INTRODUCTION TO THE LABORATORY OBJECTIVES OF THE LABORATORY WORK

The Objectives of the laboratory work are

1. To provide opportunity for study of the chemical and physical properties of certain and the more
common compounds and their solutions.

2. To show how these properties and the principles of solution chemistry can be combined into a
systematic scheme for analysis.

3. To give the students experience in laboratory technique.

4. To become familiar with analytical methods in common use and to understand the theoretical
principles on which they are based.

5. To appreciate the limitations of each method and the magnitude of the possible errors involved.

6. To acquire adequate manipulative ability in the use of the tools of quantitative analyses and analytical
operations without sacrifice of accuracy.

7. To acquire the habit of recording all data directly in a suitable notebook in such clear, systematic form
that such records may be understood by any analyst

8. To make calculations from analytical data with speed and accuracy and to a precision in keeping with
that of the data involved.

GENERAL INSTRUCTIONS
The qualities, which make for excellence in laboratory technique, are orderliness, cleanliness and
neatness. The following suggestions, if adopted and practiced by the student, will lead them toward
excellence in laboratory technique, which is one of the objectives of this course.

1. Prepare for the laboratory in advance; study the properties of the ions involved in the procedures to
be performed.

2 Upon beginning work, make certain that the top of the desk is clean. Arrange the more common and
frequently used apparatus on the desk in a convenient, orderly pattern.

3. Place several capillary syringe and calibrated medicine droppers in a beaker of distilled water. Thus,
water is to be used for diluting solutions and for washing precipitates.

4. Make certain that the reagent bottles ties at the desk are clean and in order and keep them that way.

5. If a water bath is needed during the laboratory period set it up and bring it to temperature.

6. Just before beginning work, review the laboratory directions and plan the program of work for the
day.

7. During the course of the work place all dirty glassware in definite place.
8. While the student is expected to adhere closely to directions, he should not work blindly. Some bit of
information may show how a negative test appears. Divide the blank test between two test tubes and to
one test tube add a drop or two of test tube of the ion under consideration. This control shows how a
positive test appears. Then compare the unknown, blank, and the positive test.

POINTS AND TIPS TO REMEMBER IN MAKING OF SOLUTIONS

1. Check calculations.

2. Check label on chemical very carefully.

3. Assemble and check all glassware for cracks and cleanliness. Spatulas should be clean and dry. Never
use the same spatula for more than one chemical at a time.

4. Preferably use rain water or distilled water.

5. Label all containers, with the name, formula, concentration and date.

TIPS
1. Always add acid to water or solid to water.

2. No prepared solutions should be stored in direct sunlight.

3. It saves time to have bottles already labeled, even if they have rinsed clean immediately after use.

4. All basic solutions should be stored in rubber stoppered bottles.

5. We are aware of the need to keep the science rooms and all materials stored there, clean and tidy.
This can only be achieved if practical class is encouraged to spend a few minutes towards the end of
each session, cleaning and replacing equipment.

6. Breakages will be kept to a minimum if students are encouraged to use and clean equipment with
understanding and great care.

SOME IMPORTANT REMINDERS WHILE WORKING INSIDE THE LABORATORY (SAFETY

MEASURES)
1. Know the location of the closest fire exit, fire extinguishers, fire blanket, sand box, emergency shower,
first aid kit and eye wash solution. Make sure that you know when and how to use them.

2. Laboratory instructions shall be properly read and understood before you start working on any
experiment.

3. Always keep your work area clean and orderly.

4. Any accident, major or minor, should be reported to your teacher.

5. Objects at books. Clothes and other inflammable materials should be kept away from a lighted
burner.
6. Use only the proper apparatus for the required experiment.

7. Reasonable spaces should be provided for each working group.

8. Never direct a test tube to your classmates or at yourself. Seldom formation of a gaseous substance
may throw the content several feet away

9. Never return unused chemicals to reagent bottles. This will contaminate the contents. Furthermore,
do not interchange covers, spatulas and droppers of chemical containers.

10. If any part of your body comes in contact with an acid or base, wash it with water and inform your
teacher immediately.

11. Large bottles of chemical should be properly handled. The base of the bottle should be supported by
one of your hands.

12. Do not add water to an acid or base. Acids and bases should be added to water

13. Class tubing should be properly fire-polished to remove sharp edges. If your glassware have chips or
cracks, request your laboratory technician or your teacher to replace them.

14. Wash your hands thoroughly before leaving the laboratory area.

GENERAL MANIPULATIVE PROCEDURE

1 Cleaning Glassware

2 Observation

3 Measurement of reagents

4. Identification of Vessels

5. Mixing solution

6. Heating solution

7. Evaporation of solution & Regulation and Testing of Acidity

9. Flame Tests

10. Precipitation

THE NOTEBOOK
1. The Notebook should contain all recorded data and all calculations.

2. Records of weights, burette readings and major calculations should be written on the right-hand page.

3. Minor calculations such as the computation of molecular weights and theoretical volumes of reagents
required should be written on the left-hand page

4. All records should be dated and all observations and data should be recorded at once, in the
notebook, in neat and orderly fashions.
5. The making of records upon loose paper is bad practice, as is also the copying of original entries into a
second notebook.

REAGENTS
Reagents-are substances used to bring about a reaction. Chemical reagents are sold in various grades
and the analyst should have a complete understanding of the significance of the terms used to express
their degree of purity

A. Technical or commercial reagents - Technical-grade reagents have been subjected to only superficial
purification and are seldom used in analytical work, except for such purposes as the preparation of
cleaning solution and other solution not directly involved in analytical purposes.

B. USP and NF Reagents - reagents marked U.S.P conform to the standards set up by the United States
Pharmacopoeia Similar to these are the NF. Chemicals that meet the standards of the National
Formulary

C. CP Reagents - the term C.P. stands for chemically pure and has no exactly definable meaning beyond
the implication that the chemical so marked is of high degree of purity, probably to the extent that the
amounts of impurities are too small to cause interference in the processes in which the reagent is used

D. Reagent Grade Chemicals - Reagents which have been analyzed by the analysis of which are given on
the labels of the containers are favored by analytical chemists. Such highly purified chemicals are
referred to as reagent grade, analytical reagent, certified reagent, tested purity reagent. The analysis of
a reagent of this type is given either in terms of the actual percentages of the impurities present or in
terms of maximum limiting percentages of the various impurities

E. Primary Standards - chemical of said purity that it can be weighed out and used to standardize a
solution to a very high degree of accuracy is referred to as primary standard Ordinarily, a primary
standard has purity greater than 99.95% The National Bureau of Standards can preside several standards
of the nature and there are desirable for very precise work for routine determination, however, the
analyst is likely to find "reagent rade" standards to be satisfactory.

CARE IN THE USE OF REAGENT

1. The stopper of a reagent bottle should never be placed on the desk. It may be placed on a clean towel
or clean wash glass, but it is kore common practice to hold the stopper with the hot portion between
the index and second fingers and with the plug projecting from the back of the hand. Stopper with
horizontally flat tape may, of course be phased on the instead on the desk. It is also important to
keep the mouth of reagent bottles scrupulously clean.
2. the measuring out a liquid reagent, if more than the desired amount is purred out, it is best to
describe the excess rather the be return it to the reagent bottle
3. the laboratory desk and all apparatus should be scrupulously neat and clean at all times. A sponge
should always be at hand and desk and filter stand should be kept dry and in good order.
4. Funnels should never be allowed to dig upon the desk.
5. Glass ware should always be wiped clean with a ——— towel just before use.
6. All filters and solution should be covered to protect them from dust as far
as_______________________________

VOLUMETRIC METHODS

(Titrimetric methods)

Volumetric method is a technique in which the result of analysis depends upon accurate
measurement of the volume of an added chemical reagent of known concentration through the process
of titration. Volumetric process is a rapid technique compared to other analytical methods and yields very
reliable results.

Volumetric - is a process whereby a standard solution delivered through an upwards called burette into
reaction with an analyzed solution. It is used to determine volumetrically, the evaluation of the desired
substance in solution by adding a standard solution of known volume and concentration until the reaction
is complete, usually as indicated by a color change due to a chemical indicator.

Volumetric process involves the following steps:

a. for solids, accurate weighting of the sample using an analytical balance or for liquids, accurate
measurement using a pipette
b. bringing the sample into solution
c. removal/separation of interfering substances, if any
d. addition of inductors
e. titration of the analyte using standard solution

THE FOUR CLASSIFICATIONS OF A VOLUMETRIC PROCESS

1. neutralization
2. oxidation-reduction
3. precipitation
4. complex formation

Neutralization
Neutralization is a reaction between an acid and a base. It is based on the union of the hydrogen ion
from the acid and the hydroxyl ion from the base to form water, i.e.,

H + OH -----------> H₂O

In volumetric analysis, acidimetry denotes the titration of an acid sample with a base, while alkalimetry,
the sample is a base and is titrated with acid. To indicate the point at which the amount of the titration
added is stoichiometrically equivalent to the analyte, called the equivalence point, a chemical indicator
is added which change color at this point. The point at which a chemical indicator changes color is called
the end point and must coincide with the equivalence point, Common indicators used for neutralization
are phenolphthalein (Hph), methyl orange (MO) and methyl red.
 Metal Ions Flame Colors

1. Silver None (because it is belong in noble metal that

does not produce a characteristic flame)

2. Lead (II) Gray- White

3. Bismuth (III) Azure

4. Cobalt (II) Silver- white

5. Arsenic (III) Blue

6. Strontium Crimson to scarlet, yellowish through green

glass and violet through blue cobalt

7. Sodium Yellow

8. Cesium Blue/Violet

9. Barium Pale/ Apple Green

10. Chromium Silver-white

11. Cadmium Brick red

12. Nickel Silver-white

13. Magnesium Intense white

14. Copper Blue-green

15. Iron Gold

What are the conjugate acids and bases?

An important feature of the Bronsted-Lowry concept is the idea that the species produce when an acid
gives up a proton is a potential proton acceptor called the conjugate base of the parent acid.

Oxidation and reduction method – may be defined in terms of transfer of electrons. A substance is
iodized when it loses electrons. A substance is reduce when it gains electrons

Reduction-oxidation involves the titration of a reducing agent with an oxidizing agent or vise-versa, the
equivalence point of which is usually indicated by indicators such as diphenylamine or starch (except for
permanganate acid)

Redox methods include permanganate, dichromate, ceric and iodometric processes.

Permanganate process

Potassium permanganate is a powerful oxidizing agent and is useful for many redox processes by direct
or indirect method. It can oxidize ferrous ions, mercurous mercury, oxalates, nitrate and sulfites.
Permanganate titrations can be done in acidic or alkaline conditions.

Oxidation-Reduction Method
(REDOX TITRATION)
Oxidation and reduction may be defined in terms of transfer of electrons. A substance is
oxidized when it loses electrons. A substance is reduced when it gains electrons.

Reduction-oxidation involves the titration of a reducing agent with an oxidizing agent, or vice
versa, the equivalence point of which is usually indicated by indicators such as diphenylamine or starch
(except for permanganate process).

Redox methods include permanganate, dichromate, ceric and iodimetric process.

Permanganate Process

Potassium permanganate is a powerful oxidizing agent and is useful for many redox processes
by direct or indirect methods. It can oxidize ferrous ions, stannous tin, mercurous mercury, oxalates,
nitrite and sulfites. Permanganate titrations can be done in acidic or alkaline conditions. In acid,
manganese gains 5 electrons.

In alkaline conditions, permanganate is reduced to MnO2 resulting to gain of 3 electrons only.

 If potassium permanganate is standardized in acid medium and is used to titrate samples in
alkaline medium, the concentration of the permanganate is multiplied with 3/5 to convert the
concentration to alkaline medium.

The intense purple color of permanganate solution affords it an inherent advantage of acting as
the indicator itself. An excess of one drop permanganate gives a pink color to the sample solution which
indicates the end point. Its disadvantage is the tendency to decompose on standing or exposure to light
which is further hastened in the presence of acid.

Iodimetry

The titration of iodine against sodium thiosulfate, with starch used as the indicator, is one of the
most accurate of volumetric process and a determination involving it, is call iodimetric or iodometric
process.
The usual indicated for the iodimetric titration is a colloidal dispersion of starch which, in the
presence of iodide ions, gives a deep blue color with even minute amounts of free iodine, although the
sensitivity is impaired by the presence of certain organic solvents such as alcohol.

The iodometric process can be applied in two ways:

1. certain reducing substances like hydrogen sulfide, sulfites, arsenates and stannous salts can be
titrated directly with standard iodine solution.
2. Number of substances that can be so titrated is less than in the case of the permanganate
process.

Trituration is the process whereby a solid is grounded in contact with a liquid.

Precipitation Methods

Precipitimetry is a volumetric method of analysis in which a solution of unknown concentration

is titrated with a standard solution of a precipitating agent. The product formed in the reaction between
the analyte and the standard solution separates out as precipitate.
The most common application of precipitimetry is the determination of the amount of the
chlorine as chloride ion in water. Ground water contains different soluble salts of alkali and alkaline
earth metals in the form of CH, CO32, HCO3 and SO42. Among these, chloride ion is the most abundant.
The analysis of chloride ion by precipitimetry uses a standard solution of silver nitrate as the
titrant.

Silver chloride appears as curdy, white precipitate. This precipitate is very insoluble. Ksp =
10
1x10 , and the presence of this in the titration mixture do not affect the determination of the end
point.
End point in precipitimetry is indicated by three commonly employed methods as follows:
a. Formation of second precipitate
b. Formation of colored complex
c. Adsorption indicator
 The Mohr method uses potassium chromate, K2CrO4, as indicator. This forms a brownish-red
AgCrO4 precipitate. Silver chromate is more soluble than AgCl, therefore AgCl will precipitate first after
all the chloride ions has been precipitated, the excess silver nitrate will then precipitate the chromate
which indicates the end point.
In Volhard method an excess of AgNO3 is added. This ensures the complete precipitation of the
chloride. This excess is titrated with KSCN, the end point of which is indicated by ferric alum solution. A
drop of excess KSCN will color the whole mixture red-brown. This is due to the formation of Fe(SCN)
complex. The amount of KSCN added is stoichiometrically equivalent to the excess AgNO3 and this is
subtracted from the total silver nitrate added to precipitate the chloride.
Fajan’s method uses adsorption indicator, the most common of which is the organic dye
fluorescein, or any of its salt. This imparts a distinctive color on the surface of the precipitated AgCl. A
change in the color of the precipitate indicates the end point.

Compleximetry
EDTA titration

Compleximetry uses a titrating agent that forms a complex with the substance being analyzed.
This titrant forms a chelate with the iron being analyzed and the amount of titrant is directly
proportional to the concentration of that ion.

Of the numerous chelating agents widely used, Ethylenediaminetetraacetic acid, also known as
EDTA, is one of the commonest and most useful.

EDTA is not very soluble in water, so the sodium salt is commonly employed. EDTA is a
tetrabasic acid and is often represented as H4Y. the disodium salt is written Na2H2Y and this ionizes to
give H2Y ions which react with Ca or Mg as well as other divalent ions.

The CaY2 and MgY2 are chelates and are very slightly ionized that the calcium and magnesium
ions are efficiently removed from solution by EDTA. This is the principle where the compleximetric
determination of the total hardness of water is based.

Water hardness is ascribed chiefly to the presence of calcium and magnesium carbonate,
bicarbonate, chloride and sulfate. The most common method used for the determination of total
hardness of water is by direct titration with EDTA. The indicator used in this process is Eriochrome Black
T, existing as blue in solution. It renders the water containing calcium and magnesium ions red because
it reacts with some magnesium ions and produce a red colored complex. During titration, EDTA
preferably binds with calcium and then with free magnesium ions. When these ions are consumed, EDTA
displaces the complexed magnesium ions and Eriochrome Black goes back to its characteristic blue
color.
Analysis of water by this method has the total hardness reported in terms of ppm CaCO3.