REPORT

MODULE GRANTS WRITING

COURSES
ANALYTICAL CHEMICAL PRACTICE

by:
SYARIFUDDIN LIONG

CHEMISTRY DEPARTEMENT
FACULTY OF MATHEMATICS AND SCIENCE
HASANUDDIN UNIVERSITY
DESEMBER
2018

1
 FOREWORD

The Analytical Chemistry practicum module is a textbook intended for

chemistry students in particular and other fields of science that use chemical
analysis. The material presented in this module is a gravimetric analysis method
which describes how to prepare, weigh, dissolve, settle, filter, heat up / massage,
weigh, and calculate the results of the analysis.
As ordinary people, we have limited ability to realize that this module is still
far from perfection. We hope that for the users of this module, if there is
something that is unclear and difficult to understand, please ask for an explanation
on the reference book written in this module's bibliography. You can also contact /
ask directly to the module writer, in shaa Allah we are ready to serve your
questions
Hopefully the author of this module, hopefully can be useful for all interested
people, analytical chemistry, and hopefully what we have done is worth
worshiping by Allah SWT, Aamiin, aamiin Ya Rabbal Alamiin

Makassar, December 2018

Author
Syarifuddin Liong

2
 EDUCATIONAL IDENTITY

Department : Chemistry
Name of course : Analytical Chemistry Practice
Number of credits :2
Lecture of courses : 1. Dr. Hj Nursiah La Nafie, M.Sc
2. Dr. Syarifuddin Liong, M.Sc.
3. Wa Ode Rustiah, S.Si., M.Sc.

LEARNING GOALS:
Explain the work principles of qualitative and quantitative chemical
analysis both conventionally and modern using Electrochemical
(conductometry) tools, spectrophotometers UV-VIS, SSA, GC. or
IR.
Prerequisite courses: Measurement and Separation Techniques I and II
Course Description:
Discusses qualitative analysis, separation of cation groups and
anions and their identification. Conventional quantitative chemistry
includes, Gravimteri, volumetry consisting of acid-base,
precipitation, oxidimetry and complexometry titration. The principle
of application of UV-VIS, SSA, GC and IR spectrophotometers in
chemical analysis is also used to identify a compound both
qualitatively and quantitatively
Gravimetric scope:
Gravimetric analysis includes the method of weighing using
analytical balance and sample containers (weighing bottles, watch
glass, and petri dish), then dissolving the sample with various
kinds of solvents and tools that are adjusted for the nature of the
sample to be dissolved in containers (glass cups, crucible perselin,
teflon, bomb colimeter). Deposition systems can be used either
inorganic or organic substances which are adjusted to the material

3
being analyzed. Filters can be used with non-gray filter paper,
Gooch or glass crucible. Then warm up in the oven at 110 – 120
o
C for deposits that generally use organic reagents as settling.
Spawning in electric furnaces at temperatures of 800 – 1000 oC for
deposits of organic reagents. The last part is weighing and
calculating to determine the percentage of the material being
analyzed.

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 TABLE OF CONTENTS TITLE
PAGE .................................................................................................................... i
FOREWORD ........................................................................................................ ii
COURSE IDENTITY ........................................................................................... iii
TABLE OF CONTENTS ...................................................................................... iv
LABORATORY CONDITIONS .......................................................................... v
GRAVIMETRY ANALYSIS ............................................................................... 1
1. SAMPLE PREPARATION TECHNIQUES.................................................... 1
2. METODE CONTROL ..................................................................................... 3
3. REFERENCE REAGENT ............................................................................... 8
4. FILTER TECHNIQUES .................................................................................. 15
5. APPLICATION WASHING ............................................................................ 17
6. HEATING / BREAKFASRING ...................................................................... 19
7. CALCULATIONS IN GRAVIMETRY ANALYSIS ...................................... 19
8. APLICATION OF ANALYSIS GRAVIMETRY METHODE ....................... 20
8.1 SULFAT ANALYSIS ................................................................................ 22
8.2 MAGNESIUM ANALYSIS....................................................................... 25
8.3 CHLORIDE ANALYSIS ........................................................................... 29
8.4 ANALYSIS OF IRON ............................................................................... 32
8.5 COPPER ANALYSIS ................................................................................ 34
FORMATIVE TEST ............................................................................................. 37
1. MULTIPLE CHOICE ...................................................................................... 37
2. PROBLEMS OF ESSAY ................................................................................. 40

BIBLIOGRAPHY ................................................................................................. 42

ANSWER KEYS .................................................................................................. 43

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 PROCEDURES FOR PRACTICE & WORK SAFETY
IN LABORATORY
Every worker in the laboratory has the risk of various types of accidents
that can occur at any time if they do not comply with the rules that are available.
Adherence to the following rules can avoid or reduce the risk of accidents that
may occur. Therefore if you are in an Analytical Chemistry laboratory, obey the
following rules.
1. Student already in the laboratory five minutes before the practicum hour
begins, and has stopped the practical experiment 30 minutes before the time is
over to make a lab report
2. Before you work, learn in advance the location of the tap, fire extinguisher,
shower, and fire protection. Learn carefully about each work procedure and do
not hesitate in using laboratory equipment
3. Provide a log book that must be filled in from the start and after the practicum
to record all the activities that you did during the lab so that you did not forget
when writing the report.
4. Use a practice coat to protect clothing, use time glasses to dilute strong acids or
melt substances. Wear closed shoes (not sandals) while working in the
laboratory. When boiling a solution in a test tube do not point it to yourself or
to a friend. For those with long hair, tie it neatly.
5. Chemicals are generally toxic / dangerous, even some of them are very toxic
and some acids / bases are corrosive, avoid contact with skin
6. Do not bring food / drinks into the laboratory, do not drink / eat using
laboratory glassware and smoking is strictly prohibited in the laboratory.
7. Use the filler to take strong acids / bases, it is strictly forbidden to use mouth
(suck)
8. Use reagent substances as little as possible (remember green chemistry) many
experiments fail because reagents are very excessive. If only a few drops
should be applied, as much as possible use a drop pipette or drop bottle.
9. Reactions / substances that emit toxic or sharp-smelling gases or vapors may
only be done in fume hoods or open spaces

6
10. Strong acids must be diluted by pouring the acid gradually into the water
while stirring slowly. Do not reverse it can cause an explosion.
11. If you want to isolate a solution, you should use a porcelain dish on top of a
water bath, if you use direct fire, use the gauze on low heat.
12. Before and after work, the tools used must be washed before being returned /
stored.
13. Group activities:
a. Preparation of materials and tools
b. observation
c. Data collection
d. calculation of observations
e. preparation of reports
14. Don't work alone in the laboratory. If you do not understand a work
procedure, you should ask the assistant or lecturer on duty.
15. Analytical scales are only used to weigh primary raw materials, samples to be
analyzed, or the weights used in calculations. It is strictly forbidden to use
analytical scales that are only for making reagent solutions.
16. Don't forget, START YOUR WORK BY PRAYING TO GOD, I hope all
activities carried out get protection from Allah, SWT, AMIN

7
 GRAVIMETRY

The gravimetric method is a method of analysis that is based on careful

measurement of mass (weight). There are two types of gravimetric outline. 1.

Deposition method, this way the analyte or sample is converted into an insoluble,

filtered precipitate, washed so that it is free of impurities, then changed to form a

chemical composition which is known precisely through heating / flushing. This

chemical composition is weighed to be used in calculating the results of the

analysis. 2. Evaporation method. The analyte is heated at a certain temperature to

remove the content of analsized material, such as the determination of the water

content in the salt, the crystalline water in the salts contains crystalline water.

The steps that must be taken in the gravimeri analysis are as follows.

1. SETTLEMENT OF EXAMPLE SOLUTIONS

In the gravimetric analysis the samples that can be analyzed can be gases,

solutions, and solids. In this material we will discuss the procedures for preparing

solid samples which may dissolve directly with distilled water or dilute acids. For

substances that are easily dissolved, the sample is weighed and put in a glass cup

and covered with a watch glass. Then the solvent is poured carefully with the

glass stirring rod which the bottom end touches the wall of the cup glass, and the

watch glass cover is slightly shifted so that if formed gas can be free to exit. If the

gas formation is complete and the substance is completely dissolved, rinse the

8
watch glass with a small amount of distilled water in the sample solution. If

necessary, further heating is usually carried out in an acid chamber.

Substances which are difficult to dissolve or are less soluble in acid, are

usually smelted with the right reactor. The most commonly used smelting reagent

is either single anhydrous sodium carbonate (rarely done), but is generally mixed

with Potassium nitrate, sodium / potassium hydroxide, sodium peroxide. The

results of this melt are then dissolved with dilute acid.

Hydrochloric acid, nitric acid, both dilute and concentrated. If it cannot

dissolve with a mixture of concentrated hydrochloric acid and concentrated nitric

acid (aquaregia), it can be melted using sodium peroxide (Na2O2) or with a

mixture of sodium carbonate (Na2CO3) and potassium carbonate (K2CO3) and

others. The results of this melt are then dissolved with dilute acid, and the

insoluble part in general is silicate. This solution is then separated by filtration,

the filtrate is used for the desired metal analysis. The residue left on filter paper

can be used for silicate analysis.

In addition to the smelting method above, lithium metaborate can be used

as a smelter with the following advantages / benefits.

1. It does not liberate gas during smelting or when dissolving melt so that the

danger of losing the analyzed substance is very small.

2. Melting with sodium metaborate is time faster and can be done at a lower

temperature than the previous smelting method.

3. The weight loss of the platinum plate with sodium metaborate smelting is

smaller than using sodium carbonate

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4. Many elements can be analyzed in the fused acidic solution with sodium

metaborate without perly separation

5. Lack of using sodium metaborate as a smelter, just because the price is quite

expensive

2. IMPLEMENTATION METHOD

The way of settling is the most important part in gravimetry, because this is

the part that most determines the success of this analysis. The factors that

determine the success of the analysis by precipitation are as follows.

1. Precipitation should be carried out in a hot solution because solubility

generally increases with increasing temperature, (not all)

2. The solubility of sediment should not occur or its solubility must be as small

as possible so that it does not affect the percentage of analytes analyzed. The

loss / solubility does not exceed the minimum amount detected by the usual

analytic balance, which is 0.1 mg

3. Physical properties of deposits

The physical properties of sediment must be easily separated from the solution

by a filtration system, and can be washed until it is free of dissolved

impurities.

4. Deposits must be converted into a pure substance whose composition is

known with certainty. To obtain the exact and exact composition, the

precipitate must be heated or spawned at a certain temperature (will be

discussed later)

10
 The purity of the sediment depends on the substances present in the

solution, both before and after the addition of reagents and the proper deposition

conditions. To find out the factors that influence the deposition process then the

following briefly outlines the problems related to this.

2.1 FACTORS AFFECTING THE PROCESSING PROCESS

Some problems that may arise in certain deposits such as coagulation or

flocculation of a colloidal dispersion of solid substances in the form of fine grains

which allow for peptization during filtration of deposits.

2.1.1 THE COLLOIDAL STATE

The characteristics of the type of colloidal particles that are often found in

inorganic analysis are as follows.

1. The particles show the Tyndall effect when viewed with appropriate light

irradiation.

2. The particles can be separated from the solution by using a mixture of collions

or cement with the dialysis process.

3. Electrically charged particles migrate under the influence of the appropriate

differential

4. The particles have a large surface area.

For simplicity, colloids are divided into two main groups namely liophobic

and liophilic colloids. To find out the properties of each colloid is shown in the

following table

11
 Lyophobic Colloids Lyophilic colloids

1. The dispersion (or sols) are only 1. The dispertion are very viscous; they set to
slightly viscous. Example: sols of jelly-like masses known as gels, example:
metal, silver halide, metallic sols of silicic acid, tin(IV) oxide, gelatin
sulphides, etc.
2. A comparatively minute 2. Comparatively large concentration of
concentration of an electrolyte electrolytes are required to cause
results in flocculation. The change precipitation (salting out). The change is,
is, in general, irreversible; water in general, reversible, and reversal is
has no effect upon the flocculated effected by the addition of a solvent
solid (water)
3. usually this colloid is electrically 3. Most lyophilic colloids change easily
charged of definite signs, which can the electrical charge sign for example in
be changed only by special methods charged acid (+) in a charged base (-)

Colloids are flocculated with an electrolyte, the ions which are charged

opposite to the colloidal charge will be adsorbed differently on the surface, the

greater the valence of an ion being adsorbed. In all conditions the sediment will be

contaminated by surface adsorption. If the precipitate is washed with distilled

water, some of the adsorbed electrolyte will disappear, but new problems will

arise. The electrolyte concentration in the supernatant will decrease so that the

deposits can turn into colloidal solutions again. So to avoid this event, washers

containing electrolytes are usually used.

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2.1.2 THEORY OF VON WEIMARN ABOUT SUPERSATURATION

According to von Weimarn, saturated passing plays an important role in

determining the particle size of deposits. He concluded that the initial velocity of

precipitating was proportional to Q-S / S, where Q is the total concentration of the

substance to be deposited while S is the solubility of equilibrium. Q-S shows a

saturated state which is clearly illustrated in the von Wimarn results in the

formation of barium sulphate originating from barium which is reacted with

manganese sulphate. The results of this experiment show that the particle size of a

sediment will decrease with increasing concentration of reagents. To produce a

crystalline precipitate, the adsorption error must be as small as possible, so the

drying can be done easily, the Q-S/S must be small too. To reduce the value of Q -

S/S then Q must be minimized, because precipitation must be perfect in a

relatively short time and the volume of the solution should not be too large so that

precipitation can be useful in the analysis. Another way that can be done is to

increase the value of S. For example barium sulfate has a fifty times greater

solubility in 2M hydrochloric acid than in distilled water.

The procedure steps that can be done to minimize these disorders are as follows.

1. Precipitation should be done in a hot solution, because solubility in general

increases with increasing temperature.

2. Precipitation is carried out in an aqueous solution by slowly adding the reagent

while stirring. Adding slowly can cause the particles to settle first to act as the

nucleus which will be followed by the formation of the next sediment.

13
3. Reagents that are used are often added to increase the solubility of the sediment

to give rise to larger primary sediment particles.

4. Work methods commonly used to prevent the occurrence of a saturated state,

with deposition in a homogeneous solution.

2.1.3 PURPOSE OF DEPOSITS

If the sediment separates in the solution, it does not mean that the deposit

is pure enough. But it may contain various impurities which are affected by the

nature of the sediment and the conditions at the time of deposition. Sediment

contamination caused by substances that dissolve in the mother liquor, commonly

called coprecipitation. There are two different types of coprecipitation, the first is

related to the adsorption on the surface of the particles affected by the solution.

Second is occlusion is the growth of particles from foreign substances

Surface adsorption is generally greatest in deposits similar to gelatin and

the smallest in crystalline macro deposits. Deposits with ionic grids appear to

follow the rules of adsorption of Paneth-Fayans-Hahn, which states that the

strongest ion adsorbed by an ionic (crystal lattice) substance is the ion that forms

the hardest dissolved salt. For example, sulfate is very difficult to dissolve, so

calcium ions are adsorbed more strongly than magnesium ions, because calcium

sulfate is less soluble than magnesium sulfate. Silver iodide adsorbs silver acetate

stronger than silver nitrate at the same consistency, because the solubility of silver

acetate is smaller.

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2.1.4 PRECIPITATED CONDITION

There are no rules that have been established in general in the deposition

process, but we can follow the facts described earlier. To obtain the maximum

deposit we can follow the steps below.

1. Precipitation should be carried out in a dilute solution, taking into account the

solubility of the sediment, the time needed to filter which can reduce

coprecipitation error

2. Reagency must be added slowly while stirring continuously. This stirring

serves to maintain a small saturation through and helps the growth of large

crystals.

3. Precipitation is carried out in a hot solution, as long as the solubility and

stability of the sediment have no effect on temperature.

4. Crystal-shaped deposits must digest as long as possible or at least overnight,

except in cases that can lead to post-precipitation. Usually digestion is carried

out on a water bath. This process reduces the effect of coprecipitation and gives

deposits that are easier to filter.

5. The precipitate must be washed with the appropriate dilute electrolyte solution.

Aquades tend to cause peptization.

3. REFERENCE REAGENTS

Sedimentary reagents should be specific and selective for the chemical

elements or species to be analyzed so that they can reduce / eliminate disturbing

ions from the material to be tested. Sedimentary reagents that can used in

15
gravimetry there are several good types as organic and organic compounds

reagents. In this material only organic reagents are discussed because of their

specific reaction and special treatment.

3.1 ORGANIC DEVOTION FOR DEVOTION

Organic reagents generally form chelate compounds with cations, both

containing basic functional groups (electron donors) and groups containing acidic

functional groups. The metal will interact with these two groups to form a

hetorocyclic ring. Some organic sediments will be described below.

a. Dimethyl glioksima

This reagent was discovered by L. Tschugaeff but was used by O. Brunck

for the analysis of nickel in steel. This reagent forms bright red deposits

with nickel (Ni (C4H7O2N2)2). Precipitation is carried out in a buffer

ammonia base containing ammonium acetate and acetic acid buffer. The

NiDMG complex is weighed after being heated at a temperature of 110 –

120 oC. This reagent can only be used as needed, because if it is too

excessive it can cause DMG to settle because it is very difficult to dissolve

in water. Another disadvantage if the use of this reagent is excess can

increase the solubility of deposits in a mixture of water-ethanol.

Determination of nickel content in this way can be disturbed by the presence

of Fe3+, Al3+, and Bi3+ ions, but this interference can be prevented by the

addition of tartrate or citrate.

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b. Oxin (8-hydroxyquinine)

Oxine or 8-hydroxycinolin is also called 8-quinolinol (C9H7ON), forming

derivatives with metal ions that are difficult to dissolve with combination M

(C9H6ON)2 for metals with four coordination numbers such as Mg, Zn, Cu,

Cd, and Pb). If the coordination numbers are six such as Al, Fe, and the

combination Bi is M (C9H6ON)3 and M (C9H6ON)4 for eight coordination

number metals such as thorium and zirconium.

Oxin is a crystalline solid that is colorless and difficult to dissolve in water.

Making reagents if you want to be used as a sediment, can be chosen in the

following ways.

• Two grams of pro-oxin analysis were weighed and then dissolved in

100 mL of 2M acetic acid, add ammonia solution drop by drop until

turbidity arose, to clear the solution of a little acetic acid. This solution

is quite stable in the long run, especially if stored in a colored bottle.

• Two grams of pro-oxin analysis weighed then dissolved was dissolved

in 100 mL of methanol or ethanol or acetone (reagents cannot be used

for Al analysis). This solution is only stable in ten days if protected

from light.

The general condition of the experiment if using an oxin reagent as a

sediment is as follows.

Reagents are added to the sample solution in cold conditions or temperatures

around 50 – 60 oC until a yellow or orange color appears and the supernatant

shows an excess reagent

17
 1. The precipitate is coagulated in a short time at a temperature of less than 70
o
C

2. Deposits can be filtered with filter paper or one of the filtering devices

discussed at the deposit screening point.

3. The filtrate must be yellow or orange which indicates the presence of excess

settling reagents. If turbidity arises, take a few mL of filtrate then heat it. If

turbidity is lost by heating means the reagent is crystallized and does not

interfere with the analysis. But if it does not disappear means the deposition

is less than perfect, then the mother liquor is added to the reagent to

complete deposition.

4. Washing of sediment can be used hot or cold water (depending on solubility

of metal oxynate) until the filtrate is colorless.

5. Washed deposits can be dried at a temperature of 105-110 oC (if the oxinate

complex is not hydrated). If the sediment contains hydrated water, the

temperature can be increased up to 130 – 140 oC for a long time but

decomposition may occur. Sometimes it can be spawned to form the metal

oxide.

c. KUPRON (BENZOIN-α-OKSIMA)

The kupron compound forms a green-copper precipitate (CuC14H11O2N) in a

dilute ammonia base, and is dried at 110oC. To avoid interference with other

elements, the solution must be maintained in an atmosphere of ammonia base and

addition of tartrate. Kupron reagents are specific to copper so they can be

separated from metals Cd, Pb, Ni, Co, Zn, Al, Fe if the amount is continuous.

18
 In very acidic solutions, cupron acid can settle with Mo and W ions

quantitatively. The molybdate complex should be dispersed at a temperature of

500-525 oC to form stable MoO3 oxides to be weighed. Kupron is a crystalline,

white solid, 152 oC melting point, difficult to dissolve in water, easily soluble in

ethanol.

d. 1-NITROSO-2-NAFTOL

Organic reagents can precipitate quantitatively Co, Fe (III), Pd, and Zr

metals in a slightly acidic solution. This reagent can also precipitate partially (not

quantitatively) metals, Sn, Ag, Bi, Cr (III), Ti, W (IV), and V (V). Elements of Pb,

Cd, Hg, As, Sb, Be, and Mg. Reaction 1-nitroso-2-naphthol is used to separate

cobalt and nickel in large quantities but iron must be separated first. A

considerable amount of red brown color deposits can be obtained in the

atmosphere of dilute hydrochloric acid with the molecular formula Co

(C10H6O2N)3. The precipitates obtained are not of sufficient purity, so careful

spawning can give deposits with the formula Co3O4 which can be quantitatively

weighed. 1-Nitroso-2-naphthol in the form of brown powder, melting point

109 oC, water insoluble. The reagent was made by weighing 4 grams then in 100

mL glacial acetic acid then adding 100 mL of hot water, cool and strain. This

reagent must be made when use cannot be stored.

e. ACID 4-BROMOMANDELAT

4-bromomandellic acid (C6H5CH (OH) COOH) also called mandelic acid is

a reagent that is very selective and sensitive to zirconium (Zr), which settles in a

slightly acidic atmosphere. Mandelic acid must be used in large concentrations so

19
that the excess is very difficult to remove by washing, unless washed with 2%

HCl heat with 5% mandelic acid. The precipitate is then spawned so that the oxide

can be carefully weighed. The deposition system is well carried out in an

atmosphere of hydrochloric acid (3-5 M) in hot conditions. The ions that interfere

with the use of this reagent are Cu (II), Cd (II), Hg (I), Sn (II), Th (IV), Sb (III),

and Fe (III).

Mandalic acid is a solid white crystal, the melting point of 118oC, is less soluble

in water. For precipitation, a concentration of 0.1 M is used and the solution is

very stable.

f. SALISILALDEHIDA OKSIMA

Salisilaldehyde oxima compounds are used to determine copper (Cu) to

form yellow-green Cu(C7H6O2)2 deposits in an acetic acid (pH 2.6). These

deposits are very disturbed by Iron (III) because they are deposited, but other

metals such as Ag, Cd, Hg, As, and Zn do not have a significant effect.

Salisilaldehyde Oxima can also be used with metals as in the analysis of Pb, Bi,

Zn, Ni, and Pd. Acidity (pH) is a very important factor especially for separating

divalent metal from one another. Copper settles perfectly at pH 2.6, nickel settles

at pH 3.3, therefore to separate Cu and Ni the pH must be maintained between

2.6 - 3.3.

The bismuth ion reacts with this reagent to form yellow-bright base salt

deposits in a neutral atmosphere and is difficult to dissolve in water. In order to

obtain the exact and exact chemical composition, these deposits must be spawned

20
to form bismuth oxide (Bi2O3) which can be weighed. Lead can be deposited

quantitatively by reacting salicylaldehyde oxima to form a yellow PbC 7H5O2N

complex at pH 8.9 or more with an ammonia base, allowing to separate Pb, from

Ag, Cd, and Zn. Palladium is deposited as yellow Pd (C7H5O2N) 2 in an acidic

atmosphere, so it can be separated from Pt and Ni.

Salicilaldehyde oxima is a solid colored crystal, the melting point of 57 oC

is less soluble in water. The reagent is made by dissolving 1.0 gram of

salisilaldehyde oxima in 5 mL of 95% ethanol and then diluting it to a volume of

100 mL with distilled water, heating the temperature below 80 oC, the mixture is

shaken until homogeneous and filtered if necessary and storing in a colored bottle

or dark bottle. This reagent can break down in the solution so that it cannot be

stored for more than three days.

g. ACID KUINALDAT.

Organic reagents form insoluble complexes with cations of copper,

cadmium, zinc, manganese, silver, cobalt, nickel, lead, mercury, iron (II),

palladium (II), and platinum (II), and form insoluble base salts with iron (III),

aluminum, beryllium and titanium cations. The formation of complex compounds

with quarantine which is difficult to dissolve is strongly influenced by the pH of

the solution. This reagency has two types commonly used in practice, namely

quinaldic acid or in the form of sodium salt with a concentration of 2% in water.

Aluminum replaces acidic hydrogen from the hydroxyl group, when the

unused electron pair on the nitrogen atom is donated to aluminum to form a six

ring.

21
3.2 BENEFITS AND LACK OF ORGANIC CONTROL

The advantages of the technical reagent will be explained below.

1. Some organic metal compounds are difficult to dissolve in water, so the

metal can be deposited quantitatively

2. The relative molecular mass of organic settling is large enough so that

metals in small concentrations can produce considerable deposits.

3. Some organic reagents are quite selective, only precipitate certain metals.

4. The deposits obtained with organic reagents are often rough and abundant

crystals that are easy to handle.

5. In some cases, metals deposited with organic reagents, deposits can be

filtered and then dissolved and the molecules organic titrated (titrimetric

method)

While the lack of organic reagents is as follows.

1. Some chelate compounds do not have a stable form for weighing so that

they cannot be used as determination of content

2. It is possible that sediment is not sufficiently pure because the chelating

can pollute the deposits.

4. TECHNIQUES FOR FILTERING

Filtering is the separation of the sediment with the mother's solution, the

purpose is that the sediment and filtering equipment are free from the solution.

There are several types of sediment filters in gravimetry such as;

a. Non-gray filter paper using a funnel

b. Asbestos filter (Gooch cup)

22
 c. The porous plate is made of heat-resistant glass (glass filter cup masir)

Selection of filter media will be explained below.

a. Use filter paper Filter paper that can be used in gravimetric analysis is a non-

gray filter paper or very low ash content. This filter paper is placed in a funnel
o
that has an angle as close as possible or around 60 and a stirring rod that is

about 60 cm long which is used as a tool to move the sediment from the cup to

filter paper. The paper types commonly used in gravimetric analysis are shown

in the following Table

Filter Paper fast Medium Slow

holding holding holding
Coarse particles Medium particle Fine particle
No.541 No.540 No.542
Ash content (mg) 0.08 0.08 0.09
The ash content shown for filter paper is 12.5 cm in size

b. Crush Gooch

This type of crucifix is tall in shape with basically many small holes. This hole

is covered with asbestos porridge which is poured into the crucible which is

equipped with a vacuum pump so that the water contained in the asbestos pulp

will be pulled until the Gooch crucible is dried. Crush Gooch is generally used

for deposits using organic reagent deposits.

c. glass masir

glass masir is made of glass which holds porous discs made of masir glass,

which is attached by melting in crucible. These filter discs have varying pore

sizes which are expressed with numbers from 0 (roughest) to five (most

subtle). The diameter between pores is shown below.

23
 Pored 0 1 2 3 4 5

Pore dimeter 200-250 100-120 40-50 20-30 5-0 1-2

(µm)

Pore number 3 is used for medium and pore particle size deposits number 4

for fine deposits. This crucible masir glass is generally used for sediments that

cannot be released and are easily oxidized with air, so that they are easily

protected from light.

5. DEPOSIT EDUCATION

The filter and precipitate filter must be selected according to the nature of

the sediment so that the filtering time is not too long.

Washing solutions commonly used in the analysis are divided into three

groups;

1. A solution that prevents deposits from becoming colloidal.

These events tend to occur in gelatin-like deposits, or in flocculation, but

rarely occur in crystalline deposits. The washing solution should contain

eletrolite which does not react with deposits during the washing and heating /

letting process. For example, dilute ammonium nitrate solutions used to wash

iron (III) hydroxide deposits and 1% nitric acid were used to wash silver

chloride deposits.

2. Solutions that minimize sediment solubility.

Washing solutions containing one ion ally with precipitate can be used in

small concentrations. Facts show that the sediment is less soluble in the

24
 presence of these allied ions. Most salts are difficult to dissolve in alcohol and

other organic solvents, so sometimes used organic solvents can be used for

washing sediment. Often times a mixture of organic solvents with distilled

water is used, or with a dilute electrolyte.

3. A solution that prevents hydrolysis

If the sediment is a salt of weak acid and less soluble in distilled water,

then the sediment tends to undergo hydrolysis and its hydrolysis dissolves as a

base, so the washing solution used should be alkaline as well. For example

magnesium hydrogen phosphate can be hydrolyzed to produce HPO42- and OH-

ions. To avoid this hydrolysis process, a dilute ammonia solution should be

used for washing these deposits.

Before filtering, it should be noted that the sediment and supernatant are

well separated, so that when pouring supernatant through the stirring rod into the

sediment filter container does not enter into the funnel. After the supernatant is

used up, add the washing solution then stir until homogeneous, let stand for a few

moments so the sediment and superanate separate well. Then move the

supernatant to the filter tool in the same way before.

Repeat this work three to five times, so that the deposits are free from

impurities which are usually carried out qualitative tests. This process is usually

called enaptour (deposited then the supernatant is poured into a funnel). After the

preparation is done several times, the last part of the phytate is tested qualitatively.

If the results of a positive qualitative test of the material being examined, the

25
washing is continued until it is free from the tested substance. If the deposits are

clean of impurities, then follow the steps below.

6. HEATING / BREAKING ON IN

After the sediment is filtered and washed until it is free of impurities, the

precipitate must be converted into a definite and constant chemical composition

either by heating at a certain temperature or by spreading so that the results can be

carefully and precisely weighed. The next work depends on the nature of the

deposits and the nature of the filter media. Deposits that use organic reagents as

settling are generally only used for heating at a certain temperature in the oven.

Whereas an organic settling reagent is usually carried out by an exfoliation, except

for high temperature unstable deposits such as silver chloride. Furthermore, the

method of heating or injection will be explained in every experiment in the

practical reference.

7. CALCULATIONS IN ANALYSIS OF GRAVIMETRY

The results to be obtained in gravimetric analysis are generally calculated

from two measurement results (weighing), namely the mass of the sample and the

mass of the results of the analysis which is known to be a definite composition.

The following is an example of calculating the results of gravimetric

analysis.

Analysis of sulfur content from a sample weighing 0.8423 grams is converted into

sulfate form and deposited as BaSO4. After filtering, washing, burning, cooling,

then weighing until the dry weight is obtained 0.3148 grams of the remaining

26
incandescent weight. Calculate the percentage of sulfur in the sample. Ar. S = 32;

Ba= 137; O = 16

Answer.

Known: sa mple weight = 0.8423 g

Incandescent weight = 0.3148 g

Gravimetric factor = Ar S / Mr BaSO4

= 32/233

= 0.1373

Percentage S in example

Gravimetric factor x incandescent remaining weight

= 𝑥 100%
Sample weight

0.1371 𝑥 0.3146
= 𝑥 100%
0.8432

= 5.1184%

= 5.11%

Note: a gravimetric factor is a comparison between the relative atomic mass of an

element or compound that is searched for by the relative molecular mass of the

compound being weighed

8. APPLICATION OF GRAVIMETRY ANALYSIS

Gravimetric analysis can be used almost all elements in the periodic

table, both in the form of organic and organic compounds. The following table

shows some elements of each group that can be analyzed by the gravimetric

method.

Table of elements that can be analyzed by the gravimetric method

27
 Periodic Table Element Deposited as Weighed as

IA K KClO4 KClO4

IIA Ca CaC2O4 CaO, CaCO3

IIIA Al Al2O3.xH2O Al2O3

IVA Si SiO2xH2O SiO2

VA P MgNH4PO4 Mg2P2O7

VIA S BaSO4 BaSO4

VIIA Cl AgCl AgCl

IB Ag AgCl AgCl

IIB Zn ZnNH4PO4 Zn2P2O7

IIIB Sc Sc. Oxinate Sc. Oxinate

IVB Ti Ti.kufferat TiO2

VB V HgVO3 V2O5

VIB Cr Cr2O3.xH2O Cr2O3

VIIB Mn MnO2 Mn2O3

VIII Fe Fe2O3.H2O Fe2O3

Co CoS CoSO4

Ni NiDMG NiDMG

Note: DMG = dimethyl glioksima

In this module several methods of gravimetric analysis will be presented, among

others.

28
1. ANALYSIS OF SULFATE IN GIPS

Work principle;

Sulfate ions are deposited with barium ion as barium sulfate in the acid

atmosphere and weighed as barium sulfate.

Reaction:

SO42- + Ba2 + → BaSO4

BaSO4 + C → BaS + CO

BaS + H2SO4 → BaSO4

Tools used:

Analytical balance

Desiccator

Glass cupper

Erlemeyer Funnel

Non-gray filter paper

Banners

Electric heater

Furnace

Statif

Ring

Test tube

Drop pipette

Water bath

Reagent

29
Dilute hydrochloric acid

Barium chloride

Cast

Nitric acid

Procedur

1. Weigh the sample carefully around 0.5000 - 1.0000 grams using a weighing

bottle

2. Transfer it to a 400 mL glass jar and add the distilled water slightly while

stirring until all the samples are runny.

3. Add 0.5 mL concentrated hydrochloric acid and dilute with distilled water

until the volume is around 150-200 mL.

4. Heat the solution to boiling then add 10-15 ml of 5% barium chloride solution

hot while stirring.

5. Allow sediments a few minutes so that they separate between the sediment

and the supernatant.

6. Test the supernatant with the addition of barium chloride, if a new precipitate

is formed it means that the deposition is not perfect. Re-add barium chloride

until no new deposits are formed in the supernatant.

7. After settling perfectly heat (not boil) back the sediment for one hour

8. Strain with non-gray paper by using it three times, then the sediment is

transferred into filter paper.

30
9. Wash the precipitate in filter paper with distilled water 2-3 times, then test

chloride by adding silver chloride to the last filtrate, if precipitate is formed,

washing is continued until chloride is free.

10. Chloride-free deposits move into a porcelain dish that has known empty

weight then heat slowly until there is a drying of filter paper.

11. After casting, transfer the cup to the electric furnace, then heat it until the

precipitate appears pure white then cool to room temperature

12. Density of concentrated sulfuric acid after cold to oxidize carbon-reduced

sulfides at heating.

13. Heat it on the hot plate until sulfuric acid appears dry, then put it back into the

furnace and give it a few minutes

14. Cool in the eksicator for about 10 minutes then weigh,

15. Repeat the work of points 13 and 14 until you get a constant weight

Data analysis results

Example weight: 0.6575 grams

Constant weight: 0.2457 grams

Gravimetric calculation:

The gravimetric factor is the atomic / molecular mass (Ar or Mr) which is

searched compared to the relative molecular mass (Mr) of the analyte being

weighed.

Mr. SO42- = 96

Mr. BaSO4 = 233

The gravimetric sulfate factor from barium sulfate= 96/233

31
 = 0.41

0.2457 x 0.41
Levels of sulfate in alum = 𝑥 100%
0.6575

= 15.39%

2. Analysis of Magnesium as ammonium phosphate hexahydrate.

Working principle:

Magnesium salt solution in an acidic atmosphere, excess ammonia solution

is added to precipitate magnesium ammonium phosphate hexa hydrate in cold

temperatures

Reactions that occur:

Mg2+ + HPO42- + NH4+ + OH- → NH4MgPO4 + H2O

2 NH4MgPO4 → Mg2P2O7 + 2 NH3 + H2O

Tools used:

Analytical balance

Desiccator

Filter paper Goblet

glass Funnel

Stirrer

Erlemeyer flask

Statif Ring

Clamp

Test tube

Reagensia used:

Magnesium salt

32
 Diamonium hydrogen phosphate

Ammonia

Distilled water

Indicator

Prosedur

1. Carefully weigh the magnesium salt sample then dissolve it with distilled

water and acid with hydrochloric acid then dilute it to a volume of about

150 mL

2. Add a few drops of the MM indicator while stirring

3. Add 10 mL of the newly made ammonium phosphate reagent (25 grams of

ammonium phosphate pro analysis in 100 mL of distilled water).

4. Add the pro-ammonia concentrated ammonia slowly while stirring, until

the indicator turns yellow. The stirring system should not hit the glass cup

wall because the sediment will stick to the wall, stirring constantly for

about five minutes. Then ammonia is about five mL.

5. Leave the sediment in a cool or cool place for at least 4 hours or better

overnight.

6. The precipitate can be weighed as magnesium ammonium phosphate or

magnesium firo phosphate.

The screening technique carried out if the precipitate is weighed as magnesium

ammonium phosphate is as follows.

a. The precipitate is filtered using masir glass whose empty weight is known

33
 b. The sediment is taken several times using a dilute ammonia solution (1:19

equivalent to 0.8 M)

c. After three to five times taken, the final phytate is tested by taking a few

mL into the test tube then acidifying with nitric acid and adding a small

amount of silver nitrate solution, if white deposits are formed indicate

chlorine ions in the sediment

d. Washing continues until chloride free,

e. After chloride is released, the precipitate is washed three times with 10 mL

of alcohol each.

f. Finally the precipitate is washed with five x five mL diethyl ether free of

water, while sucked on the vacuum pump for 10 minutes.

g. Crucible glass is taken from the vacuum pump then cleaned with linen

cloth (tissue).

h. Leave it in the open place or in the eksicator for 20 minutes, then weigh it

as MgNH4PO4.

WEIGHING AS A PHOSPHATE MAGNESIUM FIRO

a. The filter used is non-gray filter paper using an ordinary funnel.

b. Take the precipitate three to five times using 0.8 M ammonia solution to

free chloride (chloride test is the same as before)

c. After chloride deposits are deposited and filter paper is inserted into the

porcelain crucible, the empty weight is known.

d. Heat at low temperatures until the filter paper is removed.

34
 e. Transfer it to an electric furnace, heat it to a temperature of 800-1000oC

for 20 minutes.

f. Move to the eczema, chill for 10 minutes then weigh it with an analytical

balance

g. Repeat the work e and f until a constant weight is obtained

HOW TO CALCULATE MAGNESIUM LEVELS

a. If weighed as MgNH4PO4

Example calculation:

sample weight of salt Mg = 2.5758 grams

The weight is weighed as MgNH4PO4 = 0.8275 grams

The gravimetric factor = MgNH4PO4 / Mg

= 24/137

= 0.1752

Levels of Mg in the example

Gravimetric factor x weight of residual heating

= 𝑥 100%
Sample weight

0.1752 x 0.8275
Levels of Mg in the example = 𝑥 100%
2.5758

= 5.6279%

= 5.63%

35
a. If weighed as Mg2P2O7

Incandescent weight = 0.0975

Gravimetric factor = 2 Mg / Mg2P2O7

= 48/222 = 0.2162

0.2152 x 0.0975
Levels of Mg in the example = 𝑥 100%
2.5758

= 2.1081 %

= 2.11 %

3. Determination of chlorine levels in kitchen salt

Work principle.

The chloride ion in the atmosphere of dilute nitric acid is deposited with

silver nitrate as silver chloride. Silver ions in a neutral atmosphere also settle with

phosphate ions and carbonates.

Reaction that happened

Cl- + Ag + → AgCl

Tools used,

Analytical balance
Oven
Masir glass
Glass stirrer
Electricity post
Baker Glass
Sintered glass

36
 Vacuum pump

Desiccator

Chemical reagents used:

Nitric acid

Silver nitrate

Distilled water

Procedur

Before working, the glass beaker and watch glass that will be used to precipitate

silver chloride must be protected against light because these deposits are very

sensitive to light.

1. Carefully weigh an example of about 0.2 grams, put it in a 400 mL glass

beaker equipped with a stirring rod and cover with a watch glass.

2. Add 100 mL of distilled water, stir until all samples dissolve completely,

add 0.5 mL of concentrated nitric acid while stirring.

3. Add 0.1M silver nitrate slowly until complete deposition, test the

supernatant with the addition of a silver nitrate solution, until no new

deposits are formed.

4. Heat the suspension to almost boiling, while stirring, the temperature is kept

until the precipitate is coagulated and the supernatant appears clear.

5. Store the glass cup containing the deposits in a dark place for about one

hour before filtering.

37
 6. Clean the masir glass then heat it at a temperature of 130-150oC for 30

minutes, cool it in the desiccator for 10 minutes, weigh it on the analytic

balance, the empty weight of the masked glass is known

7. Strain the sediment using masir glass (point 6) which is equipped with a

vacuum pump

8. Wash the sediment two to three times with decantation with very runny

nitric acid.

9. The last filtrate is tested with the addition of hydrochloric acid, if a white

precipitate is formed it indicates that Ag ions are still bound to the

precipitate. Washing is continued until free Ag.

10. Transfer the glass crucible to the oven at a temperature of 130-150oC for

one hour, cool in the desiccator for 10 minutes then weigh.

11. Repeat heating and cooling until a constant weight is obtained.

How to calculate chlorine levels.

The gravimetric chlorine factor from silver chloride = Cl / AgCl

= 35.5 / 142.5 = 0.2491

Example chlorine content

Gravimetric factor x weight of residual heating

= 𝑥100%
Sample weight is weighed

= ...................%

38
4. Determination of iron presentation as iron (III) oxide

General review

An example solution containing iron (III) solution was deposited with excess

ammonia to form hydrated oxide Fe2O3.xH2O. This sediment composition is

not stoichiometric because it contains different amounts of water, some are

chemically bound and others are adsorbed. The hydrated iron (III) oxide

deposition reaction equation can be written as follows,

[Fe (H2O) 6] 3+ + 3NH3 → Fe (H2O) 3(OH)3 + 3NH4-

Fe3 + + 3NH4OH → Fe (OH)3 + 3 NH4-

2 Fe(OH)3 → Fe2O3 + 3H2O

The cations that interfere in Fe (III) analysis are Al, Cr (III), Ti, and Zr and

Mn. Anions such as arsenate, phosphate, vanadate, and silica form insoluble

compounds in alkaline conditions with iron. These cations and disturbing

anions must be removed before Fe is analyzed so that the concentration

obtained is quite valid and accurate.

Iron (III) analysis procedure

1. As a form of learning for students, pure iron (II) ammonium sulfate or iron (III)

ammonium sulphate is used.

2. Carefully weigh 0.8 grams of iron (II) ammonium sulfate into a 400 mL goblet

which is equipped with a watch glass cover and stirring rod

3. dissolve this sample with 50 mL of distilled water and 10 ml of HCl (1:1)

4. Add 1-2 mL of concentrated nitric acid then heat until boiling slowly, until the

solution is clear yellow which shows that iron (II) has turned into iron (III).

5. Dilute to a volume of 150 mL with distilled water, then heat until boiling.

39
6. Add ammonia slowly while stirring until excess is shown from the odor

coming out of the solution vapor.

7. Bring to a boil for a few minutes and allow the precipitate to absorb, the

supernatant must be colorless.

8. Strain using non-gray filter paper through the decantation system (take

several times).

9. After being applied pour with ammonium nitrate nitrate several times.

10. Chloride test on the last filtrate using silver nitrate, if positive, then washing

the precipitate is continued by ammonium nitrate until chloride free.

11. While filtering also warm up until the glow on the crucible to be used, then

cool in the desiccator for 10 minutes and weigh on the analytic balance, the

results of this weighing as an empty weight crucible.

12. Fold the filter paper so that the sediment is closed, then transfer it to the

crucible where the empty weight is known

13. Heat over the electric heater or meker slowly until the paper, stretch all filter

paper without turning on.

14. Transfer to heat the furnace to a temperature of 800-1000oC for 20 minutes

15. Cool in the desiccator for 15 minutes then weigh.

16. Repeat the work of points 14 and 15 until a constant weight is obtained

17. Calculate the iron concentration in the example calculated as iron, iron (II)

oxide, and iron (III) oxide

40
 Calculation of Iron percentage

Calculate the gravimetric factor of each element / compound to be determined.

2ArFe
Gravimteri Fe and Fe2 O3 factors =
MrFe2 O3

= 112/160 = 0.7

= 72/160 = 0.45

MrFe2 O3
The Gravimteri factor of Fe2 O3 from Fe2 O3 =
MrFe2 O3

= 160/160 = 1

Concentration of Fe

The remaining weight is incandescent x the gravimetric factor

= 𝑥100%
Sample weight is weighed

Concentration of Fe2 O3

The remaining weight is incandescent x the gravimetric factor

= 𝑥100%
Sample weight is weighed

5. ANALYSIS OF COPPER AS COPPER (I) TIOSIANAT

This gravimetric medote is very well used for the analysis of copper (I) cations

with tiosinat anions because other metals such as, Bi, Cd, As, Sb, Sn, Fe, Ni,

Co, Mn, and Zn generally dissolve well. Addition of 2-3 grams of tartrate acid

can prevent hydrolysis from Bi, Sb, and Sn. To obtain maximum experimental

results, follow the following experimental conditions.

41
 a. The acidity of the solution is maintained, not too acidic because by

decreasing the pH value, the sediment solubility will increase

b. Reducing agents such as sulfite acid or ammonium hydrogen sulfite can

reduce Cu (II) to (I)

c. The advantages of adding as little as possible to the tiosinat reagent

because it is too excessive can cause it to increase the solubility of copper

thiocyanate.

d. There must be no oxidizing agent

REACTION THAT HAPPENED:

2Cu2 + + HSO3- + H2O → 2Cu + + HSO4- + 2H+

Cu+ + SCN- → CuSCN

Procedur

1. Carefully weigh 0.4 grams of copper (II) sulfate, put it in a 400 mL cup, add

50 ml of distilled water as a solvent.

2. Add a few drops of dilute hydrochloric acid, then add 20-30 mL of saturated

sulfuric acid which is just made or can be used 25 mL of ammonium

hydrogen sulfite solution but the compound contains 54% sulfite

3. Dilute the sample solution to a volume of 200 mL, then heat it to almost

boiling, add 10% ammonium thiocyanate through the burette while stirring

4. Add ammonium thiocyanate until white sediment is formed, the supernatant

must be colorless and smell of sulfur dioxia gas

5. Leave it for about two hours, but it should be stored for 24 hours.

42
6. Filter through the Gooch crucible or screw glass that was previously prepared

and the empty weight is known

7. The filter system is done by applying 3-4 times with a washing solution of

distilled water containing 1 mL of 10% ammonium thiocyanate and 5-6 drops

of saturated sulfuric acid solution

8. Sediment washing does not give a positive reaction with the Iron (III) cation,

(qualitative test).

9. The precipitate with the filter container is slowly heated in the oven at a

temperature of 110-120oC for 2 hours

10. Cool in the desiccator for about 10 minutes then weigh as copper thiocyanate

11. Repeat job no. 9 and 10 until a fixed weight is obtained

Calculation of copper content

Gravimetric factor of Cu from CuSCN = Cu / CuSCN

= 63.5 / 121.5

= 0.5226

Percentage of Cu

The remaining weight is incandescent x the gravimetric factor

= 𝑥 100%
Sample weight is weighed

43
FORMATIVE TEST

I. SELECT THE MOST ANSWER

1. If an analysis uses mass as the basis of calculation, this method is called.

A. Gravimetri

B. iodimetry

C. iodometry

D. volumetric

E. oxidimetry.

2. If the weight of the deposition of barium sulfate is obtained 0.2126 grams of 50

mL sulfuric acid technique, then the amount of sulfuric acid contained in one

liter of sulfuric acid technique is,

A. 178.6 grams

B. 17.86 grams

C. 1786 grams

D. 17860 grams

E. Everything is wrong

3. The English salt technique is analyzed by gravimetric method, from the sample

weight of 0.4285 grams, the remaining weight of the incandescent is 0.1920

grams, then the purity of British salt is,

A. 99.31%
B. 99.75%
C. 99.99%
D. 99.05%
E. 99.00%

44
4. If 0.500 grams of copper sulfate are five water molecules, then the mass of

copper iodate formed is,

A. 8,280 grams

B. 82.80 grams

C. 0.828 grams

D. 1.636 grams

E. 16.36 grams

5. A mixture of 1.5 grams of sample consisting of 38.00% magnesium carbonate

and 42.00% potassium carbonate, the weight of the released carbon dioxide is,

A. 0.248

B. 2,480

C. 4,980

D. 0.498

E. All answers are wrong

6. Analysis of chemical constituents in blood samples is an in chemistry

application,

A. Environment

B. Medicine

C. Agriculture

D. Industry

E. Security.

7. The calcium content in samples weighing 0.8342 grams would be known by

gravimetric analysis. After calcium is deposited as calcium oxalate, washed,

45
 dried, and weighed as calcium carbonate, obtained a weight of 0.3462 grams,

then the percentage of calcium is,

A. 23.00%

B. 2,34%

C. 32.00%

D. 3.20%

E. 16.80%

8. If a sample containing 14.40% chloride is analyzed gravimterially so that the

remaining heating weight is 0.4400 grams as silver chloride, then the weight

of the sample weighed is.

A. 15,1181 grams

B. 7,5590 grams

C. 0,0755 grams

D. 0.7559 grams

E. all answers

9. Phosphate rock samples contain phosphorus pentaoxide 26.26%. If 0.5428

grams of sample are analyzed gravimetric so that the sediment is obtained as

MgNH4PO4.6H2O. after the precipitate is filtered, washed, burned, cooled

magnesium ammonium phosphate compound is transformed into magnesium

firo phosphate, then the weight of magnesium ammonium phosphate and

magnesium firo phosphate, is.

A. 0.2235 and 0.4929 grams

B. 0.4929 and 0.2235 grams

46
 C. 4.929. and 0.2235 grams

D. 0.4929 and 2.2350 grams

E. 4.9290 and 2.2350 grams

10. If 200 mL of the water sample is analyzed the calcium content is gravimetric

by depositing it as calcium oxalate. The precipitate is filtered, washed, and

burned in a crucible whose empty weight is 26.6002 grams. The weight of the

crucible with calcium oxide is 26.7134 grams, so the weight of calcium in

grams per 100 mL example is,

A. 0.4050 gram / 100 mL

B. 4.0500 grams / 100 mL

C. 0.0405 gram / 100 mL

D. 40,5000 grams / 100 mL

E. 8.1000 grams / 100 mL\

ESSAY

1. Explain the difference between

a. Colloidal and crystalline deposits

b. Precipitation and coprecipitation

c. Nucleation and crystal growth

d. Peptization and coagulation of colloids

2. Define the following terms,

a. Gravimetric factor

b. Enap pour it

47
 c. Decantation

d. Too tired

3. Calculate the gravimetric factor for the following compounds,

a. ZnO from Zn2P2O7

b. FeS from BaSO4

c. Cr2O3 from Ag2CrO4

d. NH3 of (NH4) 2PtCl6

Key: a. 0.5328 b. 0.3776 c. 0.2289 d.0.0766

4. Analysis of aluminum from the ammonium aluminum sulfate technique sample,

weighed 0.910 grams. Dissolved with distilled water and then deposited with

ammonia as Al2O3. xH2O. The precipitate is filtered using non-gray filter paper

and washed until it is free of chloride and sulfate (qualitative test).

Furthermore, it is heated, heated, weighed to obtain a constant weight, 0.2001

grams as Al2O3. Calculate concentration as,

a. Percent of Al

b. Percent of Al2O3

c. Percent of NH4Al (SO4)2

Key: a. 11.64% b. 21.98% c. 83.24%

5. If 0.2121 grams of sample organic compounds are burned by flowing O2 and

the released CO2 gas is flowed into Ba(OH)2. Calculate the carbon percentage in

the example if the weight of the deposit of BaCO3 is 0.6006 grams.

Key: 17.23%

48
 BIBLIOGRAPHY

1. Alexeyev, V. Quantative Analysis A textbook, Foreign Languages

Publishing House – Moscow

2. Basset, J., Denny,R.C., Jeffry,G.H., J.Mendham;(1989) Vogel’s

textbook of Quantitative Inorganic Analysis Including Elementary

Instrumental Analysis 4Ed

3. Day, R.A. JR., A.L. Underwood, A.L., 2001. Analisis Kimia

Kuantitatif, Ed. 6 Jakarta: Penerbit Erlangga.

4. Ismono, Detlev Naroso,H., Roekmini Sadli, Bambang Sutikno, Hadi

Sangkaparan, Hiskia Ahmad. 1978. Dasa-Dasar Kimia Analitik

Kuantitatif. Penerbit ITB Bandung.

5. Skoog, D.A., West, D.M., F. James Holler, Stanley R.Crouch. 2004.

Fundamental of Analytical Chemistry, 8th edition, New York: Sanders

College Publishing

49
KEY TO ANSWER MULTIPLE CHOICE

1. A

2. C

3. A

4. C

5. B

6. D

7. E

8. D

9. B

10.C

50