Joshua Gullace

AP Chemistry Lab #2

2011

Analysis of Alum AlK(SO4)212H2O AP Chemistry Laboratory #12l

Introduction: When a compound is synthesized tests are carried out to confirm whether the compound formed is indeed the compound desired. There are a number of tests that can be performed to verify the identity of a compound. In this experiment several tests are carried out to determine if sample crystals are aluminum potassium sulfate (alum) Background: Every compound has a unique set of chemical and physical properties. To identify a compound with certainty a minimum number of the properties must be verified experimentally in this experiment three properties of a sample of aluminum potassium sulfate are determined- its melting point, the number of moles of water of hydration in the formula, and percent composition of sulfate. Materials:
Part 1 0.5g Aluminum potassium sulfate Beaker 150 mL (or Thiele melting point tube) Bunsen Burner Hot Plate Capillary tube Split Stopper to hold the thermometer Part 2 0.5g Aluminum potassium sulfate Balance .001g precision Bunsen Burner Crucible and cover Part 3 1g aluminum potassium sulfate Aspirator Balance .oo1g accuracy 2 Beaker 250 mL Bunsen Burner Filter flask and adapter Gooch Crucible with fiber glass filter pad Mortar and Pestle Ring stand, Ring and Wire Gauze Rubber Band Thermometer 0C-100C Universal Clamp

Ring stand, Ring Support Triangle, Pipe stem Wire Gauze

Graduated cylinder 50 mL Ring stand, Ring Rubber policeman Stirring rod wash bottle with distilled water watch bottle

Joshua Gullace

AP Chemistry Lab #2

2011

Safety Precautions:
Barium nitrate solution is toxic by ingestion. Wear chemical splash goggles, chemical-resistant gloves, and a chemical-resistant apron. Thoroughly wash hands with soap and water before leaving the laboratory.

Pre Lab Questions:

1. When measuring a melting point why is it necessary to raise the temperature very slowly when approaching the melting point? As you approach the melting point if you do not go slowly as you approach the theoretical melting point if you proceed to quickly you will not have an accurate measure of your labs melting point. Washing soda is a hydrated compound whose formula can be written as Na2CO3xH2O, where x is the number of moles of H2O per mole of Na2CO3. When a 2.123g sample of washing soda was heated at 130C, all of the water of hydration was lost leaving .787g of anhydrous sodium carbonate calculate the value of x. X= 9.96 here is how H2O=1.336 wash soda= .787 1.336/18.015= .074 moles water .787/105.961= .00743 moles of anhydrous wash soda .074/.00743= 9.96 moles water per one mole of was soda The formula for Epsom salts is MgSO47H2O. If 1.250 g of the compound is dissolved in water calculate the number of millimeters of .200M Ba(NO3)2 that would be required to precipitate all of the sulfate ions as barium sulfate. Make the same determination for 1g of alum.

2.

3.

Procedures: Part 1
1. Using a mortar and pestle pulverize a small amount about .5g of dry alum. 2. Pack the alum in a capillary tube to a depth of about .5 cm. to get the alum into the capillary tube push the tube down into a small pile of alum powder. 3. To pack the alum tightly at the closed end of the capillary tube turn the tube so the open end is up and bounce the tube on a desk top. 4. Fasten the capillary tube to the thermometer with a rubber band the alum should be level with the thermometer bulb 5. Using a universal clamp and cork stopper fasten the thermometer to a ring stand 6. Immerse the bottom of the capillary and the thermometer in a beaker of water (or Thiele melting point tube filled with water) and heat. If using a beaker stir the water to maintain an even distribution of temperature. The water bath may be heated rapidly in the beginning but as the temperature approaches the melting point of alum the waters bath should be heated more slowly in order to get a more accurate temperature reading of the melting point. 7. Record the temperature at which the alum melts in the part one Data table 1 8. Repeat the melting point determination , using a fresh sample of alum and a new capillary tube.

Part 2

Joshua Gullace

AP Chemistry Lab #2

2011

1. Set up a Bunsen burner on a ring stand beneath a ring clamp holding a clay pipestem triangle Do Not light the Bunsen burner 2. Adjust the height of the ring clamp so that the bottom of a crucible sitting o the clay triangle is about 1 cm above the flame when the Bunsen burner is lit 3. Place a crucible cover in the clay triangle and heat until the crucible is red hot 4. Turn off the gas and remove the burner 5. Using tongs remove the crucible cover and place it on a wire gauze on the bench top. With the tongs remove the crucible from clay triangle and place it on the wire gauze as well 6. Allow the crucible and its cover to cool completely on the wire gauze for at least 10 minutes \ 7. Find their mass using an analytical balance handle with tongs or forceps to avoid getting fingerprints on the crucible and lid 8. Record their mass in the Part 2 Data Table 9. Now add 2 g of alum crystals to the crucible weigh the crucible cover and crystals and record their combined mass in Part 2 Data Table 10. Set the crucible at an angle in the triangle held in a ring on a ring stand. Cover the crucible loosely with the crucible cover and heat very gently the alum crystals will melt and the water hydration will evaporate it is important that the escaping vapor does not carry any of the anhydrous alum along with it so be sure that the crystals are heated very gently at first 11. After the bubbling has stopped heat the sample more strongly for an additional five minutes 12. Turn off the gas source and remove the burner 13. Using the tongs remove the crucible cover and place it on a wire gauze on the bench top. With the tongs remove the crucible from the clay triangle and place it on the wire gauze as well 14. Allow the crucible and its cover to cool completely on the wire gauze for at least 10 minutes 15. Measure and record the mass of the crucible, cover, and anhydrous alum 16. Repeat the drying procedure until the constant mass is obtained 17. Record the final mass of the crucible, cover and anhydrous alum in the Part 2 Data Table 18. Dispose of the anhydrous alum according to your instructors directions carefully clean the crucible and crucible cover

Part 3
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. obtain a Gooch crucible with a fiber glass filter pad Walter adapter and filter flask. Connect the flask with vacuum tubing to an aspirator Turn on the vacuum to pull approximately 50 mL of distilled water through the filter pad. Turn off the vacuum remove the crucible and place the crucible in a 250 mL beaker Dry the beaker and Gooch crucible in a drying oven at 120C for 15 minutes Using tongs remove the beaker and Gooch crucible and set them aside to cool Determine the mass of the cooled crucible using an analytical balance record the mass in the Part 3 Data Table Use an analytical balance to accurately weigh about 1gram of alum in a 250 mL beaker Dissolve the alum in approximately 50 mL of distilled water d Obtain 50 mL of the .200M Ba(NO3)2 solution in a clean 50 mL graduated cylinder Add twice the volume of the .200M Ba(NO3)2 calculated in the Pre-lab questions #3 slowly into the alum solution while stirring

Joshua Gullace

AP Chemistry Lab #2

2011

12. Cover the beaker with a watch glass and heat the solution nearly to boiling. Keep the solution just under the boiling point for at least 15 minutes. During this time the precipitate particles should grow to a filterable size 13. Filter the precipitate through the Gooch crucible with suction. Do not fill the crucible too full as the Barium sulfate has a tendency to creep up the sides use a rubber policeman to be sure that every particle is transferred from the beaker and stirring rod into the filter crucible 14. Wash the beaker and the precipitate several times with small quantities of distilled water 15. Carefully transfer the Gooch crucible to a beaker and dry it for 15 minutes in an oven set at 120C 16. Allow the dry Gooch crucible and determine its mass. Record the mass in the Part 3 Data Table

Data Table:
Part 1 Data table: Measured melting point Literature melting point Trial 1 92.5C 92.5C Trial 2 93C 93C

Part 2 Data Table: Mass of crucible and cover Mass of crucible cover and alum crystals Mass of alum crystals Mass of crucible cover and alum after heating # 1 Mass of crucible cover and alum after heating #2 Mass of water driven off Mass of anhydrous alum AlK(SO4)2 Moles H2O Moles AlK(SO4)2 Mole ratio: moles H2O/moles AlK(SO4)2 Part 3 Data Table: Mass of alum Mass of dry Gooch crucible Mass of Gooch crucible plus barium sulfate Mass of barium sulfate Mass of sulfate in precipitate Experimental percent sulfate in alum Theoretical percent sulfate in alum

21.43g 23.43g 2g 22.52g 22.53g 1.09g .91g .0605 3.52 x 10-3 17.19 : 1

1.026g 31.548g 32.586g 1.038g 0.4272g 42.23% 37.20%

Analysis: Part 1
The literature based melting point for alum is 92.5C based off of internet source

Part 2
26.982+39.098+2(32.066+(8*15.999))=258.194g molar mass of anhydrous alum

Joshua Gullace .91/258.194=.00352 moles of alum from the experiment

AP Chemistry Lab #2

2011

.0605/.00352=17.19 which is ratio of moles of water to moles of alum aka 17.19:1

Part 3 Molar mass of Ba(SO4)2=137.33+96.062=192.114 96.062/192.114 = 41% sulfate .41(1.038) = .4272g of sulfate in precipitate .4484/1.062 = 42.23% sulfate in alum sample 96.057/258.194 = 37.2% of theoretical sulfate in alum .4223/.3720 = 113.2% Conclusion: We were able to identify that this is indeed alum crystals but the level is not that of pure alum and as a result of that along with numerous sources of error were received a percentage of sulfate that was higher than the theoretical percentage we would expect which shows that our data is off by roughly 13% which is not a wide margin of error but is still a margin from this data we can conclude that not all conditions were perfect whenever we did this experiment and as such are results reflect our findings. Through the melting point we were able to conclude that this may be some form of alum then with the second test we were able to determine through the hydration level that It was indeed alum and were able to be even more certain then with the third test we were able to determine just how off our alum sample was from pure alum crystals. This factor along with our sources of error were the reason why we obtained such a high percentage of error Post Lab Questions: 1. Why must objects be cooled before their mass is determined on a sensitive balance? When particles are heated they increase in speed which causes the mass to become less than what it would be at standard room temperature. 2. Comment on the results of the different tests used to verify that the sample was alum. Although the tests were not exactly the numbers we needed they were close enough to prove that this indeed was a sample of aluminum potassium sulfate 3. What other tests could be used to verify the composition of alum? You could test the density and its reaction with other compounds

SOE:
4 broken crucible lids 2 broken crucibles

Joshua Gullace Broken lighter Incorrect procedures

AP Chemistry Lab #2

2011