Teacher Notes

Gravimetric Analysis of Calcium and Hard Water

Inquiry Lab Kit for AP® Chemistry

Materials Included In Kit

Antacid tablets, bottle of 20
Calcium chloride, anhydrous, CaCl2, 30 g
Calcium chloride solution, CaCl2, 2 M, 500 mL
Sodium carbonate, anhydrous, Na2CO3, 30 g
Sodium carbonate solution, Na2CO3, 0.5 M, 1000 mL

Additional Materials Required

Water, deionized or distilled, 40 mL*
Water, deionized or distilled, 600 mL†
Balance, 0.001-g precision (shared)*
Beakers, 150-mL, 3*
Beakers or bottles to store water samples, 6†
Drying oven (shared)*
Filter flasks, 250-mL, 2*‡
Filter paper, 3 (to fit funnels)*
Funnel, Büchner and rubber adapter*
Glass tubing, 2*‡
Graduated cylinder, 25- or 50-mL†
Graduated cylinder, 50-mL*
Latex rubber tubing*‡
Pinch clamp*‡
Rubber stopper, 2-hole*‡
Rubber tubing*‡
Spatula*‡
Support stand and ring clamps*‡
Vacuum pump or aspirator*‡
Vacuum tubing, 2*‡
Volumetric flask or graduated cylinder, 100-mL†
Wash bottle*
Watch glasses, 2*
Weighing dishes, 2*
*for each lab group
Vacuum filtration apparatus setup*
for Prelab Preparation

Prelab Preparation

Prepare 100 mL each of six different “unknown” hard water samples for students to analyze in the guided-inquiry activity. See the calculations for the amount of 2 M CaCl2 stock solution to be diluted to prepare 100 mL of each sample.

{13766_Preparation_Table_3}
  1. Using the 2 M calcium chloride stock solution provided in the kit, measure out V1 using a graduated cylinder or volumetric pipet.
  2. Add to a 100-mL volumetric flask or graduated cylinder and fill each to equal 100 mL with deionized or distilled water.
  3. Mix well and store each solution in a labeled beaker or bottle.

Safety Precautions

Sodium carbonate is irritating to body tissues. Calcium chloride is moderately toxic by ingestion and the anhydrous generates a great deal of heat when dissolved in water. Avoid contact of all chemicals with eyes and skin. Antacid tablets used in the lab are considered laboratory chemicals and may not be removed from the lab. Do not taste or ingest any materials in the chemistry lab. Wear chemical splash goggles, chemical-resistant gloves and a chemical-resistant apron. Remind students to wash their hands thoroughly with soap and water before leaving the laboratory. Please follow all laboratory safety guidelines. Please review current Safety Data Sheets for additional safety, handling and disposal information.

Disposal

Please consult your current Flinn Scientific Catalog/Reference Manual for general guidelines and specific procedures, and review all federal, state and local regulations that may apply, before proceeding. The leftover solid calcium chloride and sodium carbonate may be packaged for landfill disposal according to Flinn Suggested Disposal Method #26a. The leftover calcium chloride or sodium carbonate solutions may be rinsed down the drain with excess water according to Flinn Suggested Disposal Method #26b.

Lab Hints

  • This laboratory activity can be completed in two 50-minute class periods. It is important to allow time between the Introductory Activity and the Guided-Inquiry Activity for students to discuss and design the guided-inquiry procedures. Also, all student-designed procedures must be approved for safety before students are allowed to implement them in the lab. Prelab Questions may be completed before lab begins the first day.
  • Quantitative transfer techniques are essential for accurate results in this investigation. Students should practice pouring liquids, rinsing beakers or flasks and filtering mixtures. The type of glassware used will also affect the precision of the results.
  • If a vacuum filtration apparatus is not available, students may filter the precipitates by gravity filtration. For smaller amounts of precipitate, such as 0.10 M and 0.05 M samples of CaCl2 (samples 4 and 5), it is best to filter by gravity in order to prevent loss of product.
  • If some of the solid CaCO3 precipitate goes through the filter paper, students should stop the filtration, pour the filtrate back into the beaker, and use two filter papers to filter a second time.
  • Quantitative filter paper is needed for this lab. We recommend Extra-Fine Quantitative Filter Paper (11 cm) from Flinn Scientific, Catalog No. AP7628, if it fits the funnel being used.
  • Experimental errors can result if the students do not dissolve the reactants completely in distilled water before mixing. Some of the solid filtered out may be the undissolved reactant(s). Tap water should not be used because the impurities in it, such as calcium and magnesium ions in hard water, can also precipitate out and interfere with the desired results. The filter paper and precipitate must be completely dried and any water of hydration must be removed by the drying process. Usually, the most accurate method to ensure complete dehydration is by heating until a constant mass is achieved.

Teacher Tips

  • Students may calculate mass and mass percent of Ca2+ in the hard water samples collected.

  • Students may choose to bring their own samples of over-the-counter calcium tablets for analysis. Results may be compared with the manufacturer’s label.
  • Students can compare results obtained via EDTA titration versus gravimetric analysis for hard water determination. In the Water Softening—Guided-Inquiry Kit, available from Flinn Scientific, Catalog No. AP7352, students treat water samples of unknown hardness with ion-exchange resin and analyze by EDTA titration. The guided-inquiry format allows students to identify the minerals that are removed through ion exchange and understand the practical benefits of water softening.
  • If there is a swimming pool in the school, talk with the swimming pool supervisor about having the chemistry students perform the water hardness test on the pool water. The recommended water hardness level for swimming pools and spas is 200–300 ppm. Compare the results obtained in the lab with those obtained poolside using typical “dip and read” test papers or methods. Also, schedule an in-house field trip to the pool to learn about the routine tests used to monitor pool chemistry and water quality: chlorine, pH, alkalinity, total dissolved solids, cyanuric acid, copper and iron.
  • The three principal ions that contribute to water hardness are calcium, magnesium and iron. While there are no national, state or local standards for calcium and magnesium in drinking water, the EPA recommends a limit of 0.3 mg/L for the concentration of iron in drinking water. This is a recommended value and is not legally enforceable.
  • Set up a collaborative classroom research project. Using the Internet, look up typical surface water, groundwater, or municipal water hardness levels in major cities or geographic areas for every state. Plot the data on a large map of the United States using a color-coded system for the USGS water hardness categories (see the Background section). Analyze the resulting national map in terms of geographic features and properties. Although about 85% of the country has hard water, there are wide variations depending on geography. New England and the Pacific Northwest generally have soft water, while very hard water (≥1000 ppm) is common in many areas of the Southwest such as Texas, New Mexico, Arizona and Utah.

Further Extensions

Alignment to the Curriculum Framework for AP® Chemistry

Enduring Understandings and Essential Knowledge

Atoms are conserved in physical and chemical processes. (1E)

1E2: Conservation of atoms makes it possible to compute the masses of substances involved in physical and chemical processes. Chemical processes result in the formation of new substances, and the amount of these depends on the number and the types and masses of elements in the reactants, as well as the efficiency of the transformation.

Matter can be described by its physical properties. The physical properties of a substance generally depend on the spacing between the particles (atoms, molecules, ions) that make up the substance and forces of attraction among them. (2A)

2A3: Solutions are homogenous mixtures in which the physical properties are dependent on the concentration of the solute and the strengths of all interactions among the particles of the solutes and solvent.

Chemical changes are represented by a balanced chemical equation that identifies the ratios with which reactants react and products form. (3A)

3A1: A chemical change may be represented by a molecular, ionic, or net ionic equation.

3A2: Quantitative information can be derived from stoichiometric calculations that utilize the mole ratios from the balanced chemical equations. The role of stoichiometry in real-world applications is important to note, so that it does not seem to be simply an exercise done only by chemists.

Learning Objectives

1.19 The student can design, and/or interpret data from, an experiment that uses gravimetric analysis to determine the concentration of an analyte in a solution.

2.10 The student can design and/or interpret the results of a separation experiment (filtration, paper chromatography, column chromatography, or distillation) in terms of the relative strength of interactions among and between the components.

3.2 The student can translate an observed chemical change into a balanced chemical equation and justify the choice of equation type (molecular, ionic, or net ionic) in terms of utility for the given circumstances.

3.3 The student is able to use stoichiometric calculations to predict the results of performing a reaction in the laboratory and/or to analyze deviations from the expected results.

Science Practices

1.5 The student can re-express key elements of natural phenomena across multiple representations in the domain.

2.2 The student can apply mathematical routines to quantities that describe natural phenomena.

4.2 The student can design a plan for collecting data to answer a particular scientific question.

5.1 The student can analyze data to identify patterns or relationships.

5.3 The student can evaluate the evidence provided by data sets in relation to a particular scientific question.

6.2 The student can construct explanations of phenomena based on evidence produced through scientific practices.

6.4 The student can make claims and predictions about natural phenomena based on scientific theories and models.

7.1 The student can connect phenomena and models across spatial and temporal scales.

7.2 The student can connect concepts in and across domain(s) to generalize or extrapolate in and/or across enduring understanding and/or big ideas.

Answers to Prelab Questions

  1. Define the term gravimetric analysis. Describe the procedure used in this activity, and identify two other common examples of gravimetric analysis.

    Gravimetric analysis is used to determine the amount of a substance in a sample by measuring the mass of a solid product or precipitate obtained by reaction of the substance with a precipitating agent. In this investigation, calcium is determined by precipitation of calcium carbonate upon addition of sodium carbonate to a solution of the sample. Other common gravimetric analysis procedures include the determination of sulfate ions by precipitation of barium sulfate and the determination of silver ions by precipitation of silver chloride.

  2. Write the balanced chemical equation for the reaction between calcium chloride and sodium carbonate.

    CaCl2(aq) + Na2CO3(aq) → CaCO3(s) + 2NaCl(aq)

  3. Calculate the number of moles of each reactant in the Introductory Activity (see steps 1 and 2). Identify the limiting reactant in the reaction and determine the theoretical amount of CaCO3 that should be produced.

    2.0 g CaCl2/110.98 g/mole = 0.0180 moles of CaCl2
    2.5 g Na2CO3/105.9 g/mole = 0.0237 moles of Na2CO3
    The limiting reactant is calcium chloride. Sodium carbonate is present in approximately 31% excess relative to the amount needed based on the stoichiometric mole ratio.
    [(0.0237 moles – 0.0180 moles)/0.0180 moles] x 100% = 32%
    The molar mass of CaCO3 is 100.1 g/mole, and the theoretical yield of calcium carbonate is
    0.0180 moles x 100.09 g/mole = 1.80 g.

  4. As noted in the Background section, hardness levels are calculated by assuming that all the “hard” metal ions come from dissolved calcium carbonate and are reported in mg CaCO3/L. Calculate the equivalent water hardness in mg CaCO3/L for a calcium chloride solution containing 0.1 M Ca2+ ions.

    The number of moles of calcium ions is obtained by multiplying the solution molarity by the volume. Since water hardness is expressed in terms of equivalent weight of calcium carbonate per liter of water, it is convenient to start with the moles per liter of calcium ion, or 0.1 moles.
    (0.1 moles CaCl2/liter of solution) x 1 L = 0.1 moles Ca2+
    Multiply the moles of calcium by the molar mass of calcium carbonate to determine the equivalent mass of calcium carbonate. Convert the result to mg/L.
    (0.1 moles/L) x (100.09 g/mole) x (1000 mg/g) = 10,000 mg/L of CaCO3

Sample Data

Sample Data for Introductory Activity

Mass of calcium carbonate obtained = 1.774 g
Percent yield = (1.774 g/1.80 g) x 100% = 98.6%

Sample Data and Results for Gravimetric Analysis to Determine Water Hardness

{13766_Data_Table_4}

aPercent yield calculated based on the known molarity of CaCl2 provided to the students.
bWater hardness is calculated in units of mg/L of calcium carbonate based on the assumption that the water samples analyzed by the students actually represented a 100-fold concentration of the original water sample. Thus, for sample 5, which gave 0.072 g of CaCO3 from a 20-mL solution, the calculated water hardness is:

{13766_Data_Equation_2}

where the factor 1/100 accounts for the fact that the sample analyzed was 100 times more concentrated than the original water sample.

Conclusion
The gravimetric analysis procedure is not accurate for “soft” water samples containing < 100 mg/L.

Sample Procedure for Analyzing Antacid Tablets

Antacid tablets are provided in this advanced inquiry kit as an optional guided-inquiry extension. Antacid tablets should be ground using a mortar and pestle. Collect the pulverized solid and measure the mass. In a 100-mL beaker, dissolve the solid with 20 mL of 3 M hydrochloric acid and 20 mL of deionized or distilled water. Stir the mixture for 5–6 minutes on a stir plate or using a stirring rod. Heating gently, on a low heat setting, is optional to aid in dissolving of the solid. After stirring, filter the binder and other insoluble material. To the resulting filtrate, slowly add about 60 mL of 1 M sodium carbonate solution. During this step, the filtrate will bubble and a white solid, calcium carbonate, precipitates. Isolate the precipitate by gravity or vacuum filtration. Allow to dry and mass.

Sample Data for Analyzing Antacid Tablets

Mass of calcium carbonate: 0.541 g
According to the manufacturer’s label, the antacid tablet kit contains 500–675 mg of calcium carbonate.

Answers to Questions

Guided-Inquiry Discussion Questions

  1. The ideal precipitate in a gravimetric analysis procedure should be insoluble and have a known composition. Using reference texts such as The Merck Index or the Handbook of Chemistry and Physics, look up the properties of calcium carbonate and discuss its advantages and possible disadvantages for gravimetric analysis of calcium.

    Calcium carbonate is considered virtually insoluble in water and is thus an ideal candidate for the gravimetric determination of calcium ions. (The Handbook of Chemistry and Physics lists the solubility as 0.0014 g in 100 mL of cold water and 0.0019 g in 100 mL of hot water.) It has a stable composition, but also exists as a potential hexahydrate. This could complicate the percent yield determination if the solid is not thoroughly dried to remove waters of hydration. The anhydrous solid is easily obtained by heating to approximately 100 °C. Another potential disadvantage of calcium carbonate is that heating at elevated temperatures (> 800 °C) may cause decomposition to give calcium oxide and carbon dioxide. As long as the solid is dried in an oven, and not in a burner flame, to drive off residual water, decomposition of the product is not likely to affect the results.

  2. Based on solubility rules, what ions in water might interfere with the analysis of calcium ions by precipitation of calcium carbonate?

    Other carbonate salts that are insoluble in water and might interfere with gravimetric determination of calcium include the alkaline earth metal cations Mg2+, Sr2+ and Ba2+ as well as Fe3+ and other transition metal cations, such as Cu2+ and Ag+. Of these cations, only Mg2+ and Fe3+ are likely to be present in water.

  3. Precipitate particles in gravimetric analysis must be large enough to be collected by filtration—smaller particles may pass through or clog the filter. Discuss how the following techniques will help prevent product loss and ensure product purity in a gravimetric procedure.
    • Add the precipitant slowly with vigorous mixing.
    • “Digest” the precipitate by allowing it to stand in contact with the solution and/or heating the mixture for 10−15 minutes.
    • Rinse the precipitate with a small amount of water after filtration.

    The precipitating agent (sodium carbonate in this example) should be added slowly to ensure even mixing and avoid local areas of supersaturation, which would lead to small particles or even a colloidal solution. Digesting the precipitate allows time for the particles to coagulate into larger particles. Heating and then cooling the mixture essentially promotes recrystallization of the solid, which leads to larger crystal or particle growth and also helps remove impurities that might be adsorbed on the surface. Finally, rinsing or washing the precipitate with water also helps remove impurities.

  4. Calculate the number of moles of Ca2+ ion in 20 mL of each solution and the theoretical amount of CaCO3 that can be obtained by reacting 20 mL of each solution with excess sodium carbonate. Enter the results in the table.

    Sample Calculation (Sample 1):
    0.400 moles/L x 0.020 L = 0.008 moles Ca2+
    0.008 moles Ca2+ x 100.09 g/mole CaCO3 = 0.801 g (theoretical yield)
    See the table for the results of all calculations.

  5. Excess sodium carbonate solution (precipitant) is recommended to ensure that all of the calcium ions in solution are converted to product. For each sample, determine the volume of 0.5 M sodium carbonate solution providing the stoichiometric number of moles of Na2CO3 to react completely with 20 mL of the CaCl2 solution. Multiply the result by 1.2 to provide a 20% excess, and enter the results in the table.

    Sample Calculation (Sample 1):

    {13766_Answers_Equation_3}

    See the table for the results of all calculations.

  6. Calculate the theoretical water hardness in mg CaCO3/L for each water sample. Recall that each sample has been concentrated by a factor of 100 to provide the solution shown in column 2. The calculation for sample 1 is shown below as a guide.

    Sample Calculation (Sample 1): (0.801 g CaCO3/0.020 L) x (1000 mg/g) x (1/100) = 400 mg CaCO3/L
    Note that the factor 1/100 accounts for the concentration of the original water sample to the final analyzed volume of 20 mL.
    See the table for the results of all calculations.

    {13766_Answers_Table_5}

Review Questions for AP® Chemistry 

  1. Calculate the number of moles of (a) copper(II) chloride and (b) aluminum that reacted.
    {13766_Answers_Equation_4}
    {13766_Answers_Equation_5}
  2. What is the mole ratio of copper(II) chloride to aluminum metal? Express this to the nearest whole number ratio.
    {13766_Answers_Equation_6}

    The nearest whole number ratio of CuCl2 to Al is 3:2.

  3. What happened to the aluminum metal that was consumed in this reaction? Write the formula of the most probable aluminum-containing product.

    The aluminum metal dissolved and was converted to aluminum (Al3+) ions upon reaction with Cu2+ ions. The most probable aluminum-containing product is AlCl3.

  4. Write a balanced chemical equation for the single replacement reaction of copper(II) chloride with aluminum.

    3CuCl2(aq) + 2Al(s) → 3Cu(s) + 2AlCl3(aq)

References

AP® Chemistry Guided-Inquiry Experiments: Applying the Science Practices; The College Board: New York, NY, 2013.

Harris, D.C. Exploring Chemical Analysis, 3rd ed.; W. H. Freeman and Company: New York, 2005.

Student Pages

Gravimetric Analysis of Calcium and Hard Water

Introduction

In certain areas of the country, the presence of hard water poses significant problems in water supply systems. Various water softening techniques are used to remove the cations responsible for water hardness. This investigation involves the application of gravimetric analysis to test samples for the amount of water hardness and calcium ions.

Concepts

  • Water hardness

  • Double replacement reactions
  • Gravimetric analysis
  • Stoichiometry

Background

Water from natural sources may contain a number of dissolved substances. The amount and nature of these dissolved substances varies depending on the geography of the area and the journey the water has taken. As water travels through the ground or over the surface of the land, it can dissolve naturally occurring minerals. As minerals dissolve in the water, the compounds separate into their respective cations and anions. Common cations in water include Na+, Ca2+, Mg2+ and Fe3+ while the principal anions in water are Cl, HCO3, NO3 and SO42–. The main ions contributing to water hardness are Ca2+, Mg2+ and, to a lesser extent, Fe3+. Their presence makes it difficult for soaps to lather and also causes a “scum” to form. Equation 1 (where R is a long hydrocarbon chain) shows the precipitation reaction between alkyl sulfate anions in a typical soap with calcium ions in hard water. The main problem due to water hardness in industrial pipes or boilers is the buildup of solid CaCO3, which precipitates out and causes thick deposits to form in pipes and other appliances.

{13766_Background_Equation_1}
There are many different ways to “soften” water. One of the most common ways to remove ions is by ion exchange. The ion exchange process uses a resin to replace some of the ions that cause hardness with ions that do not. Hardness is commonly measured in units of grains per gallon or milligrams per liter (also known as parts per million), and is classified by the U.S. Department of the Interior and the Water Quality Association as follows in Table 1:
{13766_Background_Table_1}
Although several ions contribute to water hardness, the units of mg/L or ppm are defined in terms of the equivalent mass (milligrams) of CaCO3 that would be present per liter of water. In this investigation, gravimetric analysis will be used to precipitate and isolate solid CaCO3 from water samples and determine water hardness. Many municipal water treatment plants use soda ash (sodium carbonate, Na2CO3) and lime (calcium hydroxide, Ca(OH)2) to chemically remove calcium and magnesium ions, respectively, from hard water.

Experiment Overview

The purpose of this advanced inquiry lab is to investigate the suitability of gravimetric analysis for determining the amount of water hardness in the form of calcium carbonate, CaCO3, in various water samples. Six samples, representing a wide range of potential water hardness, from 50 ppm to 500 ppm, will be analyzed by various student groups as part of a cooperative class investigation to determine the accuracy and sensitivity of gravimetric analysis for water hardness testing. Note that all water samples have been concentrated by a factor of 100 for the purpose of quantitative analysis. The lab begins with an introductory activity to develop skill in the calculations and techniques of gravimetric analysis, in particular, quantitative transfer and vacuum or gravity filtration. The precipitation reaction involves preparing and combining solutions of Na2CO3 and CaCl2. The balanced chemical equation for this reaction predicts the amount of precipitate that will be formed. Careful isolation, drying and weighing of the precipitate will confirm the calculations and the percent yield. The procedure provides a model for guided-inquiry design of the cooperative class investigation described above. Antacid tablets are also provided as an opportunity for further inquiry—the use of gravimetric analysis to determine the amount of calcium in an over-the-counter medication.

Materials

Antacid tablets (optional)
Calcium chloride, anhydrous, CaCl2, 2 g
Sodium carbonate, anhydrous, Na2CO3, 2 g
Sodium carbonate solution, Na2CO3, 0.5 M
Water, deionized or distilled
Balance, 0.001-g precision (shared)
Beakers, 150-mL, 3
Drying oven (shared)
Filter flask, 250-mL
Filter paper, 3
Funnel, Büchner and rubber adapter
Graduated cylinder, 50-mL
Hard water samples, 20 mL, 2
Spatula
Vacuum filtration apparatus setup
Wash bottle
Watch glasses, 2
Weighing dishes, 2

Prelab Questions

  1. Define the term gravimetric analysis. Describe the procedure used in this activity, and identify two other common examples of gravimetric analysis.
  2. Write the balanced chemical equation for the reaction between calcium chloride and sodium carbonate.
  3. Calculate the number of moles of each reactant in the Introductory Activity (see steps 1 and 2). Identify the limiting reactant in the reaction and determine the theoretical amount of CaCO3 that should be produced.
  4. As noted in the Background section, hardness levels are calculated by assuming that all the “hard” metal ions come from dissolved calcium carbonate and are reported in mg CaCO3/L. Calculate the equivalent water hardness in mg CaCO3/L for a calcium chloride solution containing 0.1 M Ca2+ ions.

Safety Precautions

Sodium carbonate is irritating to body tissues. Anhydrous calcium chloride is moderately toxic by ingestion and generates a great deal of heat when dissolved in water. Avoid contact of all chemicals with eyes and skin. Antacid tablets used in the lab are considered laboratory chemicals and may not be removed from the lab. Do not taste or ingest any materials in the chemistry lab. Wear chemical splash goggles, chemical-resistant gloves and a chemical-resistant apron. Wash hands thoroughly with soap and water before leaving the laboratory. Please follow all laboratory safety guidelines.

Procedure

Introductory Activity

Precipitation Reaction and Vacuum Filtration

  1. Weigh 2.5 g of sodium carbonate and place in a clean, dry 150-mL beaker. Record the precise mass and dissolve the solid in 20 mL of deionized or distilled water.
  2. Weigh 2.0 g of calcium chloride and place in a clean, dry 150-mL beaker. Record the precise mass and dissolve the solid in 20 mL of deionized or distilled water.
  3. Combine the two solutions by slowly adding the sodium carbonate solution to the calcium chloride solution. Record all observations about the reaction.
  4. Separately weigh a piece of filter paper and a watch glass and record their masses.
  5. Set up a vacuum filtration apparatus as shown in Figure 1. The second filter flask is used to prevent back-up of water from the aspirator to the filter flask when the vacuum is released.
    {13766_Procedure_Figure_1_How to set up a vacuum filtration}

    For help in setting up a vacuum filtration and tips for carrying out the procedure, please see the following How-To Videos on the Flinn Scientific website under Teacher Resources: “How to Set Up a Vacuum Filtration” and “How to Perform a Vacuum Filtration” (at www.flinnsci.com).

  6. Isolate the precipitate by vacuum filtration. Careful transfer techniques are essential for accurate results! Precipitate may also be collected by gravity filtration.
  7. Place the watch glass and filter paper containing precipitate in a lab oven to dry at 100 °C for 10–20 minutes. Monitor and carefully break up the solid with a spatula to ensure complete drying.
  8. Calculate the percent yield of calcium carbonate.

Guided-Inquiry Design and Procedure

Accuracy and Sensitivity of Gravimetric Analysis to Determine Water Hardness

Form a working group with other students and discuss the following questions.

  1. The ideal precipitate in a gravimetric analysis procedure should be insoluble and have a known composition. Using reference texts such as The Merck Index or the Handbook of Chemistry and Physics, look up the properties of calcium carbonate and discuss its advantages and possible disadvantages for gravimetric analysis of calcium.
  2. Based on solubility rules, what ions in water might interfere with the analysis of calcium ions by precipitation of calcium carbonate?
  3. Precipitate particles in gravimetric analysis must be large enough to be collected by filtration—smaller particles may pass through or clog the filter. Discuss how the following techniques will help prevent product loss and ensure product purity in a gravimetric procedure.
    • Add the precipitant slowly with vigorous mixing.
    • “Digest” the precipitate by allowing it to stand in contact with the solution and/or heating the mixture for 10−15 minutes.
    • Rinse the precipitate with a small amount of water after filtration.

    Six water samples containing known concentrations of calcium chloride are available for analysis as part of a cooperative class activity. Each student group should analyze two different samples. The recommended sample volume for the precipitation reaction is 20 mL. Complete the following table with the results of the calculations from Questions 4−6.

    {13766_Procedure_Table_2}
  4. Calculate the number of moles of Ca2+ ion in 20 mL of each solution and the theoretical amount of CaCO3 that can be obtained by reacting 20 mL of each solution with excess sodium carbonate. Enter the results in the table.
  5. Excess sodium carbonate solution (precipitant) is recommended to ensure that all of the calcium ions in solution are converted to product. For each sample, determine the volume of 0.5 M sodium carbonate solution that provides the stoichiometric number of moles of Na2CO3 needed to react completely with the CaCl2 solution. Multiply the result by 1.2 to provide a 20% excess, and enter the results in the table.
  6. Calculate the theoretical water hardness in mg CaCO3/L for each water sample. Recall that each sample has been concentrated by a factor of 100 to provide the solution shown in column 2. The calculation for sample 1 is shown as a guide. Sample Calculation (Sample 1): (0.801 g CaCO3/0.020 L) x (1000 mg/g) x (1/100) = 400 mg CaCO3/L Note that the factor 1/100 accounts for the concentration of the original water sample to the final analyzed volume of 20 mL.
  7. Write a detailed, step-by-step procedure for analyzing the concentration of calcium in the water samples. Include the reagents needed, the glassware and equipment that will be used, and the appropriate measurements and observations that must be made.
  8. Review the hazards of the chemicals used in the procedure and write appropriate safety precautions that must be followed during the experiment.
  9. Carry out the procedure and record the results in an appropriate data table.
  10. Repeat the analysis as needed to check for reproducibility.

Analyze the Results

Calculate the percent yield of calcium carbonate and determine the experimental water hardness in mg/L for each sample. Classify the water hardness of each sample according to the criteria established by the U.S. Department of the Interior and the Water Quality Association (see the Background section). Compile the class data for all the samples that were analyzed and compare the accuracy and sensitivity of the gravimetric analysis procedure over the range of possible water hardness from 50 to 500 mg/L.

Opportunities for Inquiry

Gravimetric Analysis to Determine the Mass of Calcium Ion in an Antacid Tablet


The amount of calcium in an antacid tablet may also be determined using gravimetric analysis. Note that antacid tablets contain binders and other inert ingredients or additives. Design a procedure to dissolve and separate the calcium carbonate from the binders in the tablet and analyze the amount of calcium.

Student Worksheet PDF

13766_Student1.pdf

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