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VI-1 Chem 2115 Experiment # 6 PERIODIC RELATIONSHIPS

VI-1 Chem 2115 Experiment # 6 PERIODIC RELATIONSHIPS

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<strong>Chem</strong> <strong>2115</strong> <strong>Experiment</strong> # 6<br />

<strong>PERIODIC</strong> <strong>RELATIONSHIPS</strong><br />

OBJECTIVES: Gaining insight into property and reactivity trends within families and across periods for the<br />

chemical elements through experimental observation.<br />

SKILLS: Observations, manipulation and preparation of solutions<br />

EQUIPMENT: Clean test tubes<br />

REFERENCE: : <strong>Chem</strong>istry: Matter and its Changes, Brady & Senese, 5 th ed, pp. 127–135; 273–281; 284–291<br />

SAFETY AND DISPOSAL: The vigorous exothermic reactions of Li, Na, and K with water will be demonstrated.<br />

Everyone must wear safety goggles during the demonstration. Small pieces of unreactive metals (EXCEPT Na, Li,<br />

K) may be rinsed with water and placed in the trash can. Acid solutions should be diluted with water and can be<br />

flushed down the sinks. Solid elemental oxides should be combined with water and diluted before disposal down<br />

the sinks. Organic solvents (i.e., hexane) containing halogens should be placed in the waste jar in the hoods. All<br />

halide salts can be disposed of in the trash.<br />

INTRODUCTION: The periodic table provides a useful theoretical and experimental summary of the behavior of<br />

the chemical elements. It was developed from observations of reactivity similar to those that will be made during<br />

this experiment. In particular, observations of similar behavior permits grouping of different elements into chemical<br />

families, while noting trends within families allows ordering of elements in each column. These groupings, based<br />

on experimental observations, are in agreement with theoretical descriptions of the atom.<br />

From a theoretical view, atoms have protons and neutrons in the nucleus, surrounded by electrons grouped into<br />

shells. Filled shells are stable, and atoms may react by gaining or losing electrons to complete their outer shells and<br />

become ions. The periodic table arranges elements with electrons in different outer shells into different rows, and<br />

puts elements with similar outer shell electron configurations into the same column. Thus going down columns of<br />

the periodic chart, elements behave similarly because of their similar electron configurations; going across rows,<br />

elements show changing properties because of different electron configurations.<br />

Trends in each column, or Group as they are known, are governed by the ability of an atom to gain or lose electrons.<br />

Smaller elements, near the top of the chart, have electrons (negatively charged) closer to the nucleus (positively<br />

<strong>VI</strong>-1


charged). Thus electrons will be attracted more strongly and in metals electrons will be lost with more difficulty<br />

than elements lower in each column. Conversely, for non-metals, which gain electrons to from ions, the elements<br />

near the top of the group will be more active since fewer electrons screen the positive nucleus. This theoretical<br />

prediction can be used to understand and explain the experimentally observed behavior.<br />

Trends in the behavior of elements in each group are governed by the preference to have a complete outer shell.<br />

Elements closer to complete shells tend to be more reactive than elements with electron configurations farther from<br />

completion. The noble gas elements, which are generally unreactive, all have complete electron shells.<br />

This experiment begins with observations of the reactivity of some metals and simple oxides (to gain insight into<br />

trends). It then focuses on the halogen family, showing the behavior of three of these elements plus their salts and<br />

solutions in water and hexane. Reactions between them are used to illustrate trends and to permit identification of<br />

unknown samples.<br />

I. Reactivity of Metals<br />

The reactivity of Na, Li, and K from Group IA, of Mg and Ca from Group IIA, and of Al from Group IIIA<br />

will be compared by observing some of their reactions with water and hydrochloric acid. From the<br />

observations, comparisons between Groups and within Groups can be made.<br />

II. Halogens<br />

The properties of chlorine (Cl2), bromine (Br2) and iodine (I2) will be observed. Chlorine is a greenish gas<br />

at room temperature and is commonly used in the laboratory. Aqueous solutions of chlorine will be used to<br />

illustrate some of the properties of chlorine. Bromine will be observed in a closed tube. Iodine will be<br />

sublimed (converted directly from the solid to the gaseous phase) and recrystallized to study its behavior.<br />

Solutions of each of these elements in water and in hexane will be examined.<br />

III. Halide Salts<br />

Halide salts are compounds formed from metals and halogen elements. The potassium halide salts will be<br />

studied by comparing their colors, solubilities, and reactivities, both alone and in combination with water,<br />

hexane, and aqueous solutions of chlorine, bromine, and iodine.<br />

Halide ions are formed when neutral halogen molecules are reduced (gain electrons from some other<br />

species, which loses them). Halide ions may lose their electrons to a more active halogen. In this<br />

experiment, chloride (Cl - ), bromide (Br - ), and iodide (I - ) ions will be combined with aqueous (water)<br />

solutions of Cl2, Br2, and I2 molecules to observe when these reactions will occur. Hexane will be added to<br />

provide evidence of reaction, since the halogen molecule which remains after reaction (or lack of reaction)<br />

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can be inferred from observing the color of the hexane layer.<br />

There is a clear trend in halogen reactivity that is related to its position on the periodic chart. This trend can<br />

be interpreted in terms of the distance between the nucleus and the outer shell electrons for each atom. The<br />

experimental observations can also be used to identify an unknown halide by comparing its behavior to that<br />

of a known sample.<br />

IV. Determination of an Unknown Halide Salt<br />

An unknown solution of either KCl, KBr, or KI in water will be assigned to each student. Students will be<br />

able to determine which of the unknown salts they have by applying the tests used in Part III D.<br />

Since the focus of this experiment is observation, be careful to write down what you see in your lab notebook as you<br />

do each step. Some of the observations in early sections will be needed to answer questions in later sections of this<br />

experiment.<br />

EXPERIMENTAL PROCEDURES<br />

BE SURE TO WEIGH YOUR CRUCIBLE AND PRODUCT FROM EXPERIMENT 5 THAT HAS DRIED<br />

OVER THE WEEK IN YOUR LOCKER. RECORD THE MASS AND ENTER THE DATA ON THE LAB<br />

COMPUTER.<br />

I. Reactivity of Metals<br />

A. (This section will be demonstrated by your instructor.) Observe freshly cut pieces of sodium, lithium<br />

and potassium. Record the physical state, color and consistency of each element. Observe the reactivity of<br />

each metal when your instructor places a small piece of each metal in separate beakers containing water<br />

and phenolphthalein. (NOTE: This is a demonstration of the reactivity of the metals with water. This is<br />

NOT an appropriate method of disposal because of the explosion potential related to the very high<br />

reactivity of these elements compared to Ca, Mg and Al.)<br />

B. Place one small piece of Ca, Mg and Al into separate test tubes. Slowly add 3-4 mL of distilled water<br />

and a drop of phenolphthalein to each test tube. Phenolphthalein will identify one of the products formed;<br />

it changes to a pink or red in the presence of a base ( OH - ) and remains colorless in an acidic ( H + )<br />

solution. Note that some reactions happen very quickly while others take much more time. If you do not<br />

observe any reaction initially, check the test tube after 15 minutes to see if a slow reaction occurred.<br />

Did any of the solutions become basic? Observe the reactivity of each metal. Which is more reactive?<br />

<strong>VI</strong>-3


C. Place a small piece of Mg and Al into separate test tubes. Carefully add 3 mL of 6 M HCl<br />

(hydrochloric acid) drop by drop. Observe the reactivity of each metal. Which is the most reactive?<br />

Notebook observations:<br />

I. Reactivity of Metals: Observations for this section should include color changes, bubbling (gas<br />

formation), temperature changes, formation/disappearance of a precipitate, and color when phenolphthalein<br />

is added.<br />

II. Halogens (Parts II A and IIB will be demonstrated by your instructor)<br />

A. Observe and describe the color and physical appearance of bromine in a closed tube when the end of the<br />

tube is immersed first in ice water and then in warm water.<br />

B. A few crystals of iodine will be placed in a small beaker and heated. The beaker will be covered with a<br />

watch glass that has some ice on it. Observe what happens to the iodine in the beaker and the formation of<br />

iodine crystals on the watch glass. The violet fumes are gaseous I2 vapor. CAUTION: Iodine is a toxic<br />

material; avoid breathing the fumes.<br />

C. Place 2 mL of aqueous solutions of Cl2, Br2, and I2 into separate test tubes. Observe the characteristic<br />

colors of each of the aqueous solutions. To each tube add 1 mL of hexane. (note which layer is the<br />

hexane layer. Is it on top or bottom?) Water and hexane are immiscible (not mutually soluble). Stopper<br />

the tube (do not use your fingers) and shake vigorously. Observe the color of each halogen in the hexane<br />

layer. Halogens are more soluble in hexane than in water, so the halogen (Cl2, Br2, or I2) will move to the<br />

hexane layer. The colors in hexane are characteristic of the halogen and can be used to identify which<br />

halogen is present in a sample.<br />

Notebook observations:<br />

IIA and B. Observations for these sections should include changes in state and colors observed.<br />

II C. Prepare a table of observations with three columns (Halogen, color of water layer, and color of<br />

hexane layer) and with rows for Cl2, Br2 and I2 Since water is denser than hexane, the aqueous layer is on<br />

the bottom of the test tube.<br />

<strong>VI</strong>-4


III. Halide Salts<br />

A. Observe the appearance of three halide salts - KCl, KBr, and KI - as solids and in solution (if any).<br />

Put a few crystals of each one into separate test tubes, add water, and shake to see if they dissolve.<br />

Put a few crystals of each one into separate test tubes, add hexane, and shake to see if they<br />

dissolve.<br />

B. Using clean test tubes, prepare the following set of nine systems:<br />

3 test tubes, each containing 2 mL of 0.1 M KCl and 1 mL of hexane.<br />

3 test tubes, each containing 2 mL of 0.1 M KBr and 1 mL of hexane.<br />

3 test tubes, each containing 2 mL of 0.1 M KI and 1 mL of hexane.<br />

To study the reactivity of the halide salts, mix each of their solutions with 1 mL of aqueous<br />

solutions of Cl2, Br2, and I2. (Put 1 mL of Cl2 solution into a test tube with KCl solution, 1 mL of<br />

Cl2 solution into a test tube with KBr, and 1 mL of Cl2 solution into a test tube with KI solution.<br />

Then do the same for Br2 and I2 solutions.) It may be helpful to construct a table similar to the<br />

one shown below to record your observations. Each box in the table represents one of your nine<br />

test tubes.<br />

Cl - Br - I -<br />

Cl2 Cl2 + Cl - Cl2 + Br - Cl2 + I -<br />

Br2 Br2 + Cl - Br2 + Br - Br2 + I -<br />

I2 I2 + Cl - I2 + Br - I2 + I -<br />

Observe the color of the hexane layer after mixing, comparing it to the results in Part IIC. If the<br />

color is the same as would be expected for the added halogen, then no reaction has occurred. If it<br />

is not, then this is evidence of a reaction.<br />

<strong>VI</strong>-5


Notebook observations:<br />

IIIA. Halide Salts: Prepare a table of observations with three columns (solid, with water, and with hexane)<br />

and with rows for KCl, KBr and KI. Your observations should include color (distinguishing the color<br />

white from “colorless”), whether or not the solid dissolves, and the color of liquids.<br />

IIIB. Halide Salt Reactions: Prepare a table of observations with three columns (for Cl2, Br2 and I2) and<br />

with rows for KCl, KBr and KI (similar to the table shown above). In each of the 9 boxes, put your<br />

observations of the colors of the (bottom) water layer and the (top) hexane layer. The hexane layer color<br />

will be crucial in determining what halogen is present after any possible reaction has taken place. (Note:<br />

Five of these systems should have I2 in the hexane layer after the halogen addition, three should have Br2<br />

and one should have Cl2. If your results do not agree with this, check with your instructor.)<br />

At this point you should be able to write the chemical reactions for samples that exhibited a reaction. For<br />

example, when chlorine (Cl2) is mixed with the iodide ion (I - ) a reaction should be observed (after shaking,<br />

the hexane layer is the characteristic color if iodine, I2). Since you began with the iodide ion (KI) and<br />

ended up with the iodine molecule (I2), this is evidence of a reaction:<br />

In many cases you will not observe any reaction (the color of the hexane layer exhibits the characteristic<br />

color of the halogen you began with). In this case, no reaction took place between the halogen and the<br />

halide.<br />

IV. Determination of an unknown halide<br />

Take one of the unknown solutions, which will contain KCl, KBr, or KI, and determine which it is by<br />

applying a test used in Part IIIB. To do this, it will be necessary to plan a procedure to distinguish between<br />

the solutions.<br />

Notebook observations:<br />

IV. Unknown halide salt determination. Write the unknown number of your salt solution. Include a<br />

clear description of the procedure you have chosen in your lab notebook. Write down your observation of<br />

the outcome of this procedure and your conclusion about the identity of your unknown.<br />

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