Gravimetric Analysis of Chloride Experiment

Chem 111

I.Purpose To obtain a qualitative gravimetric analysis of chloride. Also to determine the percentage in an unknown sample. II.Experimental Procedure Experimental procedure was conducted in reference to the CHM 111Gravimetric Chloride Experiment (r7) handout. Getting Started: 1. Obtained materials, chemicals and equipment needed for experiment. 2. Obtained unknown: B. Sample Preparation and Analysis: 1. Weighed 3 samples of the unknown. 2. Dissolved samples in deionized water to make 150 mL of solution. 3. Added 15 drops (half a milliliter) of nitric acid, HNO3, to each solution. Stirred using separate rods. 4. Prepared 150 mL of 0.1 M Ag NO3 using 2.54 g AgNO3 (s) and 150 mL deionized water. 5. Added 45 mL of 0.1 M AgNO3 solution to each sample solution while stirring. Each formed a cloudy white PPT. 6. Boiled the sample solutions on a hot plate. The precipitates in each beaker clumped together and the solutions cleared. 7. Removed the beakers from the hot plates and allowed to cool for 3 minutes. 8. Added a few drops of 0.1 M AgNO3 to check for a new precipitation. No new PPTs formed. 9. Placed the beakers in a dark lab drawer for 45 minutes. Prepared a wash solution of 1 mL of concentrated HNO3 with 300 mL of deionized water. 10.Labeled and weighed three filter crucibles. Prepared the suction flasks for filtration. Secured the flasks to rings stands to prevent them from falling over. 11.Slowly filtered each sample, rinsing with the HNO3 solution.

12.Placed the 3 crucibles into a beaker to prevent them from falling over, then placed the beaker into the drying oven set on 125o C. Left to dry for 12 days. 13.Removed crucibles from the drying oven and allowed to cool. 14.Weighed the crucibles. I.Results 1. Table Measurements and Calculations Unknown ID: B Trial 1 Trial 2 Mass of Unknown .2308 g .2303 g Mass of Crucible 24.4003 g 24.4066 g Mass of Crucible + 24.8402 g 24.8468 g AgCl PPT Mass of AgCl PPT .4399 g .4402 g Mass of Chloride .1089 g .1090 g % Cl in Sample 47.18% 47.33% Average % Cl 47.24% Standard Deviation .08155 of Cl Trial 3 .2320 g 23.1337 g 23.5762 g .4425 g .1095 g 47.20%

2. Sample Calculations Mass of AgCl Trial 2 Trial 3

Trial 1

24.8402 g crucible + AgCl 24.8468 g crucible + AgCl 23.5762 g crucible + AgCl -24.4003 g empty crucible -24.4066 g empty crucible 23.1337 g empty crucible .4399 g AgCl 4425 g AgCl Trial 1 % Cl in AgCl .4402 g AgCl .

.1 0 8 9g C l .4 3 9 9g A gC l

100%= 24.76%

Trial 2

.1 0 9 0g C l .4 4 0 2g A gC l .1 0 9 5g C l .4 4 2 5g Ag C l

100% = 24.76%

Trial 3

100%= 24.75%

Mass of Cl in AgCl PPT

Trial 1 .4399 g AgCl g Cl

1mol A g Cl 1 m o l C l 13 4 .4 g A g C l 3 .5 5 1 mol A g C l 1 m o l C l

g C l =

.1089

Trial 2 .4402 g AgCl g Cl Trial 3 .4425 g AgCl g Cl Trial 1

1mol A g Cl 1 m o l C l 13 4 .4 g A g C l 3 .5 5 1 mol A g C l 1 m o l C l

g C l =

.1090

1mol A g Cl 1 m o l C l 13 4 .4 g A g C l 3 .5 5 1 mol A g C l 1 m o l C l

g C l =

.1095

% Cl in Sample

.1 0 8 9g C l .2 3 0 8g S a m pl e .1 0 9 0g C l .2 3 0 3g S a m pl e .1 0 9 5g C l .2 3 2 0g S am pl e

100%= 47.18%

Trial 2

100% = 47.33%

Trial 3

100%= 47.20%

Standard Deviation Xi di=(xi-x) di2

47.18 47.33 47.20 Sum X I.Discussion 141.71 47.24

-.06 +.09 -.04 Sum

.0036 .0081 .0016 .0133

S= (.0133/3-1)1/2 = .08155

The average percent of the chloride in the unknown was 47.24%. The labels on the beakers that contained the unknown A and B were switched. According to the experimental data, unknown B in this experiment was NaCL. Due to labeling error, the unknown B of this experiment was supposed to be KCl. Other errors may have occurred during the transfer of the AgCl from the beaker to the crucible after heating, leading to loss of some of the product.