A.

Title of Experiment
Spot Test
B. Objective of Experiment
The student can be known:
1. Mercury through the examine of Cu(II) iodide
2. Arsen through the examine with Gutzeit method and silver nitrate
3. Cobalt through the examine with ammonium thiocyanate and the examine
there are Fe
4. Chloride through the examine with precipitation as silver chloride and
examine with the volatile of hydrochloric acid
5. Sulphate through the examine with barium carbonate
6. Hydrogen peroxide through the examination with Fe(III) cyanide
C. Literature Review
Sample be tested analysis by using edx analysis ( energy dispersive x-ray )
.The principal of anode lithium-ion battery is LiCoO 2. From the analysis edx it
can be seen the heavy metals besides lithium and cobalt. Based on an analysis edx
another metal contained in anode lithium-ion battery is aluminum. An analyzer
conducted using edx still in the form of qualitative analysis. To get composition is
anode lithium-ion battery and aas analysis. The metals are that analysis use aas
analysis was Co, and Li. The results of the analysis. The results of the analysis aas
shows that largest concentration contained in anode lithium-ion battery is cobalt
and aluminum, while lithium contained small making on trial , metal lithium not
analysis (Yuliusman, 2008:150).
The importance of obtaining a representative sample for analysis cannot be
overemphasized. Without it, results may be meaningless or even grossly
misleading. Sampling is particularly crucial where a heterogeneous material is to
be analyzed. It is vital that the aims of the analysis are understood and an
appropriate sampling procedure adopted. In some situations, a sampling plan or
strategy may need to be devised so as to optimize the value of the analytical
information collected. This is necessary particularly where environmental samples
of soil, water or the atmosphere are to be collected or a complex industrial process
is to be monitored. Legal requirements may also determine a sampling strategy,

particularly in the food and drug industries. A small sample taken for analysis is
described as a laboratory sample (Kealey, 2002:10).
Independently of the monitoring aim, samples should be representative of
the water studied. Sampling strategies, as well as the techniques, the requirements,
and the recommendations for the routine collection of representative water
samples, are described in the U.S. National Field Manual and elsewhere.
Strategies for sampling water from an aquatic environment, several factors should
be looked at. Which of these should be taken into account in a given situation
depends on the objective of sampling and the type of water body to be analyzed.
The most important factors are the selection of sampling location (general
position in the water body) and sampling sites (exact position), the size of samples
and the number to be taken at each site, the frequency and timing of sampling, and
the manner in which the sample is taken (Namiensink, 2010:8).
The scientific method originated in the seventeenth century with such
people as Galileo, Francis Bacon, Robert Boyle, and Isaac Newton. The key to the
method is to make no initial assumptions, but rather to make careful observations
of natural phenomena. When enough observations have been made so that a
pattern begins to emerge, a generalization or natural law can be formulated
describing the phenomenon. Natural laws are concise statements, often in
mathematical form, about natural phenomena. The form of reasoning in which a
general statement or natural law is inferred from a set of observations is called
induction (Petrucci, 2010:2).
The comparisons of cyclohexanol conversion over parent and modified
catalyst showed lowered conversion levels at all temperatures except at 430
where all samples showed nearly complete conversion due to higher temperature.
A comparison at lower temperature where dehydrogenation is prominent depicted
in indicates that modified catalyst exhibit improved values of selectivity to
cyclohexanone due to cyclohexanol dehydrogenation. Itis generally accepted that
higher charge to radius ratio of the metallic ion gives a more acid (less basic)
oxide (Vyawahare, 2010:46).

Significance tests involve a comparison between a calculated experimental

factor and a tabulated factor determined by the number of values in the set(s) of
experimental data and a selected probability level that the conclusion is
correct.Tests are based on a null hypothesis an assumption that there is no
significant difference between the values being compared. The hypothesis is
accepted if the calculated experimental factor is less than the corresponding
tabulated factor, otherwise it is rejected and there is said to be a significant
difference between the values at the selected probability level. The conclusion
should always be stated clearly and unambiguously (Kealey, 2002:34).
For measuring the quantity of pollutants carried by a river, the sampling
sites should represent the water body as a whole. Boundaries such as banks,
surface, bottom, and the confluences of streams or other rivers should thus be
avoided, since any samples collected there will generally be unrepresentative. For
studying the effect of the discharge of wastewater, industrial effl uents, and so on,
on river water quality, samples should be taken downstream, at a location where
mixing is complete. For monitoring the quality of water taken for a particular
purpose, the sampling site should be situated close to the abstraction point. In the
case of lakes and reservoirs, the heterogeneity related to thermal stratification, infl
owing streams, morphology, and even wind needs to be taken into consideration
during site selection (Namiensink, 2010:9).
Matter is anything that occupies space and displays the properties of mass
and inertia. Every human being is a collection of matter. We all occupy space, and
we describe our mass in terms of weight, a related property. All the objects that we
see around us consist of matter. The gases of the atmosphere, even though they are
invisible, are matter they occupy space and have mass. Sunlight is not matter;
rather, it is a form of energy. Energy is discussed in later chapters. Sometimes a
sample of matter undergoes a change in its physical appearance. In such a
physical change, some of the physical properties of the sample may change, but its
composition remains unchanged. When liquid water freezes into solid water (ice),
it certainly looks different and, in many ways, it is different. Yet, the water
remains 11.19% hydrogen and 88.81% oxygen by mass (Petrucci, 2010:4).

Can be seen that the percentage of leaching will increase in line with the
decline in the ratio of solid or liquid. The increase in the percentage of leaching
happened because with increasing volume hcl , then the possibilities of contact
between metal ions Cl- with will be bigger. In addition if the ratio of solid or
liquid too big then solution would be too saturated .On observation appears that
the ratio of solid on or liquid of 1 / 25, there are still many remnants of the
sample are not dissolved (Yuliusman, 2008:152).
When selecting equipment for sampling water, the prime consideration is
the material from which the parts in contact with the sample have been made. This
can be various organic polymers, metals, and glass. The material selected should
not release compounds interfering with the determination of target analytes and
should neither adsorb nor react with these analytes. Hence, the nature of the
analytes and the properties of the sampler material will be crucial factors in
selecting the equipment for a given task. In general, organic polymers are
incompatible with most organic analytes, which can dissolve in or be leached out
of such materials, and this may lead to negative or positive errors, respectively
(Namiensink, 2010:12-13).
Whether or not an aqueous solution is a conductor of electricity depends
on the nature of the solute(s). Pure water contains so few ions that it does not
conduct electric current. However, some solutes produce ions in solution, thereby
making the solution an electrical conductor. Solutes that provide ions when
dissolved in water are called electrolytes. Solutes that that do not provide ions in
water are called nonelectrolytes. All electrolytes provide ions in water but not all
electrolytes are equal in their tendencies for providing ions. A strong electrolyte is
a substance that is essentially completely ionized in aqueous solution (Petrucci,
2010:152).
D. Apparatus and Chemicals
1. Apparatus
a.
b.
c.
d.

React tube
Tube Rack
Stir bar
Spiritus Burner

(4 pieces)
(2 pieces)
(1 piece)
(1 piece)

e.
f.
g.
h.
i.
j.
k.

Tripod and Gauze

Spot Plate
Spray Bottle
Rough and Smooth Cloth
Spatula
Porselain
Clamp

(@1 piece)
(1 piece)
(1 piece)
(@1piece)
(1 piece)
(5 pieces)
(2 pieces)

2. Chemicals
a.
b.
c.
d.
e.
f.
g.
h.
i.
j.
k.
l.
m.
n.
o.
p.
q.
r.
s.
t.
u.
v.
w.
x.
y.

Potassium Iodide-Sodium Sulphate solition (KI-Na2S2O3)

Copper (II) Sulphate solution (CuSO4)
Chloride Acid solution (HCl)
Nitric Acid solution (HNO3)
Zink solid (granul)(Zn)
Sulphuric Acid solution (H2SO4)
Silver Nitric solution (AgNO3)
Ammonium Hydroxide solution (NH4OH)
Hydrogen Peroxyde solution (H2O2)
Acetic Acid solution (CH3COOH)
Silver Nitric solution 1% (AgNO3)
Ammonium thiocyanate solution (NH4SCN)
Ammonium Flouride solution (NH4F)
Oxyn (C6H9NOH)
Barium Carbonate solid (BaCO3)
Phenolphtalein indicator (pp)
Sodium Chloride solid (NaCl)
Hydrargirum (II) Chloride solution (HgCl2)
Aresen Oxyde solution (As2O3)
Cobalt Nitric solution (Co(NO3)2)
Stannum Chloride solution (SnCl2)
Potassium Ferricyanaide solution (K4Fe(CN)6)
Aquadest (H2O)
Tissue
Matches

E. Work Procedure
1. Mercury Test with Cu (II) Iodide
a. 2 drops of KI-Na2SO3 solution was added into spot plate
b. 2 drops of CuSO4 was added into spot plate
c. 2 drops of HgCl2 was added and the mixture solution was stirred
2. Arsenic Test
a. Gutzeit Method
1) 2 drops of dilluted H2SO4 was added into test tube
2) Solid Zn was added into test tube
3) 2 drops of As2O3 was added into test tube
b. Silver Nitric

1) 2 drops of As2O3 was added into porcelain

2) 2 drops of H2O2 and 2 drops of NH4OH was mixtured and heated at
another test tube
3) The mixture of H2O2 and NH4OH solution wa added into porcelain
4) 2 drops of AgNO3 was added into porcelain
3. Cobalt Test
a. Ammonium Thiocyanate and Aceton
1) 1 drop of Co(NO3)2 was dropped into spot plate
2) 1 drop of NH4SCN 10% was added into spot plate
b. The Existence of Fe ion
1) 5 drops of Co(NO3)2 was dropped into spot plate
2) Some mg of NH4F was added into spot plate
3) 5 drops of NH4SCN 10% was added into test tube
4. Chloride Test
a. Silver Chloride Precipitation
1) 5 drops of SnCl2 was dropped into test tube
2) 1 drop of oxyn was added to test tube and it was shaken
3) 1 drop of HNO3 was added into test tube
4) 1 drop of H2O2 solution was mixed with above test tube
5) Heat was done during 4 minutes
6) 1 drop of AgNO3 1% was mixed and it was shaken in test tube
b. Volatilization of Chloride Acid
1) NaCl solid was put into test tube
2) 2 drops of HNO3 was added into test tube
3) Heat was done during 2 minutes
4) 3 drops of AgNO3 was added again into test tube and it was shaken
5. Sulphuric Test with BaCO3 and pp
a. 5 drops of H2SO4 was dropped into porcelain
b. 5 drops of BaCO3 was added into porcelain
c. Some drops of pp was added into porcelain and it was shaken
d. Heat was done during 3 minutes
6. Hydrogen Peroxyde with Ferricyanide and PbS
a. 5 drops of K3Fe(CN)6 was dropped into test tube
b. 5 drops of H2O2 was added into test tube and it was shaken
c. 5 drops of SnCl2 was added into test tube and it was shaken again
d. Color change of all experiment was noted and it was observed clearly
F. Observation Result
N
o
1

Experiment

Result

Determination of Hg in Cu (II) Iodide

1 drop of KI-Na2S2O3 (colorless) + 1
drop of CuSO4 (blue)

The color of solution is

yellow

+ 1 drop of HgCl2 (colorless)

Arsenic Test
a. With Guitzet Method
As2O3 (colorless) + Zn (granul)
+ H2SO4 (colorless)
b. With Silver Nitrate
3 drops of As2O3 + 3 drops NH3
+ 3 drops H2O2 (heated)
+ 2 drops CH3COOH + 2 drops
of AgNO3

Not formed yellow spot

Colorless
Colorless and white
precipitate

Cobalt Test
a. With Ammonium Thiocyanate
and Acetone
Co(NO3)2 (pink) + NH4SCN
(yellow brownish)
b. With Cobalt in Iron
Co(NO3)2 (pink) + NH4F (white)
+ NH4SCN (yellow brownish)

The color of solution is

red

Chloride Test
a. With Precipitation AgCl
HCl (colorless) + oxyn
(colorless)
+ H2O2 (colorless) + HNO3
(colorless)
(heated) + AgNO3 1%
b. Volatilization of HCl
NaCl (white crystal) + HNO3
+ 1 stirrer wet by AgNO3
(colorless) and cooled
Sulphate Test with BaCO3 and pp
H2SO4 (colorless) + BaCO3 (heated)
dry (colorless) + pp (colorless)

Green-blue solution
Pink solution
Green-blue solution

Colorless
Colorless
White precipitate
Colorless
Buble formed, and clear
yellow color solution

Colorless

G. Discussion
1. Uji raksa dengan Cu(II) Iodida
Percobaan ini dilakukan untuk mengetahui secara kualitatif ada atau tidaknya
raksa (Hg) pada suatu sampel. Kedalam tabung reaksi dimasukkan larutan

KINa 2 S 2 O3

tidak berwarna dan larutan

Cu SO 4

yang berwarna biru.

Kemudian direaksikan dan terbentuk larutan yang berwarna kuning-kecoklatan,

Hg Cl 2
lalu campuran ini ditambahkan larutan
yang tidak berwarna dan
terbentuk endapan yang berwarna merah. Reaksi yang terjadi yaitu:
Hg I 2
2+ +2 I
terbentuk endapan merah merkurium (II) iodida
Hg
2
Hg I 4

Hg I 2+ 2 I
Endapan akan melarut pada reagensia berlebihan pada ion
tetraiodomerkurat (II). Larutan kalium tetraiodomerkurat (II) yang basa dipakai
sebagai reagensia selektif dan peka untuk ion ammonium. Reaksi yang terjadi:
NH4+ + 2[HgI4]2- + 4OH- HgO.Hg(NH2)I + 7I- + 3H2O
Hal ini telah sesuai dengan teori yang menyatakan bahwa Setetes larutan atau
suspensi yang dihasilkan dan direaksikan dengan reagensia Nessler maka akan
menghasilkan noda berwarna merah-jingga atau kuning (Svehla, 1979:215).
2. Uji arsen
a. Metode Gutzeit
Percobaan ini dilakukan menggunakan metode Gitzeit bertujuan untuk
mengetahui secara kualitatif adanya arsen dalam suatu sampel. Pertama larutan
sampel dimasukkan kedalam tabung reaksi dan ditambahkan beberapa butir Zn
granul dan

H 2 SO 4

ditetesi dengan larutan

encer kemudian ditutup dengan kertas saring yang telah

Ag NO 3

20% dan hasil yang didapatkan tidak terjadi

perubahan atau dengan kata lain tidak ada bercak yang timbul pada kertas saring.
Hal ini tidak sesuai dengan teori yang menyatakan bahwa akan diperoleh suatu

bercak berwarna kuning dari senyawa kompleks Ag3As.2AgNO3 sesuai dengan

persamaan reaksinya yaitu:
2+

+ As H 3 +3 Zn
3+ +3 Zn+3 H
As
4 As H 3 ( panas ) 4 As + 6 H 2
(Svehla, 1979:273).
b. Dengan perak nitrat ( Ag NO 3)
Pada perobaan ini juga ingin mengetahui mengetahui secara kualitatif
adanya arsen dalam suatu sampel. Kedalam cawan ditambahkan larutan sampel
lalu larutan ammonia

( NH 4 OH )

dan hidrogen peroksida

( H 2 O2 )

dan

dipanaskan pada api langsung yang bertujuan untuk mempercepat reaksi yang
terjadi. Kemudian ditambahkan asam asetat

CH 3 COOH

dan

Ag NO 3

1%

dan terbentuk endapan merah-coklat

3. Uji kobalt
a. Dengan ammonium tiosianat dan aseton
Pengujian ini dilakukan untuk mengetahui secara kualitatif adanya kobalt
dalam suatu sampel yang akan diuji dengan menggunakan pereaksi ammonium

tiosianat dan aseton. Pertama, kobalt(II) nitrat

ammonium tiosianat

(NH 4 SCN )

NO3 2 }
{Co

direaksikan dengan

menghasilkan larutan yang berwarna hijau-

kebiruan. Hal ini telah sesuai dengan teori yang menyatakan bahwa larutan garam
kobalt dalam suasana asam yang mengandung aseton yang cukup, pada
penambahan ammonium tiosianat akan memberikan warna biru yang intens

karena terbentuknya kompleks tiosianat (Tim Dosen Kimia Organik II, 2016:20).
Reaksi yang terjadi yaitu: : Co(NO3)2+4NH4SCN

Co(SCN)4(NH4)2 +

2NH4NO3
b. Uji kobalt dengan adanya besi
Pengujian ini dilakukan untuk mengetahui secara kualitatif adanya kobalt
dalam sampel yang akan diujikan dengan adanya ion besi. Pertama, kobalt(II)

nitrat

NO3 2 }
{Co

direaksikan dengan ammonium fluorida (NH 4F) dan kemudian

ditambahkan larutan ammonium tiosianat (NH4SCN) yang berwarna kuningkecoklatan dan terbentuk larutan yang berwarna hijau-kebiruan. Hal ini telah
sesuai dengan teori yang menyatakan bahwa dengan menambahkan beberapa butir
kristal ammonium tiosianat kepada larutan kobalt(II) yang netral atau asam, maka
muncul warna biru karena terbentuk io tetratiosianatokobaltat(II):
2
SCN 4
Co

2++ 4 SCN
Co
(Svehla, 1979:279).
4. Uji klorida
a. Pengujian dengan pengendapan sebagai

AgCl

dengan adanya halida lain

Pengujian ini bertujuan untuk mengetahui adanya kandungan anion klorida

Cl

dalam suatu sampel yang ditandai dengan terbentuknya endapan

yang berwarna putih. Pertama dimasukkan larutan

HCl

AgCl

kedalam tabung reaksi

dan diteteskan larutan oksin yang tidak berwarna

AgNO 3

dipanaskan dan diteteskan larutan

H 2 O2

dan

HNO3

lalu

1% dan dihasilkan endapan yang

AgCl . Hal ini telah sesuai dengan teori yaitu

berwarna putih yaitu endapan

endapan perak klorida AgCl berwarna putih, tak larut dalam air dan dalam asam
nitrat encer tetapi larut dalam larutan ammonia encer dan juga pada ion-ion
kompleks (Svehla, 1979:346).
Cl- + C6H9NOH

C6H9NCl + OH

C6H9NCl + H2O2

C6H9NOH + HCl

HCl + AgNO3

AgCl + HNO3

Cl + AgNO3

AgCl + NO3

b. Pengujian dengan volatilitas asam klorida

Pengujian ini dilakukan untuk mengetahui secara kuantitatif ada atau
tidaknya klorida

Cl

dalam suatu sampel berdasarkan volatilitas atau

kemudahan menguapnya larutan

NaCl

direaksikan dengan

HCl yang terbentuk. Pertama, padatan kristal

HNO3

dan dipanaskan terbentuk gelembung dan

larutan berubah menjadi warna kuning. Hasil ini tidak sesuai dengan teori yang
mengatakan bahwa klorida itu terurai banyak dalam keadaan dingin, dan
penguraian sempurna dalam pemanasan, yang disertai dengan hidrogen klorida.

Reaksi yang terjadi yaitu:

+ H 2 SO 4 HCl + HSO4
Cl

(Svehla, 1979:345).

Kesalahan yang terjadi dikarenakan karena alat yang digunakan belum bersih dari
zat pengotor lainnya yang mengakibatkan kesalahan dalam reaksi.
5. Uji Sulfat dengan Barium Karbonat dan PP
Pengujian ini dilakukan untuk mengetahui secara kualitatif ada atau
tidaknya sulfat dalam sampel yang akan diuji. Pertama, larutan
direaksikan dengan barium karbonat

(BaCO3)

H 2 SO 4

kemudian dipanaskan hingga

hampir kering dan diteteskan dengan indikator phenolphatalein (PP) dan

dihasilkan larutan yang tidak berwarna. Hal ini tidak sesuai dengan teori yang
mengatakan bahwa barium karbonat bereaksi cepat terhadap larutan alkali sulfat
netral, sesuai denga reaksi yaitu: BaCO3 + Na2SO4

BaSO4 + NaCO3

berlangsungnya reaksi dapat dideteksi dengan indikator PP yang berubah akibat

sifat basa dari natrium karbonat hasil reaksi (Tim Dosen Kimia Organik II,
2016:22).
H. Conclusion and Suggestion
1. Conclusion
After conducted all of the test we can concluded that:
a. The existence of mercury can be determine by using Cu(II) Iodide and positive
reaction is formed red or orange solution
b. The existence of arsenic can be determine by using Gutzeit method which is the
postive reaction is formed yellow spot on filter paper and with used silver nitrate
the positive reaction is formed red-brown precipitation
c. The existence of cobalt can be determine by using ammonium thyocianate and
aceton that signed is will be formed green to blue solution and with there are Fe is
signed by the solution became green
d. The existance of chloride can be determine by examining with precipitation of
AgCl with another halide that signed by will be turbidity solution or formed
precipitation and with used the examine based on volatility of hydrochloric acid is
signed by formed precipitation

e. The existance of sulphate can be determine by using barium carbonate and

phenolphatalein that signed is the solution became red solution
2. Suggestion
a. Before conducted the experiment we must known about the MSDS of the tools
and chemicals and understand the work procedure so that, can be minimalized
error while the experiment conducted
b. The tools that will be used must be checked before experiment conducted so
that if damaged is happened on the tools we can know before experiment
conducted

BIBLIOGRAPHY

Petrucci, Ralph. H and Herring, F. Geoffrey,. Madura, Jeffry. D,. Bissonette,

Carey. 2007. General Chemistry Principle and Modern Applications
Tenth Edition. Kanada : Pearson. ISBN: 978-0-13-206452-1
Namiesnik, Jacek and Szefer, Piotr. 2010. Analytical Measurements in Aquatic
Environments. London : Iwa Publishing. ISBN-13: 9781843393061
Kealey, D and Haines, P. J. 2002. Instant Notes Analytical Chemistry. United
States : BIOS Scientific Publisher. ISBN:0-203-68109-6
Vyawahare, Y. K and Chumbhale, V. R., et all. 2010. Gas-phase oxidant-free
oxidation of cyclohexanol over

V 2 O5

Mo O3

M 2O

(M= Na,

K, Cs) catalyst. Indian Journal of Chemical Technology. Vol. 17

Yuliusman and Hidayatullah, Muhammda Resya. 2008. Uji kinerja larutan HCl
pada proses leaching logam kobalt dari limbah baterai Lithium-ion.
2008. Department teknik kimia : Lampung. ISBN: 978-979-1165-74-7