Mohammad Ismail

BSPh3B

EXPERIMENT 9
ANALYSIS OF AN ANION OF A SOLUTION
CONTAINING ONLY ONE INORGANIC
COMPOUND

PROCEDURE:
Detection of Acid Constituents:
1. Determine the group in which the acid
constituents belong.

A. 1mL original sample + 1-2 drops silver
nitrate = precipitate + 10 drops 6N HNO
3
= dissolve precipitate (if not dissolve, try
boiling the mixture for 1min.)

B. Repeat Step 1-A using BaCl
2
. From the
results from Step 1-A and 1-B,
establish the group in which the acid
constituents belong, as described under
the classification.

2. Silver nitrate produced precipitate,
insoluble in HNO
3
, BaCl
2
produced no
precipitate: GROUP I is present.

A. Orange precipitate: FERRICYANIDE
1mL original sample + 1-2 drops ferrous
sulfate
Blue precipitate: FERROCYANIDE

B. Yellow precipitate: BROMIDE or
IODIDE
1mL original sample + 1mL chloroform
+10 drops 6N HNO
3
+ a drop at a time
of potassium permanganate (until
solution acquired pink coloration) +
shake
Orange to brownish-red in the
chloroform layer: BROMIDE
Violet color in the chloroform layer:
IODIDE

C. White ppt: CHLORIDE, CYANIDE,
FERROCYANIDE, THIOCYANATE,
and HYPOCHLORITE
a. 1mL original sample + 1-2 drops Ferric
chloride.
Blue coloration: FERROCYANIDE
Blood-red coloration: THIOCYANATE
b. 1mL original sample + 6N acetic acid (a
drop at a time for acidic solution) + 1mL
lead acetate + heat mixture + stand for 5
min
Brown precipitate: HYPOCHLORITE
c. 1mL original sample + 6N NaOH
(alkaline) + few drops of ferrous sulfate
+ 1 drop ferric chloride + heat to boiling
+ cool + acidify with HCl
Blue precipitate: CYANIDE
d. All of the above tests negative = add
mercurous nitrate solution in STEP C-c
White precipitate: CHLORIDE


3. Silver nitrate produced a precipitate,
soluble in HNO
3
, BaCl
2
produced no
precipitate: GROUP II is present.

A. Black precipitate: SULFIDE
1mL original sample + HCl (acidify)
Evolution of H
2
S gas: SULFIDE
1mL original sample + few drops of lead
acetate
Black precipitate: SULFIDE

B. White precipitate, rapidly changing to
brown or black: HYPOPHOSPHITE
1mL original sample + 1mL 6N NaOH +
boil for 1min + HNO
3
and ammonium
molybdate (acidify strongly) + heat
Yellow precipitate: HYPOPHOSPHITE

C. White ppt: NITRITE and ACETATE
1mL original sample + dilute H
2
SO
4
+
stand the mixture
Brown gasses: NITRITE

D. 1mL original sample + 1mL conc. H
2
SO
4

+ 5 drops ethyl alcohol + warm mixture
Evolution of gas with fruity odor:
ACETATE

4. Silver nitrate produced white precipitate,
soluble in HNO
3
, BaCl
2
produced a
precipitate also soluble in HNO
3
:
GROUP III is present.

A. 1mL original sample + HCl (acidify)
SO
2
produced and solution remains
clear: SULFITE
1mL original sample + 3-5 drops BaCl
2
+
drop of HCl (redissolve the precipitate)
or filter (not completely dissolve
precipitate) = filtrate + 1ml bromine
water + boil for 1-2 min
White precipitate: SULFITE

B. Effervescence produced in Step 4-A,
gas evolved is odorless + expose a drop
of limewater in the stirring rod to the
issuing gas
White precipitate in the limewater:
CARBONATE

C. 1mL original sample (evaporating dish)
+ 1mL conc. H
2
SO
4
+ 3 mL methyl
alcohol + stir mixture + light the alcohol
Green flame: BORATE

D. 1mL original sample + CaCl
2

(precipitation complete) + acetic acid
(acidify)
White precipitate insoluble in acetic
acid: OXALATE

E. Precipitate produced in Step 4-D,
soluble in acetic acid: TARTRATE
1mL original sample + potassium
acetate + acetic acid (acidify)
White crystalline precipitate:
TARTRATE

F. CaCl
2
produced no precipitate in Step 4-
D, without adding acetic acid + boil for
1-2 min
White precipitate: CITRATE

5. Silver nitrate produced colored
precipitate, soluble in HNO
3
, BaCl
2

precipitate (colored or white) also
soluble in HNO
3
: GROUP IV is present.

A. Reddish-brown silver nitrate precipitate:
ARSENATE and CHROMATE
1mL original sample + 5 drops conc.
HCl + 5 drops KI + 2-3 drops starch
solution
Blue coloration: ARSENATE

B. 1mL original sample + few drops lead
acetate
Yellow precipitate: CHROMATE

C. Yellow silver nitrate precipitate:
PHOSPHATE and ARSENITE
1mL original sample + 10 drops NH
4
Cl +
1mL magnesia mixture + excess NH
4
OH
+ stand for 10 min
White crystalline ppt: PHOSPHATE

D. 1mL original sample + HCl (acidify) +
saturate with 10% thioacetamide
solution
Yellow precipitate: ARSENITE

E. White silver nitrate precipitate rapidly
turning black: THIOSULFATE
1mL original sample + few drops iodine
Iodine sol. decolorized: THIOSULFATE

6. Silver nitrate and BaCl
2
produced no
precipitate: GROUP V is present

A. 1mL original sample + 1mL conc. H
2
SO
4

+ copper wire + warm the mixture
Evolution of brown gas: NITRATE

B. 1mL original sample + 2-3 drops KNO
2

and AgNO
3
+ HNO
3
(acidify)
White precipitate: CHLORATE

7. Silver nitrate produced no precipitate,
BaCl
2
produced white precipitate
insoluble in HNO
3
: GROUP VI is
present.

A. 1mL original sample + few drops lead
acetate + 1-2 mL ammonium acetate
solution + warm mixture
White precipitate soluble in ammonium
acetate solution: SULFATE

B. 1mL original sample + several drops
CaCl
2

White, slimmy precipitate difficult to
dissolve in HCl and HNO
3
but soluble in
acetic acid: FLOURIDE