Anions Illinois Central College CHEMISTRY 132 Laboratory Section: _______ Page 1 Name:___________________________ Anion Analysis Equipment 1-tray of dropper bottles 2-wooden test tube blocks 12-16 micro test tubes 2-10 mL beakers 2-micro spatulas 4-medicine droppers 2-micro test tube brushes 1-small graduated cylinder Make labels for 6 dropper bottles and fill them with the following solutions: 6 M HCl 6 M HNO3 6 M HC2H3O2 6 M NaOH 6 M NH4OH distilled water Make 6-8 capillary droppers and 2-3 stirring rods. Helpful tips Centrifuge In order to facilitate the separation of solid precipitate from supernatant liquid, a sample must be centrifuged. For the centrifuge to spin smoothly, it must be balanced. Be sure to place a like test tube with approximately the same amount of liquid just opposite your sample tube. Complete Precipitation When instructions require that a solution be made alkailne or acidic (in order to precipitate selected ions) , be sure that you've added enough acid or base by swabbing a drop of the solution across a strip of litmus paper. Litmus turns blue when exposed to basic solutions and red when exposed to acidic solutions. Then THROW THE LITMUS PAPER AWAY. Drop Size It should be noted that the drops delivered by a cpillary pipette are much smaller than a medicine dropper. When instructed to add a given number of drops of unknown or a necessary reagent, be sure to use a medicine dropper for big healthy drops. Saftey Precautions Some unknowns contain solutions that may stain the skin. Treat them with care. The concentrated acids and bases will naturally cause skin irritations or burns, so if you should contact them, wash the solution off immediately. Anions Page 2 Tests for Common Anions Pre-test: To several drops of the unknown sample, add 2 drops of BaCl2 solution. Then, to a second sample, add 2 drops of AgNO3 solution. These are results obtained with some common anions. (NR= no reaction) Cl-1 Br-1 I-1 NR NR NR NO3-1 C2H3O2-1 White White White precipitate. precipitate. precipitate. Insoluble Soluble in Soluble in in HCl. HCl HCl. NR NR Yellow White Pale White Yellow precipitate. precipitate. precipitate. precipitate. yellow Soluble in precipitate. (maybe) Slightly NH4OH. soluble in Insoluble Soluble in Soluble in Soluble in in HNO3 HNO3. Insoluble NH4OH. HNO3 HNO3. Insoluble in HNO3 in HNO3. NR Colorless (white) crystals. (may form slowly. BaCl2 test White AgNO3 precipitate. test SO4-2 PO4-3 CO3-2 Chloride test To 2 drops of solution add 1 drop of AgNO3. A white precipitate that dissolves completely in 6M NH4OH, then reappears when 6M HNO3 is added confirms Cl-1 ion. Bromide test To 3 drops of solution add 6 drops of CCl4. Then add 2 drops of 6M H2SO4 and 3 drops of chlorine water. Shake tube gently. An orange color the CCl4 (bottom) layer confirms Br-1 ion. in Iodide test Repeat the test for bromide ion. A pink to purple color in the CCl4 layer confirms I-1 ion. Sulfate test To 2 drops of solution add 2 drops of BaCl2. A whicte precipitate that does not dissolve in 6M HCl confirms SO4-2 ion. Phosphate test To 2 drops of solution add 3 drops of 6M HNO3 and 3 drops of ammonioum molybdate solution. Heat in a water bath. A fine yellow precipitate confirms PO4-3 ion. (AsO4-3 also gives test.) Carbonate test To 2 drops of solution add 2 drops of 6M HCl. Evolution of a colorless, odorless gas (bubbles) confirms CO3-2 ion. Nitrate test To 3 drops of solution add 3 drops of FeSO4. Holding the test tube at a 45o angle, allow 5-6 drops of conc. sulfuric acid to flow down the inside of the tube. Formation of a brown ring at the junction of the two liquids confirms NO3-1 ion. Acetate test To 3-4 drops of solution add 3 drops of conc. sulfuric acid and 3 drops of ethyl alcohol. Carefully heat in a flame until gentle boiling begins. A fruity (apple-like) odor of ethyl acetate confims C2H3O2-1 ion. Anions Illinois Central College CHEMISTRY 132 Laboratory Section: _______ Name:___________________________ REPORT SHEET Analysis of Unknown-Anions 1. Unknown Sample Number _____________ Reagent Added Result Conclusion 1. 2. 3. 4. 5. Sample Contains:_____________ 1. Unknown Sample Number _____________ Reagent Added Result Conclusion 1. 2. 3. 4. 5. Sample Contains:_____________ 1. Unknown Sample Number _____________ Reagent Added Page 3 Result 1. 2. 3. 4. 5. Sample Contains:_____________ Conclusion Anions Page 4