Gravimetric Analysis of a Metal Carbonate
Introduction
How do chemists determine the identity of a compound? A large variety of analytical techniques and procedures,
ranging from instrumental methods such as spectroscopy and chromatography to more classical processes, such as
qualitative and gravimetric analyses, have been created to accomplish that task. In this laboratory, the identity of a
Group 1 metal carbonate is determined gravimetrically using a double-replacement precipitation reaction.
Experimental Overview
The purpose of this lab is to determine the identity of a Group 1 metal carbonate compound by gravimetric analysis.
The unknown is weighed and dissolved in water. A solution of calcium chloride is added to the metal carbonate solution
to precipitate the carbonate ions as calcium carbonate. The precipitate is filtered, dried and weighed. From the data,
the formula weight and identity of the unknown metal carbonate is determined.
Materials
Unknown sample, M2CO3, 2 g
0.4 M CaCl2 solution, 125 mL
Distilled water
Ring stand with iron ring
Funnel
Stirring rod
Bunsen burner
Crucible tongs
Crucible
Analytical and Electronic Balance
Wash bottle
2 Beakers, 400 mL or 250 mL
Drying oven
Filter paper
Clay triangle
Watch glass
Procedure
1. Obtain a clean, dry crucible.
2. Set up a Bunsen burner on a ring stand beneath a ring clamp holding a clay
triangle. Place the crucible in the clay triangle.
3. Light the Bunsen burner and heat the crucible for about 1 minute. Allow
crucible to cool.
4. Using tongs to handle the crucible, measure the mass of the clean, empty
crucible to the nearest .01g using an electric balance.
5. While the crucible is still on the balance, add approximately 2 g of the
unknown carbonate to the crucible.
6. Place the crucible on the clay triangle as shown in figure 2.
Light the Bunsen burner again and slowly heat the crucible for 2-3 minutes.
Allow crucible to cool before weighing.
7. Repeat step 6 until the mass of the crucible and unknown carbonate no longer decreases. Note: the Group 1
carbonates are hygroscopic – they absorb water from the air. These heating steps are necessary to ensure the crucible
is dry and the carbonate samples are anhydrous when massed.
8. Add the crucible contents to a 400-mL beaker.
9. Add about 50 mL of distilled water to the beaker and stir to dissolve the unknown carbonate. If it does not fully
dissolve, add more water.
10. Add about 125 mL of the 0.4 M CaCl2 solution to the 400-mL beaker with the dissolved carbonate and stir.
11. Let the precipitate settle (5 minutes).
12. Obtain a piece of filter paper and determine its mass to the nearest 0.0001g using an analytical balance.
13. Place the filter paper into a Buchner funnel. Moisten with about 5 mL of distilled water from a wash bottle.
14. Set up the Buchner funnel apparatus: http://www.youtube.com/watch?v=1JygPCD8bKE
15. Using a stirring rod, decant the liquid from the 400-mL
beaker slowly into the center of the funnel.
16. When all but about 10 mL of the liquid has been transferred,
swirl the beaker to suspend the precipitated CaCO3. Transfer this
to the center of the filter paper in the funnel.
17. Rinse the beaker with small amounts of distilled water from
the wash bottle and then transfer the washings to the filter.
18. When all the solid has been transferred to the filter paper,
rinse the solid with three small portions of distilled water. Allow
the funnel to drain completely.
19. Obtain a watch glass. Use a sharpie to put your initials on it.
Using a microspatula, take the filter paper out of the funnel and
place it in the center of the watch glass. Be careful not to tear
the paper or to lose any part of the solid. Place the watch glass
and filter paper in a drying oven set at 110 C and allow to dry
overnight.
Before lab:
Create a table to record all necessary data.
Watch the video on how to set up a Buchner funnel.
After lab:
Show all your calculations and determine the identity of the Group 1 metal carbonate.