Ontario Tech University CHEM 1010U / 1800U, W24; Exp. 1-17.

28

1. LABORATORY SAFETY AND ORIENTATION

Objectives

1) To become familiar with the safety equipment and procedures in the laboratory; 2) to recognize
the glassware and equipment in the lockers; 3) to prepare a standard solution of sodium chloride; 4)
CHEM 1010 - to practise using a pipette and to assess the variability of the volume delivered.

Introduction

This experiment is divided into three distinct “parts”: i) general laboratory safety and
orientation; ii) preparation of a standard solution; iii) pipetting practice (for CHEM 1010).

Everyone’s safety and security in a chemistry laboratory depend on each student knowing and
obeying the safety rules and working safely. The introductory pages of the manual and the First-Year
Laboratory Safety Video outline the safety rules and procedures. You should thoroughly familiarize
yourself with the safety rules and procedures of the laboratory in order to ensure your own safety and
the safety of others. The rules discussed here are applicable to all undergraduate chemistry
laboratories. Be aware that failure to comply with the safety rules may result in your dismissal from
a laboratory.

Two very important roles of the teaching assistant are to ensure all students are informed of
the safety rules of the laboratory and to ensure they are followed. At the beginning of this laboratory
period the teaching assistant will spend some time explaining the safety aspects of the laboratory,
pointing out safety equipment, and describing procedures.

79
 Ontario Tech University CHEM 1010U / 1800U, W24; Exp. 1-17.28

At the beginning of the semester, the technicians ensure that all the equipment on the locker
equipment list is in each locker and in good repair. After the safety talk, please check your locker.
If you discover anything is missing or broken, ask the teaching assistant or the technician for a
replacement. At the end of each laboratory period, make sure all the equipment that is supposed to
be in the locker (no more, no less!) is there and that your bench top has been wiped clean with a
damp sponge. The first-year chemistry technician or your TA may do inspections of lockers and
benches and if the workspace is dirty or equipment is missing, marks will be deducted from the last
student who used the locker (2.5 marks from the laboratory report).

In the second part of the experiment, students will prepare a “standard” solution - a solution
of accurately known concentration - of sodium chloride, NaCl. Many solutions in chemistry need
to have accurately known concentrations and are made by dissolving a known mass of a solid (the
solute) in a known volume of liquid (the solvent). These solutions are called primary standards and
are used to determine the concentrations of compounds in other solutions. Therefore, the primary
standard solutions must be made with great care and great accuracy. Preparing a standard solution
is a fundamental skill in chemistry. The calculation of the concentration of the chemical species in
the primary standard solution is straightforward. The number of moles of the compound is given by:

(1.1)

where:
mcompound = mass of the compound (in g)
Mcompound = molar mass of the compound (in g mol-1)

The concentration (in mol L-1) is given by:

(1.2)

80
 Ontario Tech University CHEM 1010U / 1800U, W24; Exp. 1-17.28

where:
Vsolution = volume of the solution (in L)

Concentration is an “intensive” property which means it does not change as the amount of solution
changes. In other words, the concentration of solute in 10.0 mL of the solution is the same as the
concentration in 20.0 mL of the same solution. An “extensive” property does change with the
amount of material. The number of moles of a compound is an extensive property: 2 g of NaCl
contain more moles of NaCl than 1 g of NaCl.

In this experiment a solution of ~0.1 mol L-1 NaCl will be prepared. Sodium chloride is not
commonly used as a primary standard, but the technique used to prepare the sodium chloride solution
is the same as would be used for making a primary standard.

Finally, in this laboratory period CHEM 1010 students will practise using a pipette. A
transfer pipette is used to transfer an accurate volume of liquid from one vessel to another. This is
a crucial aspect of performing a volumetric analysis and a technique that is employed extensively
in subsequent experiments in CHEM 1010 and in analytical chemistry.

All pipettes will have some systematic error associated with them. A 25.00 mL pipette, even
when used properly, will probably not deliver exactly 25.00 mL. It may deliver a volume that is
slightly higher or slightly lower. This “systematic error” can be measured by pipetting several
portions (“aliquots”) of a liquid of known density and measuring the mass transferred. The volume
transferred is calculated from the mass transferred using the density. Theoretically, if the pipette is
used exactly reproducibly, the volume, therefore the mass, transferred will be the same for each
aliquot. The difference between the volume actually transferred and the volume given on the pipette
is the systematic error and it can be taken into account in subsequent calculations (a process known
as “calibration”). In practice, variations in technique lead to variations in volume transferred. The
“variability” of the amount transferred (or “random error”) will be small if good technique is

81
 Ontario Tech University CHEM 1010U / 1800U, W24; Exp. 1-17.28

employed and high if poor technique is used. Good technique should lead to good agreement
amongst the volumes (or masses) transferred and poor technique leads to poor agreement. In this
experiment several aliquots will be pipetted to practise and assess technique. Good pipetting skills
are important in many aspects of analytical chemistry.

Procedure

The techniques used in this experiment are: open-pan balance, analytical balance, weight-by-
difference, pipetting, and preparing a standard solution.

In chemistry laboratories preparation of aqueous (“of, or in, water”) solutions requires

deionized water. It is provided in large carboys at the end of each laboratory bench.

Part I: Safety Orientation

You should watch the laboratory safety video posted on Canvas and review the safety rules
and procedures outlined at the beginning of the laboratory manual. In the first part of the laboratory
period the teaching assistant will briefly review the safety protocols and procedures that are outlined
in the introduction of this manual. You should answer and submit questions 1 - 8 on p. 91.

Part II: Locker Equipment Check

In the introductory pages of the laboratory manual is a list of equipment (p. 77) that should
be in each locker. Pictures are provided in the introduction to help you identify the equipment.
Review this list and ensure that all the equipment on the list is in your locker kit. If you do not
recognize a piece of equipment, ask the teaching assistant. If a piece of equipment is missing, ask
the teaching assistant or technician for a replacement.

82
 Ontario Tech University CHEM 1010U / 1800U, W24; Exp. 1-17.28

During the semester the technicians and teaching assistants may perform random checks of
the lockers to ensure all the equipment that should be in the lockers has been returned. If equipment
is missing, damaged or if there is extra equipment, you will have marks deducted from your report.
Likewise, if your work area is not cleaned after the experiment, you will lose marks.

Part III: Preparation of a Standard Solution of NaCl

For this part of the experiment you should watch the following videos: open-pan balance,
analytical balance, weight by difference, the meniscus, the volumetric flask, and preparing a standard
solution.

The volumetric flasks for preparing the NaCl solution will be provided in the laboratory. The
TA will point them out.

1. Place a 50 mL beaker on the open-pan balance and “tare” (zero) the balance. Add ~1.5 g of
NaCl to the 50 mL beaker.

2. Weigh the 50 mL beaker + NaCl on the analytical balance. The analytical balance will give
a mass to four decimal places. Write down all these numbers.

3. Pour the NaCl into a clean 250 mL beaker. Be careful not to spill any of the NaCl. It is more
important not to spill any of the NaCl than to get it all out of the 50 mL beaker.

4. Re-weigh the now (mostly) empty 50 mL beaker on the same analytical balance. Again,
write down all the numbers. The difference between this number and the number recorded
in step two is the mass of NaCl transferred. This technique to determine a mass is “weight-
by-difference”.

83
 Ontario Tech University CHEM 1010U / 1800U, W24; Exp. 1-17.28

5. Add ~125 mL of deionized water to the 250 mL beaker (this volume does not have to be
measured accurately).

6. Using a glass stirring rod, carefully stir the solution until all the NaCl dissolves. Do not
splatter the solution. If, at any point, you remove the stirring rod from the beaker, rinse it
with deionized water from a wash bottle so that the rinsings flow into the beaker. This
ensures no NaCl is lost from the beaker.

7. Obtain a 250.0 mL volumetric flask and rinse it thoroughly three times with small portions
of deionized water.

8. Now the quantitative transfer of the NaCl solution in the beaker must be performed. You
need to transfer all the dissolved NaCl to the flask.

9. Place a funnel in the neck of the volumetric flask and, using the stirring rod as a guide,
carefully pour the NaCl solution so that it runs down the rod through the funnel and into the
flask. Do not place the stirring rod on the bench once you have completed this step; put it
in the beaker.

10. Using a wash bottle carefully wash the inside walls of the beaker with deionized water.
Using the stirring rod as you did in step 9, transfer the washings to the volumetric flask.
Repeat the washings twice more. Do not use too much deionized water at this stage - the
total volume added to the flask must be less that 250 mL!

11. Rinse the end of the stirring rod so that the rinsings go through the funnel into the flask.

12. Finally, rinse the inside surface of the funnel with deionized water.

84
 Ontario Tech University CHEM 1010U / 1800U, W24; Exp. 1-17.28

If steps 9 - 12 have been performed properly, all the NaCl transferred to the 250 mL beaker
(step 3) should have been transferred to the flask.

13. Carefully fill the flask with deionized water so that the bottom of the meniscus is exactly on
the mark. If this is done properly, there will be 250.0 mL of solution in the flask (within the
systematic error in the flask). The bottom of the meniscus cannot be above nor below the
mark. Be very careful as the solution nears the mark. The last few millilitres should be
added with a medicine dropper. If the flask is overfilled, the procedure should be started
again. If you overfill the flask, consult with a TA before proceeding.

14. Once the solution is prepared, stopper it and have the teaching assistant check your work.
The stopper needs to fit snugly but should not be put in with excessive force. To do so, risks
injury or jamming the stopper in the neck of the flask.

15. Invert the flask 20 - 25 times (while holding the stopper in place with your hand) to ensure
thorough mixing.

Part IV: Use of the Transfer Pipette (CHEM 1010 only)

For this part of the experiment you should watch the video on transfer pipettes.

25.00 mL pipettes will be provided in the laboratory. The teaching assistant will point them
out.

1. Obtain a 25.00 mL transfer pipette and rinse it three times with tap water. The pipette is
rinsed by using the bulb to half fill the pipette, holding the pipette horizontally and rotating
it to allow the liquid inside to contact the inner surface of the pipette. Allow the liquid to
drain through the tip of the pipette. Do NOT pour the liquid out the top of the pipette or

85
 Ontario Tech University CHEM 1010U / 1800U, W24; Exp. 1-17.28

allow liquid to enter the bulb.

2. Collect ~150 mL of deionized water in a 250 mL beaker. Rinse the pipette once with
deionized water.

3. Weigh an empty 250 mL Erlenmeyer flask on a tared (zeroed) open-pan balance (two
decimal places) and record the mass.

4. Pipette 25.00 mL of deionized water into the flask. Tare an open-pan balance and weigh the
flask + water.

5. Repeat step 4 four more times (for a total of 5 transfers). Good pipetting technique should
give nearly identical masses for each transfer.

86
 Ontario Tech University CHEM 1010U / 1800U, W24; Exp. 1-17.28

Experiment 1 - Laboratory Safety and Orientation

Name: _______________________

Course: _______________________

Day: _______________________

Time: _______________________

TA Name: _______________________

You must submit this sheet with your report.

87
 Ontario Tech University CHEM 1010U / 1800U, W24; Exp. 1-17.28

88
 Ontario Tech University CHEM 1010U / 1800U, W24; Exp. 1-17.28

89
 Ontario Tech University CHEM 1010U / 1800U, W24; Exp. 1-17.28

DATA SHEET - Laboratory Safety and Orientation

If you are submitting your lab report electronically, you must scan or photograph all the data sheets
with your data as recorded in the laboratory period, signed and dated by the teaching assistant, and
submit them with your report.

Student Name: _____________________________

Student Number: _____________________________
Date: _____________________________
TA Signature: _____________________________

Part III - Preparation of Standard Solution

mass of 50 mL beaker + NaCl / g: ____________________________________

mass of “empty” 50 mL beaker / g: ____________________________________
mass of NaCl used / g: ____________________________________
Final volume of solution / L: ____________________________________
Checked by the TA (TA initials): ____________________________________

Part IV - Pipette Practice (CHEM 1010 only)

First Aliquot Second Third Fourth Fifth Aliquot

Aliquot Aliquot Aliquot
Mass before
transfer / g
Mass after
transfer / g
Mass
transferred / g

90
 Ontario Tech University CHEM 1010U / 1800U, W24; Exp. 1-17.28

Calculations and Questions

Part I - Safety Orientation

1. Using the laboratory template provided (see pp. 88 - 89) for your room, indicate the
location(s) of:
a. The fire extinguisher(s)
b. The eyewash stations
c. The first aid kit
d. The fire blanket
e. The spill kits

2. List five (5) restrictions and / or requirements for clothing in a chemistry laboratory.

3. Students must never pipette by mouth. Why not?

4. Sadio is a student working in a first-year chemistry laboratory. When making a solution of

sodium carbonate, he weighs out too much. What should he do with the excess sodium
carbonate? Why?

5. Kaitlyn needs to store a solution in her laboratory locker for a week. What information must
be on the label? What other information should be on the label?

6. What is the proper way to dispose of broken glass?

7. What steps should you take if the fire alarm sounds?

8. What are the appropriate treatments for i) cuts and ii) minor burns?

91
 Ontario Tech University CHEM 1010U / 1800U, W24; Exp. 1-17.28

Part III - Preparation of Standard Solution

1. Calculate the concentration of the NaCl solution in mol L-1 and with the correct number of
significant digits.

2. Why is it desirable to use the same analytical balance to weigh the weighing vial + NaCl and
to weigh the “empty” weighing vial?

3. Avoiding spilling the NaCl in the weighing vial is more important than getting all of the
NaCl out of the vial. Why?

4. When transferring the dissolved NaCl from the beaker to the volumetric flask, all the
glassware (beaker, stirring rod, funnel) are thoroughly rinsed with deionized water. Why?

Part IV - Pipette Practice (CHEM 1010 only)

1. Calculate the average mass of water transferred with the pipette.

2. Assuming the density of water is 1.00 g mL-1, calculate the average volume of water
transferred.

3. Calculate the percent error between the average volume transferred and the volume stated
on the pipette (25.00 mL).

4. Describe at least three flaws in your technique that may have led to variability in the volume
of water transferred.

92