Bicol University East Campus

College of Engineering
Legazpi City
A.Y. 2019-2020

DEPARTMENT OF CHEMICAL ENGINEERING

DETERMINATION OF PERCENT NITROGEN

(Laboratory Plan)

CIELO, Manlyn
EDMA, Anthony Justin
BIRON, Juan Raymond
BUSTAMANTE, Shaquille Marc Burt
OCAMPO, Neza
BSChE 1- A
I. INTRODUCTION

II. OBJECTIVES

III. MATERIALS AND APPARATUS

Materials Definition Specifications Quantity

Burette set- Essentially a long, graduated 50 mL burette 2
up (burette, measuring tube with a stopcock and
clamp, a delivery tube at its lower end;
stand) utilized in titrations.
Volumetric Are designed to very accurately 5 mL 2
Pipet transfer a specific amount of
solution. These pipets can only be
used to deliver the volume of liquid
for which it is calibrated.
Measuring Used for dispensing a variable 10 mL 2
Pipet volume of aqueous liquid.
Aspirator Also known as an educator -jet 1
pump, or a filter pump. This is a
device that is able to produce a
vacuum by using the venturi effect.
Erlenmeyer A flask having a wide base, narrow 250 mL 6
Flask neck, and conical form, convenient
in laboratory experimentation for
swirling liquids by hand.
Volumetric a piece of laboratory glassware that 50 mL, 500 mL 3, 4
Flask is used to prepare and measure
chemical solutions. It is used to
make up a solution to a known
volume.
Beaker A cylindrical container used to store, 100 mL 1
mix and heat liquids in laboratories.
Analytical Highly sensitive lab instruments 1
Balance designed to accurately measure
mass. Their readability has a range
between 0.1mg - 0.01mg.
Wash bottle A squeeze bottle with a nozzle, used 1
to rinse various pieces of laboratory
glassware, such as test tubes and
round bottom flasks.
Dropper Is a pipette consisting of a small tube 1
with a vacuum bulb at one end for
drawing liquid in and releasing it a
drop at a time.
Stirring A piece of laboratory equipment 1
Rod used to mix chemicals and liquids
for laboratory purposes.
Glass Can be used to guard against spillage 1
Funnel when pouring chemicals from one
vessel to another, and they can also
 be fitted with a filter to separate
solids from liquids.
Distillation A piece laboratory equipment that is 1
Flask used to separate mixtures of two
liquids with different boiling points.
condenser It is a device used in the laboratory 1
to cool hot gases into liquids.
Alcohol Used to produse an open flame that 1
Lamp is used for heating, sterilization and
combustion in a laboratory.
Tong Used for grasping and lifting vessels 1
of heat-resistant material used in
high temperature chemical reaction.
Meat 200 mg

Reagents Specifications MSDS Emergency Overview

Sodium 10 grams Appearance: Solid, White
Hydroxide Immediate effects: ND
(NaOH) Potential health effects
Primary Routes of entry: Ingestion, inhalation,
skin and eye contact.
Signs and Symptoms of Overexposure: ND
Eyes: Causes eye damage.
Skin: Causes severe skin burns.
Ingestion: Harmful if swallowed.
Inhalation: Harmful by inhalation.
Chronic Exposure: ND
Hydrochloric 20.5 mL DANGER! Corrosive. Causes severe skin, eye,
Acid Solution and digestive tract burns. Harmful if swallowed.
(HCl(aq)) Mist or vapor extremely irritating to eyes and
respiratory tract.
Ethanol 50 mL Appearance: colorless clear liquid.
(C2H5OH) Flash Point: 16.6 deg C.
Warning! Causes severe eye irritation.
Flammable liquid and vapor. Causes respiratory
tract irritation. This substance has caused
adverse reproductive and fetal effects in
humans. May cause central nervous system
depression. May cause liver, kidney and heart
damage. Causes moderate skin irritation.
Target Organs: Kidneys, heart, central nervous
system, liver.
Distilled water 2.5 L
(H2O)

IV. PROCEDURES
1. Gather all the equipment indicated in the laboratory borrower’s form from the laboratory
technician, Mr. Joel Ilagan.
2. Clean the glassware to be utilized using a wash bottle with distilled water.
3. Before the conduct of the experiment proper, the Taichou and Fuku-Taichou must ensure
 that all members of the group are aware of the MSDS of the chemicals to be utilized. Also, it
must also be ensured that all members are wearing the proper PPE.
4. To prepare 250 mL of 0.5 M NaOH solution 10g of NaOH pellets must be dissolved. Firstly,
make a paper box and place it on top of the analytical balance. Set the balance to tare. Weigh
10g of NaOH pellets. Then, transfer the pellets to a beaker. Add distilled water to the beaker
just enough to dissolve it completely using a stirring rod. After this, transfer this solution
into a 500 mL volumetric flask. Add distilled water to the flask until it reaches the mark. Use
a wash bottle in adding distilled water to the flask to avoid spillage and to ensure that it will
not go above the mark. Cover the flask tightly and swirl it lightly until the solution is fully
mixed.
5. Using the analytical balance, weigh 200 milligrams of the sample and transfer it to the
distillation flask.
6. Pipette 3 mL of sulfuric acid (H2SO4) and add it to the sample. Set aside.
7. Weigh 1.4 grams of potassium sulfate and a catalyst which is the copper sulfate, then add
them to the sample and mix well.
8. Set-up the ring stand and the wire mesh or gauze together with the alcohol lamp.
9. Put the distillation flask with the mixture at the top of the wire mesh then start heating the
mixture until white fumes can be seen. Continue the heating process for about 12-18
minutes. (Take note that this process will reach end point when the mixture became liquid
and translucent, and the brownish smoke stop being released).
10. Afterwards, set aside the mixture and let it cool at room temperature.
11. Pipette 50 mL of distilled water then add it in the mixture. Set aside.
12. For the trapping solution, prepare an Erlenmeyer flask. Pipette 3 mL of hydrochloric acid
(Hcl) and transfer it to the Erlenmeyer flask. Add 14 mL of water in it. Set aside.
13. Pipette 25 mL of sodium hydroxide from the mother solution then add it to the mixture to
raised its pH to change ammonium (NH4) to ammonia (NH3) which is a gas.
14. To separate the nitrogen away from the digestion mixture, heat again the mixture and raised
its temperature to boiling point. (Use a thermometer to determine its temperature).
15. Put the Erlenmeyer flask containing the HCl solution at the tip of the condenser along the
trapping flask to trap the distilled vapors of the mixture.
16. Stop the distillation process before the flask becomes completely dry.
17. Afterwards, remove the trapping flask and rinse the condenser with distilled water to make
sure that all the ammonia has been dissolved.
18. Add two drops of methyl orange that will serve as the indicator to the acid/ ammonia
trapping solution. A strong color must be seen to indicate that a significant amount of the
original trapping acid is still present. Set aside.
19. Prepare the burette set-up for the titration process. Rinse the 50 mL burette with distilled
water up and allow the water to flow to the tip. Rinse it again with NaOH.
20. Fill the burette up to the 50 mL mark with NaOH solution with eye-level.
21. Put the acid/ ammonia trapping solution below the tip of the burette. Slightly turn the spigot
in a horizontal manner to slowly add a small amount of sodium hydroxide (NaOH) solution
to the acid solution with the dye.
22. Stop adding when the acid solution turns to orange color. It indicates that the acid solution
reached its end point and all the acid have been neutralized.