Microscale Chemical Reactions – Solubility Introduction: Today we will perform twenty-eight chemical reactions! Not bad for one lab period. While exploring the reaction of several combinations of chemicals we will generate less than 20 milliliters of chemical waste per student. We will practice writing balanced chemical equations for each reaction that we perform to represent double replacement (aka metathesis) reactions and we will use this information to devise a set of solubility rules. Learning Objectives: (a) Observe a reaction mixture and distinguish between soluble and insoluble compounds. (b) Learn to classify compounds as soluble and insoluble. (c) Learn to balance chemical reactions of salts. Materials: -0.1 M solutions of eleven different salts in dropper bottles or with droppers -Sheet protector -Reaction grid -Safety goggles Hazard Information: Solution Health Hazards Physical Hazards 0.1 M AlCl3 0.1 M KCl 0.1 M NH4Cl 0.1 M MgCl₂ 0.1 M CaCl2 0.1 M FeCl₃ 0.1 M SrCl2 0.1 M NaBr 0.1 M Na2CO3 0.1 M Na2SO4 0.1 M Na₃PO₄ Irritant Irritant Low hazard Irritant Low hazard Irritant Irritant Low hazard Irritant Low hazard Low hazard Mildly corrosive Low hazard Low hazard Low hazard Low hazard Mildly corrosive Low hazard Low hazard Low hazard Low hazard Low hazard Siena Green Chemistry Summer Institute Lucas Tucker, Ann Klotz V2 Environmental Hazards Low hazard Low hazard Low hazard Low hazard Low hazard Low hazard Low hazard Low hazard Low hazard Low hazard Low hazard Page 1 Waste: Description of Material Quantity per group 0.1 M Salt solution 3 mL mixture Sheet Protector 1 Hazard Disposal Method Low Low Curl the reaction sheet and allow the drops to drain into a beaker. Trash Procedure: 1. Obtain an 8 1/2" x 11" plastic pouch and a laminated paper grid. The grid will look like the Data Collection Table for this experiment. The plastic sheet will serve as the reaction vessel for all of your reactions simultaneously. Slip the grid sheet into the pocket of the plastic sheet protector. Wipe the plastic sheet carefully with a dry towel to remove any residue from previous experiments. Tape the plastic sheet down flat on the bench. 2. A box containing small dropper bottles of solutions will be provided for each pair of students. All the starting materials are soluble, so a precipitate in the reactant bottle indicates that the bottle is contaminated with some other substance. If any of the bottles contains a precipitate or cloudiness, show it to your instructor and the bottle will be replaced. 3. Place a drop of each cation on the grid. Start with the potassium chloride solution and working your way across with one drop in each box. Continue to the next row of boxes and put a drop of ammonium chloride solution in each of the boxes in the next row. Continue until there is a drop of cation in each box. 4. Add a drop of anion solution next to, not on top of, the drop of cation, starting with bromide ion. Be careful not to touch the drop on the sheet with the tip of the dropper! Add anions down each column until the there is a drop of anion and a drop of cation in each box. 5. Use a toothpick to nudge the pairs of drops together and then stir with the same end of the toothpick. Use the fresh toothpick for each reaction. 6. Record your observations for each reaction in the table below. What is the color of the starting solutions? What is the color of the reacted solution? Is there a precipitate? What color is the precipitate? Cleanup: Remove the tape. Carefully curl the plastic sheet, and empty as much as possible of the solutions and solids into a large beaker. Pour the contents of the beaker into the labeled waste container. Siena Green Chemistry Summer Institute Lucas Tucker, Ann Klotz V2 Page 2 Student Name:___________________ Date: ___________________ Observations Data Summary Fill in the following table with the data gathered from the experiment. Look for the formation of solid precipitate, color change and gas bubbles. Na+ →- ↓ Cl- Br- CO32- SO42- PO43- Al3+ NH4+ Ca2+ 3+ Fe K+ Mg2+ Sr2+ Siena Green Chemistry Summer Institute Lucas Tucker, Ann Klotz V2 Page 3 Lab Questions 1) Which cations seemed to be soluble when mixed with any of the anions and which seemed to be insoluble? Soluble Insoluble 2) Which anions seemed to be soluble when mixed with any of the cations and which seemed to be insoluble? Soluble Insoluble 3) Green Question(s) List three ways that running these reactions on microscale makes this lab greener. References Siena College Chemistry Department Lab book. Solubility Rules. Written in fall 2004. Siena Green Chemistry Summer Institute Lucas Tucker, Ann Klotz V2 Page 4 TEACHER INFORMATION Solution preparation Chemical Name Molecular Weight To prepare 100 mL of 0.1M solution KCl NH4Cl MgCl₂.6H₂O CaCl2 AlCl3. 6H₂O FeCl₃·6H₂O SrCl·6H₂O NaBr Na2CO3 Na2SO4 Na₃PO₄·12H₂O 74.55 Grams/m 53.49 ole 203.3 110.98 241.43 270.3 266.62 102.89 105.99 142.04 380.12 0.74 0.53 2.03 1.10 2.41 2.70 2.66 1.02 1.05 1.42 3.80 Data Summary ↓ → Cl Al 3+ Br - CO3 2- SO4 2- PO4 3- No precipitate Precipitate + No precipitate No precipitate No precipitate No Precipitate 2+ No precipitate Precipitate Precipitate Precipitate 3+ No precipitate Precipitate No precipitate Precipitate No precipitate Precipitate No precipitate Precipitate No precipitate Precipitate No precipitate No precipitate No precipitate Precipitate Precipitate Precipitate Mg + Sr + Precipitate Ca K Na No precipitate NH4 Fe - + 2+ Siena Green Chemistry Summer Institute Lucas Tucker, Ann Klotz V2 Page 5 Balanced Chemical reactions that form precipitates: 2 AlCl3 (aq) + 3 Na2CO3 (aq) è Al2(CO3)3 (s) + 6 Na+ (aq) + 6 Cl- (aq) AlCl3 (aq) + Na3PO4 (aq) è AlPO4 (s) + 3 Na+(aq) + 3 Cl-(aq) 2 KCl (aq) + Na2CO3 (aq) è K2CO3 (s) + 2 Na+(aq) + 2 Cl-(aq) MgCl2 (aq) + Na2 CO3 (aq) è MgCO3 (s) +2 Na+(aq) + 2 Cl-(aq) 3 MgCl2(aq) + 2 Na3PO4(aq) è Mg3(PO4)2 + 6 Na+(aq) + 6 Cl-(aq) CaCl2 (aq) + Na2 CO3(aq) è CaCO3(s) + 2 Na+(aq) + 2 Cl-(aq) CaCl2 (aq) + Na2SO4(aq) è CaSO4 (s) + 2 Na+(aq) + 2 Cl-(aq) 3CaCl2(aq) + 2 Na3PO4(aq) è Ca3(PO4)2 (s) + 6 Na+(aq) + 6 Cl-(aq) 2 SrCl2(aq) + Na2CO3(aq) è Sr2CO3(s) + 2 Na+(aq) + 2 Cl-(aq) SrCl2(aq) + Na2SO4(aq) è SrSO4 (s) + 2 Na+(aq) + 4 Cl-(aq) 3 SrCl2(aq) + 2Na3PO4(aq) è Sr3(PO4)2 (s) + 6 Na+(aq) + 6 Cl-(aq) 2 FeCl3(aq) + 2 Na2 CO3(aq) è Fe2(CO3)2 (s) + 4 Na+(aq) + 6 Cl-(aq) FeCl3(aq) + Na3PO4(aq) è FePO4 (s) + 3 Na+(aq) + 3 Cl-(aq) 1) Which cations seemed to be soluble when mixed with any of the anions and which seemed to be insoluble? Soluble: Na+, NH4+ Insoluble: None 2) Which anions seemed to be soluble when mixed with any of the cations and which seemed to be insoluble? Soluble : Cl-, BrInsoluble : None Green Question 3 List three ways that running these reactions on microscale makes this lab greener. 1) Reduces the volume of material created 2) Reduces the volume of waste material 3) Reduces the amount of salt that must be created. Siena Green Chemistry Summer Institute Lucas Tucker, Ann Klotz V2 Page 6 MICROSCAL SOLUBILITY Reaction Grid Na+ ↓ →-­‐ Br-­‐ I-­‐ CO32-­‐ SO42-­‐ PO43-­‐ Cl-­‐ Al3+ NH4+ Ca2 Fe3+ K+ Mg2+ Sr+ Siena Green Chemistry Summer Institute Lucas Tucker, Ann Klotz V2 Page 7 Which of the 12 principles of Green Chemistry were employed to make this lab greener? VPrevention It’s better to prevent waste than to treat or clean up waste afterwards. mAtom Economy Design synthetic methods to maximize the incorporation of all materials used in the process into the final product. VLess Hazardous Chemical Syntheses Design synthetic methods to use and generate substances that minimize toxicity to human health and the environment. VDesigning Safer Chemicals Design chemical products to affect their desired function while minimizing their toxicity. mSafer Solvents and Auxiliaries Minimize the use of auxiliary substances wherever possible make them innocuous when used. mDesign for Energy Efficiency Minimize the energy requirements of chemical processes and conduct synthetic methods at ambient temperature and pressure if possible. mUse of Renewable Feedstock’s Use renewable raw material or feedstock rather whenever practicable. mReduce Derivatives Minimize or avoid unnecessary derivatization if possible, which requires additional reagents and generate waste. mCatalysis Catalytic reagents are superior to stoichiometric reagents. mDesign for Degradation Design chemical products so they break down into innocuous products that do not persist in the environment. mReal-time Analysis for Pollution Prevention Develop analytical methodologies needed to allow for real-time, in-process monitoring and control prior to the formation of hazardous substances. mInherently Safer Chemistry for Accident Prevention Choose substances and the form of a substance used in a chemical process to minimize the potential for chemical accidents, including releases, explosions, and fires.1 EPA: Twelve Principles of Green Chemistry. Retrieved from http://www.epa.gov/sciencematters/june2011/principles.htm Siena Green Chemistry Summer Institute Lucas Tucker, Ann Klotz V2 Page 8