Group 4: TORRES, VILLANUEVA, VILLARETE PhCh121-1 : UNKNOWN

I. Preliminary Tests A. Reaction to litmus paper Red litmus paper Blue litmus paper B. Flame test Wire cleansed with HCl C. Residue upon Evaporation Not performed D. Reactions with the precipitants 1. Diluted hydrochloric acid + Unknown + Diluted hydrochloric acid = Clear colorless solution Absence of 2+ 2+ + Pb , Hg2 , Ag ions + UNKNOWN + + Drops of test solution to the litmus paper Drops of test solution to the litmus paper No change in color of = red litmus paper = Litmus paper turns red = ORANGE FLAME Sample is ACIDIC

2. Ammonium sulfide TS + Unknown Ammonium sulfide TS

Not performed due to lack of Ammonium sulfide TS

3. Diluted sulfuric acid Unknown + Diluted sulfuric acid = Clear colorless solution Absence of Group 2 Cation

4. Silver nitrate TS Unknown + Silver nitrate TS = White, curdy precipitate Presence of Cl , SCN
-

5. Barium chloride TS Unknown + Barium chloride TS = White precipitate Presence of SO4 group
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II. Confirmatory Tests Because of the absence of Ammonium Sulfide TS, which is very important for the identification of the unknown, we just proceed to the confirmatory tests. Since our unknown is negative with dil. HCL and dil. H2SO4, therefore, it is possible that our unknown is not lead II, mercury II, silver I, and not group 2 cations. We are left with group 3, 4 and 5 cations particularly Bi , As , As , Sb , Sb , Sn , Fe , Al , Cr . Some group 1 cations were also left which includes K , Na and NH4 .
3+ + + + 3+ 3+ 5+ 3+ 5+ 4+ 3+ 3+

Here are our added procedures for the confirmatory test for cations: UNKNOWN + This indicates the absence of Bi gelatinous precipitate), Fe precipitate). Clear, colorless solution Red litmus paper turns to blue; pungent odor Ammonium ion is present
3+ 3+

NaOH TS =

Clear, colorless solution (white precipitate), Sb

3+ 3+

(white precipitate), Sn
3+

4+

(white

reddish brown precipitate, Al

(white precipitate), Cr (grey green

UNKNOWN

AgNO3 TS

Clear, colorless solution

Absence of As , 5+ As

3+

The cation of our unknown is NH4 . Sb

+

5+

was not tested due to the absence of H2S. The flame

+

test result was colored orange, so it is not Na or K . The confirmatory tests for the anions were done as followed: Precipitate dissolves White, curdy precipitate + NH3 TS = POSITIVE for Cl White, curdy precipitate White, curdy precipitate + HNO3 = Precipitate is undissolved + HCl = Yellow solution NEGATIV E for SCN
-

+ FeCl3

Blood red solution

White precipitate

HNO
3

Precipitate is undissolved POSITIVE for SO4

2-

White precipitate

HCl

Precipitate is undissolved

The presence of a white curdy precipitate indicated that there is a strong possibility that the unknown contained Cl , and testing the solubility of the precipitate with ammonia and nitric acid proved that there is indeed Cl in the unknown. Since the precipitate was white in color, there is a possibility of a mixture of AgCl and AgSCN. Confirmatory test was done for SCN , but the blood red solution with FeCl3 turned yellow with the addition of HCl, indicating that the test was negative for SCN (USP CI, 2007). The white precipitate with BaCl2 TS was undissolved with HNO3 and HCl, indicating that the precipitate formed was most likely BaSO4, and proving that there are SO4 ions in the unknown. (USP CI, 2007) In conclusion, the unknown of the group is composed of compound such as NH 4Cl and (NH4)2SO4.
2-

References SVEHLA, G., 1996. Vogels Qualitative Inorganic Analysis. 7 edition. England: Longman Group Limited,
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UNITED STATES PHARMACOPOEIAL CONVENTION, INC.2007. United States Pharnacopoeia 30 Revision and the National Formulary 25 Edition [CD-ROM]. USP Convention, Rockville, Maryland.
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