OFFICIAL REPORT OF CHEMISTRY FUNDAMENTAL

PRACTICE ANALYTIC
Anion and Cation Analysis

By :
Putri Nurjihan Najla
21030194079
PKU21

CHEMICAL
STUDY MAJOR
CHEMISTRY
FACULTY OF MATH AND SCIENCE
UNIVERSITY STATE OF SURABAYA
2022

1
 CHAPTER I
PRELIMINARY

1.1 Background Behind

In the precipitation reaction a lot of quantitative analysis is applied. In the analysis, the cations
are first separated based on the ratio of the solubility of the compounds. The soluble cations that
form the same precipitate with sufficiently different solubilities can be separated by selective
precipitation carried out with careful selection of the required anion concentration. Quantitative
analysis is a process to determine the presence or absence of cations or anions in a solution.
Examples of cations are the ions Al 3+ , H + , K + , while examples of anions are SO 4 - 2, NH 4 - , Cl -
. Identification of cations and anions is done so that we can identify the types of cations and anions
that make up something and observe whether a precipitate is formed or not. Qualitative analysis is
concerned with determining how much of a certain substance is contained in a sample. The
specified substance is expressed as the analyte (A.L, 2001). Anions are ions that have a negative
charge and are attracted to the anode (positive electrode) while cations are ions that are positively
charged and attracted to the cathode (negative electrode) during electrolysis. Specific tests are
carried out by adding certain reagents that will give color to the solution or there is a precipitate
which is characteristic for certain ions (Amin, 2016).
1.2 Destination

1. Determine the cations present in the analyte.

2. Determine the anions present in the analyte.

1.3 Formulation of the problem

1. Can determine the cations present in the analyte.

2. Can determine the anions contained in the analyte

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 CHAPTER II
LITERATURE REVIEW

2.1 Definition

Many dissolved ions that we encounter around us, for example in sea water, rivers,
sewage, or also in solid form such as in soil and fertilizers. Metal elements in solution will
form positive ions or cations, while non-metal elements will form negative ions or anions. The
method used to ascertain the presence of these cations and anions in chemistry is called
qualitative analysis. For inorganic compounds called inorganic qualitative analysis. Qualitative
analysis based on chemical properties involves some chemical reactions such as acid-base
reactions, redox, complex, and precipitation. The law of mass balance is very useful for
determining which direction a reaction is going.
Cations and anions are ions that have a positive and negative charge. systematic
qualitative analysis cations are classified into 5 groups based on the properties of the cations to
some of the reagents. By using the so-called group reagents systematically, we can determine
the presence or absence of cation groups, and can also separate these groups for further
examination.
Cations are ions that are positively charged for the purpose of systematic qualitative
analysis. cations are classified into 5 groups based on their properties. The group reagents used
for the classification of very common cations are hydrochloric acid, hydrogen sulfide,
ammonium sulfide, and ammonium carbonate. This classification is based on whether a cation
reacts with the reagents to form a precipitate or not.
Anion is an ion/group that has a negative charge. The reaction in the anion is used to
facilitate the reaction of organic acids. Anions are broken down into 3 groups, sulfate groups:
SO 4 2- , SO 3 2- , PO 4 3- , Cr 2 O 4 2- , BO 2- , CO 3 2- , C 2 O 4 2- , AsO 4 3 - , halide group: Cl – , Br –
, I – , S 2- and nitrate group: NO 3 – , NO 2– , C 2 H 3 O 2– . Salts BaSO 4 , BaSO 3 , Ba 2 ( PO 4 ) 3,
BaCr 2 O 4 , Ba( BO 2 ) 2, BaCO 3 , BaC 2 O 4 , Ba 3 ( AsO 4 ) 2 are insoluble in water in an
alkaline state, on the other hand Other anionized barium salts are readily soluble.
The method in conducting this qualitative analysis is done conventionally, namely
using a visual method based on solubility. Solubility test is carried out first by grouping ions
that have similar properties. The grouping is carried out in the form of precipitation in which
the addition of certain reagents is able to precipitate a group of ions. This method produces 6
groups whose names are adjusted to the precipitating reagent used to precipitate these ionic
groups. The groups of these ions are: chloride group (I), sulfide group (II), hydroxide group
(III), sulfide group (IV), carbonate group (V), and residual group (VI) (Anonim, 2010). In this
qualitative analysis method, we use several reagents including group reagents and specific
reagents, these two reagents are carried out to determine the type of anion / cation. Anion
analysis is not much different from cation analysis, it's just that anion analysis does not have a
standard systematic analysis method such as cation analysis. Initial preliminary tests on anion

3
analysis are also based on physical properties such as color, odor, gas formation, and solubility.
Some anions produce weak volatile acids or are oxidized with concentrated sulfuric acid. To
make it easier to analyze the anion, it is first attempted in the form of a compound that is easily
soluble in water. Generally, sodium salts are easily soluble in carbonate salts of heavy metals
and are difficult to dissolve in water, so that if the substance to be analyzed is a substance that
is difficult to dissolve or give a precipitate with Na 2 CO 3 , then it is made first in the form of
soda extract, then separated from the disturbing precipitate (Widiarto, 2011). To facilitate the
identification of cations and anions, a systematic qualitative analysis method is used. This
method is a classification of cations into 5 groups. The five groups of cations and the
characteristics of this group are as follows: a. Group I, cations of this group form precipitates
with dilute hydrochloric acid. The ions of this group are Lead, Mercury (I) (mercury), and
silver. b. Group II, the cations of this group do not react with hydrochloric acid, but form
precipitates with hydrogen sulfide in dilute mineral acids. The ions of this group are mercury
(II), copper, bismuth, cadmium, arsenic (III), arsenic (V) , stibium (III), stibium (V), tin (II),
and tin (III) (IV).c. Group III cations of this group do not react with dilute hydrochloric acid,
nor with hydrogen sulfide in dilute conditions. However, these cations form precipitates with
ammonium sulphide in neutral or amonical conditions. The cations of this group are cobalt (II),
nickel (II), iron (II), iron (III), chromium (III), aluminum, zinc and manganese (II). d. Group
IV, cations of this group do not react with group I, II, and III reagents. These cations form
precipitates with ammonium carbonate in the presence of ammonium chloride, in neutral or
slightly acidic conditions. The cations of this group are: calcium, strontium, and barium.e.
Group V, the common cations, which do not react with the reagents of the previous group, are
the last group, which includes magnesium, sodium, potassium, ammonium, lithium, and
hydrogen ions.

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 CHAPTER III
RESEARCH METHODOLOGY

3.1 Tools
- 20 test tubes
- 1 test tube rack
- 20 drop pipettes
- 1 glass beaker
- Centrifuge 1 piece
- Hose 1 piece
- 1 piece of filter paper
- 1 piece of Pt/Ni-Cr wire
- Spirit burner 1 piece

3.2 Ingredient
a. Group I
- 6M . HCl solution
- Dilute HCl solution
- 6M . CH3COOH solution
- K2CrO4 . solution
- 0.5ml 6M . ammonium hydroxide
b. Group II
- 3% H2O2 solution
- H2S . gas
- Saturated Hydrogen Solution
- Dilute nitric acid (HNO3) solution
- Concentrated NH3 solution
- Aquades
- 1M . NaOCl Solution
- Dilute HCl solution
- SnCl2 . solution
- NH3 . solution
- NaOH solution
- Dilute CH3COOH solution
- Na-Stannit reagent
- Ammoniacal solution
- K2CrO4 . solution
- Potassium ferrocyanide solution
- CH3COOH . solution
- KCN solution
- HCl Larutan solution

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 - Dilute HCl solution
- Dilute NH3 solution
- Mg(NO3)2 . solution
- Oxalic acid solution
- NaNO3 . small crystal
- Rhodamine B . indicator
- 20mg iron filings
- HgCl2 . solution
- 5-10 g Mg powder
- FeCl3 . solution
- 5% tartaric acid solution
- Dimethyl glyoxin indicator
c. Group III
- H2S . gas
- HNO3 . solution
- 20% NH4Cl solution
- Concentrated NH3 solution
- Dilute NH3 solution
- NaOH solution
- 2% NH4NO3 solution
- Dilute HNO3 solution
- 3% H2O2 solution
- Saturated H2SO3 solution
- K4Fe(CN)6 solution or KSCN . solution
- Aquades
- 10 mg NaBiO3
- Dilute CH3COOH solution
- Pb(CH3COO)2 . solution
- Dilute HCl solution
- 1M . HCl solution
- 1M . NaOCl Solution
- Amyl alcohol indicator
- 50 mg solid NH4SCN
- NH4Cl . solution
- NH4OH . solution
- Concentrated HNO3 solution
- 250 mg PbO2
d. Group VI
- 20% NH4Cl solution
- 6M . NH4OH solution
- Solution (NH4)2CO3
- Aquades

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 - CH3COOH . solution
- K2CrO4 . solution
- 6M . HCl solution
- Pt/Ni-Cr . Wire
- Ethyl alcohol
- Solution (NH4)2SO4
- 6M . HCl solution
- Dilute NH4OH solution
- Ammonium oxalate solution
- NA2HPO4 . solution
e. Group V
- 6M . NaOH solution
- NA2HPO4 . solution
- Concentrated HNO3 solution
- 6M . CH3COOH solution
- Sodium cobalt nitrite solution
- Uracil acetate solution
- NaOH solution
- red litmus

3.3 Trial Procedure

Carry out a preliminary analysis of the analyte that Mr. Obtain, observe and
record all observations obtained. Determine the appropriate solvent for the analyte to be
analyzed. Work systematically, completing the analysis of each cation in one group
until it is complete according to the steps of each group. Leave the analyte to identify
the presence of NH 4 + cations and for anion analysis. Perform a flame test for several
cations that will give a characteristic color.

CATION ANALYSIS IN GENERAL

First Add a few drops of dilute hydrochloric acid (6M) to the solution. If a
precipitate occurs, add another 1-2 drops of dilute hydrochloric acid. Centrifuge and
wash the precipitate with a few drops of aquadest. Both precipitates contain group I
cations which can consist of Hg 2 Cl 2 , AgCl, or PbCl 2 (all white). All three filtrates
may contain group II, III, IV, or V cations. Add 4 drops of 3% hydrogen peroxide
solution. Make the concentration of H + ions about 0.3 M. Check with a universal
indicator. Heat in a water bath for 2-3 minutes, then run off hydrogen sulfide gas.
Centrifuge and wash the precipitate with ammonium nitrate solution (1 g in 2 mL and
flush with hydrogen sulfide gas). The four group II deposits can consist of HgS (black),
Bi 2 S 3 (black/brown), CuS (black), CdS (yellow), SnS 2 (yellow), SbS 3 (orange), As 2
S 3 (yellow). The five filtrates contain group III, IV, and V cations. Boil the analyte

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solution to remove hydrogen sulfide gas. Add 3 drops of concentrated nitric acid and
bring to a boil again, then add 50-100 mg ammonium chloride or 0.25-0.5 mL 20%
ammonium chloride solution. Heat on a water bath. Add concentrated ammonium until
it becomes alkaline. Place the tube in a water bath for 2-3 minutes. Centrifuge and wash
the precipitate with hot water or a 2% ammonium nitrate solution. The six precipitates
contain group IIIA which can consist of Fe(OH) 3 (brown), Cr(OH) 3 (green), Al(OH) 3
(white), or MnO 2 .xH 2 O (brown). The seven filtrates may contain group IIIB, IV and
V cations. Add 1-2 drops of dilute NH3 solution . Heat and flow with hydrogen sulfide
gas for 1 minute. Centrifuge and wash the precipitate with 1% ammonium chloride
solution which has been added with 1% ammonium sulfide. The eight group IIIB
deposits can consist of CoS (black), NiS (black), MnS (pink), ZnS (white). The nine
filtrates may contain group IV or V. Acidify with acetic acid, evaporate to a paste, cool
and add 5-10 drops of concentrated nitric acid. Carefully heat, add 5 drops of dilute
hydrochloric acid and 0.5 mL of water. Transfer the clear solution to a centrifuge tube.
Add 25 mg solid ammonium chloride or 0.25 mL 20% ammonium chloride and
concentrated NH 3 until alkaline. Add 0.3 mL of ammonium carbonate solution, place
on a 50-60oC water bath and stir the mixture well. Centrifuge and wash the precipitate
with a few drops of hot distilled water. The ten group IV precipitates may consist of
BaCO 3 (white), SrCO 3 (white), CaCO 3 (white). The eleven filtrates contain group V
cations, namely K + , Na + , Mg 2+ , NH 4 + . Finally, the NH 4 + cation is examined for its
original substance by adding a NaOH solution. The resulting NH 3 vapor will turn wet
litmus paper blue and form a white mist with concentrated HCl. After finding the group
in question, do the analysis according to the cation of the group.

CATION ANALYSIS GROUP I

First Add a few drops of 6 M HCl to a solution containing group I cations. If a

precipitate occurs, add another 1-2 drops of dilute HCl. Centrifuge and wash the
precipitate. Both precipitates contain group I cations. Heat the mixture (precipitate and
filtrate) in a boiling water bath for about 1 minute. Centrifuge, separate the precipitate
and the filtrate. The third filtrate contains PbCl 2 which is soluble in hot water. Add 2
drops of 6M acetic acid solution and 1 drop of potassium chromate solution. The
yellow precipitate that occurs (PbCrO 4 ) indicates the presence of Pb. The four
precipitates were dissolved in 0.5 mL of 6M ammonium hydroxide, heated (until
boiling), stirred, centrifuged. A black precipitate from a mixture of Hg and Hg(NH 2 )Cl
indicates the presence of Hg(I). The last five filtrate (no. 4) contains Ag(NH 3 ) 2 + . Add
dilute HCl or HNO 3 until the solution is acidic. A white precipitate of AgCl indicates
the presence of Ag + .

CATION ANALYSIS GROUP II

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 First, the solution containing group II cations or the filtrate resulting from group
I precipitation is added with 4 drops of 3% hydrogen peroxide solution. Make a
concentration of [H+] about 0.3 M. Heat in a water bath for 2-3 minutes. Flow H 2 S
gas. Centrifuge and wash the precipitate. The two group II deposits can consist of group
IIA (HgS, PbS, Bi 2 S 3 , CuS, da CdS) or group IIB (SnS, Sb 2 S 3 , and AsS 3 ). Add 4
drops of freshly made saturated hydrogen sulfide, centrifuge and wash the precipitate
with water. All three deposits contain group IIA. While the filtrate contains group IIB.
Add 1-1.5mL of dilute nitric acid to the Group IIA precipitate, place it in a water bath
for 1-3 minutes while stirring. Centrifuge and wash the precipitate with 0.5 mL of water
and discard the washing water. The four black precipitates indicate the presence of
HgS. Add 5 drops of 1M NaOCl solution and 1 drop of dilute HCl. Heat in a water bath
for 1 minute. Add 1-2 drops of SnCl 2 to the clear solution. A white precipitate that
turns gray/black indicates the presence of Hg(II). The five filtrates (no. 3) can contain
Pb 2+ , Bi + , Cu 2+ , and Cd 2+ cations, then added with an excess of concentrated NH 3 solution.
Centrifuge and separate the precipitate. The six precipitates may contain Bi(OH) 3 , or
Pb(OH) 2 . Add 1 mL of NaOH solution, place on a water bath for 2 minutes.
Centrifuge and separate the precipitate from the filtrate. The seventh deposit that occurs
is Bi 2 S 3 . Wash with 5 mL of water and discard the washing water. Add 1 mL of Na -
Stannit reagent (1-2 mL of SnCl 2+ NaOH solution dropwise until the precipitate
Sn(OH) 2 dissolves. The color change of the precipitate to black indicates the presence
of Bi(III). Furthermore, the filtrate (no. 6) contains Pb(OH) 4 2+ was acidified with
dilute acetic acid, then 2 drops of potassium chromate solution were added. A yellow
precipitate of PbCrO 4 indicated the presence of Pb(II). The nine filtrates (no. 5)
contained Cu(NH 3 ) 4 2+ or Cd(NH 3 ) 4 2+ If no blue color means no Cu. Stream H 2 S
gas for 10 seconds in ammoniacal solution. A yellow precipitate of CdS indicates the
presence of Cd(II). If the solution is blue, the filtrate is divided into two. The first part
is acidified with acetic acid and a drop of potassium ferrocyanide solution is added. A
reddish brown precipitate indicates the presence of Cu(II). The second part is dripped
with KCN while stirring until the blue color disappears. Flow H 2 S gas for 30-40
seconds. CdS yellow precipitate indicates the presence of Cd(II).The ten filtrates
containing the cation go longan IIB can contain AsO 3 2- , AsS 3- , SbO 2- , SbS 3 2- ,
Sn(OH) 2 - , SnS 3 2- , and a small amount of Hg 2 2- . Add HCl into the filtrate dropwise
until the solution is acidic, then flow H2S gas for 30-60 seconds. The precipitate indicates
the presence of group IIB cations. Wash the precipitate with water. Add 0.5-1 mL of
concentrated HCl, place in a water bath for 2-3 minutes. Centrifuge and wash the
precipitate with 0.5 mL dilute HCl. Mix the washing water into the filtrate. Then wash
the sediment with water, discard the washing water. Add 0.5 mL of dilute NH3, stir and
centrifuge. Separate the precipitate and the filtrate. Twelfth If the precipitate (no. 11) is
dark in color it indicates the presence of HgS. Confirmation test is the same as no. 4.
Then add dilute HNO3 to the filtrate (no. 11) until it is acidic. As2S3 yellow precipitate
indicates the presence of As(III). Dissolve the precipitate in 0.5 mL of hot dilute NH3.
Add 0.5 mL of 3% H2O2 and heat on a water bath for 3 minutes. Add 4 drops of

9
Mg(NO3)2. There was a white precipitate of Mg(NH4)AsO4. Centrifuge and discard
the filtrate. Add 2 drops of AgNO3 and 1 drop of dilute acetic acid. A reddish brown
precipitate indicates the presence of As(III). Finally, the filtrate (no.10) contains Sb3+
and Sn4+ divided by two. The first part is added with NH3 until just alkaline, then add
oxalic acid, and flow H2S gas for 20-30 seconds. An orange precipitate indicates the
presence of Sb(III). Confirmation of the presence of Sb(III) can also be done by adding
small crystals of NaNO3 and 2 drops of Rhomanine B to 2 drops of the solution. The
purple color indicates the presence of Sb(III). The second part can be tested in two
ways as well. The first method, put 2 cm of iron wire or 20 mg of iron file into the
solution, heat it in a water bath for 3-5 minutes. Add 2 drops of HgCl2 solution to the
clear solution. A white precipitate of Hg2Cl2 indicates the presence of Sn(IV). The
second method is to add 5-10 mg of Mg powder, 2 drops of FeCl3, 2-3 drops of 5%
tartaric acid solution, 2 drops of dimethyl glyoxin, then alkaline with dilute NH3. The
red color indicates the presence of Sn(IV).

CATION ANALYSIS GROUP III

First, the solution contains group III cations and the remaining group II is boiled
until the H2S gas disappears. Add 3 drops of concentrated HNO3 and bring to a boil
again. Add 1 drop of 20% NH4Cl, heat on a water bath. Add concentrated NH3 until it
is basic. Place the tube in a water bath for 2-3 minutes. Centrifuge and wash the
precipitate. Separate the precipitate and the filtrate. Second Wash the precipitate (no.1)
with dilute NH3 and discard the washing water. The precipitate is group IIIA which
may contain Fe(OH)3, Cr(OH)3, Al(OH)3, or MnO2.xH2O. while the filtrate may
contain group IIIB cations. Add 2 mL of NaOH, 1 mL of 2% H2O2. Simmer until the
O2 is gone. Centrifuge and separate the precipitate from the filtrate. The three
precipitates (no. 2) may contain Fe(OH)3 or MnO2.xH2O. Wash the precipitate with
hot water or 2% NH4NO3. Dissolve the precipitate with dilute HNO3. If necessary add
2 drops of 3% H2O2 or a drop of saturated H2SO3. Divide the solution into two. The
first part is added with a drop of K4Fe(CN)6. Blue precipitate indicates the presence of
Fe. To determine Fe(II) or Fe(III), the original solution is tested with K4Fe(CN)6 or
KSCN. The second part is diluted with 1 mL of water (aquadest), cooled, add 10 mg
NaBiO3, shake and let the solids drop. A purple solution of MNO4- indicates the
presence of Mn. The fourth filtrate (no. 2) may contain Al(OH)4- or CrO42-. Divide
the solution into two. The first part is acidified with dilute acetic acid. Add 1 drop of Pb
acetate. PbCrO4 yellow precipitate indicates the presence of Cr. The second part is
acidified with dilute HCl. Add dilute NH3 until just alkaline. Add another drop and
heat on a water bath for 1 minute, a white precipitate of Al(OH)3 indicates the presence
of Al. The five filtrates from the addition of HNO3, NH4Cl and NH3 above may
contain cations group IIIB. Add 1-2 drops of dilute NH3 solution, heat and flow with
H2 gas. Centrifuge and wash the precipitate. Separate the precipitate and the filtrate.
The six precipitates (no. 5) may consist of CoS, NiS, MnS, or ZnS. Stir the precipitate

1
0
with 1 mL of 1 M HCl. Centrifuge, separate the precipitate from the filtrate. The seven
deposits (no. 6) can be CoS, NiS. Add 10-15 drops of dilute HCl and 5 drops of 1 M
NaOCl. Stir on a water bath for 1-2 minutes. Bring to a boil to remove Cl2. Divide the
solution into two. The first part is added 1-2 drops of amyl alcohol and 50 mg solid
NH4SCN and shaken. The blue color in the alcohol layer indicates the presence of Co.
The second part is added with 1 drop of NH4Cl solution, then NH4OH is added until it
is basic. Add 2-3 drops of dimethyl glyoxin reagent. A pink precipitate indicates the
presence of Ni. The eight filtrates (no. 6) may contain Mn2+, or Zn2+. Bring the
solution to a boil to remove H2S. Cool and add 1 mL of NaOH and 4 drops of 3%
H2O2. Centrifuge, separate the precipitate and the filtrate. The nine precipitates (no. 8)
contain MnO2.xH2O. Identify as in group IIIA, or dissolve the precipitate in 0.5 mL of
dilute HNO3 with the addition of 1-2 drops of H2O23% and 0.3 mL of water. Bring to
a boil to remove excess H2O2. Cool, add 0.5 mL concentrated HNO3 and 250 mg
PbO2. Simmer for 1 minute and leave. A purple solution of MnO4- indicates the
presence of Mn. Finally the filtrate (no. 8) may contain Zn(OH)22+. Flow with H2S
gas white precipitate indicates the presence of Zn.

CATION ANALYSIS GROUP IV

First, the solution containing group IV cations or group III filtrate was added
with 5 drops of 20% NH4Cl and 6 M NH4OH dropwise, then added 6 drops of
(NH4)2CO3. Place it on a hot water bath for a few minutes. Centrifuge, separate the
precipitate from the filtrate. Both group IV precipitates may contain BaCO3, SrCO3, or
CaCO3. Wash the precipitate with a few drops of water and 1 drop of (NH4)2CO3.
Dissolve the precipitate in 3-4 drops of 6 M acetic acid. Add 2 drops of K2CrO4, stir
for about 1 minute. A yellow precipitate indicates the presence of Ba. Centrifuge,
separate the precipitate and the filtrate. The three precipitates (no. 2) contained
BaCrO4. Wash the precipitate with water until the washing water is colorless. Add 2
drops of 6 M HCl. Test the flame reaction using Pt/Ni-Cr wire. A green glow indicates
the presence of Ba. The four filtrate (no. 2) may contain Sr2+ or Ca2+. Add NH4OH
dropwise until alkaline. Concentrate the solution to 0.5-1 mL. Add ethyl alcohol with
the same volume while stirring. Cool under running tap water, let stand for 5 minutes.
Yellow precipitate indicates the presence of Sr. Centrifuge, separate the precipitate and
the filtrate. The precipitate should not be washed. The five precipitates (no. 4)
contained SrCrO4. Add 10 drops of ammonium sulfate and simmer for 1 minute. Cool
and centrifuge. Wash the sediment with water and discard the washing water. Add 2
drops of 6 M HCl and perform a flame test. Red flame indicates the presence of Sr. The
six filtrates may contain Ca2+ or Ag2+. Evaporate to a volume of 0.5 mL and discard
the precipitate. Add 2 drops of dilute NH4OH and 2 drops of ammonium oxalate. A
white precipitate indicates the presence of Ca. Centrifuge, separate the precipitate and
the filtrate. React the precipitate with 2 drops of 6 M HCl and perform the flame test. A

1
1
brick red flame indicates the presence of Ca.
*The possibility of Ag 2+ ions being precipitated in group IV. Add 2 drops of
Na2HPO4 to the filtrate. Leave it for 5 minutes. The formation of white crystals
indicates the presence of Ag.

CATION ANALYSIS OF GROUP V

First, the solution containing group V cations or group IV filtrate is divided into
four parts. In the first part add 1 drop of 6 M NH4OH and 1 drop of Na2HPO4. Leave a
few minutes. The formation of white crystals of MgNH4PO4 indicates the presence of
Mg. Second In the second part, vaporize 2 drops of the solution. Add 2 drops of
concentrated HNO3. Steam again. Drop the residue with a drop of 6 M acetic acid and
3-4 drops. Stir well, transfer the solution to a watch glass. Add a drop of sodium cobalt
nitrite solution. A yellow precipitate indicates the presence of K. In the third section,
vaporize 2 drops of the solution. Add 1 drop of 6 M HCl to the residue. Perform a
flame test, check the flame through the cobalt glass. Reddish purple flame color
through the glass indicates the presence of K. Third If there is a yellow flame (without
gauze) at the last second, it indicates the presence of Na. In the fourth section, add 8
drops of zinc uranyl acetate to the solution. Cool under running tap water. Let stand for
10 minutes or so, then centrifuge. A yellow precipitate indicates the presence of Na.
Fourth, the test for NH4+ cations cannot be tested from the filtrate from the previous
group separation because of the addition of these cations from NH4OH, NH4Cl,
(NH4)2SO4, and others. This cation is tested from the original substance. If the original
substance is a solution, take 3 drops and if it is a solid, take some of the crystals, put it
in the bottom of the test tube. Carefully add 6 drops of NaOH (be careful not to let the
NaOH hit the tube wall). Place the red litmus paper on top of the tube, and put half of it
into the tube. Carefully heat the tube. The color change of the bottom of the litmus
paper to blue indicates the presence of NH4+ ions. Instead of litmus paper, the solution
is heated and smelled. The smell of ammonia is very obvious in the presence of NH4+
ions.

ANION ANALYSIS IN SOLUTION

1. Prepare the preparation solution :

The substance to be checked for anion is heated with saturated Na2CO3. The
precipitate is filtered, the filtrate (preparatory solution) is used for further
analysis.
2. Proof of sulfate ion (SO42-) :
The preparation solution was added with 6 M HCl until acidic, then brought to a
boil. Add BaCl2 solution. A white precipitate indicates the presence of sulfate

1
2
 ions
3. Proof of nitrate ion (NO3-) :
The preparation solution was added with concentrated H2SO4, then added the
saturated FeSO4 solution slowly through the tube wall. The formation of a
brown ring indicates the presence of nitrate ions.
4. Proof of chloride ion (Cl-) :
The preparation solution was added with AgNO3 solution. A white precipitate
soluble in ammonia indicates the presence of chloride ions.
5. Proof of bromide ion (Br-) :
The preparation solution was added with AgNO3 solution. A light yellow
precipitate soluble in concentrated ammonia indicates the presence of bromide
ions.
6. Proof of iodide ion (I-) :
The preparation solution was added with CuSO4. A brown precipitate occurs
which is a mixture of copper (I) iodide and iodine. The brown color that
disappears with the addition of sodium thiosulfate indicates the presence of
iodide ions.
7. Proof of sulfide ion (S2-) :
The preparation solution was added with Pb-acetate solution. A black precipitate of
lead (II) sulfide indicates the presence of sulfide ions.
8. Proof of sulfite ion (SO32-) :
The preparation solution was added with silver nitrate solution. A white precipitate
dissolved in excess sodium sulfate indicates the presence of sulfite ions. When
the solution is boiled, a gray precipitate of Ag occurs.
9. Proof of thiosulfate ion (S2O3) :
The preparation solution was added with a brown I2 solution. The loss of brown
color indicates the presence of thiosulfate ion.
10. Proof of carbonate ion (CO32-) :
The preparatory solution is supplemented with calcium chloride. The white
precipitate that occurs indicates the presence of carbonate ions.
11. Proof of phosphate ion (PO43-) :
The preparation solution was added with MgCl2, NH4Cl, NH4OH. The occurrence
of a white precipitate of MgNH4PO4 indicates the presence of phosphate ions.
12. Proof of acetate ion :
The preparation solution was added with FeCl3. The solution is brown. Dilute and
heat. A brown precipitate is formed from Fe(OH)2CH3COO.

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4
 CHAPTER IV
RESULTS AND
DISCUSSION

4.1 Results Observation

No. Procedure Test Results Observation Allegation/Reacti Conclusion
Perc. Before After on
1. Cation Analysis (group 1) -Sample x is - sample x + - Pb 2+ + 2Cl - PbCl 2 From the experimental
white (grain)? distilled water - Ag + + Cl - AgCl group I cations, it can be
Sample Solution - colorless = colorless - Hg + 2Cl HgCl 2 concluded that sample x
2+ -

aquadest solution, no - Pb 2+ + CrO 4 PbCrO 4 shows group I cations as

1 . Added a few drops of 6M . HCl - 6M HCl precipitate (yellow precipitate) evidenced by the formation
2 . Added 1-2 drops of dilute HCl 2+ cations.
solution is - sample -Hg 2 Cl 2 + 2NH 3 Hg + of Pb
3 . centrifuged
colorless solution + 6M Hg(NH 2 )Cl + NH 4 + + Cl -
- Colorless HCl = there is a (black precipitate)
dilute HCl colorless - AgCl + 2Nh 3 [Ag(NH
sediment Group II,III,IV,V filtrate CH3COOH solution precipitate -
3 ) 2 ]+Cl
is colorless - sample [Ag(NH 3 ) 2 ] + + Cl - +
4 . Washed sediment - K 2 CrO 4 solution x + 5 HNO AgCl + NH NO
3 4
5 . Heated in a boiling water bath for 1 minute solution is yellow drops of 6M
6 . centrifuged 3
HCl + 2 drops
-[Ag(NH 3 ) 2 ] + + Cl
of dilute Hcl =
AgCl + NH 4 +
there is a
PbCl2 filtrate Sediment colorless
precipitate
7 . Add 2 drops of 6M . CH3COOH 7. dissolved in 0.5 ml NH4OH >Sediment
solution 8. heated washed
8. Add 1 drop of K2CrO4 . solution 9. stirred - sample
10. centrifuge
PbCrO4 yellow solution x + 5
precipitate drops of HCl +
Filtrate Black precipitate 2 drops of
Hg(NH2)Cl dilute HCl is
11. addition of dilute HCl or HNO3 heated, no
change occurs
+ decanted the
AgCl white precipitate precipitate &
filtrate are
separated
- filtrate + 2
drops of CH 3
COOh 6M =
colorless, no
precipitate
- filtrate + 2
drops of Ch 3
COOH 6M + 1
drop of K 2 CrO
4 = filtrate is
yellow, there is
a yellow
precipitate
(+++)
 No. Procedure Test Results Observation Allegation/Reaction Conclusion
Perc. Before After
Anion analysis Sample x + Na 2 sample x + Na 2 Na2CO3 _ _ _
1. Making preparation solution Co 3 saturated CO 3 is heated =
Na 2 CO 3 = a white
Sample colorless precipitate is
solution formed
1 . heated with full Na2CO3 HCl = colorless
2. filtered the sediment solution
Concentrated H 2
SO 4 = colorless
Sediment (not used) Preparation solution solution
Saturated FeSO4
3. divided into 11 test
tubes
= colorless

SO Cl- I- SO32- PO3- CH3COOH

42-

Br- S2- S2O32- CO32-

NO3-
-preparation
2. Proof of sulfate ion (SO 4 2- ) -preparation solution + 6M -SO 4 2- + Ba 2+
solution = HCl 4 drops = BaSO4 _
Preparation solution
colored (cloudy precipitate and
1 . 6M HCl solution was added until acidic white) no bubbles form
2. bring to a boil precipitate
3. Add BaCl2 . solution
- preparation
BaSo4 white precipitate
solution + 3
3. Proof of nitrate ion (NO 3 - ) - preparation drops of -2NO 3 - + 4H 2 SO 4 + From the anion experiment on
Preparation solution
solution = concentrated 6Fe 2+ 6Fe 3+ +2NO NO 3 - it can be concluded that
colorless, no H2SO4 + 3 drops + 4SO 4 2- + 4H 2 O sample x shows the presence
1 . concentrated H2SO4 added precipitate of saturated - Fe 2+ + NO of NO 3 - anion , as evidenced
2. Add saturated FeSO4 slowly through the FeSO4 = a [Fe(NO)] 2+ by the presence of a brown
wall brown ring is ring.
Brown ring formed and there - So sample x spans
is a green compound Pb(NO 3 ) 2
precipitate, there
are 2 layers
4.2 Analysis and Discussion
For cation analysis, we use group 1 cations with a few drops of 6M
HCl added to the sample solution. Then add 1-2 drops of dilute HCl and
centrifuge. Produces sediment and filtrate goals II, III, IV, V. The
precipitate was washed and heated with a boiling water bath for 1 minute
and centrifuged. To produce PbCl 2 filtrate , 2 drops of 6M CH 3 COOH
solution were added, then 1 drop of K 2 CrO 4 solution was added to produce a
yellow precipitate of PbCrO 4 . And the precipitate was dissolved in 0.5 ml
of NH 4 OH heated, stirred, and centrifuged to produce the filtrate and black
precipitate of Hg(NH 2 )Cl. The filtrate is added with dilute HCl or HNO 3 to
produce a white precipitate of AgCl. Before analysis, sample x was white
after adding distilled water, the solution was colorless and there was no
precipitate. The solution plus HCl has a colorless precipitate. The solution
was added with 5 drops of HCl and 2 drops of dilute HCl when heated,
there was no change. The filtrate was added with 2 drops of CH 3 COOH
6M which was colorless and there was no precipitate. The filtrate was added
with 2 drops of CH 3 COOH 6M and then 1 drop of K 2 CrO 4 was added which
was yellow and there was a yellow precipitate. The conclusion from the
group 1 experiment can be concluded that sample x shows group I cations,
as evidenced by the formation of Pb 2+ cations .
To analyze the anions, it is necessary to make a preparation
solution first by heating the sample with full Na 2 CO 3 then filtering the
precipitate to get an unused precipitate and the preparation solution divided
into 11 test tubes. 11 preparation solutions namely SO 4 2- , NO 3 - , Cl - , Br -
, I - , S 2- , SO 3 2- , S 2 O 3 - , PO 4 3- , CO 3 2- , CH 3 COOH . Then prove the
sulfate ion with the preparation solution added with 6M HCl solution until
the acid boils and the BaCl 2 solution is added to form a white precipitate of BaSO
4 . And prove the nitrate ion with the preparation solution added with
concentrated H 2 SO 4 and added saturated FeSO 4 slowly through the wall to
produce a brown ring. Prior to the observation, Na 2 CO 3 , HCl, H 2 SO 4 were
saturated, and FeSO 4 was saturated colorless. The solution of the sulfate ion
preparation was cloudy white in color and there was no precipitate. The
nitrate ion preparation solution is colorless and has no precipitate. After
completion of sample x added saturated Na 2 CO 3 was heated to form a
white precipitate. Then the preparation solution of sulfate ion + 6M HCL 4
drops to form a precipitate and bubbles. The preparation solution of nitrate
ion was added with 3 drops of concentrated H2SO4 plus 3 drops of saturated
FeSO4 to form a brown ring and there was a green precipitate and there were
2 layers. In conclusion, from the anion equation for NO 3 - it can be
concluded that sample x shows the presence of NO 3 - anion as evidenced by
the presence of a brown ring. So sample x spans the compound Pb(NO 3 ) 2 .

4
 CHAPTER V
CONCLUSION AND
SUGGESTION

5.1 Conclusion
From group 1 experiments, it can be concluded that sample x
shows group I cations, as evidenced by the formation of Pb 2+ cations . From
the anion equation for NO 3 - it can be concluded that sample x shows the
presence of NO 3 - anion as evidenced by the presence of a brown ring. So
sample x spans the compound Pb(NO 3 ) 2 .
5.2 Suggestion
Suggestions for this Anion and Cation analysis practicum is to pay
attention to the cleanliness of the tools to be used, we are also expected to
be more careful in observing changes that occur in the sample and must be
careful in determining the sample group .

LIST REFERENCES

Amin, M. 2016. “Analysis of cation minor elements in natural water samples

using ion chromatography techniques”, Journal of Techno05 (1), 1 -8
(2016).
Day, RA and AL, Underwood. Quantitative Analysis . Terj, Dr. Ir. Lis Sopyan,
M. Eng. Qualitative Chemical Analysis. Jakarta: Erlangga, 2001.
Widiarto, Sonny. 2011. Anion and Cation analysis. UNILA Staff : Lampung
Anonymous. (2010). Practical Guide to Analytical Chemistry at the Muslim
University of Indonesia. Makassar.

ATTACHMENT

a. Answer Question
1. Write the general reaction for each group!
Answer: (Group I: M + + Cl - MCl (s) white)
a. Group I : M + + Cl - MCl
M + + 2Cl - MCl 2
Where:
M + = Ag + and Hg 2+
M2 + = Pb +
b. Group II:
M 2+ + S 2- MS
5
 3M 3+ + 2S 2- M 2 S 3
M 4 + + 2S 2- MS 2
Where:
M 2+ = Cu 2+ , Cd 2+ , Pb 2+
M 3+ = Bi 3+ , As 3+ , Sb 3+
M 4 + = Sn 4 +
c. Group IIIA:
M 2+ + S 2- MS
Where:
M 2+ = Zn 2+ , Co 2+ , Ni 2+
d. Group IIIB:
M 3+ + 3OH - M(OH) 3
Where:
M 3+ = Fe 3+ , Al 3+ , Cr 3+
e. Group IV:
M 2+ + CO 3 2- MCO 3
Where:
M 2+ = Ba 2+ , Sr 2+, Ca 2+
f. Group V:
M 2+ + 2OH - M(OH) 2
Where :
M2 + = Mn2 +
2. 2S cation analysis system H 2 O 2 or bromine water, and not HNO 3 ?
Answer: Because in oxidizing a compound, HNO 3 will form Ammonia gas
which will give a small solubility of the compounds formed so that the
precipitate formed between group 1 and other groups cannot be distinguished.
3. How do you know if H 2 S, H 2 O 2 , or Br 2 are no longer in the solution?
Answer: H2S is no longer present in the solution if the heated solution no longer
emits the smell of hydrogen sulfide which smells of rotten eggs or by using filter
paper dipped in lead acetate and placed over the mouth of the heated solution
tube.
H2O2 is no longer present in the solution , it can be determined by dipping filter
paper in HCl, then facing the hose that is channeled to H2O2 . If there is no black
stain on the filter paper, then H 2 O 2 is not present.
Br2 is no longer present in the solution can be determined by the way the
solution is evaporated . The smoke that comes out is placed on paper moistened
with starch. If the wet starch paper turns orange red, then Br 2 is still there, but if
6
 it is orange then Br 2 is gone.
4. Why is it necessary to use the analyte directly to determine the presence of NH 4
+ cations?

Answer: Because in the previous test, the analyte has been added NH 4 +
(functions as a reagent) repeatedly so that if the filtrate from the previous group
test is used, it is clear that there will be NH 4 + in it, so the analyte is needed
directly to test for NH 4 +
5. What is the general reaction in the preparation of a preparatory solution to
determine the presence of anions?
Answer: MA 2+ Na 2 CO 3 MCO 3 + 2NaA
6. The precipitation of sulfide salts in the analysis of group II and group IIIB
cations was carried out in different solution conditions. Explain?
Answer: In group II, H2S is flowed into an acidic solution because the filtrate
used to get the sulfide salt precipitate comes from the group I filtrate which still
contains dilute HCl.
In Group IIIB the solution is alkaline, because the filtrate used to precipitate the
sulfide salt comes from the group IIIA filtrate which still contains NH 3 and NH
4 Cl.

7. Why should the group IV deposition be carried out in an alkaline environment?

Answer: Precipitation of group IV must be in an alkaline environment, because
in an acidic environment bicarbonate salts will be formed where the solubility is
greater.
b. Documentation

 Cation

No Picture Information

1. Put sample x into the test tube

7
2. Put distilled water into a test tube containing sample x

3. Shake until sample x dissolves in distilled water

4. Result of sample x + aquades

5. Transferred to a test tube sufficiently

8
6. Added a few drops of HCl 6 M

7. Shake to mix the sample solution and 6 M . HCl

Result of sample solution x + HCl 6 M = form a precipitate

8.
and colorless solution

9. Added 1-2 drops of dilute HCl

9
10. Shake so that the solution is completely mixed

The results of the sample solution x + HCl 6 M + 1-2 drops

11.
of dilute HCl formed a precipitate and a colorless solution

12. Centrifuge

13. Washed sediment

1
0
 The precipitate is heated in a water bath until it boils,
14.
approximately 1 minute

15. The result of the precipitate after heating

16. Centrifuge produces precipitate and filtrate

The filtrate was added with 2 drops of M . CH3COOH

6
17.
solution

1
1
18. The result of adding 2 drops of CH COOH 6 M . solution
3

The filtrate was added with 2 drops of 6 M CH COOH 3

19.
solution and then 1 drop of K CrO 2 4 solution was added.

The result of the filtrate + 2 drops of CH COOH 6 M

3

20. solution + 1 drop of K CrO

2 = the filtrate is yellow and
4 solution

there is a yellow precipitate (+++)

 Anions
No Picture Information

1. Put sample x into a test tube to make a preparation solution

1
2
2. Add saturated Na CO until it reaches test tube
2 3

3. Heated with saturated Na2CO3 _

The result of sample x + saturated Na CO 2 3 solution when heated

4.
= a precipitate is formed

5. Filtered the sediment

1
3
 Proof of ion NO 3
-
6.
Preparation solution + concentrated H2SO4

Preparation solution + concentrated H2SO4 + FeSO4

7.
saturate slowly

The final result of the NO3- anion experiment was

8.
evidenced by the presence of a brown ring

c. Plot handwritten

1
4
d. Report temporary write hand

1
5
1
6
1
7