GRAVIMETRIC ANALYSIS OF A CHLORIDE SALT

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1 PURPOSE The goal of this experiment is to quantitatively determine the amount of chloride in an unknown sample by precipitation with silver nitrate. INTRODUCTION: Silver chloride is a water-insoluble ionic compound. As a result, chloride can be quantitatively precipitated from solution by the addition of silver nitrate, as shown below. AgNO3(aq) + Cl (aq) AgCl(s) + NO3 (aq) The AgCl precipitate is collected on filter paper, dried, and massed. The mass of AgCl can then be used to calculate the mass of chloride as well as the percent chloride in the original unknown sample. Percent Chloride = mass of chloride (g) mass of unknown (g) 100 AgCl is photosensitive and slowly decomposes in the presence of light, as shown below. As such, the lights in the laboratory need to be dimmed and the samples protected with foil. 2AgCl(s) 2Ag(s) + Cl2(g) EQUIPMENT: 250-mL Beakers (3) Hot Plate Glass Stirring Rods (3)* Beakers, any size (3) Funnel Clamp Weighing Bottles* Watch Glasses (3) Analytical Balance Funnels (3)* Filter Paper (3) Plastic Wash Bottle Rubber Policeman (3)* Ring Stand/Rings Weighing Paper Unknown Sample* *Obtain from Stockroom. CHEMICALS M AgNO3 6M HNO3 Acetone (60 ml) DI water SAFETY NOTES 1. Silver nitrate can stain your skin and clothing. 2. Acetone is flammable. Keep it away from open flames! 1

2 PROCEDURE A. Mass By Subtraction 1. Obtain three clean 250-mL beakers and label them #1, #2, and #3 with a pencil. 2. Using a weighing paper, mass out 0.1 to 0.2 g of the unknown sample on a top-loading balance. 3. Carefully transfer the sample from the paper into the weighing bottle. 4. Record the mass the weighing bottle + sample using an analytical balance. 5. Transfer the contents of the weighing bottle to one of the 250-mL beakers. 6. Using the same analytical balance, record the mass of the now empty weighing bottle. 7. Calculate the mass of the unknown sample by subtracting the mass of the empty weighing bottle from the mass of weighing bottle + sample. 8. Repeat steps 2 through 7 with the two other samples. B. Precipitation of AgCl 1. Add between 75 and 100 ml of deionized water and 1 ml of 6 M HNO3 to each of the beakers containing the unknown samples. 2. Stir each of the solutions with a different glass, stirring rod until the entire sample has dissolved. Leave the stirring rods in the beakers to avoid sample loss. 3. Slowly (dropwise) add 30 ml of M AgNO3 to one of the beakers, stirring constantly. Place a watch glass over the beaker and then cover both the beaker and watch glass with foil to protect it from light. Repeat with the other two beakers containing the unknown samples. 4. Warm the solutions gently using a hot plate and keep them warm for approximately 30 minutes. DO NOT BOIL THE SOLUTIONS! C. Gravity Filtration 1. Obtain three filter papers and label them as #1, #2, or #3 using a pencil. 2. Fold each filter paper into a cone shape, as demonstrated by the instructor. 3. Using the analytical balance, record the mass of each filter paper. 4. Fit each filter paper into a separate funnel. Wet the filter paper with a small amount of deionized water to hold it in place. Place an empty beaker under each funnel to collect the filtrate. 5. Completely and quantitatively transfer the precipitate from beaker #1 on to filter paper #1. Use a rubber policeman and a wash bottle filled with deionized water to remove the last traces of precipitate from the beaker. Repeat with beakers #2 and #3 (and filter papers #2 and #3). Never allow the liquid to rise above the top edge of the filter paper! 6. Wash each precipitate with two or three 5-mL portions of water from the wash bottle. 7. Test for complete precipitation by adding a few drops of AgNO3 to the clear filtrate. If it clouds, refilter. 8. Pour three 5-mL portions of acetone through each filter paper. Once the acetone has completely passed through the sample, remove the filter paper from the funnel and place it on a numbered watch glass (#1, #2, or #3). Store the watch glasses in your locker until the next lab period. D. Calculation of Percent Chloride 1. Record the mass of each filter paper/agcl using the analytical balance. 2. Calculate the mass of AgCl; use the mass of AgCl to calculate the moles of Cl and mass of Cl in each sample. 3. Calculate the percent Cl in each sample; then calculate the average and standard deviation of the percent Cl. REFERENCE Nelson, J., Chemistry: The Central Science, 3ed. Prentice-Hall,

3 Name: Date: PRELABORATORY ASSIGNMENT 1. Give the balanced molecular, total ionic, and net ionic equations for the reaction of potassium chloride with lead(ii) nitrate. a. Molecular: b. Total Ionic: c. Net Ionic: 2. A g sample containing the chloride ion is treated with excess lead(ii) nitrate. The precipitate is filtered using a g piece of filter paper. After washing and drying, the mass of the precipitate and filter paper was g. Calculate: a. The mass of the precipitate that formed. b. The number of moles of precipitate that formed. c. The number of moles of chloride in the sample. d. The mass of chloride in the sample. e. The mass percent chloride in the sample. 3. Why was excess lead(ii) nitrate used in the above procedure? 4. Why is the mass of the precipitate different from the mass of the sample? 3

4 Name: Date: RESULTS Unknown Number: Mass of Weighing Bottle + Sample (g) Mass of Weighing Bottle (g) Mass of Sample (g) Mass of Filter Paper + AgCl (g) Mass of Filter Paper (g) Mass of AgCl (g) Sample 1 Sample 2 Sample 3 Moles of Cl Mass of Cl (g) Percent Cl Show one complete sample calculation here: Average Percent Cl : Standard Deviation of Percent Cl : 4

5 QUESTIONS 1. A g sample of a compound containing the Ba 2+ ion was treated with excess H2SO4, precipitating all of the barium as BaSO4. If g of BaSO4 precipitated, what is the mass percent of barium in the original sample? 2. A g sample of impure table salt was dissolved in water and treated with excess AgNO3, forming g of AgCl. What is the mass percent of NaCl in the impure sample? 5

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