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Unknown Analysis Cheat Sheet (Anion)
Unknown Analysis Cheat Sheet (Anion)
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Procedures: A. + 2-3 drops 6 M H2SO4 to test soln (if no reaction observed warm in water bath) B. + 6 M HCl to test soln til acidic (use litmus paper to check) + one drop K3Fe(CN)6 and + one drop 0.10 M FeCl3. Observe C. + 5 drops satch MnCl2H2O in 12 M HCl to test soln (heat if needed). Observe D1. + 3 M CH3COOH to test soln til acidic and in excess (use litmus paper to check)(warm to remove anions positive In A). remove ppt, + drop 0.10 M CaCl2, if ppt forms cont pption D2. Repeat prod D1 but w/ 0.10 M BaCl2(warm and stir to induce pption) D3. To soln from D2 w/o ppt, + 6 M NH3 until soln is basic(mix after each drop) E1. + 3 M HNO3 to test soln til acidic (use litmus paper to check)(warm to remove anions positive In A).+drop 0.10 M AgNO3. If ppt forms, cont adding to complete pption. Centrifuge. Discard centrifuge and wash ppt w/ 1 mL h2o E2. Test solblty in E1 in 1 mL 3 M NH3. E3. If ppt dissolves in E2, acidify with 3 M HNO3
Confirmatory test (For anions not absent) Do in 5-10 drops unknown soln (UNK). if in doubt, use control for anions being tested. If same results, then pos. 1. CH3COO + 10 drops UNK in evap dish. Evap til only few drps remain. Allow to cool. + 2-3 drops 18 M H2SO4 and warm over water bath. + few drops ethyl alcohol and warm. POS RESULT:Fruity odor(another test, is elim test A, vinegar smelling gas) 2. Br Acidify 1 drop of 0.01 KMnO4 w/ 2 dropd 3 M HNO3, + this to 5 drops UNK. + 6-8 drops baby oil, shake well allow to stand til immiscible layers form. POS RESULT: decolorization MnO4 and formation of yellow non-aqueous layer. 23. CO3 Perform test A in elim exp to 10 drops UNK, + 5 drops 6 M H2SO4 and warm in bath. POS RESULT: effervescence. 4. ClDo E1 to E3 from elim test. After test if white ppt AgCl persists, POS RESULT. 25. CrO4 Perform D2 fro elim test. Acidify each test soln w/ 3 M CH3COOH, + few drops in excs. Warm in bath. Remove any ppt that may form. + 1 drop 0.10 M BaCl2 and in excs. POS RESULT: formation of yellow ppt BaCrO4 6. I To 5 drops UNK, + 2 drops 3 M HNO3. + 3 drops 0.1 M FeCl3. + 6-8 drops baby oil. Shake well and let stand til immisc layers form. POS RESULTS: pink non-aqueous layer. 7. NO3
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Acidify 5 drops UNK by +ing 1 drop 6 M H2SO4. + 3 drops FeSO4. Til test tube 60 deg allow 2 drops 18 M H2SO4 slide down side of tt. Do not shake, slowly bring tt upright. POS RESULT: brown ringt at interface of concentrated acid soln.(I, BR, CNS, nitrite interferes with test.) 2C2O4 Perform D1 from elim test. Acidify 10 drops UNK with 3 M CH3COOH, +ing 2-3 drops acid in xcs. Warm in bath. Remove any ppt formed. + drop 0.10 M CaCl2. If white ppt froms, complete pptation. POS RESULT: white ppt CaC2O4 2PO4 + magnesia mixture dropwise to 10 drops UNK. White ppt MgNH4PO4 confirms presence of phosphate. +ing of AgNO3 to ppt transforms ppt to yellow. 2SO4 Acidify 10 drops UNK w/ 3 M HCl and + drop BaCl2. If white ppt forms, cont +ing BaCl2 til ppt comp. this indicates presence of SO4. (interferes with CrO4. To elim interference, CrO4 must ppted out first wth 20 drops 0.10 M AgNO3) CNSTo 5 drops UNK, + 3-5 drops 0.1 M FeCl3. POS RESULT: formation of blood red complex. 2S perform A from elim test to 10 drops UNK. + 5 drops 6 M H2So4 and warm in bath. POS RESULT: colorless gas w/ rotten-egg smell. 2S2O3 perform test A from elim test. POS RESULT: Aside from burnt rubber smell, formation of milky yellowish ppt.
Results
Anions Cl S
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A 6M H2SO4
B FeCl3/ K3Fe(CN)6
D1 CaCl2/ HoAc
D2 BaCl2/ HoAc
D3 BaCl2/ NH3
-2
-2 S2O3 -
Rotten egg/fruit smell Burnt rubber w/ milky yellow ppt Vinegar bubbles Orange soln
NVR
NVR
No change
Colorless Colorless Brown soln Dark blue ppt. in yellow soln Brown soln
NVR NVR
NVR NVR
NVR NVR NVR Yellow ppt. NVR NVR NVR NVR White ppt. Yellow ppt.
No change
No change
NO3 C2O4
2-
NVR
No ppt. Yellow soln Colorless Colorless Blood red soln No ppt. yellow soln
2-
NVR
White ppt