+ = (NH4)3PO4.12MOO3 + 21 NH4+ + 12H20 (NH4)3PO4.12MoO3 + SnCl2 = Molybdenum blue (Blue color) + Sn4+ SnCl2 acts as reducing agent

Record: S.No 1. 2. 3. Sample Blank Tap pond Absorbance at 690 nm 0 0.242 0.506 Concentration 0 ~0.39 ppm ~0.85 ppm

6. Estimation of Cu using AAS (Atomic Absorption Spectroscopy) Table: Absorbance and concentration of Cu Slit size: 2.7/0.8 mm =324.75 nm Sl. no. 1. 2. 3. 4. Sample Std 1 Std 2 Std 3 Blank Concentration of Cu 1 ppm 2 ppm 4 ppm 0 Absorbance at 324.75 nm 0.0791 0.1577 0.3082 0.0

Using these standard solutions, we can plot a calibration curve of concentration of Cu vs. absorbance. The concentration of Cu in unknown sample can be known by measuring absorbance using AAS and taking the concentration of Cu from the calibration curve.