Experiment 2

Identification of
a Compound:
Chemical Properties
Jo A. Beran

A potassium chromate solution added to a silver nitrate solution results in the formation
of insoluble silver chromate.

• To identify a compound on the basis of its chemical properties Objectives

• To design a systematic procedure for determining the presence of a particular Chemical property: characteristic of
compound in aqueous solution a substance that is dependent on its
chemical environment

The following techniques and safety practices are used in the Experimental Procedure: Techniques
and Safety
Practices

Chemists, and scientists in general, develop and design experiments in an attempt to Introduction
understand, explain, and predict various chemical phenomena. Carefully controlled (labo- and
ratory) conditions are needed to minimize the many parameters that affect the observations.
Chemists organize and categorize their data and then systematically analyze the data to reach
Applications
some conclusion; often, the conclusion may be to carefully plan more experiments!
It is presumptuous to believe that a chemist must know the result of an experiment
before it is ever attempted; most often, an experiment is designed to determine the pres-
ence or absence of a substance or to determine or measure a parameter. A goal of the Substance: a pure element or
environmental or synthesis research chemist is, for example, to separate the substances of compound having a unique set of
chemical and physical properties
a reaction mixture (one generated in the laboratory or one found in nature) and then iden-
tify each substance through a systematic, or sometimes trial-and-error, study of their Trial-and-error study: a method that
chemical and physical properties. As you will experience later, Experiments 35, 37–39 is often used to seek a pattern in the
accumulated data
are designed to identify a specific ion (by taking advantage of its unique chemical prop-
erties) in a mixture of ions through a systematic sequence of analyses.
In this experiment, you will observe chemical reactions that are characteristic of var-
ious compounds under controlled conditions. After collecting and organizing your data,
you will be given an unknown compound, one that you have previously investigated. The
interpretations of the collected data will assist you in identifying your unknown compound.
What observations will you be looking for? Chemical changes are generally
accompanied by one or more of the following:
• A gas is evolved. This evolution may be quite rapid, or it may be a “fizzing”
sound (Figure 2.1). Experiment 2 69
 • A precipitate appears (or disappears). The nature of the precipitate is important.
It may be crystalline, it may have color, or it may merely cloud the solution.
• Heat may be evolved or absorbed. The reaction vessel becomes warm if the
reaction is exothermic or cools if the reaction is endothermic.
• A color change occurs. A substance added to the system may cause a color
change.
• A change in odor is detected. The odor of a substance may appear, disappear,
or become more intense during the course of a chemical reaction.
The chemical properties of the following compounds, dissolved in water, are
investigated in Part A of this experiment:
Jo A. Beran

Sodium chloride NaCl(aq)

Sodium carbonate Na2CO3(aq)
Magnesium sulfate MgSO4(aq)
Figure 2.1 A reaction Ammonium chloride NH4Cl(aq)
mixture of NaHCO3(aq) and Water H2O(l)
HCl(aq) produces CO2 gas. The following test reagents are used to identify and characterize these compounds:
Silver nitrate AgNO3(aq)
Sodium hydroxide NaOH(aq)
Hydrochloric acid HCl(aq)
Reagent: a solid chemical or a In Part B of this experiment, the chemical properties of five compounds in aque-
solution having a known ous solutions, labeled 1 through 5, are investigated with three reagents labeled A, B,
concentration of solute
and C. Chemical tests will be performed with these eight solutions. An unknown will
then be issued and matched with one of the solutions, labeled 1 through 5.

Experimental Procedure Overview: In Part A, a series of tests for the chemical properties of known
Procedure compounds in aqueous solutions are conducted. A similar series of tests are conducted on
an unknown set of compounds in Part B. In each case, an unknown compound is identified
on the basis of the chemical properties observed.
You should discuss and interpret your observations on the known chemical tests with
a partner, but each of you should analyze your own unknown compound. At each circled
superscript 1–7 in the procedure, stop and record your observation on the Report Sheet.
To organize your work, you will conduct a test on each known compound for the
five aqueous solutions and the unknown compound with a single test reagent. The Report
Sheet provides a “reaction matrix” for you to describe your observations. Because the
Andy Washnik

space is limited, you may want to devise codes such as the following:
• pc—precipitate + color • g—gas, no odor
• cc—cloudy + color • go—gas, odor
A mix of AgNO3 and NaCl • nr—no reaction
solutions produce a white AgCl
precipitate.

A. Chemical Properties of 1. Observations with silver nitrate test reagent

Known Compounds a. Use a permanent marker to label five small, clean test tubes (Figure 2.2a) or
set up a clean 24-well plate (Figure 2.2b). Ask your instructor which setup
you should use. Place ~1 mL of each of the five “known” solutions into the
labeled test tubes (or wells A1–A5).
b. Use a dropper pipet (or a dropper bottle) to deliver the silver nitrate solu-
tion to each of the known solutions. (Caution: AgNO3 forms black stains on
the skin. The stain, caused by silver metal, causes no harm.) If after adding
several drops you observe a chemical change, then add 5–10 drops to see
Avoid Skin Contact if there are additional changes. Record your observations in the matrix on

70 Identification of a Compound: Chemical Properties

 AgNO3 1 2 3 4 5 6
A
B Silver nitrate tests
C Sodium hydroxide
D tests
Hydrochloric acid
tests

Figure 2.2b Arrangement of test solutions in the 24-well plate for testing salts.

NaCl Na2CO3 MgSO4 NH4Cl H2O

Figure 2.2a Arrangement of test
tubes for testing with the silver
nitrate reagent.

the Report Sheet.1 Save your test solutions for Part A.4. Write the formula
for each precipitate that forms. Ask your lab instructor for assistance. For
example, a mixture of NaCl(aq) and AgNO3(aq) produces AgCl(s) as a Appendix E
precipitate. The insolubility of AgCl is noted in Appendix E.
2. Observations with sodium hydroxide test reagent
a. Use a permanent marker to label five additional small, clean test tubes
(Figure 2.3). Place ~1 mL of each of the five “known” solutions into this
second set of labeled test tubes (or wells B1–B5, Figure 2.2b).
b. To each of these solutions, slowly add 5–10 drops of the sodium hydroxide
solution; make observations as you add the solution. Check to see if a gas
evolves in any of the tests. Check for odor. What is the nature of any precip-
itates that form? Observe closely.2 Save your test solutions for reference in
Part A.4. Write the formula for each of the precipitates that formed. Appendix E

3. Observations with hydrochloric acid test reagent

a. Use a permanent marker to label five additional small, clean test tubes (Fig-
ure 2.4). Place ~1 mL of each of the five “known” solutions into this third
set of labeled test tubes (or wells C1–C5, Figure 2.2b).
b. Slowly add 5–10 drops of the hydrochloric test reagent to the solutions and
record your observations. Check to see if any gas is evolved. Check for odor.
Observe closely.3 Save your test solutions for reference in Part A.4. Write
the formula for any compound that forms.

NaOH HCl

NaCl Na2CO3 MgSO4 NH4Cl H2O NaCl Na2CO3 MgSO4 NH4Cl H2O
Figure 2.3 Arrangement of test Figure 2.4 Arrangement of
tubes for testing with the sodium test tubes for testing with the
hydroxide reagent. hydrochloric acid reagent.

Experiment 2 71
 4. Identification of unknown. Obtain an unknown for Part A from your laboratory
instructor. Repeat the three tests with the reagents in Parts A.1, 2, and 3 on your
unknown. On the basis of the data from the “known” solutions (collected and sum-
marized in the Report Sheet matrix) and that of your unknown solution, identify
the compound in your unknown solution.4

Disposal: Discard the test solutions in the Waste Salts container.

CLEANUP: Rinse the test tubes or well plate twice with tap water and twice with
deionized water. Discard each rinse in the Waste Salts container.

B. Chemical Properties of The design of the experiment in Part B is similar to that of Part A. Therefore, 15 clean
Unknown Compounds test tubes or a clean 24-well plate is necessary.
1. Preparation of solutions. On the reagent shelf are five solutions labeled 1
through 5, each containing a different compound. Use small clean test tubes or the
well plate as your testing laboratory. About 1 mL of each test solution is neces-
Avoid Skin Contact sary for analysis.
2. Preparation of reagents. Also on the reagent shelf are three reagents labeled
A, B, and C. Use a dropper pipet (or dropper bottle) or a Beral pipet to deliver
reagents A through C to the solutions.
3. Testing the solutions
a. Test each of the five solutions with drops (and then excess drops) of
reagent A. If, after adding several drops, you observe a chemical change,
add 5–10 drops more to see if there are additional changes. Observe closely
and describe any evidence of chemical change; record your observations.5
b. With a fresh set of solutions 1–5 in clean test tubes (or wells), test each with
reagent B.6 Repeat with reagent C.7
4. Identification of unknown. An unknown solution will be issued that is one of the
five solutions from Part B.1. On the basis of the data in your reaction matrix and
Ken Karp

the data you have collected, identify your unknown as one of the five solutions.

A dropper pipet. 20 drops is

~1 mL of solution.

Disposal: Discard the test solutions in the Waste Salts container.

CLEANUP: Rinse the test tubes or well plate twice with tap water and twice with
deionized water. Discard each rinse in the Waste Salts container.

The Next Step This experiment will enable you to better understand the importance of “separation
and identification,” a theme that appears throughout this manual. For example, refer to
Experiments 3, 35, 37–39. These experiments require good experimental techniques
that support an understanding of the chemical principles involved in the separation
and identification of the various compounds or ions. Additionally, the amounts of a
substance of interest are also determined in other experiments.
Obtain a small (~50 cm3) sample of soil, add water, and filter. Test the filtrate with
the silver nitrate test reagent. Test a second soil sample directly with the hydrochloric
acid test reagent. What are your conclusions?

72 Identification of a Compound: Chemical Properties

 Experiment 2 Prelaboratory Assignment
Identification of a Compound:
Chemical Properties
Date __________ Lab Sec. _____ Name ____________________________________________ Desk No. __________

1. Experimental Procedure, Part A.

a. What is the criterion for clean glassware?

b. What is the size and volume of a “small, clean test tube”?

2. Experimental Procedure, Part A.2. Describe the technique for testing the odor of a chemical.

3. Identify at least five observations that are indicative of a chemical reaction.

4. Depending upon the tip of a dropper pipet, there are approximately 20 drops per milliliter of water. The Experimen-
tal Procedure, Parts A and B, indicates the addition of 5–10 drops of each solution (Figure 2.2a) to the test tubes.
Calculate the volume range in milliliters for the solution.

Experiment 2 73
5. Experimental Procedure, Part A. The substances NaCl, Na2CO3, MgSO4, and NH4Cl, which are used for test solutions, are
all soluble ionic compounds. For each substance, indicate the ions present in its respective test solution.
NaCl:

Na2CO3:

MgSO4:

NH4Cl:

6. Three colorless solutions in test tubes, with no labels, are in a test tube rack on the laboratory bench. Lying beside the
test tubes are three labels: potassium iodide, KI; silver nitrate, AgNO3; and sodium sulfide, Na2S. You are to place the
labels on the test tubes using only the three solutions present. Here are your tests:
• A portion of test tube 1 added to a portion of test tube 3 produces a yellow silver iodide precipitate.
• A portion of test tube 1 added to a portion of test tube 2 produces a black silver sulfide precipitate.
a. Your conclusions are:
Test tube 1

Test tube 2

Test tube 3

b. Write the balanced equation for the formation of silver iodide, AgI, from a mix of two selected solutions provided
above.

c. Write the balanced equation for the formation of silver sulfide, Ag2S, from a mix of two selected solutions provided
above.

74 Identification of a Compound: Chemical Properties

 Experiment 2 Report Sheet
Identification of a Compound:
Chemical Properties
Date __________ Lab Sec. _____ Name ____________________________________________ Desk No. __________

A. Chemical Properties of Known Compounds ADDITIONAL NOTES

Indicate your observations in the reaction matrix.
A. _________________
Test NaCl(aq) Na2CO3(aq) MgSO4(aq) NH4Cl(aq) H2O(l) Unknown

1
AgNO3(aq) ___________ ___________ ___________ ___________ ___________ ___________

2
NaOH(aq) ___________ ___________ ___________ ___________ ___________ ___________

3
HCl(aq) ___________ ___________ ___________ ___________ ___________ ___________

Write formulas for the precipitates that formed in Part A. (See Appendix E)

Part A.1 ___________ ___________ __________ ___________ ___________ ___________

Part A.2 ___________ ___________ __________ ____________ ___________ ___________

Part A.3 ___________ ___________ __________ ____________ ___________ ___________

Sample no. of unknown for Part A.4 ______________________

4
Compound in unknown solution ______________________

B. Chemical Properties of Unknown Compounds B. _________________

Indicate your observations in the reaction matrix.
Sample no. of unknown for Part B.4 ______________________
Solution No. 1 2 3 4 5 Unknown
5
Reagent A ___________ ___________ ___________ ___________ ___________ ___________

6
Reagent B ___________ ___________ ___________ ___________ ___________ ___________

7
Reagent C ___________ ___________ ___________ ___________ ___________ ___________

Compound of unknown is the same as Solution No. ______________________

Experiment 2 75
Laboratory Questions
Circle the questions that have been assigned.
1. Identify a chemical reagent used in this experiment that can be used to distinguish solid CaCl2 (soluble) from solid
CaCO3 (insoluble). What is the distinguishing observation?
2. What test reagent used in this experiment will distinguish a soluble Cl− salt from a soluble SO42− salt? What is the dis-
tinguishing observation?
3. Predict what would be observed (and why) from an aqueous mixture for each of the following (all substances are water
soluble).
a. potassium carbonate and hydrochloric acid
b. zinc chloride and silver nitrate
c. magnesium chloride and sodium hydroxide
d. ammonium nitrate and sodium hydroxide
4. Three colorless solutions in test tubes, with no labels, are in a test tube rack on the laboratory bench. Lying beside
the tests tubes are three labels: 0.10 M Na2CO3, 0.10 M HCl, and 0.10 M KOH. You are to place the labels on the test
tubes using only the three solutions present. Here are your tests:
• A few drops of the solution from test tube 1 added to a similar volume of the solution in test tube 2 produces no
visible reaction but the solution becomes warm.
• A few drops of the solution from test tube 1 added to a similar volume of the solution in test tube 3 produces carbon
dioxide gas.
Identify the labels for test tubes 1, 2, and 3.
5. Three colorless solutions in test tubes, with no labels, are in a test tube rack on the laboratory bench. Lying beside the
test tubes are three labels: silver nitrate, AgNO3; hydrochloric acid, HCl; and sodium carbonate, Na2CO3. You are to
place the labels on the test tubes using only the three solutions present. Here is your analysis procedure:
• A portion of test tube 1 added to a portion of test tube 2 produces carbon dioxide gas, CO2.
• A portion of test tube 2 added to a portion of test tube 3 produces a white silver carbonate precipitate.
a. On the basis of your observations how would you label the three test tubes?
b. What would you expect to happen if a portion of test tube 1 is added to a portion of test tube 3?
6. For individual solutions of the cations Ag+, Ba2+, Mg2+, and Cu2+, the following experimental observations were
collected:
NH3(aq) HCl(aq) H2SO4(aq)
Ag+ No change White ppta No change
Ba2+ No change No change White ppt
Mg2+ White ppt No change No change
Cu2+ Blue ppt/deep blue soln with excess No change No change
a
Example: When an aqueous solution of hydrochloric acid is added to a solution containing Ag+, a white precipitate (ppt) forms.

From these experimental observations,

a. identify a reagent that distinguishes the chemical properties of Ag+ and Mg2+. What is the distinguishing
observation?
b. identify a reagent that distinguishes the chemical properties of HCl and H2SO4. What is the distinguishing
observation?
c. identify a reagent that distinguishes the chemical properties of Ba2+ and Cu2+. What is the distinguishing
observation?
*d. identify a reagent that distinguishes the chemical properties of Cu2+ and Mg2+. What is the distinguishing
observation?

76 Identification of a Compound: Chemical Properties