ACS Chemistry Laboratory Supplement

Project-Based Labs

Contaminated Soil
Introduction
Your team of chemists has been called out to a local farm. The farmer tells you that she is
having problems with the crops in one of the fields. She thinks that the soil has become
contaminated after a road accident that occurred doing the winter. A truck jackknifed and spilled
some of its contents on the field. However, she does not know the nature of the spilled chemicals
and there are no longer any visible clues on the surface of the soil. She does know that the truck
was carrying bulk chemicals for a company that produced inorganic fertilizers, ice melting
compounds for roads, inorganic industrial cleaners, and additives for making cement. The farmer
has asked for your help in identifying the contaminants and suggesting how to alleviate the
problems.
Project Tasks
Some of these tasks will be accomplished experimentally and some by library or web-based
research in appropriate resources.
1. Confirm the observation that there is a problem with the soil.
2. Determine the identity of the contaminant or contaminants.
3. Determine the amount of the contaminant present in the soil.
4. Suggest possible remedies for the existing problems.

Learning and Performance Objectives

1. Record data and observations accurately.
2. Prepare solutions by mass and by molar concentration.
3. Analyze for simple ions in solution using titration techniques.
4. Draw conclusions based on correct interpretation of data.
5. Understand and explain the importance of correct sampling techniques.
6. Understand and explain the importance of a reference sample.
7. Determine the buffer capacity of a complex mixture.
8. Separate and analyze ions in a complex mixture.
9. Decolorize a mixture with a small amount of colored impurity.
10. Determine the pH of heterogeneous mixtures.
11. Use your chemical knowledge to solve a real world problem.
Resources Available
1.
2.
3.
4.
5.
6.
7.

Background on plant growth.

Strategies for drying soil samples.
Suggested strategy for qualitative analysis of soil samples.
Suggested method for testing pH of a soil sample.
A method to determine buffer capacity.
A method to decolorize a soil solution.
Methods to analyze for carbonate, chloride, and phosphate ions.

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Reports
1. Planning sheets are to be completed as directed by your instructor.
2. The final report for this project should follow the basic guidelines given previously.
Be sure to include:
a. data and observations from all group experiments.
b. evidence showing there is a problem with contamination
c. qualitative and quantitative documentation for all contaminants in the soil.
d. suggestions for effective and environmentally acceptable remediation.
3. Be sure you support your conclusions and recommendations with data from the various
aspects of the project.

Materials Available: Chemicals

Bucket of soil from the contaminated area of the farm; Bucket of soil from the adjacent
uncontaminated area of the farm
Radish seeds
Possible contaminants: NaCl, KCl, CaCl2, Ca(OH)2, Na2CO3, Na3PO4, NaH2PO4, K2HPO4,
For test solutions: concentrated HCl, H2SO4, HNO3; AgNO3, K2CrO4, phenolphthalein solution,
5% ascorbic acid, 0.12 M sodium molybdate in 12% acetic acid
Safety Information
You may encounter some or all of these materials during your experimentation for this project.
Hydrochloric, sulfuric, and nitric acids are corrosive and causes severe burns if concentrated.
Notify your instructor if any acid is spilled. Flush the affected area with running water for 15
minutes if you should spill any on your skin. Be sure to read the label carefully and use the
concentration called for.
When mixing acids and bases use extreme care mix drop wise with plenty of stirring. If the
solution gets hot, stop mixing for a while and let the solution cool.
When mixing concentrated acid and water, always add the acid to the water and not the other
way around. Gentle stirring while adding the acid is also recommended.
Potassium chromate is a strong oxidizing agent and a suspected carcinogen. Discard the solid
residue and chromate solutions in the designated disposal container.
Techniques You May Need
Dilution processes
Decolorizing procedures
Drying techniques for soil
Extracting soluble ions from soil
Measuring pH
Soil sample preparation
Small-scale chemistry techniques

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Project-Based Labs

Testing procedures for ions in soil

Titration
Use of a spectrophotometer
Use of volumetric glassware
Resource: Plant Growth
Plants require the presence of water and several different nutrients for proper growth. These
essential foodstuffs must also be found in the proper proportions for the healthy sustainability of
the plant. You may want to consider cultivating radishes, or other fast-growing plants, and
monitor their growth in your soil samples. This will provide one way to see if there is a problem
with soil contamination.
Resource: Strategies for Drying Soil Samples
Soils sampled from the field contain water in varying amounts depending on soil properties
and the preceding weather conditions. Even when the soil is air-dried, some water remains.
Before further testing, soil samples are usually dried at about 105 C and their water content
determined. Results of soil analyses are normally expressed in the literature relative to a mass of
oven-dry soil, making comparisons among analyses possible. The samples used for
determining water content can be placed in flat glass dishes and dried in a drying oven.
Alternatively the samples in their dishes can be place on a hot plate set fairly low for several
hours. The test is complete when a constant weight is achieved for each sample. If you decide
achieving constant weight is essential, be patient because this might take time!
When an oven-dry soil is heated to 500C, organic matter is burned off and there is further
loss of water. The mass lost between 105C and 500C is called the loss on ignition. If you
decide to use these tests, you will want to use about 10 g of the soil in a porcelain crucible with a
loosely fitting lid. The samples are heated to red heat in the hottest part of a Bunsen burner flame
until a constant weigh is achieved.
Resource: Suggested Strategy for Qualitative Analysis of Soil Samples.
For the qualitative analysis of the soil samples, you will want to test for the presence of
various anions. Anions will often complex with various reagents and then precipitate out of
solution. Thus, the presence of a precipitate for an anion test will indicate the presence of that
particular anion. These ion tests should be done with the soil in solution. A small amount on the
end of a spatula of the soil sample mixed with approximately 1ml of water in a test tube will be
sufficient for the tests. Alternatively, use small-scale techniques including a 24-cell well plate
and Beral-type pipets to perform the tests.
Resource: A Strategy for Testing the pH of Soil Samples
The extent of a soils acidity or basicity can be determined via a pH reading. These pH
values can be altered by some contaminants. Make a solution of your soil using about 10 g of
the soil sample mixed with 20 mL of water. In this part of the experiment, you will want to use a
pH meter. Remember to calibrate the probe before collection of values. Ask your teacher for
more information about the care and proper use of pH meters.

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Resource: A Method to Determine Buffer Capacity

A buffer helps resist change in pH. Some contaminants can affect the way a soil solution
responds to the addition of acid. To test the buffer capacities of your soil samples, make a
solution of your soil with KCl (0.1M) as the solvent. To make the solution, combine 5 g of your
soil sample with 10 mL of the KCl solution. Consider why KCl is better than H2O for this
purpose. Set up several runs with varying amounts of added HCl (0.1M). Allow the mixtures to
react for approximately 2 hours, stirring occasionally. Record pH values and plot the buffer
curve. How could you regraph the data and obtain a linear relationship in order to compare
slopes?
Resource: Strategy for Decolorizing Solutions
If soil samples are extracted with aqueous solvents, a darkly colored solution is usually
obtained. Since most acid-base indicators and many spot tests depend on color or color change,
this can cause problems in interpreting experimental results. There are two simple approaches to
dealing with this problem. The first is to remove the organic substances responsible for the color
by absorbing them on activated charcoal. Another alternative is to heat the soil sample at red heat
for 30-60 minutes to burn off all the organic materials.
Resource: Carbonate Analysis
To quantitatively determine the amount of carbonate in your soil samples, mix 10 g of soil
with 20 mL of 2 M HCl and allow the mixture to react for approximately 15 minutes. What do
you observe happening in the flask? Heat the solution on a hot plate and allow the mixture to
react for approximately another 15 minutes. Filter with a Hirsch funnel and then transfer the
filtrate to a 100 mL volumetric flask and fill to mark. Use a sample of this soil solution with a
few drops of phenolphthalein indicator and titrate with 0.1 M NaOH.
Resource: Chloride Analysis
A microscale approach is less accurate, but much faster and less expensive than a standard
titration. Obtaining good results requires counting uniform drops very accurately. Add exactly
25 drops of unknown chloride solution to each of three wells. Then add 5 drops of 0.5 M
NaHCO3 and 2 drops of 5% KCrO 4 indicator. Titrate the individual sample with 0.050 M AgNO3
solution by adding the AgNO 3 solution drop by drop with stirring after the addition of each drop.
The stirring is essential to redissolve the transient red-orange precipitate, which has a tendency to
clump if not stirred. The titration is complete when the red-orange precipitate no longer
disappears when the mixture is stirred. The sample typically will require at least 20 drops of
AgNO3 solution. If less is required, adjust the amount of unknown chloride.
You will need only about 1 mL of 5% potassium chromate for each titration. Prepare only
what you think you will need. Caution: Potassium chromate is a strong oxidizing agent and a
suspected carcinogen. Discard the solid residue and chromate solutions in the designated
disposal container.
Resource: Phosphate Analysis
This analysis procedure is the most complicated one of those used in this project. All
solutions must be carefully prepared using distilled or deionized water. You must keep track of
all dilutions and make all volume measurements and dilution using volumetric glassware such as
volumetric flasks, pipets and burets. Sample selection must be made carefully.

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Contaminated Soil: Planning Sheet 1
To be completed before starting experimentation.

Project-Based Labs
Group Name

State the overall purposes of this project in your own words.

1. What possible compounds could the jackknifed truck have been carrying? Recall that the
manufacturer produced inorganic fertilizers, ice melting compounds for roads, inorganic
industrial cleaners, and additives for making cement. Give references for any resource used
to answer this question.

2. There are no longer any visible remains of the spill on the surface of the farmers field. What
information does that give you about the chemical nature of the contaminants? Explain.

3. It is not possible to analyze all of the contaminated soil in your bucket. How will you take a
representative sample of the contaminated soil? Will the same strategy work to obtain a
representative sample of the uncontaminated soil? Why or why not?

4. Soil analysis usually begins with drying the soil. Why do you think this step is necessary?

5. Soil normally contains most of the ions found in the possible contaminants spilled on the
farmers field. How will you plan to determine which ions are the contaminants and which
ions are part of the natural soil of the field?

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6. Which contaminants could change the pH of the soil? Explain your reasoning.

7. If soil samples are extracted with aqueous solvents, a darkly colored solution is usually
obtained. This color will interfere with ion identification. How do you plan to deal with this
problem?

8. Briefly outline how you plan to determine the pH of the soil. Include a list of reagents and
equipment you will need.

9. What procedures do you plant to use to separate and identify the soluble components from
the soil?

10. If you plan to test the viability of the seeds in the soil samples, the end of the first laboratory
period is a good time to plant the radish seeds. How will you set up this part of your
experimental tests? You will need to be able to follow this experiment for 2-3 weeks.

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Contaminated Soil: Reflection and Planning Sheet 2
To be completed after the first laboratory period.

Project-Based Labs
Group Name__________________

State the purposes of this weeks lab in your own words.

1. What procedures were used to obtain a representative sample of contaminated soil? Of

uncontaminated soil?

2. What procedures were used to determine the pH of the soil samples? Was the pH of the
contaminated soil the same as that of the uncontaminated soil? Why or why not?

3. What procedures were used to extract soluble ions from the soil sample? Are there any
modifications to these procedures that you will implement in next weeks lab? Explain.

4. What procedures were used to decolorize the aqueous solution extracted from a soil sample?
Was the resulting solution colorless? Why or why not?

5. What ions have you found so far in the soil samples? What evidence supports your
identifications?

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6. During the next laboratory period, you will move from qualitative identification of ions to
quantitative determination. How will you determine the concentration of some of the ions in
the soil samples? Briefly outline the standard method your group has decided to use to
extract soluble ions from a soil sample and what analysis methods you plan to use. (Hint:
Consult the Resources sections in this experiment and the Techniques section elsewhere in
this Laboratory Supplement. You will likely want to analyze the soil sample for phosphate,
carbonate, and chloride ions.)

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Contaminated Soil: Reflection and Planning Sheet 3
To be completed after the second laboratory period.

Project-Based Labs
Group Name__________________

State the purposes of this weeks lab in your own words.

1. Outline and discuss the analytical procedures you used today to determine the concentration
of ions in the soil.

2. What is the purpose of adding NaHCO3 when analyzing for chloride ion? Explain.

3.

How did your group decide how much soil sample to use for your tests? Was this a
satisfactory size or were modifications made in the plan as you proceeded?

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4. Most analytical procedures are performed on at least three samples of the material to be
analyzed. What do you think is the reason for repeating a test several times? Was this part of
your plan or will you need to repeat some determinations?

5. Given that your team has identified the soil contaminants, what suggested remedies are you
prepared to test in next weeks lab period? Consider not only the chemical effectiveness of
your suggested remedy, but possible environmental impacts. The farmer will definitely not
appreciate exchanging one problem for another! Briefly outline your plans.

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Project-Based Labs

Contaminated Soil: Reflection and Summary Sheet 4

To be completed after the third laboratory period.

Group Name___________________

State the purposes of this weeks lab in your own words.

1. What procedures were carried out to test your teams suggested remedies? Were they both
successful and environmentally safe? Explain.

2. After discussion of all team results, decide how to tabulate and interpret your experimental
results. Prepare the table and write a bulleted outline of the important points to be made in
your report to the farmer.

(over)

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3. Write a summary statement for the farmer. Be sure you communicate how you confirmed
there was indeed a problem, how you identified the contaminants both qualitatively and
quantitatively, and what suggestions you have for remediation.

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