Advanced Chemistry The Determination of Copper in Brass Purpose: To calculate the % of copper in Brass. Background: Brass is a combination of copper and >>>>. When a brass sample is dissolved in nitric acid the result is the following reaction. 8 H+ (aq) + 2 NO3- (aq) + 3 Cu (s) 2 NO (g) + 4 H2O (l) + 3 Cu2+ (aq) The concentration of copper (II) ion, and hence the concentration of copper in the brass sample can be measured by evaluating the intensity of the blue color. The color intensity will be measured visually by a comparison of the sample’s color with that of a series of copper (II) ion solutions of known concentrations. Alternatively, since the absorbance of the colored solutions is directly proportional to its concentration (A=abc), a Beer’s Law plot can be constructed using solutions of known concentration. The copper (II) ion concentration of the brass sample may then be read directly from this plot. Materials: 1.00 M Cu(NO3) 2 5 mL volumetric flask 24 well plates toothpicks 15.8 M HNO3 10 mL volumetric pipettes 96 well plates ¼ x #2 brass screw spectrophotometer Beral thin-stem pipets Safety Precautions: 15.8 M nitric acid is very corrosive to all body tissues and toxic by ingestion and inhalation. Nitric acid is also a strong oxidizing agent. Cupric nitrate is an oxidizing agent and moderately toxic by ingestion. NO 2 is a colorful gas therefore POISONOUS. Lab should be performed in the fume hood. Wear goggles, gloves and aprons at all time during lab. Procedure: First Things First 1. Measure the mass of a brass screw to ± 0.001 g using an analytical balance. 2. Assuming your brass sample is 100 percent copper by mass (even though it isn’t…), calculate the minimum volume, in mL, of concentrated 15.8 M HNO3 (aq) that needs to be added to react completely with the brass. SHOW YOUR TEACHER THIS CALCULATION, then have them measure it out carefully in the fume hood and add it to a 10.000 – mL volumetric flask. 3. Allow the screw to react completely. Pre-Experiment Procedure You will be collecting data between wavelength, concentration, and absorbance. The interaction of light with solutions to determine the concentration of an absorbing species is an important aspect of this experiment. 1. You will be given 0.100 M solutions of salts: a. copper (II) sulfate b. copper (II) nitrate c. zinc nitrate d. zinc sulfate e. iron (III) nitrate f. iron (III) sulfate Choose either salts a and d, b and e, or c and f. 2. Using a spectrophotometer (you will be shown how to do this), take measurements every 20 nanometers from 400-700 nm in order to generate a spectrum and to determine the “best” wavelength at which to measure the absorbance of the two solutions. 3. Print your data and bring it to the front of the room so that we can have a class discussion about absorbance, Beer’s Law, and the spectra you created. Method A 1. Prepare comparison samples of copper (II) nitrate solutions by serial dilution. Using the 24 well plate and a Beral pipet, begin with 20 drops of the copper (II) nitrate solution provided in one well, and where each subsequent well has been diluted by one drop while maintaining an overall volume of 20 drops. 2. Calculate the concentration of Cu+2 ions in each cell. 3. When the screw has completely dissolved, carefully add distilled water to the mark on the volumetric flask and invert several times to mix. Let any solids settle, then draw out the solution with a clean pipet and place it in a well of a 24-well plate. Visually match the color intensity of this well with the closest standard dilution and record the appropriate Cu2+ ion concentration. 4. Use solution stoichiometry to calculate the amount of grams of Cu and then the % of Cu in the brass screw. Method B A standard curve of absorbance versus concentration must be prepared by determining the absorbance of a set of standard solutions. A Beer’s Law graph then is plotted to determine the unknown solution. Prepare the stock solutions in the following way: 1. Find the wavelength of maximum absorbance of the Cu2+ ion using the standard 1.00 M Cu(NO3) 2 solution (this was done in the pre-experiment procedure). 2. Obtain 10.00 mL of 1.00 M Cu(NO3)2 stock solution using a volumetric pipette. Place the solution in a test tube. 3. Determine what volume is required to make 10.00 mL of 0.8000 M Cu(NO3)2. Use a volumetric pipette to transfer this volume of the stock solution into a clean test tube, and pipette the appropriate amount of water as well. Thoroughly mix the solution. 4. Repeat the dilution process to make 10.00 mL each of three additional dilute solutions (0.600 M, 0.400 M, 0.200 M). 5. Place each of these solutions into cuvettes and determine their respective absorbance. Create a graph of absorbance vs. concentration (a standard curve). Determining % copper in brass of your sample: 6. Using your copper ion solution from your lab, Find its absorbance simply by looking and reading the number off of the computer and writing it down in your written data table. Using the graph constructed determine the concentration of of the copper ions in the solution. 7. Place your sample in a clean cuvette and determine its absorbance value. 8. Using the equation of the line on your standard curve, determine the concentration of your sample. 9. Use solution stoichiometry to calculate the amount of grams of Cu and then the % of Cu in the brass screw. Data Table: 1) Method A 2) Method B 3) All results data from calculations Calculations: 1) Beer’s Law = A=abc Find the molar absorptivity of Cu+2 ions using the pre-experiment data, choosing the maximum wavelength and appropriate absorbance (the path length is 1.00 cm). 2) Method A concentration of copper ions in each well reasoning used to determine concentration of your sample moles of copper in screw grams of copper in screw % copper in brass screw 3) Method B molarity of aliquots y = mx + b to find concentration of copper ions in unknown moles of copper in screw grams of copper in screw % copper in brass screw Questions: 1) Give the advantages and disadvantages of both methods. 2) Error Analysis a) Effect of not preparing your solutions accurately in method B on % brass? b) Effect of not using 20 uniform drops in method A on % brass? Vocabulary: Brass, Alloy, Beer’s Law, Aliquot, & Molar absorptivity Lab modified from Flinn Scientific Workshop-St. Xavier Univ.