AP Chemistry Lab — Precipitation Reactions and Solubility Rules Prelab: 1. To be done on a separate piece of paper and turned in before lab starts! Write balanced molecular equations for each of the reactions you will be performing in Parts I and II. (There should be a total of 42 equations .) You will be mixing each compound with each other compound, but not with itsel f. It does not matter what order in which you react the compounds. (For exam ple. silver nitrate ± barium chloride will give the same results as barium chloride + silver nitrate!) 2. Prepare two data tables in your lab notebook one for Part I and one for Part II. Use a full page for each table! For Part I. label 7 columns (1-7 to correspond to the top of the 48-well reaction plate you will use) with the corre ct formulas of each of the seven solutions for Part I, starting with silver nitrate. Labe l 6 rows (A-F to correspond to the side of the 48-well reaction plate you will use) with the correct formulas of six solutions for Part I, starting with barium chloride since you will not mix silver nitrate with itself. For the second data table, repeat with the seven solutions for Part II. Each square in each data table must be large enough to record the observations and also to write the formulas of the two possible prod ucts formed! — Introduction: Discover some general rules of solubility for ionic subs tances. Conduct 42 chemical reactions, determine the solubility of the prod ucts. analyze the patterns, and formulate the rules. Background: An ionic salt is a compound composed of two parts caflons (positively-charged ions) and anions (negatively-charged ions). When an ionic salt is dissolved in water, the salt crystal dissociates or separates into its correspon ding cations and anions. For example, potassium iodide (KI) dissociates into potassium cations (K) and iodide anions (F) according to equation 1: — KI (s) K (aq) + F (aq) Equation 1 Similarly, the ionic salt lead nitrate 3 [Pb(N0 dissociates into lead cations (Pb j 2 ) ) and 2 nitrate anions (N0 ) according to equation 2: 3 3 Pb( 2 ) N0 (s) 2 (aq) Pbt ± 2 N0 3 (aq) Equation 2 When two ionic salts are mixed together in water. two new combinations of cations and anions are possible. In some cases, the cation from one salt and the anion from the other salt may combine to form an insoluble solid product. whic h is called a precipitate. For example. if the solutions of potassium iodide and lead nitrate are mixed together. a solid precipitate of lead iodide (Pb1 ) forms, as shown in equation 3: 2 2Kb(aq) + 21 2 (aq)+ ( iq Pb ) + 2N0 (aq) Pb ( 2 s)2K 1 (aq) +2N0 3 (aq) Equation 3 Notice that the potassium cations (K) and the nitrate anions (N0 ) remain dissolved in 3 solution. These ions are referred to as spectator ions. Spectator ions do not partici pated in the overall reaction (hence the term spectators) and are often omitted from the net ionic equation. A net ionic equation is one that includes only the ions participating in the reaction. Thus, equation 3 can be reduced to equation 4: 2 (aq) Pb + 2F (aq) 2 (s) Pb1 -‘ Equation 4 The example described above shows that a precipitate of Pb1 2 forms when a solution of KI is mixed with a solution of 3 Pb(N0 However, when two salt solutions are mixed . 2 ) together and no visible precipitate forms (indicating that no reaction occurs), it can be concluded that all combinations of the cations and anions from the two salt solutions are soluble in water. It must be noted that every salt has some degree of solubility. Some salts dissolve readily in water while others will not. Even if a salt is considered insoluble (formi ng a solid precipitate). there is still some small amount of that salt dissolved in the water. (Hence the double arrow” in the equations above. A more correct representation would have a top arrow to the right which is longer than a lower arrow to the left.) Tables of solubilities are available to predict whether or not a precipitate will form when two salts are mixed together. However, observing precipitation reactions in a laboratory setting and becoming familiar with the general rules of solubility can be extremely valuable. In this laboratory experiment, 14 salt solutions will be combined, two at a time seven in Part I and seven in part II totaling 42 chemical reactions. Observations will be recorded as to which combinations form a precipitate and which do not undergo a reaction. From these results, a list of soluble substances and a list of insoluble substan ces will be generated. This list will be analyzed and some general rules of solubility will then be developed. — — Materials Needed: Chemicals — Part I Silver nitrate solution, 0.1 M Barium chloride solution, 0.1 M Sodium carbonate solution. 0.1 M Ammonium sulfate solution, 0.1 M Lead nitrate solution. 0.1 M Calcium nitrate solution, 0.1M Potassium phosphate solution. 0.1 M Chemicals — Part II Iron (III) chloride solution. 0.1 M Sodium hydroxide solution, 0.1 M Magnesium bromide solution, 0.1 M Potassium carbonate solution, 0.1 M Lead nitrate solution. 0.1 M Sodium sulfate solution, 0.1M Sodium chromate solution. 0.1M Equipment Reaction plate. 48-well Pipet (cassette) holder, with labeled beral pipets. for Part I Pipet (cassette) holder, with labeled beral pipets, for Part II Distilled water bottle and Q-tips for cleaning well plate Safety Precautions: Barium chloride, lead nitrate, and sodium chromate solu tions are toxic by ingestion. Silver nitrate solution is toxic, corrosive, light-sens itive, and stains skin and clothing. Sodium hydroxide solution is corrosive and a body tissue irritant. Avoid all eve and body tissue contact with all solutions, Wear chem ical splash goggles. chemicalresistant gloves, and a chemical-resistant apron. Procedure: Part I — Mixing Pairs of Solutions in Data Table 1 1. Take the pipet holder with the 7 labeled pipets for Part I to the stock solutions table. Fill (about half-way) the 7bpipets with the appropria te solutions and take them back to your lab bench. 2. Place a 48-well reaction plate on top of a black table or black piece of paper. 3. Using your Part I Data Table as a guide. place 4 drop s of silver nitrate solution into well Al. Be sure to hold the pipet vertically for unifo rmly-sized drops. Continue adding 4 drops of silver nitrate solution to each well down the vertical column 1. wells Bi to Fl. 4. Fill each vertical column in the well plate as follows: Place 4 drops of barium chloride solution into wells B2-F2 . Place 4 drops of sodium carbonate solution into wells C3-F3. Place 4 drops of ammonium sulfate solution into wells D4-F4 . Place 4 drops of lead nitrate solution into wells E5-F5. Place 4 drops of calcium nitrate solution into well F6. (Remember. it doesn’t matter which order you mix the chem icals so only half of the reactions need to be performed!) 5. Now add 4 drops of barium chloride solution to the solu tion already in well Al. Record your observations immediately. (Note: If a prec ipitate appears, write “PPT” in the correct box of Data Table I. Record the colo r of the precipitate. If no precipitate appears to have formed, write NR” for No Reaction in the correct box of Data Table I. Make sure to leave space in each box whether or not a precipitate was formed!- to write the two possible products of the reaction.) — 6. Continue the process of mixing solutions by adding 4 drops of each of the solutions listed along the left side of your Data Table I to the correct well. Record your observations immediately, as described in Step #5. 7. Once Data Table I is complete. turn your well plate upside down on several thicknesses of paper towel and tap it on the towel to empty the wells. Immediately flush the reaction plate with tap water. The remaining solutions may be flushed down the drain with plenty of water. Rinse the well plate with distilled water (use a Q-tip if this doesn’t completely clean out a well!) and tap it on a paper towel to dry it out your plate is now ready for Part II. — Part II — Mixing Pairs of Solutions in Data Table H 8. Take the pipet holder with the 7 labeled pipets for Part II to the stock solutions table. Fill (about half-way) the 7bpipets with the appropriate solutions and take them back to your lab bench. 9. Place a 48-well reaction plate on top of a black table or black piece of paper. 10. Using your Part II Data Table as a guide, place 4 drops of iron (III) chloride solution into well Al. Be sure to hold the pipet vertically for uniformly-sized drops. Continue adding 4 drops of iron (III) chloride solution to each well down the vertical column 1, wells Bi to Fl. 11. Fill each vertical column in the well plate as follows: Place 4 drops of sodium hydroxide solution into wells B2-F2. Place 4 drops of magnesium bromide solution into wells C3-F3. Place 4 drops of potassium carbonate solution into wells D4-F4. Place 4 drops of lead nitrate solution into wells E5-F5. Place 4 drops of sodium sulfate solution into well F6. (Remember, it doesn’t matter which order you mix the chemicals so only half of the reactions need to be performed!) 12. Now add 4 drops of sodium hydroxide solution to the solution already in well Al. Record your observations immediately. (Note: If a precipitate appears, write “PPT” in the correct box of Data Table I. Record the color of the precipitate. If no precipitate appears to have formed, write ‘NR” for No Reaction in the correct box of Data Table 1. Make sure to leave space in each box whether or not a precipitate was formed!- to write the two possible products of the reaction.) — 13. Continue the process of mixing solutions by adding 4 drops of each of the solutions listed along the left side of your Data Table I to the correct well. Record our observations immediately, as described in Step #5. 14. Once Data Table I is complete, turn your well plate upside down on several thicknesses of paper towel and tap it on the towel to empty the wells. Immediately flush the reaction plate with tap water. The remaining solutio ns may he tiushed down the drain with plenty of water. Rinse the well plate with distilled water (use a Q-tip if this doesn’t completely clean out a well!) and tap it on a paper towel to dry it out. Analysis: Part I — Making a List of Soluble, Insoluble, and Unknown Substances I. In each box where a reaction was performed in Data Tables I and II. write the formulas for the two possible double replacement products. This should be done even for those combinations that produced no reaction. 2. Use a full page in your notebook to make the following table: Categories of Substances Soluble Substances [ Insoluble Substances ] Unknown Substances Use this table to make a list of all the substances that you know to be soluble in water. Generate this list of soluble substances in two ways. a. Write down each solution that you used in this experiment from the materials list. (Since these are all solutions with no precipitates. you can assume they are all soluble.) h. Look at your recorded observations in the data tables. For each reaction that did not produce a precipitate (NR), four substances are now known to be soluble the two starting substances and the two possible products. For example. when mixing two soluble substances such as sodium carbonate and ammonium sulfate, no reaction occurs. This tells you that sodium sulfate and ammonium carbonate are also soluble. — 3. Generate a list of all substances that you know to be insoluble. Look at your data tables. Examine each of the reactions that did produce a precipitate. Each pair of solutions mixed together can produce 2 new possible substances, as discussed in the background section. Make the assumption that if a precipitate is formed when mixing two solutions, the precipitate is formed by only 1 of the 2 new substances. Compare each of the new substances to the list of soluble substances. If one of the new substances appears on the soluble list, the other must be the precipitate and can be add to the insoluble column. If neither one of the new substances appears on the soluble list, then place both substances in the unknown column. Write the two substances together as a pair. This way. later you will know that if one substance is found to he soluble, the other must be insoluble. 4. Look at your lists of soluble and insoluble substances. Cross out any duplicate entries, using a different colored pen. Leave the list of unknown substances unchanged. 5. In ‘our notebook. make a separate table like the one above. This time categorize and alphabetized column 1 (soluble substances) and then column 2 (insoluble substances) by the anionic part (second work!) of the salt. For example. potassium chloride would be listed as ‘chloride, potassium” and would be grouped with all the other chlorides in that column. Leave column 3 (unknown substances) as is, with the salts written in pairs. Do not mix up the pairs! 6. Examine the pairs of substances in the unknown column of your table. Remember, if one substance is found to be soluble, the other must be insoluble. Look for any substances that can now be definitely determine to be soluble or insoluble. Move these into the appropriate column of your table, and crossing out the old entry, using your different colored pen. 7. Look for any common relationships among the substances in the unknown column and that of the soluble or insoluble substances. The key objective at this point is to remove all of the substances from the unknown column and place them in either the soluble or the insoluble column using logic and the process of elimination. There will be a point where no more substances can be moved from the unknown column by simply looking at laboratory data. At this point, some inferences and generalizations will need to he made. For example, are most (or all) of the nitrate compounds in the same column? How about the ammo nium or potassium compounds? Use the following categories to help with this step: carbonates: chlorides and bromides: chromates; hydroxides; nitrates; phosphates; sulfates: ammonium. potassium and sodium compounds. As you remove a substance. cross out the old entry and place the substance in its new colum n using your different colored pen. Under your tinal table. for each substa nce that you remove from the unknown column by generalization/inference, list the reason that you used to move the substance. 8. After completely eliminating the unknown column, examine the substances in the soluble and insoluble columns. Each column should be organized by group (i.e.. carbonates, chlorides, etc.) if you completed step #5 correctly. In your notebook. make a final table like the one below with the solubility of each group, including any exceptions that you observe. Be sure that your final table matches your experimental data and not what you “think” you should get! - - General Solubilitv Rules Substances Carbonates Soluble or Insoluble Exceptions Chlorides and Bromides Chromates Hydroxides Nitrates Phosphates Sulfates Ammonium, Potassium, and Sodium Compounds 9. Write balanced net ionic equations for each metathesis (doubl e replacement) reaction that produced a precipitate in this experiment. Be sure to include states of matter (aq. s. 1. g). 4 .3 -* j’ (i ), 3 Ni 4 ,SJ t ) 3 fC O PANO, () U U U i .3 Lu 4 ede the ciAelcs on th tabLe. 1cu iJ all cuIus that fudil. If aiy soli pie. use the a[bieviiian ppt. If d ipiiaLus no i eaction at nil oceucs, use [he ntbA e’ inucn NR. Wine (lie two possible produc rcj’ ose nLS eniply chls. ts in enh circle, as sho eii iii well A I observatb)L[ i 1 0 00cz00 C)OOC)0 Reoid &LalcJ ) Q ZZ’ZZ) SU 2 ) 4 i i)aia a 1 ‘ Lil l c I :000 U A I/ r 2. ‘: •‘\ ( \J \) —- r’. = t \7 r — (1 - \ E’) N 7 7 C \ \ = Th - = — = CuOCC;C Z L) C,: C CZ DC C C, C : C C’CC C C 1 C ‘C C C*C )C 7 7 : — 7 ____ ____ ____ ____ ____ ____ _ /arne: Categories oi Substances :5oluble Substances insoluble Substances Unknown Substances ____ ____ ____ ____ ____ ____ ____ 1 a me. Categories of Substances •1 Soluble Substances Insoluble Substances Unknown Substances ________________ ___________ £‘Ialne. General Solubility Rules 3ubstances Soluble Carbonates Chlorides and Bromides I Chromates iydroxides I I I I , “itrates Phosphates uIfates ! Xmmonium, 2odium Potassium arid or Insoluble Exceptions