AP Chem U2-2 Hand In Lab on Hydrates

 

Objective

Chemical compounds that contain discrete water molecules as part of their crystalline structure are called hydrates. Hydrates occur quite commonly among chemical substances. More often than no, some compounds are either prepared in, or are recrystallized from, aqueous solutions. Hydrates exist for ionic compounds most commonly, but hydrates of polar and nonpolar covalent molecules are also known. In this experiment, you will study some of the properties and characteristics of several ionic hydrates.

 

Introduction

Hydrates are most commonly encountered in the study of metal salts, especially those salts of the transition metals. Water is bound in most hydrated in definite, stochiometric proportions, and the number of water molecules bond per metal ion is often characteristic of a particular metal ion.

            A very commonly encountered in the general chemistry laboratory is copper(II) sulfate pentahydrate, CuSO4.5H2O. The word “pentahydrate” in the name of this substance indicates that five water molecules are bound in this substance per copper sulfate formula unit. Hydrated water molecules are generally indicated in formulas as shown above for the case of the copper sulfate, using a dot to separate water molecules from the formula of the salt itself.

            Many hydrated salts can be transformed to the anhydrous (without water) compound by heat. For example, if a sample of copper sulfate pentahydrate is heated. The bright blue crystals of the hydrate are converted to white powdery, anhydrous salt.

 

CuSO4.5H2O(s)ŕ CuSO4(s) + 5H2O(g)

Blue                  white                         

 

During the heating of copper sulfate pentahydrate, the water of crystallization is clearly seen escaping as steam from the crystals.

            It is also possible to reconstitute the hydrate of copper sulfate: if water is added to the white anhydrous salt, the solid will reassume the blue color of the hydrated salt. Anhydrous salts are sometimes used as chemical drying agents, or desiccants, because of their ability to with and remove water from their surroundings. For example, most electric equipment (and even at least one brand of ground coffee) comes packed with small envelopes of a desiccant to protect the equipment from moisture. Substances that absorb moisture and are able to be used as desiccants are said to be hygroscopic.

            Not all hydrated salts are converted simple into the anhydrous compound when heated, however. Some hydrated metal salts will decompose upon loosing the water of crystallization; subsequently they are usually converted into the metal oxide if the heating is carried out in air. Most covalent hydrates decompose rather than simply loose water when heated.

            The water molecules contained within the crystals of a hydrate may be bound by several different means. For the case in which water molecules are bound with a metal salt, generally a nonbonding pair of electrons on the oxygen atom of the water molecule forms a coordinate covalent bond with empty, relatively low energy d-orbitals of the metal ion. In the case of copper sulfate pentahydrate, for example, four or five of the water molecules form such coordinate bonds with the copper (II) ion. In other situations, water molecules of the hydrate may be hydrogen-bonded to one or more species of the salt. This is especially common for covalently bonded hydrates.

 

Safety Precautions

Wear safety glasses at all times while in the laboratory

Copper, cobalt, nickel, chromium, and barium compounds are all highly toxic. Wash hands after use.

When you are heating the hydrated metal salts, they may splatter if heated too strongly. To avoid this, Heat the solids with as small as flame as possible at first, and do not heat strongly with the full heat of the burner until most of the water has been driven from the hydrate. Make certain that the mouth of the test tube used to heat the hydrate is not pointed at yourself or anyone else.

Dispose of the metal salts as directed by the instructor. Do not wash the salts down the drain, and do not place them in the wastebasket.

 

Apparatus/Reagents Required

Nickel (II) chloride hexahydrate, cobalt (II) chloride hexahydrate, copper (II) sulfate pentahydrate, chromium (III) chloride hexahydrate and anhydrous chloride.

 

Procedure

            Part 1

Record all data and observations directly in your notebook in ink.

Your grade will in part be influenced by how accurate your data is…be painstakingly careful with measurements (lose up to 4 points).

            Determine the mass of a clean, dry casserole or small evaporating dish to the nearest milligram (0.001 g). Add to the casserole or evaporating dish a spatula tip-full of copper (II) sulfate pentahydrate, CuSO4.5H2O, and reweigh. Calculate the mass of CuSO4.5H2O taken. Record the appearance of the crystals.

            Based on the mass of CuSO4.5H2O taken and its formula, calculate the theoretical mass of water that should be lost from the crystals if all the water were driven off.

            Set up a wire gauze on a metal ring, are prepare to heat the casserole/evaporating dish in the burner flame. Begin the heating with a very small flame.  If there is any evidence that the material is about to spatter, remove the heat immediately. Record any changes in color/appearance as the hydrate is heated.

            When it is apparent that most of the water has been driven from the sample, increase the size of the flame. Stir the salt with a clean stirring rod until the sample is uniform in texture and appearance.

            Remove the heat and allow the casserole to cool completely to room temperature. When the casserole has cooled completely, reweigh and calculate the mass of water driven off from the crystals. Using theoretical mass loss calculated above, along with the experimentally determined mass loss, determine the percent error in your experiment.

            After all mass determinations for the CuSO4.5H2O sample have been completed, add water drop wise to the sample. Record any changes in appearance/color.

            For the hydrates listed below, first record the appearance of the crystals. Then transfer tiny amounts of the hydrates to each separate, clean borosilicate test tubes.

            Part 2

Repeat this procedure for a Nickel or a Cobalt Chloride hydrate compound. Determine the % composition for the hydrate. Take note that the grade will reflect how close you are to the correct percent.

 

Analysis Questions part 1

 

1. Use a handbook of chemical data to find the number of water molecules bound per formula unit in the common hydrates of the following salts:

Strontium Chloride, SrCI2

Sodium Chromate, Na2CrO4

Nickel (II) Nitrate, Ni(NO3)2

Iron (II) Ammonium Sulfate, Fe(NH4)2(SO4)2

 

2. As described in the introduction to this experiment, when copper (II) sulfate pentahydrate is heated, the deep blue color of the hydrate changes to the white color of the anhydrous salt. Use the sections of your textbook discussing the chemistry of the transition elements to determine why such a vivid change in color is common when such elements’ hydrated compounds are heated. 

 

 

 

 

3. Suppose 2.3754 g of copper(II) sulfate pentahydrate is heated to drive off the water crystallization. Calculate what weight of anhydrous salt will remain.

 

 

 

 

 

 

4. CuSO4.5H2O, it was mentioned that four of the five water molecules held per formula unit of the salt were attached by coordinate covalent bonds to the copper ion. The fifth water molecule is attached to the sulfate ion, but by a different mechanism. Use your textbook or a chemical encyclopedia to determine how a water molecule might be bonded to a sulfate ion.

 

 

 

 

 

 

 

Results/Observations

Data Part 1

Copper (II) sulfate pentahydrate

Mass of empty casserole/evaporating dish, g

Mass of casserole/evaporating dish plus CuSO4.5H2O, g

Mass of taken CuSO4.5H2O, g

Appearance of CuSO4.5H2O

Theoretical mass loss expected on heating CuSO4.5H2O

Mass of casserole/evaporating dish after heating, g

Mass of water lost from CuSO4.5H2O crystals, g

% error in mass water lost from CuSO4.5H2O, g

Appearance of CuSO4 after heating

Appearance of CuSO4 on adding water

 

Data Part 2

 

 

 

 

 

 

 

 

 

 

 

 

Analysis Questions part 2

5. Use a chemical dictionary or your book to distinguish between the terms desiccant, hygroscopic, and deliquescent.

 

 

 

 

 

6. Sugars and starches belong to a class of biological compounds called carbohydrates, indicating that the general formula for such compounds is of the sort (CH2O)n. Use your book to find out why such compounds are not really hydrates of carbon as the family name suggests and record you findings here.

 

 

 

 

 

 

 

7. Generalize the colors of the above solutions and use any other reference source to cite generalized solution colors.

 

 

 

Chance of Vindication (add up to 4 points)

Repeat the procedure of above with the other chloride • unknown hydrate sample. Take mass readings before and after heating. Determine the mass driven off from the sample and hence the amount of water. Work backwards as before to determine the amount of water in the hydrate molecule. Label and record your data below and show any/all calculations.