CHM 2046 lab manual 8.9 (21) 8

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St. Petersburg College *

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2045

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Chemistry

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Feb 20, 2024

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CHM2046 Equilibrium Constant Determination St. Petersburg College Purpose Students will use UV-Visible spectroscopy to determine concentrations and calculate an equilibrium constant. Introduction Typically, reactions do not go to completion. Instead, the concentrations of reactants and products will reach a level where their concentrations remain constant. This is called equilibrium. The equilibrium that will be studied in this lab is the reaction of the iron (III) ion and thiocyanate ion to form a complex ion FeSCN 2+ . Fe 3+ (aq) + SCN - (aq) ҡ FeSCN 2+ (aq) The equilibrium equation for this reaction is Equation 1 ܭܿ = [ ி௘ௌ஼ே మశ ] [ ி௘ యశ ][ ௌ஼ே ] The value of K c is constant at a given temperature, and it does not depend on the initial concentrations of the reactants. The complex ion FeSCN 2+ is red in color, and the intensity of the color can be measured by UV-Visible spectroscopy. The intensity of this red color can then be used to calculate the concentration of this ion by a method to be described later. Firstly, the initial moles of the reactants (Fe 3+ and SCN - ions) are calculated. Secondly, the moles of the product (FeSCN 2+ ) at equilibrium are calculated. Thirdly, equilibrium moles of the reactants can be calculated by subtraction using the initial moles of the reactants and the equilibrium moles of the product. Fourthly, the equilibrium moles of reactants and products can be converted into concentrations. Lastly, the value of K c is calculated using these concentrations. 23
CHM2046 Equilibrium Constant Determination St. Petersburg College Calibration Curve Use this pre-made data set of concentration of FeSCN 2+ and the corresponding absorbance values (and its equation in the graph below to help with calculations. This set of data/graph is the calibration curve data/graph. Concentration of FeSCN 2+ (X axis) Absorbance (Y axis) Percent Transmittance (%T) 0 0 100 1.00E-04 0.495 32 2.00E-04 0.955 11.1 3.00E-04 1.398 4 FeSCN 2+ ion is red in color and can be detected at 447 nm using a spectrophotometer. The higher the concentration of this complex ion, the higher the absorbance value. The absorbance is related to the concentration of the solution by Beer’s Law: Equation 2 ܣ = ߝܿ or ܿ = tŚĞƌĞ ± ŝƐ ĂďƐŽƌďĂŶĐĞ͕ Đ ŝƐ ĐŽŶĐĞŶƚƌĂƚŝŽŶ ĂŶĚ ɸ ŝƐ ƚŚĞ ŵŽůĂƌ ĂďƐŽƌƉƚŝǀŝƚLJ͕ ǁŚŝĐŚ ŚĂƉƉĞŶƐ ƚŽ ďĞ the slope of the graph. In this way, concentration of any solution of this ion may be found from any absorbance value. 24
CHM2046 Equilibrium Constant Determination St. Petersburg College Experimental Procedure Materials x 5 clean and dry test tubes x 2.00 x 10 -3 M Fe(NO 3 ) 3 in 1 M HNO 3 solution x 2.00 x 10 -3 M KSCN solution x Cuvettes and UV-Visible Sprectrophotometer 1. Obtain 5 clean and dry medium test tubes. Label them 1, 2, 3, 4, and 5. 2. Obtain two clean and dry small beakers. 3. Pour ~30 mL of 2.00x10 -3 M Fe(NO 3 ) 3 (this comes dissolved in 1M HNO 3 , so be very careful! Nitric acid is extremely corrosive and toxic. Use gloves!) into the first beaker. 4. Pour ~20 mL of 2.00 x10 -3 M KSCN into the second beaker. 5. Measure out the beaker solutions and deionized water into each test tube according to Table 1. The total solution in each test tube will be 10.00 mL each. Use a clean graduated cylinder for each solution and for deionized water to avoid cross- contamination. Table 1. Test tube mixture ratios, measured absorbance at 447 nm and calculated concentration of FeSCN 2+ . 6. After the solutions are made in the test tubes, stir/mix well so a homogeneous solution is made. If a glass rod is used, be sure to clean and dry the glass rod before reusing it in the next test tube. 7. Leave the test tubes on your test tube rack. Obtain a plastic pipet for each test tube. 8. Obtain a clean and dry cuvette from the instructor, or from inside the spectrophotometer. Remember, the cuvettes may look like small test tubes but they are different from test tubes. 25
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CHM2046 Equilibrium Constant Determination St. Petersburg College 9. To ensure there are no stains/marks on the cuvette, wipe the cuvette with a KimWipe. Do not use regular paper towels as this will scratch the cuvette. Scratched cuvettes result in inaccurate absorbance values. 10. Fill the cuvette with deionized water about ¾ of the way. Wipe the sides with a KimWipe. The following procedures may vary depending upon the model of the UV-Visible Spectrophotometer used at your location. Please ask your instructor to demonstrate the use of the spectrophotometer used at your specific location. 11. Bring the test tubes, their associated plastic pipets, your cuvette filled with deionized water, some KimWipes, and a waste beaker to the spectrophotometer area. Figure 1. Spectrophotometer 12. Make sure the spectrophotometer is set to measure absorbance at 447nm. Use Knob C to adjust to 447 nm if it has not been set correctly for you. 26
CHM2046 Equilibrium Constant Determination St. Petersburg College 13. Bring the cuvette of deionized water to the spectrophotometer (which should have been warming up for at least 20 minutes by now) and make sure that when the lid is ĐůŽƐĞĚ͕ ƚŚĞ ĂƌƌŽǁ ŝƐ ƉŽŝŶƚŝŶŐ ƚŽ njĞƌŽ ƉĞƌĐĞŶƚ ƚƌĂŶƐŵŝƚƚĂŶĐĞ ;ь ±ďƐŽƌďĂŶĐĞͿ͘ /Ĩ ŝƚ ŝƐ ŶŽƚ zero transmittance, use the knob A to adjust the needle to zero transmittance. (Knob A is also the power knob) 14. Open the lid and place your cuvette of deionized water in. Close the lid. 15. The needle should now move to 100 percent transmittance (0 Absorbance). If it is not 100 percent transmittance (0 Absorbance) use knob B to adjust the needle to 100 percent transmittance. 16. Take the cuvette out and close the lid. The needle should point back to zero transmittance. If not, repeat steps 11-13 again until the needles are where they should be. This is the calibration process. 17. After calibrating with the deionized water cuvette, empty the deionized water into your waste beaker. 18. Dry the cuvette with a KimWipe. 19. Using the plastic pipet for test tube 1, transfer some solution 1 into the cuvette until about ¾ way filled. Wipe the cuvette with a KimWipe to remove any fingerprints/stains. 20. Open the lid, put the cuvette in the spectrophotometer and close the lid. 21. Read the absorbance value and record it in Table 1. 22. Take the cuvette out, empty the solution back into test tube 1. 23. Rinse the cuvette with deionized water into the waste beaker. 24. Then repeat steps 18-23 for test tube 2. After that, do the same again for test tubes 3, 4, and 5. Record all absorbance values in Table 1. 25. Clean all glassware, return the cuvette dry, and discard all solutions into the appropriate liquid waste container. 27
CHM2046 Equilibrium Constant Determination St. Petersburg College Recorded Data Test Tube 1 Test Tube 2 Test Tube 3 Test Tube 4 Test Tube 5 Absorbance Reading Calculated Data Step 1: Calculate the initial moles of Fe 3+ and SCN - in the solutions. Equation 3 ܫ݊݅ݐ݈݅ܽ ݉݋݈݁ݏ ܨ݁ ଷା = 2.00 × 10 ିଷ ܯ ܨ݁ ଷା × ܸ݋݈ݑ݉݁ ܷݏ݁݀ ( ݉ܮ ) × ଵ଴଴଴ ௠௅ Equation 4 ܫ݊݅ݐ݈݅ܽ ݉݋݈݁ݏ ܵܥܰ ି = 2.00 × 10 ିଷ ܯ ܵܥܰ ି × ܸ݋݈ݑ݉݁ ܷݏ݁݀ ( ݉ܮ ) × ଵ଴଴଴ ௠௅ Test Tube 1 Test Tube 2 Test Tube 3 Test Tube 4 Test Tube 5 Initial moles Fe 3+ Initial moles SCN - Step 2: Calculate the equilibrium concentration of FeSCN 2+ and equilibrium moles of FeSCN 2+ Equation 5 ܧݍݑ݈ܾ݅݅ݎ݅ݑ݉ [ ܨ݁ܵܥܰ ଶା ]( ݅݊ ௠௢௟ ) = ௔௕௦௢௥௕௔௡௖௘ ସ଻ଵଷ . / ௠௢௟ Equation 6 ܧݍ ݉ ݉݋݈݁ݏ ܨ݁ܵܥܰ ଶା = ܧݍ ݉ [ ܨ݁ܵܥܰ ଶା ] × 10.00 ݉ܮ × ଵ଴଴଴ ௠௅ Test Tube 1 Test Tube 2 Test Tube 3 Test Tube 4 Test Tube 5 Equilibrium [FeSCN 2+ ] Equilibrium moles FeSCN 2+ Step 3: Calculate the equilibrium moles of Fe 3+ and SCN - Equation 7 ܧݍ ݉ ݉݋݈݁ݏ ܨ݁ ଷା = ܫ݊݅ݐ݈݅ܽ ݉݋݈݁ݏ ܨ݁ ଷା െ ܧݍ ݉ ݉݋݈݁ݏ ܨ݁ܵܥܰ ଶା Equation 8 ܧݍ ݉ ݉݋݈݁ݏ ܵܥܰ ି = ܫ݊݅ݐ݈݅ܽ ݉݋݈݁ݏ ܵܥܰ ି െ ܧݍ ݉ ݉݋݈݁ݏ ܨ݁ܵܥܰ ଶା Test Tube 1 Test Tube 2 Test Tube 3 Test Tube 4 Test Tube 5 Equilibrium moles Fe 3+ Equilibrium moles SCN - 29 0.24 0.42 0.60 0.78 0.94
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CHM2046 Equilibrium Constant Determination St. Petersburg College Step 4: Calculate the equilibrium concentration of Fe 3+ , SCN - and FeSCN 2+ Equation 9 ܧݍݑ݈ܾ݅݅ݎ݅ݑ݉ [ ܨ݁ ଷା ] = ா௤௨௜௟௜௕௥௜௨௠ ௠௢௟௘௦ ி௘ యశ ଵ଴ . ଴଴ ௠௅ × ଵ଴଴଴ ௠௅ Equation 10 ܧݍݑ݈ܾ݅݅ݎ݅ݑ݉ [ ܵܥܰ ି ] = ா௤௨௜௟௜௕௥௜௨௠ ௠௢௟௘௦ ௌ஼ே ଵ଴ . ଴଴ ௠௅ × ଵ଴଴଴ ௠௅ Equation 11 ܧݍݑ݈ܾ݅݅ݎ݅ݑ݉ [ ܨ݁ܵܥܰ ଶା ] = ܵ݁݁ ݒ݈ܽݑ݁ݏ ݂݋ݑ݊݀ ݅݊ ࡿ࢚ࢋ࢖ Test Tube 1 Test Tube 2 Test Tube 3 Test Tube 4 Test Tube 5 Equilibrium [Fe 3+ ] Equilibrium [SCN - ] Equilibrium [FeSCN 2+ ] Step 5: Calculate the values of K c Equation 1 ܭܿ = [ ி௘ௌ஼ே మశ ] [ ி௘ యశ ][ ௌ஼ே ] Trial 1 Trial 2 Trial 3 Trial 4* Trial 5* K c Average K c = ___________________________ 30