Experiment-1

Object: To understand the Standard laboratory devices for weight and volume measurement and
Caliberation of Analytical Equipment.

The experiment is divided into two parts. The purpose of this experiment is to make the students:
● familiar with commonly used laboratory glassware and equipments,
● learn to take observations,
● analyze data and
● prepare standard solution.
● Learn to Caliberate Analytical Instument.
Learning objectives:
By the end of this experiment the student shall be able to:
● understand the safety measures of laboratory.
● know how to make correct measurements using burette, pipette and graduated cylinder.
● know the mass of compound weighed out and transferred to volumetric flask
● volume of the volumetric flask used to make the standard solution 
● know how to use digital analytical balance.
● record experimental observations.
● prepare standard solution.
● Caliberate Equipment

(A) Use of laboratory equipments and understanding the standard units of measurement.

Measurement of Weight:
Units of Weight: e.g. Milligrams (mg), Grams (g)
Analytical Balance: An Instrument used for measurement of weight in laboratory is analytical balance.
It is an accurate and precise instrument to measure weight.
The most commonly used analytical balance is beam balance, precision scales, and moisture
analyzers.
An analytical balance  measures masses to within 0.0001 g.
The balance is enclosed in a glass case in order to avoid disturbances due to air (fig. 1).

Precautions:
1. Do not exceed capacity.
2. Use tong/forceps to transfer sample and weights.
3. Protect from hot/corrosive substance.
4. Cleaning the balance after every use.
5. Vibration free table. Figure 1: A Beam Balance

Measurement of Volume:

Units of Volume: e.g. Milli liter (mL), liter (L)

For accurate measurement of volume of solutions, volumetric analysis require various types of
apparatus as:

1
Titration Flask: It is a conical flask made of borosil glass. It is available in different capacities like
100mL, 250mL, etc.
Pipette: It is a cylindrical glass tube with a bulb in the middle. It is used to measure and transfer definite
volume of the solutions. The capacity of the pipette is marked on the bulb.
Burette: It is laboratory equipment used to dispense and measure volume of a chemical solution. The
burette used in our laboratory is graduated from 0 to 50ml and each ml is further subdivided into 10
equal divisions. Thus the least count of burette is 0.1ml and with the help of it we can measure volume
accurately upto 0.1ml.
Guidelines for reading the burette correctly: The reading should be taken by keeping the eye at the
same level as the meniscus.
For colorless solution: Lower meniscus is read
For colored solution: Higher/upper meniscus is read

Precautions:
1. Clean the burette thoroughly.
2. Rinse the burette with the solution to be taken into it before use.
3. Clamp the burette vertically on the burette stand.
4. Do not blow the last drop from the pipette.
5. Ensure that there are no air bubbles in the burette.
Figure 2: Reading a burette
Measuring Cylinder: A graduated cylinder, measuring cylinder or mixing cylinder is a common piece
of laboratory equipment used to measure the volume of a liquid. Each marked line on the graduated
cylinder represents the amount of liquid that has been measured. Typical capacities of graduated
cylinders are from 10 mL to 1000 mL.

Measurement of Concentration:

Strength: Strength of a solution is defined as the amount of the solute in gms, present in one litre of the
solution. It is expressed as gramsLiter-1.
Strength of the solution is expressed in following ways:

Molarity (M): Molarity is the concentration of a solution expressed as the number of moles of solute per
liter of solution
no of moles of solute(n) Mass∈grams
M= where n =
liters of solution (V ) Molecular weight

Normality (N): Normality is defined as the number of gram equivalents of solute present
per liter of solution. Normality formula is given by:

gram Equivalent of solute

N=
Liters of solution

Molality (m): Molality of a given solution is defined as the total number of moles of solute per
kilograms of solvent present in the solution. Molality is represented by m, which is termed as molal.
One molal is the molality of solution where one mole of solute is present in 1000 grams of solvent.

2
 no . of moles of solute
m=
Weight of solvent ∈Kg

Equivalent Weight: Defined as the number of parts by weight of chemical species combined with or
displaced by one parts of hydrogen or 8 parts of oxygen.
Equivalent Weight of Acid = Molecular Weight/Bascicity
Equivalent Weight of Base = Molecular Weight/Acidity
Equivalent weight of oxidizing or reducing agent = Molecular Weight/Change in oxidation number
Equivalent weight of Ion(cation or anion) = Molecular Weight/Charge on the ion

Types of standard solutions

i) Primary Standard Solution

Primary standard is a reagent that is very pure, representative of the number of moles and can be easily
weighed. Their solutions are used in titration to determine the concentration of unknown solution.
Primary standards are often used to make standard solutions for an experiment.
A good primary standard solution has following properties:
● high level of purity
● low reactivity (high stability)
● high equivalent weight (to reduce error from mass measurements)
● not hygroscopic (to reduce changes in mass in humid versus dry environments)
● non-toxic

ii) Secondary Standard solution:

A secondary standard is a chemical that has been standardized against a primary standard for use in a
specific analysis. Secondary standards are commonly used to calibrate analytical methods and its
solution remains stable for a long time. e.g. Sodium hydroxide, once its concentration has been
validated through the use of a primary standard, is often used as a secondary standard.
A secondary standard is a chemical or reagent which has certain properties:
● Less pure than primary standard.
● Hygroscopic
● High reactivity
● Less stable and more reactive than primary standard.
● Titrated against primary standard to calculate exact concentration.

Procedure of preparation of standard solution

● Step 1: Place a small amount of distilled water into a clean, dry 250mL volumetric flask. 
Swirl the water around the whole interior of the flask to rinse it. Discard the water and dry the
flask before use.
● Step 2: Weigh the calculated amount of the salt (the solution of which is to be prepared) onto a
clean, dry watch glass. 

3
 ● Step 3: Position a clean, dry glass funnel into the neck of the volumetric flask. 
Leave a small air gap around the stem of the funnel inside the neck of the volumetric flask.
● Step 4: Place the weighed salt into funnel and wash it into the volumetric flask with a little
distilled water. Repeat this process until all the salt has been transferred to the volumetric
flask. Finally, position the watch glass over the funnel and run a little distilled water over this to
transfer any microscopic amounts of it that might be still adhering to the watch glass to the
volumetric flask. Repeat this process. Swirl the volumetric flask gently to dissolve the salt. Do
not shake the flask. Do not invert the flask.
● Step 5: Pour distilled water through the funnel slowly until the water level in the volumetric
flask reaches the base of the neck. Allow any water still remaining in the funnel to run through
(there shouldn't be any if you maintained the air gap, and, if you poured slowly.) Carefully pour
distilled water through the funnel very slowly until the bottom of the meniscus is about 1 cm
from the graduation mark on the neck of the volumetric flask.
● Step 6: Remove the funnel from the volumetric flask.
● Step 7: Use a pipette to transfer distilled water drop by drop to the volumetric flask until the
bottom of the meniscus sits on the graduation mark on the neck of the volumetric flask when
viewed at eye level.
● Step 8: Stopper the volumetric flask and invert it several times to ensure thorough mixing and
label it with the name of reagent and date of preparation.

(Part B)
Calibration of Analytical Equipment and Apparatus

Analytical intruments are used for a specific analysis. To ensure the accuracy in performance or
validation of the intrument, calibration is being done. In simple words, Calibration is the demonstration
by which, we ensure that an instrument is suitable for its intended purpose (i.e. its readings are accurate
the reference to establish standard).
Calibration is performed using primary reference standards.Instrument need to be calibrated before use.
The specific calibration procedures of few intruments are discussed below:

1. Weighing Balance
Balance or scale calibration is essential to achieve accurate weighing results. To calibrate, you simply
need to place a calibration weight on the pan and record the result. If it is within pre determined limits
then no further action is required. If the result is not within limits then the balance should be adjusted to
the value of the calibration weight.

2. pH meter
A pH meter is used to measure the pH of a solution. Depending on the laboratory, this device may be
analog or digital. A pH meter should be calibrated in solutions of known pH before use.

4
To calibrate and use a pH meter, prepare a neutral buffer with a pH of 7 and a second buffer with a pH
of 4 for acidic samples or 9.2 for base samples. Next, put a clean electrode in the neutral buffer and
press the “Measure” or "Calibrate" button.

3. Colorimeter
A Colorimeter is a device which is used to measure the transmittance and absorbance of light that
passes through a liquid sample. It also measures the intensity or colour concentration that develops upon
introducing a perticular reagent into a solution.
To Calibrate the Colorimeter, slide the lid of the Colorimeter open to reveal the cuvette slot. Insert a
cuvette, filled with distilled water or other solvent used to prepare your solutions, for your calibration
blank (100% transmittance or 0 absorbance).
The result of the calibration is a correction with its uncertainty. This correction is the difference
between the reference standard value and the value measured by your equipment.

Viva Questions

1) Name the different types of titrations.

2) What is equivalent weight? Find the equivalent weight of K2Cr2O7 and KMnO4.

3) Define Indicator. Give examples of different types of Indicator.

4) Define Normality. Also give its mathematical expression.

5) What is a standard solution? What are the differences between primary and secondary standards?

6) Why can’t we use NaOH as a primary standard?

7) Why we need to calibrate analytical instruments?

GENERAL SAFETY PRECAUTIONS TO BE FOLLOWED IN

CHEMISTRY LAB

1. Except in emergency do not run in laboratory.

5
2. Do not eat or drink in the laboratory to avoid the risk of ingestion of toxic
substances.
3. Note the place of fire extinguisher and know the method of using it.
4. Always keep the chemicals and reagent at proper place after use. Never
leave them on the bench.
5. Never use chemicals or reagent from unlabelled bottle.
6. Never use broken edged or minute cracked glass apparatus.
7. Never taste any chemical; most of them are injurious in nature.
8. Keep a distance while smelling a gas.
9. Put –off the open flame while using inflammable liquids like ethyl alcohol,
ethers etc.
10. For diluting any acid, always add acid to the water. Never add water in
acid.
11. While heating, keep away the mouth of test tube from face and also from
your neighbour’s face.
12. Avoid direct contact of solvents/chemicals with the skin.
13. Always wear Lab coat while performing experiment.
14. Wear gloves while working with corrosive chemicals.