Timothy Scott Unknown Analysis 5: Scheme Possible Ions: Cations: Na+, K+, NH4+, Ca2+, Mg(OH2)62+, Al(OH2)63+ Anions:

Cl-, NO3-, SO42-, HSO4-, OH-, CO32-, HCO3Possible Insoluble: Ca(OH)2, CaSO42H2O, CaCO3, MgCO3, Mg(OH)2 Alums: K[Al(OH2)6](SO4)2 6H2O, NH4[Al(OH2)6](SO4)2 H2O Description of Sample, in terms of: Phase, color, odor, solubility, crystal shape if crystalline, etc.

Ning Zhao

Preparation: Ensure an adequate stock of the necessary solutions: o 6M NaOH o 6M HAc o 16M & 6M HNO3 o Cobaltinitrite o 0.02M AgNO3 o Ba(NO3)2 o Fe(OH2)5(NH4)2(SO4)2

Flame Test: Clean wire loop with 16M HNO3 o Flame test the clean loop to ensure no contamination o REMEMBER: Dry the loop after each test, and remember Nings advice regarding false positives Yellow Flame: Na+ present; test for K+ & NH4+ Purple Flame: K+ present; Na+ not present, test for NH4+ Red Flame: Ca2+ present; Na+ not present, test for NH4+ and K+ Colorless Flame: test for NH4+; Ca2+, K+, Na+ not present Note: a positive HCO3-/CO32- test means carbonate interferes with Na/Ca flame test

HCO3-/CO32- (in conjunction with flame test): Treat with excess HNO3 Bubbles indicate positive test o Be careful: as small bubbles may be caused by a false positive! Refer to the pH chart to differentiate which anion

Timothy Scott

Ning Zhao

Make Solution: Dissolve half of remaining sample in 10 mL deionized water Stir for 30 seconds, or until the sample has dissolved *For insoluble samples, place the mixture into a test tube and centrifuge to create a condensed mass and supernatant liquid* Sample 5A: o Soluble: perform cation/anion tests only o Insoluble: perform insoluble test, discard supernatant liquid Sample 5B: o Soluble: perform cation/anion test only o Insoluble: centrifuge, separate supernatant liquid and solid Supernatant liquid: perform cation/anion test Solid: perform insoluble test pH Test: Add a few drops of DIW to small portion of sample Use the following chart to estimate possible ions: o 1-2: HSO4No OH-, HCO3-, CO323+ o 3: Al(OH2)6 No OH-, HCO3-, CO32o 5: NH4+ and/or Mg(OH2)62+ o 7: Na+, K+, Cl-, NO3-, SO42-, Ca2+ o 8.5-9: HCO3No HSO4-, Al(OH2)63+, OHo 12: CO32No HSO4-, Al(OH2)63+, NH4+ o 13-14: OHNo HSO4- or NH4+

NH4+ Test: Put a small portion of sample in a spot plate, or vial Add 2-3 drops NaOH o Perform sniff test Suspend damp red litmus paper above solution o Leave for approximately a minute to allow sufficient time for a more accurate test If red litmus paper turns blue, NH4+ present

Insoluble Soild Test: Treat with 1M HCL o Dissolves without bubbling: perform flame test Red flame: Ca(OH)2

Timothy Scott No color: Mg(OH)2 o Dissolves with bubbling: perform flame test Red flame: CaCO3 No color: MgCO3 o Doesnt dissolve: CaSO42H2O Mg(OH2)62+ vs. Al(OH2)63+: Treat with excess NH3 Treat resulting precipitate with 2M NaOH o Insoluble: Mg(OH2)62+ o Soluble: Al(OH2)63+ Test resulting supernatant liquid for cations

Ning Zhao

Ca2+: K+:

Treat with excess 0.5 M Na2CO3 Indicated by white precipitate Test resulting supernatant liquid for remaining cation

If NH4+ present: o Heat amount of sample in crucible until no longer smoking o Dissolve residue in 1-2 mL of deionized water o Treat as if NH4+ not present If NH4+ not present: o Put small amount of solution in spot plate o Add 2 drops of 6M HAc and 4-6 drops sodium cobaltinitrite solution o If yellow/orange precipitate forms, K+ present

Cl-: 10-20 drops of solution in vial Acidify with 6M HNO3 (blue litmus paper turns red) Add AgNO3 If cloudy white precipitate, then Cl- present

HSO4-/SO42-: Add 10-20 drops of solution to vial Add 6M HNO3 until acidic (blue litmus paper turns red) Add .25M Ba(NO3)2 If white precipitate, then HSO4-/SO42- present

Timothy Scott NO3-: Place crystal Fe(OH2)5(NH4)2(SO4)2 in spot plate Add 2-3 drops of solution Add 18 M H2SO4 If brown precipitate forms, then NO3- is present SAMPLE 5A _ Na+________________ _ K+_________________ _ NH4+_______________ _ Ca2+_______________ _ Mg(OH2)62+__________ _ Al(OH2)63+___________ _ Cl-__________________ _ NO3-________________ _ SO42-________________ _ HSO4-_______________ _ OH-_________________ _ CO32-________________ _ HCO3-________________ _ Ca(OH)2______________ _ CaSO42H2O ___________ _ CaCO3________________ _ MgCO3_______________ _ Mg(OH)2______________ _ K[Al(OH2)6](SO4)2 6H2O _ _ NH4[Al(OH2)6](SO4)2 H2O _ ___________ ___________ ___________ ___________ ___________ ___________ ___________ ___________ ___________ ___________ ___________ ___________ ___________ ___________ ___________ ___________ ___________ ___________ ___________ ___________ SAMPLE 5B ____________ ____________ ____________ ____________ ____________ ____________ ____________ ____________ ____________ ____________ ____________ ____________ ____________ ____________ ____________ ____________ ____________ ____________ ____________ ____________ Determine ion by pH indication

Ning Zhao

Timothy Scott

Ning Zhao