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Tim Unknown Analysis 5

The document provides instructions for analyzing two unknown samples (5A and 5B) to identify what ions are present. It describes preparing necessary solutions and outlines a testing process including flame tests, pH tests, and tests using reagents to identify specific cations and anions. The process will determine if ions such as Na+, K+, NH4+, Ca2+, Mg2+, Al3+, Cl-, NO3-, SO42-, HSO4-, OH-, CO32-, or HCO3- are present, as well as any insoluble compounds like Ca(OH)2, CaCO3, or Mg(OH)2. The results of the analyses will be recorded on tables provided for samples 5A and 5B.

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550 views5 pages

Tim Unknown Analysis 5

The document provides instructions for analyzing two unknown samples (5A and 5B) to identify what ions are present. It describes preparing necessary solutions and outlines a testing process including flame tests, pH tests, and tests using reagents to identify specific cations and anions. The process will determine if ions such as Na+, K+, NH4+, Ca2+, Mg2+, Al3+, Cl-, NO3-, SO42-, HSO4-, OH-, CO32-, or HCO3- are present, as well as any insoluble compounds like Ca(OH)2, CaCO3, or Mg(OH)2. The results of the analyses will be recorded on tables provided for samples 5A and 5B.

Uploaded by

Blake Freda
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© Attribution Non-Commercial (BY-NC)
We take content rights seriously. If you suspect this is your content, claim it here.
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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

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