CHE 117L

Spring 2009

Determination of Water Hardness

Introduction Approximately 75% of our planet's surface is covered with water. Most of that water is found in the ocean and various seas and is undrinkable because of its salt content. Ocean water contains on average 35 ppt (parts per thousand) NaCl. This means that for every thousand grams (about one liter) of seawater 35 grams of NaCl are present. There are many inland lakes on earth that do not have outlets and are found to be even saltier than the ocean. The Great Salt Lake in Utah is an example, with a salt concentration eight times that of the ocean (280 ppt); it can be better thought of as 28 % salt! Of all the water found on earth, 97% of it is in the ocean, 2% is found locked in the polar ice caps, and less than 1% is available as fresh water for drinking, bathing, and brushing your teeth. This fresh water is found in rivers, lakes, streams, and underground aquifers and contains very little salt content, but can contain relatively high concentrations of other ions such as calcium and magnesium. If water has a high content of these two ions it is termed "hard water". Historically the hardness of water was a measure of its capacity to precipitate soap. We will talk about the interaction between water and soap in an upcoming lab, but for now it is safe to say that when you see the soap scum in your bathtub you are looking at the chemical interaction between soap molecules and these ions found in the water. In this experiment you will be analyzing the water samples that you brought back from spring break. We will be measuring the total combined concentration of calcium and magnesium ions, known as "total water hardness." We will use a titration method of analysis that is based on the chemical reaction between calcium and magnesium ions and another ion called disodiumethylenediaminetetraacetate or simply called (Na2EDTA or just EDTA). The chemical reaction involves a one-to-one interaction between a calcium (or magnesium) ion and an Na2EDTA: Ca+2 + Na2EDTA -----> Ca(EDTA) + 2Na+

In this titration, a specific volume of the unknown water sample is carefully measured out and an EDTA solution of known concentration (called the titrant) is added dropwise from the buret until just enough EDTA has been added to react with all of the calcium and magnesium ions in solution. To find this specific point we need to add an indicator to our solution. Eriochrome Black T is a large dye molecule that, when in an alkaline (basic) solution will also bind with these ions and produce a red color. As the EDTA is slowly added to the solution it will "grab" the calcium and magnesium ions away from the Eriochrome Black T dye molecules and form a more stable complex. When the dye is alone in solution and not complexed with either a calcium or magnesium ion it produces a blue color as is represented in the below chemical equation. (Ca-Dye) + EDTA-2 ------> CaEDTA + (red) Dye -2 (blue)

The strategy in this experiment is to first use the EDTA solution to titrate a solution of MgCl 2 of known concentration to test your experimental procedure and to be sure your calculations are

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Spring 2009

correct. Once you are satisfied with your technique you will begin titrating your unknown sample of water to examine for water hardness and compare it to the table provided. For simplicity, the amounts of calcium and magnesium ions that are present in the unknown sample of water will be lumped together. It is a common practice in reporting water hardness to report the results in milligrams of CaCO3 per liter of water. This does not indicate that there is solid calcium carbonate present but that, if given a chance, that amount of solid could form from the ions in the water sample. The hardness of each water sample can be classified using the following table where total hardness is represented as a sum of all the calcium and magnesium ions in solution. Description Very Hard Hard Moderately Hard Soft Concentration Over 300 mg/L of calcium carbonate 150 to 300 mg/L of calcium carbonate 50 to 150 mg/L of calcium carbonate 0 to 50 mg/L of calcium carbonate

CHE 117L PROCEDURE A. TITRATION OF A KNOWN SOLUTION OF MgCl2 1. Rinse your 50 mL buret with a small amount of EDTA solution.

Spring 2009

2. Fill the buret with the EDTA solution. Note in your lab book the correct concentration of the solution from the bottle and record the initial level of your solution in the buret to the nearest 0.01 mL. 3. Use a graduated cylinder to add EXACTLY 5.00 mL of the magnesium chloride solution to an Erlenmeyer flask. 4. Dilute this solution with 50 mL of DEIONIZED water. Do NOT use regular tap water. 5. Now add 5 mL of the buffer solution to bring the solution to a pH of 10. 6. Stir or swirl this solution gently while adding the Eriochrome Black T solution (3 to 5 drops) to get an easily visible color. 7. Carefully titrate this solution with the EDTA solution from the buret until the color of the sample changes from red to purple to blue. Remember to swirl the flask constantly to see a uniform color. 8. Near the endpoint add drop by drop from the buret. As soon as the color of the solution has changed to a uniform blue, stop the titration and record the final level of EDTA solution in the buret to the nearest 0.01 mL. 9. Repeat the above experiment so that each person has done two titrations of the known solution of magnesium chloride. 10. Find an average of the volume of EDTA for each trial to titrate 5.00 mL of magnesium chloride solution. 11. Use this average volume to calculate the experimental concentration of magnesium chloride. B. TITRATION OF AN UNKNOWN SOLUTION OF WATER 1. Measure and record the pH of your solution. 2. Use the same procedure above EXCEPT in step 3 use exactly 10.00 mL of your unknown water sample if it is fresh water OR 2.00 mL sample size if your unknown is salt water. Each person will do two titrations of the same unknown solution. 3. Find an average of the volume of EDTA for each trial that was used to titrate your unknown water sample. 4. Use this average volume to calculate the experimental concentration of calcium and magnesium ions in the unknown water solution.

CHE 117L Section________________________

Spring 2009 Name_____________________________________

PRE-LAB QUESTIONS. (10 pts) Answer on this page, before coming to lab. 1. Why is the ocean salty?

2. What is the mole ratio between magnesium ion and EDTA in this experiment?

3. Why shouldnt you use tap water to dilute your experimental solution?

CHE 117L Section________________________

Spring 2009 Name_____________________________________

Beginning questions & ideas: What do you want to know or already know? (4 pts)

Tests & Procedures: What did you do to answer your questions or prove your idea? (4 pts)

Observations: What did you observe from each test and procedure? (10 pts)

CHE 117L

Spring 2009

Claims: What are the answers to your questions or the ideas that you claimed? (4 pts)

Evidence: What evidence supports your claims? (6 pts)

Reflection: What have you learned from this activity? (2 pts)

CHE 117L POSTLAB QUESTIONS (10 pts)

Spring 2009

1. How did the pH and hardness of your water sample relate to the hardness of the other water samples done in your class?

2. If you step outside and catch rain drops in a bucket what would you expect the water hardness of this water to be?

3. What do you think was the most significant source of systematic error in this experiment?