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Spottest Yuyun Bundelan
Spottest Yuyun Bundelan
TITLE OF EXPERIMENT
Spot Test
B. OBJECTIVE OF EXPERIMENT
1. Identification to the mercury with Cu (II) Iodide.
2. Identification to the existence of Arsenic with the experiment of Gutzeit
method and Silver Nitric.
3. Identification to the existence of Cobalt with the Experiment of Ammonium
Thyosianat and testing with Iron.
4. Identification to the existence of Chloride using testing with precipitation as a
Silver Chloride and testing with volatilization of Chloride acid.
5. Identification to the existence of Sulphate using testing with Barium Carbonate
and phenolftalein.
6. Identification to the existence of Hydrogen peroxide using testing with
Ferrisianide and Lead sulphide.
C. LITERATURE REVIEW
Chemistry is the study of matter, Including its composition, structure,
physical properties, and reactivity. There are many approaches to studying
chemistry, but, for convenience, we traditionally divide it into five fields: organic,
inorganic, physical, biochemical, and analytical. Although this division is historical
and arbitrary, as witnessed by the current interest in interdisciplinary areas such as
bioanalytical and organometallic chemistry, Reviews These five fields Werner the
simplest division spanning the discipline of chemistry. We begin this section with
a deceptively simple question. What is analytical chemistry? Like all fields of
chemistry, analytical chemistry is too broad and active a discipline for us to Easily
or completely define in an introductory textbook. Instead, we will try to say a little
about what is analytical chemistry,
According to Kealey (2002: 1) Analytical chemistry is a scientific discipline
used to study the chemicalcomposition, structure and behavior of matter. Analytical
chemistry involves the application of a range of techniques andmethodologies to
Obtain and assess qualitative, quantitative and structuralinformation on the nature
of matter.
a. qualitative analysisis the identification of elements, species and /
orcompounds present in a sample.
b. quantitative analysisis the determination of the absolute or relative
amountsof elements, species or compounds present in a sample.
c. structural analysisis the determination of the spatial arrangement of atoms
in an element or molecule or the identification of characteristic groups of
atoms (functional groups).
d. An element, compound or species that is the subject of analysis is known as
ananalyte,
e. The remainder of the material or sample of the which the analyte (s) form
(s) a partis known as the matrix,
As a broad outline chemistry analysis work can be classified two categories
large items, namely qualitative analysis and the quantitative analysis.Through the
qualitative and quantitative analysis, we can detect and identify the kind and
number of components Analyzed material or more commonly known as analite.
Composition analite who is learned in every process of analysis includes a variety
of species, can be elements, ions, molecules, radicals and isotope.The development
of the instrument as a result of technological development, an analysis Allows us
in various forms composition analite.The the main objective of qualitative analysis
is to identify the component in a chemical substance (Ibn 2004: 1).
Any chemical analysis can be broken down into a number of stages
thatinclude a consideration of the purpose of the analysis, the quality of theresults
required and the individual steps in the overall analyticalprocedure. quantitative
analysis.Preparation of standards containing known amountsof the analyte (s) or of
pure reagents to be reacted with the analyte (s) .Calibration of instruments to
Determine the responses to the standards under controlled conditions. Measurement
of the instrumental response for eachsample under the same conditions as for the
standards. All measurementsmay be replicated to improve the reliability of the data,
the andtime but this has cost implications. Calculation of results and statistical
evaluation (Kealey, 2002: 4).
Precipitation Reaction Occurs when two or more soluble species combine to
form an insoluble product that we call a precipitate. The most common reaction is
metathesis reactio precipitate; in the which two compounds soluble ionic exchange
parts. When a solution of lead nitrate is added to a solution of potassium chloride,
for example, a precipitate of lead chloride forms. We usually write the balanced
reaction as a net ionic equation, in the which only the ions precipitate and Reviews
those Involved in the reaction are included. Thus, the precipitation of PbCl2 is
written as
Pb 2+ (aq) + 2Cl- (aq) PbCl2 (s)
In the equilibrium treatment of precipitation, how ever, the reverse reaction
describing the dissolution of the precipitate is more frequently encountered.
PbCl2 (s) Pb 2+ (aq) + 2Cl- (aq)
It is important to remember (Harvey, 2000: 139-140).
Inspection of a set of replicate measurements or results may reveal that one
ormore is considerably higher or lower than the remainder and Appears to be
outsidethe range expected from the inherent effects of indeterminate errorsalone.
Such values are termedoutliers, or suspect values, Because It is possiblethat they
may have a bias due to a determinate error. On occasions, the source oferror may
already be known or it is discovered on investigation, and the outlier an be rejected
without recourse to a statistical test. Frequently, however, this isnot the case, and a
test of significance such as the Q-test should be applied to asuspect value to
Determine whether it should be rejected and therefore not includedin any further
computations and statistical assessments of the Data (Kealey, 2002 : 35).
Analytes with high vapor pressures, such as volatile organics and dissolved
gases (eg, HCN, SO2) Easily can be lost by evaporation. Filling sample
containers to the brim so that they Contain no empty space (headspace) is the most
common method of minimizing volatilization. Solid samples can be topped with a
liquid to Eliminate headspace. The volatiles can not equilibrate between the sample
and the vapor phase (water) at the top of the container. The samples are Often held
at low temperature (40C) to lower the vapor pressure. Agitation Also during sample
handling should be avoided (Mitra, 2003: 19).
Significance tests involve; a comparison between a calculated
experimentalfactor and a tabulated factor determined by the number of values in
the set (s) ofexperimental of data and a selected probability level that the conclusion
is correct.They Several are used for purposes, such as:
a. To check individual values in a set of the data for the presence of
determinateerrors (bias);
b. To compare the precision of two or more sets of the data using Reviews their
variances;
c. To compare the means of two or more sets of the data with one another or
withknown values to establish the levels of accuracy.
Tests are based on a null hypothesis an assumption that there is no
significantdifferenceCompared being between the values. The hypothesis is
acceptedif the calculated experimental factor is less than the corresponding
tabulatedfactor, calculated experimental factor is less than the corresponding
otherwise it is rejected and there is said to be asignificant differencebetween the
values at the selected probability level. The conclusion shouldalways Clearly and
unambiguously be stated (Kealey, 2002: 34).
Determination of Cu (II) in Environmental and Industrial WaterEach
filtered environmental water sample (1000ml) was evaporated nearly to dryness
with a mixture of 5 mL of concentrated H2SO4 and 10 ml of concentrated HNO 3
in a fume cupboard following a method recommended by Greenberg et al. and was
then cooled to room temperature. The residue was then heated with 10 ml of de-
ionized water in order to dissolve the salts. The solution was then cooled and
neutralized with dilute NH4OH in the presence of 1 ?? 2mL of a 0.01% (w / v)
tartarate solution. The the resulting solution was then filtered and quantitatively
transferred into a 25ml calibrated flask and made up to the mark with de-ionized
water. An aliquot (1 ?? 2mL) of this pre-concentrated water sample was pipette into
a 10 ml flask Ca librat ed a nd the Cu (II) content (Sarker, 2013: 10)
Factors that Affect the condition of the water quality, etc. items, namely the
chemical components in the water that can be toxic to the organisms that live in
them. Chemicals that Affect water quality items, namely arsenic (As) the which are
naturally sourced from nature itself, and Also from human activities. The results of
arsenic measurements in the form of suspension and dissolved at 3 sampling
locations are shown in. It appears, either as a form of suspension or dissolved
remains in very low concentrations (lower than the device detection limit (Lasut,
2016: 34).
According Kealey, (2002: 26), numerical Reviews These two characteristics of
the data are the most important and the most frequently confused. It is vital to
understand the difference between them, and this is best illustrated
diagrammatically as in. Four analysts have each performed a set of five titrations
for the which the correct titer is known to be 20:00 cm3. The titers have been plotted
on a linear scale, and inspection reveals the following:
1. The average titers for analysts B and D are very close to 20:00 cm3 - Reviews
These two sets are therefore said to have good accuracy;
2. The average titers for analysts A and C are well above and below respectively
cm3 20:00 - These are therefore said to have poor accuracy;
3. The five titers for Analyst A and the five for analyst D are very close to one
another within each set. Reviews These two sets therefore both show good
precision;
4. The five titers for the five analyst, B and C are for analyst Widely spread within
each set - Reviews These two sets therefore both show poor precision.
An analyte and an interferent can be separated if there is a significant difference
in least one of Reviews their chemical or physical properties. Provides a partial list
of Several separation techniques, classified by the chemical or physical property
that is exploited. The simplest of physical properties that can be exploited in a
separation is size. The separation is accomplished using a porous medium through
the which only the analyte or interferent can pass. Filtration, in the which gravity,
suction, or pressure is used to pass a sample through a porous filter is the most
commonly encountered separation technique based on size. If there is a difference
in the mass or density of the analyte and interferent, then a separation using
centrifugation may be possible. The simplest of physical properties that can be
exploited in a separation is size. The sample, as a suspension angular (Harvey, 2000:
205-206).
D. APPARATUS AND CHEMICALS
1. apparatus
a. Test tube (4 units)
b. Test tuberack (1 unit)
c. Stir bar (1 unit)
d. Spiritus Burner (1 unit)
e. Tripod and Gauze (1 set)
f. Spot Plate (1 unit)
g. Spray Bottle (1 unit)
h. Rough Cloth (1 unit)
i. Smooth Cloth (1 unit)
j. Spatula (1 unit)
k. Porcelain (1unit)
l. Clamp (2 units)
m. Drop pipette (19 units)
2. Chemicals
a. Potassium Iodide-Sodium Sulphate solution (KI-Na 2S2O3)
b. Copper (II) Sulphate solution (CuSO4)
c. Acid chloride solution (HCl)
d. Nitric Acid solution (HNO3)
e. Zink solid (granules) (Zn)
f. Sulfuric Acid solution (H2SO4)
g. Silver Nitric solution (AgNO3)
h. Ammonium hydroxide solution (NH4OH)
i. Hydrogen Peroxyde solution (H2O2)
j. Acetic Acid solution (CH3COOH)
k. Silver Nitric solution 1% (AgNO3)
l. Ammonium thiocyanate solution (NH4SCN)
m. Ammonium Fluoride solution (NH4F)
n. Oxyn (C6H9NOH)
o. Barium Carbonate solid (Baco3)
p. Phenolphtalein indicator (pp)
q. Solid Sodium Chloride (NaCl)
r. Hydrargirum (II) chloride solution (HgCl2)
s. AresenOxyde solution (As2O3)
t. Nitric solution Cobalt (Co (NO3) 2)
u. Distilled water (H2O)
v. tissue
w. matches
x. filter paper
E. WORK PROCEDURE
1. Mercury Test with Cu (II) Iodide
a. 1 drop of KI-Na2SO3 solution was added into the spot plate
b. 1 drop of CuSO4 was added into the spot plate
c. 1 drops of HgCl2 was added and the mixture solution was stirred
2. Arsenic Test
a. Gutzeit Method
1) 3 drops of As2O3 as the sample was added into a test tube
2) Solid Zn was added into the test tube
3) 3 drops of H2SO4 was added into the test tube
4) Filter paper was added with 1 drop of AgNO3and covered at test tube
b. Silver Nitric
1) 3 drops of As2O3 was added into porceline
2) 3 drops of H2O2 and 3 drops of NH3 was mixtured and heated
3) Added 2 drops of CH3COOH
4) 2 drops of AgNO3 was added into porceline
3. Cobalt Test
a. Ammonium Thiocyanate and Aceton
1) 1 drop of Co(NO3)2 was dropped into the spot plate
2) 1 drop of NH4SCN 10% was added into the spot plate
b. The Existence of Fe ion
1) 1 drops of Co(NO3)2 was dropped into the spot plate
2) Some mg of NH4F was added into the spot plate
3) 5 drops of NH4SCN 10% was added into test tube
4. Chloride Test
a. Silver Chloride Precipitation
1) 1 drops of HCl was dropped into a test tube
2) 1 drop of oxyn was added to the test tube and it was shaken
3) 1 drop of HNO3 was added into the 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 1% AgNO3 was mixed and it was shaken in a test tube
b. Volatilization of Chloride Acid
1) NaCl solid was put into a test tube
2) 1 drops of HNO3 was added into the test tube
3) 3 drops of AgNO3 was added again into test tube
4) Heat was done and shakeen until bubbly
5. Sulfuric Test with BaCO3 and pp
a. 1 drops of H2SO4 was dropped into porcelain
b. 1 drops of BaCO3 was added into porcelain
c. Heat until dry
d. Some drops of pp was added into porcelain and it was shaken
F. OBSERVATION RESULT
NO ACTIVITY RESULT
4 AgNO3 + 3 drops 1%
G. DISCUSSION
Spot test is a qualitative analysis used to test micro and semi-micro to
compounds or ions. Spot tests were used in this experiment because it can identify
the components in a chemical substance that produces sediment, color, and gas.The
basic principle in experiments spot test is the analysis of the levels of a substance
based on the intensity of color or precipitation of the complex formed solution.
While working principle that is by adding a reagent to a material suspected to
contain ingredients that will be identified, with the end result that a typical color
change or precipitate is formed.
1. Test mercury with Cu (II) Iodide
This experiment aims to identify the presence of mercury with a solution of Cu
(II) iodide.Solution to be tested, namely mercury. In this experiment used KI.
Na2SO3 solution that serves to liberate iodide then CuSO4 solution that frees Cu 2+
ions causing color changes to yellow solution. This color change occurs due to the
iodide ion that is as a reducing agent, so that the iodide ion will reduce copper (II)
to copper (I).
The next process solution was added with HgCl2. Addition with HgCl2 will
yield an orange. The addition of HgCl2 was caused by copper ions reduce mercury
(II) to their metal. That produce color depending on the amount of mercury
contained in the test solution HgCl2. The solution obtained shows the presence of
mercury in the solution of this. Its can show in a solution containing mercury. Occur
discoloration caused because iodide ions precipitate mercury (II) from the solution
as a precipitate orange (HgI2), this precipitate soluble iodide ion redundant because
of the formation of the complex tetra iodo merkurat (II) (HgI4)2.
This is consistent with the theory that if mercury is reacted with CuI2 will
change color to red or orange color (Sugiyanto, 2003: 164). The full reaction:
4KI.Na2SO3 + 6CuSO4 2CuI2 + 4CuSO3 + 4Na2S2O4 + 2K2SO4
(Potassium Iodide- (Copper (II) (Copper (II) (Copper (II) (Sodium (Potassium
Sodium Sulphate) Sulphate) Iodide) sulfites) Thiosulfate) Sulphate)
(colorless) (blue) (yellow)
In this experiment, no iron was added, but because cobalt has the same
2+
properties as the iron so that when the NH4F reacts with nitrate and Co cobalt
into cobalt ion Flurida which reacts with NH4 SCN forming cobalt tiosionat dark
green.
4. test chloride
In this experiment aims to identify the presence of chloride in the sample
with the two methods, namely precipitation as silver chloride in the presence of
other halide and testing with hydrochloric acid volatilization.
a. With sebaal precipitation of silver chloride in the presence of other halides
Test chloride by precipitation as silver chloride in the presence of other
halides, indicating a positive test containing chloride characterized by the formation
of white sediment and turbidity in the solution. Where HCl solution was treated
with a solution of H2O2 and HNO3 then heated and then added 1% AgNO3 produce
white precipitate and turbid solution. HCl solution serves as a test solution, a
solution H2O2 serves as an oxidant that will oxidize free halogen Bromide (Br) and
iodide (I-) becomes Brom and Iod. Oksin solution to function when progress will
halogenated phenolic compounds by halogen-free (Br- and I-). HNO3 solution
serves to provide an atmosphere in hydrochloric acid that does not oxidize by H2O2
and heating functions for vaporation other halides (Br- and I-) accelerate the
reaction and also causes the formation of salt stick to the porcelain crucible. AgNO3
solution serves to react with Cl- forming AgCl which precipitates and make the
solution cloudy, while the reaction is:
C6H9NOH C6H9NCl + HCl + H2O
(Nodes) (nodes) (nodes)
C6H9NCl C6H9NOH + HCl + H2O2
(Nodes) (nodes) (nodes)
Cl + AgNO3 H+ AgCl + HNO3
(Clear) (white precipitate) (clear)
BIBLIOGRAPHY
Harvey, David. 2000. Modern Analytical Chemistry. America. The McGraw-Hill
Companies
Ibnu, Sodiq, et al. 1. 2004. Analytical Chemistry Malang: The Malang State
University.
Lasut, henry e. Kawung, Nickson j. And Lasut markus t. 2016. The content of arsenic
(as), the form of the suspension and dissolved in the waters of the bay of
Manado. Journal coastal and tropical sea. volume 1 number 1 ISSN 95 115
2016.