Detection of the Acid Constituent

10-6 Determine the Group which the acid constituent belongs as follows:
a) To 1ml of the sample, add 1-2 drops of 1M AgNO
3
if a precipitate is formed, add 10 drops N
HNO
3.
If the precipitate does not dissolve, try boiling the mixture for 1 minute.
b) Repeat 10-6 using 1M BaCl
2
instead of AgNO
3
.
From the results obtained in 10-6a and 10-6b, establish the group to which the acid constituent
belongs, as described according to the table for Classification Anions into Groups on Page 34
10-7 If 10-6 produced a precipitate that is insoluble in 6 M HNO
3
, but no precipitate with BaCl
2,
GROUP 1
is present.
a) If the precipitate is orange, Ferricyanide is indicated. To 1 mL of the sample, add 1-2 drops of
FeSO
4
. Blue precipitate confirms FERRICYANIDE.
b) If the precipitate is yellow; Bromide and Iodide are indicated.
To 1 mL of the sample, add 1 mL of CHCl
3
(or CH
2
Cl
2
), 10 drops of 6 M HNO
3
and KMnO
4
a drop at a
time until the aqueous solution has acquired a pink coloration, then shake. A reddish brown
chloroform (or dichloroformethane) layer proves BROMIDE; while a violet layer confirms IODIDE.
c) If the precipitate is white; Chloride, Cyanide, Ferrocyanide, Thiocyanate Hypochlorite are
indicated. Confirmation of anion is done by elimination process.
(1) To 1 mL of the sample, add 1-2 drops of FeCl
3
; a blue coloration confirms FERROCYANIDE; while
a blood red colorization confirms THIOCYANATE.
(2) To 1 mL of the sample, add 6 M CH
3
COOH, a drop at a time until the solution is acidic then add 1
mL of Pb(CH
3
COO)
2,
heat the mixture and let it stand for 5 minutes. Brown precipitate shows
HYPOCHLORITE
(3) To 1 mL of the sample, add 1 M NaOH until alkaline then add a few drops of FeSO
4
, 1 drops of
FeCl
3
and heat the mixture to boiling. Allow to cool and acidify with HCL. A blue precipitate
proves CYANIDE.
(4) If all of the above tests are negative add Hg
2
(NO
3
)
2
in C-(3). White precipitate shows CHLORIDE.
10-8 If the AgNO
3
in 10-6 produced a precipitate soluble in HNO
3
while BaCl
2
also produced a
precipitate, GROUP II is present.
a) If the precipitate is black, Sulfide is indicated. Acidify 1 mL of the sample with 6 M HCL, evolution
of H
2
S gas which blackens Pb(CH
3
COO)
2
paper confirms SULFIDE.
b) If the precipitate is white rapidly changing to brown or black, Hypophosphite is indicated. To
1mL of the sample, add 1 mL of the sample, add 1 mL of 6 M NaOH. Boil the mixture for 1
minute, acidify strongly with HNO
3
and (NH
4
)
2
MoO
4
and heat the mixture. Yellow confirms
HYPOPHOSPHITE.
c) If the precipitate is white, Nitrate and Acetate are indicated.
Treat 1 mL of the sample with 3 M H
2
SO
4
, allow the mixture to stand. Evolution of brown gas
confirms NITRITE.
d) Treat 1 mL of the sample with 1 mL of concentration H
2
SO
4
, add 5 drops of C
2
H
5
OH and warm
the mixture. Evolution of a gas with a fruity odor confirms ACETATE.
10-9 If the AgNO
3
has produced a white precipitate soluble in HNO
3
and BaCl
2
has produced a
precipitate also soluble in HNO
3
, GROUP III is present.
a) Acidify 1 mL of the sample with HCl, if SO
2
gas is evolved and the solution remains clear, Sulfite
is indicated. To 1 mL of the sample, add 3-5 drops of BaCl
2
and a few drops of HCl to re-dissolve
the precipitate. Filter if the precipitate is not completely dissolved. To the solution filtrate, add
1 mL of bromine water and boil the mixture for 1-2 minutes. White precipitate confirms
SULFITE.
b) If effervescence is produced in (a), but the gas evolved is odourless, expose a lime water to the
issuing gas. White precipitate in the lime water indicates CARBONATE.
c) To 1 mL of the sample in an evaporating dish, add 1 mL of concentrated H
2
SO
4
and 3 mL of
CH
3
OH; stir the mixture and then set it on fire. Green Flame coloration confirms BORATE.
d) To 1 mL of the sample, add CaCl
2
until precipitation is complete, then acidify the mixture with 6
M CH
3
COOH. White precipitation insoluble in CH
3
COOH confirms OXALATE.
e) If the precipitate produced in (d) is soluble in CH
3
COOH, Tartrate is indicated. To 1 mL of the
sample, add CH
3
COOH and acidify the mixture with CH
3
COOH. White crystalline precipitate
confirms TARTRATE.
f) If the CaCl
2
in (d) has produced no precipitate, without adding 6M CH
3
COOH, boil mixture gently
for 1-2 minutes. White precipitate shows CITRATE.
10-10 If the AgNO
3
has produced a colored precipitate soluble in HNO
3
and BaCl
2
has produced a
white colored precipitate soluble in HNO
3
, GROUP IV is present.
a) If the precipitate with AgNO
3
is reddish brown, Arsenate and Chromate are indicated. To 1 mL of
the sample, add drops of concentrated HCl, 5 drops of KI and 2-3 drops of starch solution. Blue
coloration indicates ARSENATE.
b) To 1mL of the sample, add a few drops of Pb(CH
3
COO)
2.
Yellow precipitate proves CHROMATE.
c) If AgNO
3
produced yellow precipitate, Phosphate and Arsenite are indicated.
To 1 mL of the sample, add 10 drops of NH
4
Cl, 1 mL of Magnesia mixture and an excess of
NH
4
OH. Allow the mixture to stand 10 minutes. White Crystalline precipitate shows PHOSPHATE.
d) Acidify 1 mL of the sample with HCl and pass H
2
S. Yellow precipitate shows ARSENITE.
e) If the AgNO
3
has produced a white precipitate readily turning black, thiosulfate is indicated. To 1
mL of the sample, add few drops of Iodine Solution. Immediate discoloration of the Iodine
Solution proves THIOSULFATE.
10-11 If no precipitate was produced with AgNO
3
while BaCl
2,
GROUP V is indicated.
a) To 1 mL of the sample, add 1 mL of concentrated H
2
SO
4
and copper wire, then warm the mixture
gently. Evolution of brown gas confirms NITRATE.


b) To 1 mL of the sample, add 2-3 drops of KNO
2
and acidify the mixture with HNO
3
. White
precipitate shows CHLORATE.
10-12 No precipitate with AgNO
3
while BaCl
2
produced a white precipitate insoluble in HNO
3

indicates GROUP VI is present.
a) To 1 mL of the sample, add a few drops of Pb(CH
3
COO)
2
and 1-2 mL of NH
4
CH
3
COO solution,
then warm the mixture. A white precipitate soluble in the NH
4
CH
3
COO confirms SULFATE.
b) To 1 mL of the sample, add several drops of CaCl
2
. White slimy precipitate difficulty soluble in
HCl and HNO
3
but soluble in CH
3
COOH shows FLUORIDE.