Course Title: Inorganic Pharmacy sessional-1

Course code: Pharm-1012

SOUTHEASTUNIVERSITY

Department of Pharmacy

Name of the experiment:

Identification of unknown inorganic sample by semi micro qualitative analysis

1. Physical Characteristics of the supplied sample:

I. Color:

II. Odor:

III. Solubility:

IV. Solid sate:

V. Hygroscopic or not:

: Dry test for acid radicals:

Sl. No. / Experiment / Observation / Inference
1
2
3
4
5 / Take a small quantity of the sample in a test tube and 1 cc of conc. H2SO4 and 1 cc of CH3 OH. Mix well by stirring with a glass rod. Heat the test tube and ignites the issuing gas wit the burner flame.
Take a small quantity of the sample in a test tube and 1 ml dilute HCl drop by drop. Warm gently.
Take a small quantity of the sample in a test tube and add 0.5 ml conc. H2 SO4 warm, warm gently.
Add a few piece of copper turnings in a test tube in a test tube of expt. No. 3, heat gently.
Take a small quantity of the sample in a test tube and add MnO2, mix well. Add 0.5 ml of conc. H2SO4, heat gently. Add a little amount of Na- nitroprusside solution. / A green edged flame.
a) A colorless gas evolves which turns lime water milky. (When takes on a glass rod)
b) A color less gas with smell of rotten eggs turn lead acetate paper black.
a) Same as 2a
b) Colorless gas turns blue moist litmas paper red and produce white fumes with ammonium hydroxide taken on a glass rod.
c) Brown vapor
d) Violet vapor
Brown vapor ( Turns blue moist litmas red from white form with ammonia)
a)Evolution of a gas. Turn red moist to yellow color with pungent.
b) Raddish brown vapor turns starch iodine paper blue.
c)Violet vapor turns starch iodine paper blue.
c) A violet coloration / Borate present (BO3-3) Conformity test.
Na2 B4 O7 + H2SO4 + H2 O  H3BO3 + Na2So4.
H3BO4 + CH3 OH 
B(OCH3) + 3 H2O
Burns with green edged flame.
CO3-2 present
Na2 CO3 + HCL = 2NaCl + Cl2 + H2 O
CO3-2 present
Cl-, SCN-, NO3- present
( For conformity test wet test 1,2,4 may be carry out.)
Br- present
I- present
NO3- ( Nitrate) present
Cl- Present
(carry out expt.1 & 2 of wet test)
Br- present
I-present
S- 2 Present

: Wet test for acid radicals:

Preparation of the stock solution for wet test of the acid radicals. Dissolve the sample (0.5 gm) in 15 ml of dist. Water and carry out the following test. (Experiment 1 to 5)

If the sample is not soluble in water, prepare the solution as follows:

Take 0.5 gm of solid sample and mix thoroughly with 5 times its weight of solid Na2CO3. Add 10 ml of water and boil for 15 minutes, cool and dilute to 10 ml and filter. The filtrate will serve as stock solution. Carry out the following experiments for the detection of acid radicals (Experiment 1 to 5)

Sl. No. / Experiment / Observation / Inference
1
2
3
4
5 / Take 1 ml of the solution in a test tube and acidify with dil. HNO3 . Boil off CO2 and add few drops of AgNO3 solution.
Take 1 ml of the solution in a test tube and acidify with dil. Nitric acid. Boil off CO2 ( 0.5 minute) Make the solution just alkaline and add FeCl3 solution drop by drop.
Take 1 ml of the solution and acidify with dil. HCl. Boil off CO2 . Add a few drops of BaCl2.
Ring test: Take 1 ml of the solution and add 2 ml of conc. H2 SO4, cool under tap water to room temperature. Add continuously freshly prepared FeSO4 solution down the side of the test tube without disturbing the whole mass of the solution in the test tube.
Take a small portion of the solution 9 1 ml) in a test tube. Add 3 ml of the HNO3 solution, boil for 1 minute, cool. Add excess NH4 molybdate solution and warm at 600 C if necessary.
If no yellow coloration or ppt, boil for few minutes. / a) white ppt soluble in NH3 solution and reappears on adding HNO3 .
b) Yellow or dirty ppt slightly soluble in NH3 solution.
c) Yellow ppt soluble in NH3 solution.
Blood red coloration.
A heavy white ppt insoluble in acids( Do not use H2 SO4)
A brown ring a t the junction of the two liquids.
a)Yellow ppt.
b) Yellow ppt, appears on boiling / a) Cl-/SCN- present.
Cl- + AgNO3 = AgCl + NO-3
b) Br- present
( AgBr is dirty yellow)
c) I- present
AgI is yellow.
SCN- present
[Fe(SCN)6]-3
( If SCN- is present, then presence of chloride is quantitative)
SO4-2 present
Ba+2 + SO4-2 = BaSO4 ppt
NO-3 present.
NaNO3 +3H2SO4 + 6 FeSO4 =
3 Fe2(SO4)3 = NO + 4H2O
FeSO4 + NO = Fe(NO)SO4 ( brown)
If NO-3 is found to be present, confirm NO-3 is dry test.
a) PO4-3 present
MoHPO4 + 12 ( NH4)2 SO4 + 23HNO3 = (NH4 )3 Pmo12O40 (Yellow) + 2 NaNO3 + 21 NH4NO3 + H2O
b)AsO4-3 present
NaHAsO4 + 12(NH4)2MoO4 + 23 HNO3 = (NH4)3AsMo12O40 ( yellow) + 21 NH4NO3 + 12H2O

: Wet test for basic radicals:

Preparation of the stock solution for wet test of the basic radicals. Dissolve the sample (0.5 gm) in 15 ml of dist. Water and carry out the following test. (Experiment 1 to 5)

Sl. No. / Experiment / Observation / Inference
1
2
3
4. / Take 1 ml of the solution in a test tube and added 1-2 drops ofpotassium pyroantimonate (K2H2Sb2O7) solution.
Take 1 ml of stock solution in a test tube and added 2-3 drops of sodium cobalnitrite, Na3[Co(NO2)6] solution.
a)Take small amount of stock solution in a test tube and added of NaOH solution.Heat the solution and then added neslasr reagent (1-2 drops).
a)Take small amount of stock solution in the test tube and added continuous drop wise NH4OH solution slowly.
b)Take small amount of stock solution in the test tube and added 2-3 drops potassium Ferro cyanide solution. / a)A white ppt of sodium pyroantimonate (Na2H2Sb2O7) is observed.
Reaction:
NaCl + K2H2Sb2O7
= Na2H2Sb2O7 + KCl
white ppt
A yellow color ppt of potassium cobalnitrite K3[Co(NO2)6], is observed.
Reaction:
KNO3 + Na3[Co(NO2)6] =
K3[Co(NO2)6
Yellow ppt
+NaNO3
A brown color ppt is observed.
Reaction:
a)NH4Cl + NaOH = NH3 + NaCl +H2O
b) KHgI3 = KI + HgI2
c) 2HgI2 = Hg2I4
d) Hg2I4 + 2 NH3 =NH2[Hg2I3] +NH4I
At first pale blue color ppt is observed and later tetra ammine copper sulfate concentrated blue color solution is produced.
Reaction:
a)2 CuSO4 + NH4OH = CuSO4.Cu(OH)2 +
blue ppt
(NH4)2 SO4
b)
CuSO4.Cu(OH)2 +
(NH4)2 SO4 +NH4OH = [ Cu(NH3)4]SO4 +H2O
Cupric Ferro cyanide brown ppt is observed.
Reaction:
2CuSO4 + K4[Fe(CN)6] =
Cu2[Fe(CN)6] +K2SO4
Brown ppt / a) Na+ ion present.
K+ ion present.
.
NH4 + ion present.
Cu2+ ion present.
Cu2+ ion present