CHEMISTRY

1211/1212 and
1203/1205

LABORATORY
MANUAL

L. RUSNAK © COPYRIGHT 1989

2024 EDITION
These experiments are found in separate files and are not contained in this document.

CHEMISTRY 1211 EXPERIMENTS

Z. Introductory Laboratory Techniques Z−1

A. Formula of a Hydrate A-1
B. Standardization and Titration of Acids and Bases B−1
C. Chemical Reactions of Copper C−1
D. Redox Titrations D−1
E. Ideal Gas Constant and Molar Volume of a Gas E−1
F. Spectrophotometric Determination of Trace Iron F−1
G. Chemical Equilibrium: LeChatelier's Principle G−1
H. Chemical Equilibrium: K for I2 (𝑎𝑞) + I − (𝑎𝑞) ⇌ I3− (𝑎𝑞) H−1

CHEMISTRY 1203 EXPERIMENTS

Z. Introductory Laboratory Techniques Z−1

B. Standardization and Titration of Acids and Bases B−1
F. Spectrophotometric Determination of Trace Iron F−1
E. Ideal Gas Constant and Molar Volume of a Gas E−1
H. Chemical Equilibrium: K for I2 (𝑎𝑞) + I − (𝑎𝑞) ⇌ I3− (𝑎𝑞) H−1
CHEMISTRY 1212 EXPERIMENTS

I. Titration Curves I-1

J. Solid Unknown Acid, Buffers J-1
K. Solubility Equilibrium: Ksp of Ca(IO3)2 K−1
L. Complex Nickel Compounds L−1
N. Qualitative Identification of Cations N−1
O. Calorimetry: Enthalpy of Reactions O−1
P. Oxidation States of Vanadium P−1
Q. Electrolysis Q−1
R. The Nernst Equation R−1
S. The Kinetics of The Oxidation of Iodide Ion by Peroxydisulfate Ion S−1

CHEMISTRY 1205 EXPERIMENTS

I. Titration Curves I-1

J. Solid Unknown Acid, Buffers J-1
K. Solubility Equilibrium: Ksp of Ca(IO3)2 K−1
O. Calorimetry: Enthalpy of Reactions O−1
S. The Kinetics of The Oxidation of Iodide Ion by Peroxydisulfate Ion S−1
Table of Contents:
I. LABORATORY AND CHEMICAL SAFETY REGULATIONS
A. Chemistry Laboratory Safety Procedures 6
B. Accidents 7
C. Handling Chemicals 8

II. LABORATORY AND CHEMICAL SAFETY REGULATIONS

A. Expectations of the First Day of Lab 9
B. Before Leaving the Lab 9
C. Check-Out 9
D. Equipment List & Diagrams 11

III. ASSESSMENT
A. Expectations of Students 13
B. Lab Reports 14
1. Pre-Lab Quiz 15
2. Data/Observation Sheets 15
3. Details Regarding Lab Reports 15
C. Assessment of Lab Grades 17
D. Lab Exams 18

IV. EVALUATION OF EXPERIMENTAL DATA

a. Classification of Experimental Errors 18
b. Accuracy and Precision 19
c. Significant Digits 21
d. Propagation of Errors 21
e. Rejection Of Suspect Data Before Averaging 23

ADVANCE STUDY ASSIGNMENT 24

ACCURACY AND PRECISION EXERCISE 26

V. APPENDICES
I. Weighing, Electronic Balance 24
II. Volume Measurements 26
A. Graduated Cylinder 26
B. Use of Buret 26
C. Use of Transfer Pipet 27
D. Use of Volumetric Flask, Quantitative Transfer 30
III. Use of the Bunsen Burner 32
IV. Filtration Techniques 33
V. Use of the pH meter 34
Use of the pH meter as a Voltmeter 35
VI. Reaction of Metal Cations With Various Reagents 36
VII. Generalized Rules for the Solubility of Salts in Water 37
CHEM 12XX Laboratory Manual: Introduction and Appendices

INTRODUCTION
Welcome to the Introductory University Chemistry Laboratory!
The laboratory is an integral part of the Introductory University Chemistry curriculum for
a number of important reasons. The central role of experimentation as the basis of chemistry is
best appreciated by personal experience in the laboratory. By collecting your own data you will
gain first-hand knowledge of the effort required in obtaining reliable experimental results. The
challenge of interpreting these results and presenting them in a concise and logically written report
will enable you to become more familiar with the concepts and reasoning processes involved in
chemistry. Introductory chemistry may be the only chemistry course that you will take at the
University level and the only opportunity to learn some practical applications of chemistry which
will be of benefit in other disciplines as well.
The experiments in this manual provide a practical application of some of the principles
studied in lectures and an introduction to the laboratory techniques that are used in all chemistry
labs. In some of the experiments you will be introduced to new concepts even before they are more
thoroughly discussed in lectures. Although the lab schedule correlates closely with lectures, a
"lecture-prior-to-lab format" is not always possible. Approach each experiment as a learning
experience rather than as a confirmation of a known principle. An exposure to some concepts
prior to lectures will also help you to understand lectures better and will help you to appreciate
that chemistry is experimentally based.
You are expected to carry out each experiment independently and to arrive at your own
conclusions and answers to questions and thus you must be well prepared in advance before
coming to the laboratory. Each experiment includes a relevant theory section and pre-lab
assignments are included to guide you in your preparation. For each experiment you should think
in terms of: a) the major objective, b) the experimental approach, c) the measurements and
observations to be made, and d) the calculation and interpretation of the results. Pay particular
attention to procedures so that you can use lab time more effectively and become aware of any
hazards involved. If you prepare in advance and try to understand the chemical principle that
underlies each step of the procedure, you will learn more from the laboratory and your enjoyment
of the laboratory and course will be enhanced.
If you have difficulties, your Lab Instructor is available for help. We wish you success in
this laboratory and the course!

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CHEM 12XX Laboratory Manual: Introduction and Appendices

I. LABORATORY AND CHEMICAL SAFETY REGULATIONS

Although no specifically hazardous experiments are performed in Chemistry 1211 & 1212
it is not possible to achieve zero risk in a chemical laboratory. Potential dangers are inherent in all
chemical experimentation but the normal risks and hazards of working in a chemistry lab can be
minimized if general safety procedures are observed at all times. You are expected to know and
follow the safety procedures outlined below. In addition, comply with the "Safety Precautions"
relating to each experiment that are emphasized in the procedures.
Anyone who fails to follow these regulations will not be allowed to perform the experiment
and will be required to leave the lab.
A. CHEMISTRY LABORATORY SAFETY PROCEDURES
1. Eating, drinking, applying cosmetics (including lip balm) and smoking are prohibited in all
the labs including the Student Lab.
2. Everyone working where laboratory experiments are being performed must wear lab coats.
3. Everyone working where laboratory experiments are being performed must wear safety
glasses with side shields. Goggles and face shields are available in the labs as well. Be advised
that if you wear contact lenses in the lab you should avoid touching your eye area as you may
transfer chemical residue to the eye area. Any student wearing contact lenses must inform the
instructor.
4. Everyone working where laboratory experiments are being performed must wear appropriate
clothing and footwear. Appropriate clothing will protect the legs and feet from chemical spills
and burns.
5. Work areas will be kept free of clutter by storing coats, purses, backpacks etc in lockers
outside the labs.
6. All wastes will be collected in appropriately labeled containers and disposed of in the proper
manner.
7. Any one not following these procedures will be required to leave the lab.
8. Each lab will have a properly maintained first aid kit, a fire extinguisher, a safety shower, an
eye wash station, a phone, and or an emergency communicator and a fire blanket for use in
case of emergency.
9. Safety Data Sheets of all chemicals stored and used in the labs will be available for review by
staff and students. You can also view on line through the Loop: click on the RDC Student Life

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CHEM 12XX Laboratory Manual: Introduction and Appendices

or Work Life tab and then in the Health, Safety & Wellness section click on Material Safety
Data Sheets.
10. All accidents, chemical spills and incidents must be reported to the College Health Centre by
the supervising instructor, ASAP.
11. Each lab will have a list of emergency information and procedures posted.

B. ACCIDENTS
Fires
1. Keep flammable materials away from flames. Avoid loose-fitting clothing, long hair should
be tied back.
2. Extinguish all flames not in use. Never leave a flame unattended.
3. In case of fire, first have someone alert the lab instructor, then try to put out the fire with the
fire extinguisher. If your clothing should catch fire, try to smother the fire. This may be done
by rolling on the floor or in the case of more extreme situations use the fire blanket.
4. If the fire alarm sounds, turn off all equipment and follow the directions of the lab instructor
to leave the lab.
Cuts
1. All broken glassware should be immediately discarded in the "Glass Garbage". Never use
cracked glassware and glass with sharp edges such as broken tubing.
2. Fire-polish all glass tubing or rods to prevent cuts from the sharp edges. Tubing must be fire-
polished and lubricated before insertion into a cork or stopper. Always lubricate the tube to
be inserted with glycerin.
3. Do not attempt to force frozen glass joints, stoppers, or stopcocks. Take them to your instructor
for removal.
Acid And Alkali Burns
These should be flushed with large amounts of running water for several minutes. Then
saturated sodium bicarbonate solution (or paste) can be used for acid burns, and saturated boric
acid solution for alkali burns, while seeking medical attention. A safety shower is located in the
lab as well as an eye wash. Have a fellow student notify the lab instructor.

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CHEM 12XX Laboratory Manual: Introduction and Appendices

C. HANDLING CHEMICALS
1. All chemicals must be handled with care and in such a way that they do not come in contact
with your skin.
2. Regard all chemicals in the laboratory as poisonous and never taste them. When it is necessary
to note the odor of a substance, fan the vapors gently with your hand toward your nose. Never
smell concentrated fumes.
3. Chemical reagents are stored in labeled bottles. Read the label carefully before removing any
material. Do not take more chemical than is required. Do not, under any circumstances, return
unused chemical to the reagent bottle. When you have finished, return the bottle to its proper
place and clean up any spills.
4. Certain chemical reactions involving poisonous, irritating, or objectionable gases or vapors
must be carried out in the fume hood. Watch for the instructions in the procedures and follow
the directions.
5. Concentrated acids and bases are stored in the fume hood and must be dispensed there. Handle
them with care and do not carry them to your bench. Spilled acid or base and rings from acid
or base bottles, must be wiped up immediately. If a large quantity of an acid is spilled, inform
the laboratory instructor who will supervise the cleanup with sodium bicarbonate and water.
6. When diluting concentrated acid, add the acid slowly to the water. Never add water to
concentrated acid. The considerable heat evolved can cause the acid to spatter and result in
serious burns.
7. Dispose of wastes only in the manner prescribed by your lab instructor and lab manual. Many
solid reagents cannot be safely disposed of in trash receptacles. Toxic chemicals are collected
in the recycling waste containers provided in the fume hood. Only non-toxic water-soluble
chemicals such as dilute acids and bases can be flushed down the sink. Use the "glass garbage"
for broken glassware. If a mercury thermometer is accidentally broken, inform the lab
instructor immediately for proper disposal of the mercury.
8. When boiling liquids or carrying out chemical reactions in test tubes, keep the mouth of the
test tube pointed away from yourself and from those near you. This will prevent burns or other
injuries, should the contents of the tube spurt out.
9. Use a cork to stopper all test tubes or flasks that must be shaken; do not use your hand or
thumb as a stopper. Do not heat closed containers.
10. When pipetting never use your mouth to apply suction; always use the rubber bulb supplied.

·9· Introduction
CHEM 12XX Laboratory Manual: Introduction and Appendices

II. LABORATORY PROCEDURES

A. EXPECTATIONS FOR THE FIRST DAY OF LABORATORY

1. Arrive promptly at the scheduled hour with your safety glasses or goggles, a lab coat and a
scientific calculator.
2. Your instructor will provide a general safety orientation and review lab procedures and
assessment. There will be a video on the use of a volumetric flask, the pipet and the buret, a
virtual lab tour and significant figures you are to watch prior to the first experiment
3. Check-in: The lab instructor will assign a locker containing various glassware and equipment.
Record the locker number and lock combination for future reference. Fill out the lab
registration sheet and return it to the lab instructor. Do a quick check of the equipment in your
assigned locker against the equipment list on the following page as to quantity and condition.
Bring any deficiencies to the attention of the lab instructor. Remember to keep the equipment
clean, in good condition. Equipment broken or lost during the year must be immediately
replaced. Inform the lab instructor of any items you find missing during the term. Additional
equipment may be required for certain experiments. This equipment is stored throughout the
room and should be returned to the proper location at the end of the lab period.
4. Complete the Advance Study Assignment and submit it to the instructor at the end of the lab
period.

B. BEFORE LEAVING THE LAB

1. Your work area (work bench, sink, fume hood, balance area) is tidy.
2. Any special equipment and reagents are returned to the cart.
3. The balance which you used is clean.
4. Gas valves and water taps are shut off.
5. Your locker is securely locked.
6. Your Data Sheet is initialed by your Lab Instructor.

C. CHECK−OUT PROCEDURES
All students must check-out in order to get clearance from the course. Students withdrawing
from the course must make arrangements with the technologists for check-out.
Remove all equipment from the drawer. Clean and remove labels from glassware. Use
the equipment list to ensure everything is present. Use the lost and found at the back of the room

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CHEM 12XX Laboratory Manual: Introduction and Appendices

to retrieve missing items or drop off extra items. Inform the lab instructor or technologist when
you are ready to have your equipment checked.
Chemistry 1211/1212 Locker Equipment List
ITEM TYPE QUANTITY

Beaker 50 mL 2
Beaker 150 mL 1
Beaker 250 mL 4
Beaker 400 mL 1
Beaker 600 mL 2
Beaker 800 mL 1
Clamp, test tube 1
Flask, Erlenmeyer 50 mL 1
Flask, Erlenmeyer 125 mL 2
Flask, Erlenmeyer 200/250 mL 2
Flask, Erlenmeyer 250/300 mL 2
Funnel, filtering 65 mm 2
Graduated cylinder 10 mL 1
Graduated cylinder 25 or 50 mL 1
Graduated cylinder 100 mL 1
Scoop, lab 1
Stirring bar, magnetic 1
Stirring rod with rubber 1
policeman
Test tubes 13 x 100 mm 6
Test tubes 18 x 150 mm 6
Test tubes 25 x 150 mm 2
Thermometer, alcohol -10C to +110C 1
Wash bottle 250 mL 1
ADDITIONAL COMMUNAL LAB EQUIPMENT - located in labeled drawers and cupboards.
Clay triangles, crucible tongs, iron rings, wire gauze, test tube brushes, Bunsen burner, rubber
tubing, utility clamp, Mohr clamp, buret and buret clamp, volumetric flasks and pipets.

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CHEM 12XX Laboratory Manual: Introduction and Appendices

COMMON LABORATORY EQUIPMENT

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CHEM 12XX Laboratory Manual: Introduction and Appendices

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CHEM 12XX Laboratory Manual: Introduction and Appendices

III. ASSESSMENT
The lab component of Chemistry 1211 & 1212 (1203 & 1205) is compulsory and must be
successfully completed to obtain credit in the course.

A. EXPECTATIONS OF STUDENTS
Introduced in Fall 2023 a 10−mark performance has been added to each laboratory experiment.
The following will be considered toward this 10 mark performance grade. This purpose of this
grade is to make sure that you are prepared for the lab and listen while the pre−lab instructions are
given. Failure to be prepared for an experiment (which will be clear to your lab instructor), adhere
to safety measures (given in experiment or during pre−lab talk) or to not show up on time will
result in loss of performance marks.
i. Attendance
You are required to attend all lab periods, independently perform all experiments and hand in
all lab reports by the due date otherwise a zero grade will be assigned. If you must miss a lab for
a valid reason, you must report to your lab instructor and explain the reason for the absence in
order to be excused from that lab. In the event of illness, a medical certificate is normally required.
If a lab is missed for a valid reason, as assessed by your lab instructor, this lab will not be counted
in determining your average lab grade, otherwise missed labs will be assigned a zero grade. It may
be possible to arrange for a make-up lab with your lab instructor in another period during the week
that the experiment is scheduled, subject to available space. Written permission to attend an
alternate lab section must be first obtained from your lab instructor.
In order to obtain credit for the lab, no more than two experiments can be missed for whatever
reason. Students who are absent for more than two lab sessions, or who do not submit the reports
for more than two experiments, are not permitted to write the final lab exam.

ii. Punctuality
You are expected to arrive on time as a pre-lab quiz and lab lecture begin promptly at the
beginning of the lab period. If you arrive late you will not be given extra time for the pre-lab quiz
and you are not allowed to start the experiment without specific permission from the lab instructor.

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CHEM 12XX Laboratory Manual: Introduction and Appendices

iii. Work Independently

Come prepared to perform the experiment on your own unless otherwise directed. In
experiments in which you are directed to work with a partner, you must prepare your own data and
report sheets. All critical thinking, calculations and writing must be your own. Copying another
student's report and not thinking through the experimental results on your own will result in poor
performance on the final lab exam.

iv. Advance Preparation

For each experiment you must read the theoretical considerations and procedure, and do the
Advance Study Assignment before coming to the lab. You should think in terms of: (a) the major
objective, (b) the experimental approach, (c) the measurements and observations to be made, and
(d) the calculation and interpretation of the results. Think about the procedures so that you can use
lab time more effectively and become aware of any hazards involved. However, do not become
overly focused on just the procedures and attempt to perform the lab using a "cook-book
approach"; instead try to think about the chemical principle that underlies each step of the
procedure, the concepts being illustrated, and how these concepts fit in with you already know.
Using this approach you will learn more from the laboratory.
The Advance Study Assignment is designed to help you understand the experiment and to
give you practice with the calculations. Advance Study Assignments are generally not graded;
answers are provided to the questions. However, your lab instructor may choose to have you hand
in the Advance Study Assignment in lieu of a quiz for some experiments.

B. LABORATORY REPORTS
You will be required to submit a weekly lab report consisting of the completed data sheet,
previously initialed by the lab instructor, and the report form. Report forms with space provided
for calculations and answers to questions are given in the manual at the end of most experiments.
Reports must be written in ink.
You will be required to submit a weekly lab report consisting of the completed data sheet,
previously initialed by the lab instructor, and the report form. Report forms with space provided
for calculations and answers to questions are given in the manual at the end of most experiments.
Reports must be written in ink.

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CHEM 12XX Laboratory Manual: Introduction and Appendices

Lab Report Deadlines

Reports must be submitted weekly within two days after the lab in the appropriate deposit box
located in the hallway opposite to Room 1409 unless otherwise specified by your instructor.
Specific dead-line times will be announced by your lab instructor. You will be given a certain
number of “grace days” (depending on course) that will allow you to hand in late lab reports
provided you email your instructor before the due date.
Your lab instructor might allow (or ask) you to hand in your labs electronically via Blackboard.
They will inform you of their preferred hand−in practice on the first lab period.
TIP: Try to finish the calculations and answers to questions before leaving the lab whenever
possible. You will work more efficiently when the concepts and experimental observations are
fresh in your mind and your instructor is available to assist you with any difficulties.
For each experiment you will be assigned a mark of 30 points consisting of the following
components:
i. Pre−Lab Quiz
Generally, you will be given a 10-15 minute quiz at the beginning of each lab period
consisting of questions relating to the procedures, experimental observations and interpretations
on the current experiment. Some of the questions will be the same as or similar to the Advance
Study Assignment. The lab quiz will be valued at 4 marks towards the 30 possible marks for the
experiment.
ii. Data/Observation Sheet
Data sheets are included in the manual at the end of each experiment. The data sheet has
been prepared to simplify the recording of data and to avoid loose pages of paper. Record your
data and observations directly on the data sheet as you perform the experiment. Sheets of scrap
paper are not to be used for recording data. Enter all data neatly in pen. Numerical data must be
expressed with the correct number of significant digits and units. If an error is made simply cross
out the incorrect entry neatly and enter the correct value. The data sheet must be initialed by your
lab instructor prior to you leaving the lab.
iii. Lab Report
Report forms with space provided for calculations and answers to questions are given in the
manual at the end of most experiments. The report forms are intended to help you organize the
calculations and interpretation of the results into a professional report. The appropriate pages can

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CHEM 12XX Laboratory Manual: Introduction and Appendices

be removed from the manual as part of your report. Attach an additional loose-leaf page if more
space is required. For some experiments you will be asked to organize your own report forms.
a. Calculations
The required calculations are outlined in considerable detail but with the expectation that you know
how to perform the calculations involved. It is important that you understand the reasons behind
each step in a calculation that connects what is known (the data) with what is desired (the result).
Calculations must be presented in logical steps so that they are easy to follow using dimensional
analysis showing all units to arrive at the correct units for the final result. Report your calculated
results with the correct number of significant digits. Check your work to avoid simple mistakes in
arithmetic.
b. Graph Requirements
In some experiments you will visually display your results using a graph. Use the following
conventions when graphing:
(i) Use a full sheet of quality (1.0 mm grid) graph paper to improve the precision of the
graph. Plot the experimentally controlled variable on the horizontal axis and the
measured dependent variable on the vertical axis. Data must be plotted accurately —
don't just estimate the position of points!
(ii) Choose a convenient but largest possible scale for each axis so that you get a full-page
graph. In this process consider if it is best to display the independent variable on the
long or the short edge of the graph paper and if the scales have to start at zero or not.
(iii) Neatly print the label on both axes in ink and include the units.
(iv) Title the graph so that the title completely defines the information represented by the
graph and what experiment was performed to obtain the data; do not simply use the
title of the experiment or do not simply title your graph “y axis title vs. x axis title”.
Essentially, someone looking at the graph should not need the laboratory manual to
ascertain what information the graph is attempting to convey.
(v) Carefully plot the data points and circle the points.
(vi) If there is a linear relationship between the two variables being graphed, as is often the
case, use a transparent ruler and a pencil to draw a line of best fit through the data
points. The line should be drawn so that about the same number of points fall above as
below the line, and the line is positioned to minimize the sum of the residuals (the
distance between the points and the line). In this process any suspect data points are

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CHEM 12XX Laboratory Manual: Introduction and Appendices

given lower weighting or even ignored whereas a point such as the origin (0,0) may be
given greater weighting if the instrument was calibrated to "zero".
𝑟𝑖𝑠𝑒 𝑦2 −𝑦1
If you are required to determine the slope (𝑠𝑙𝑜𝑝𝑒 = = ) of a straight-line graph, use tick
𝑟𝑢𝑛 𝑥2 −𝑥1

lines to draw in a right-angled triangle and determine the rise and the run in units of each axis. Use
“points” on the line, not the plotted data points, to determine the slope and include the units of the
slope.
c. Discussion Requirements
No report is complete without an interpretation and evaluation of the experimental results. In
the report sheets specific questions are asked to assist you in the evaluation of your results. This
component of the report is frequently the most difficult since it requires you to reflect upon your
results in terms of identifying the possible sources of determinate experimental errors that
frequently are present (See "Section IV" below). The discussion and answers to questions are
unique for every experiment but some common features are:
i) Compare your calculated results to any known values usually given in the manual but if from
another source list the references for the literature value. Do this by calculating the experimental
% error and identify if your value is high or low.
ii) Consider some possible sources of experimental error in the design of the experiment or how
the measurements were made and assess if these can logically account for the direction (high or
low) and magnitude of the observed error.
iii)For each logically possible source of determinate error, explain how your proposed source of
error can account for the observed discrepancy.
Written explanations for the discussion and the questions asked must be concise, neat, and
with no spelling or grammatical errors.

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CHEM 12XX Laboratory Manual: Introduction and Appendices

C. ASSESSMENT OF LAB GRADES

Please see Course Outline for break down of Lab Reports and Lab Exam(s). The assessment of
your weekly lab grade will be arrived at as follows:

Lab Report 16 marks*

Lab Quiz 4 marks
Laboratory Performance 10 marks (see below)
Deductions (if any) mostly significant−figure deductions (max 10% of lab report)
Total for each lab session 30 marks
* The grading scheme for each lab report is indicated on the report sheet.

Note that in addition to penalties for late reports, points may be deducted from your weekly lab
grade (under Laboratory Performance) for any of the following (but not restricted to) reasons:
• arriving late or not being prepared for a lab
• not following safety rules
• not being tidy in the lab
• not completing an experiment on time
• data and report sheet not in ink

D. LAB EXAM(S)
One lab exam will be scheduled outside of regular lab hours and are common for all lab
sections. See the laboratory schedule for the date and time of the exams. The exams consist of
short answer questions relating specifically to the experiments performed in the lab and
interpretation of the results of each experiment. Many of the questions are like the Advance Study
Assignment questions. More information about the lab exam will be provided in the lab period.

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CHEM 12XX Laboratory Manual: Introduction and Appendices

IV. EVALUATION OF EXPERIMENTAL DATA

a. Types of Errors
1. Determinate (systematic) errors cause experimental results to be either all lower or all higher
than the actual value. Examples include error in experimental design or method and faulty
calibration of equipment. Determinate errors can often be avoided or compensated for by
calibration of the measuring device (comparison with a known standard) or improved
methods. In the experiments that you will perform in the lab, determinate errors generally fall
in the range of 0-5% assuming good technique is employed. Essentially, determine errors
would not be present if the method and/or instrumentation were perfect. You will be expected
to consider possible sources of determinate error and to assess if these can logically account
for the direction (high or low) and magnitude of the error in your results.

It is common to think of “transfer errors” (i.e. spillage, non−quantitative transfer of reagents

between containers, etc.) or “experimenter mistakes” (i.e. not reading a balance properly, not
setting up glassware properly, etc.) as determinate errors, but the latter can be removed with
good technique, and the former isn’t an error at all, as it’s impossible to completely eliminate
(transfer of substances between containers can never be 100% efficient). A good statement to
follow would be something along the lines of: “Imagine the best chemist in the world with
unlimited time performs this experiment. The flaws in the method could still be present and
thus there will be some measure of determinate and/or random errors present.”

2. Random error causes some measurements of a quantity to be higher and some lower than the
actual value. In the absence of determinate error, repeated measurements fluctuate randomly
about the average for the set. Random errors cannot be entirely eliminated but improved
technique and greater precision of the instruments used can reduce them.

3. Gross errors cause occasional suspect values (outliers) that differ significantly from the rest
of the repeated measurements of a set. Often gross errors are due to blunders, which are totally
avoidable and must be eliminated.
In designing and performing experiments the object is to reduce or ideally eliminate
determinate errors. Then, the cumulative effect of all random errors remain which can be
compensated for by averaging the results for a sufficiently large number of runs.

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CHEM 12XX Laboratory Manual: Introduction and Appendices

b. Accuracy and Precision

Accuracy refers to the agreement of a measured value with the "true" or accepted value and is
commonly expressed as a percent experimental error:

|𝑒𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 𝑣𝑎𝑙𝑢𝑒 − 𝑎𝑐𝑐𝑒𝑝𝑡𝑒𝑑 𝑣𝑎𝑙𝑢𝑒|

% 𝑒𝑟𝑟𝑜𝑟 = × 100
𝑎𝑐𝑐𝑒𝑝𝑡𝑒𝑑 𝑣𝑎𝑙𝑢𝑒

A negative value would mean a low experimental result and a positive value a high result.

Precision refers to the agreement among repeated measurements of the same quantity, i.e. their
reproducibility. Precise measurements have low random error (small deviations from the average)
but may be inaccurate due to the presence of a constant determinate error. Accurate measurements
have low determinate error and, generally, low random error as well.
In some experiments you will be asked to report the precision of your results in terms of
the % relative average deviation, which is determined as follows:

Assessing the Precision of Experimental Results: % relative average deviation:

1. For a series of n measurements (n is at least three) calculate the average value (𝑋𝑎𝑣𝑔 ).
2. For each measurement, determine its absolute deviation from the average value (i.e. ignore
the sign of the deviation).

𝐷𝐸𝑉𝑎𝑏𝑠 = |𝑋𝑖 − 𝑋𝑎𝑣𝑔 |

3. Determine the average of the absolute deviations of the ith measurement of n total
measurements:

∑|𝑋𝑖 − 𝑋𝑎𝑣𝑔 |
𝐷𝐸𝑉𝑎𝑣𝑔 =
𝑛

4. Express this as a % relative average deviation:

|𝐷𝐸𝑉𝑎𝑣𝑔 |
%𝑅𝐴𝐷 = × 100
𝑋𝑎𝑣𝑔
Example:
In a determination of the molar concentration, M, of an HCl solution by titrating with standard
NaOH, the following results were obtained. Calculate the % relative average deviation.

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CHEM 12XX Laboratory Manual: Introduction and Appendices

Run Calculated [HCl] in M 𝑫𝑬𝑽𝒂𝒃𝒔 = |𝑀𝑖 − 𝑀𝑎𝑣𝑔 |

1 0.4362 |0.4362 − 0.4259 𝑀| = 0.0103 𝑀

2 0.4271 |0.4271 − 0.4259 𝑀| = 0.0012 𝑀

3 0.4145 |0.4145 − 0.4259 𝑀| = 0.0114 𝑀

0.4362 + 0.4271 + 0.4145 𝑀

𝑀𝑎𝑣𝑔 = = 0.4259 𝑀
3
0.0103 + 0.0012 + 0.0114 𝑀 0.0229 𝑀
𝐷𝐸𝑉𝑎𝑣𝑔 = = = 0.00763 𝑀 (3 𝑠𝑖𝑔. 𝑑𝑖𝑔𝑖𝑡𝑠)
3 3
0.00763 𝑀
%𝑅𝐴𝐷 = × 100 = 1.76% (3 𝑠𝑖𝑔. 𝑑𝑖𝑔𝑖𝑡𝑠)
0.4259 𝑀

A relative average deviation of 1% or less is the expected precision for an acid-base titration
performed at the first-year level. The above results represent somewhat higher than expected
scatter and an additional titration could possibly be performed to improve the precision.
Another meaning of precision is the fineness of a measurement as indicated by the number
of decimal places and significant digits that are possible. The precision with which some simple
laboratory measurements can be made are:

Instrument Precision
10-mL graduated cylinder ± 0.05 mL
100-mL graduated cylinder ± 0.5 mL
50-mL buret ± 0.02 mL
100-mL volumetric flask ± 0.08 mL
250-mL volumetric flask ± 0.12 mL
110 ºC thermometer ± 0.2 ºC
Electronic balance * (Type in Chem. 1211/1212 lab) ± 0.003 g
pH meter (Type in Chem. 1211/1212 lab) ± 0.05 pH units
* Although the balance operates to a precision of ± 0.003 g, it is essential that the digital read-out scale be
read to ± 0.001 g. Thus, for a measurement of 9.750 g the actual mass lies in the range 9.747 - 9.753 g.

c. Significant Digits
The first uncertain digit in an experimental measurement or in a calculated result from a series
of measurements is the last significant digit. It is important to record a measurement with the
correct number of significant digits that reflects the precision of the instrument employed (no fewer

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CHEM 12XX Laboratory Manual: Introduction and Appendices

or more digits than are warranted). In general, when reading the scale of any apparatus, the last
significant digit is estimated by interpolating between the smallest scale markings. It is usually
possible to estimate the last digit of a measurement to the nearest tenth of the distance between the
markings. For example, when using a 50-mL buret, which is graduated in 0.1 mL, you should
estimate the meniscus level to the nearest ±0.01 mL although the actual uncertainty in the reading
is probably closer to ±0.02 mL.
Also, the result of a calculation from experimental measurements must be expressed with
the correct number of significant digits to reflect the overall uncertainty in that result.

d. Propagation of Errors
Since the final calculated result of an experiment is often the combination of several different
measurements the overall error of the final result is the total combined error. Although you will
not be expected to perform detailed error analysis in this course, you should apply the following
two rules:
1. The absolute error in the sum or difference of two measurements is the sum of the absolute
uncertainties in the two measurements. For example, if the uncertainty in reading a perfectly
calibrated buret is ± 0.02 mL, the error in the volume of liquid delivered due only to reading
the meniscus level is:

final buret reading 21.28 ± 0.02 mL

initial buret reading 17.32 ± 0.02 mL
volume delivered 3.96 ± 0.04 mL ← total absolute error

𝑎𝑏𝑠𝑜𝑙𝑢𝑡𝑒 𝑒𝑟𝑟𝑜𝑟 0.04

%𝑟𝑒𝑙𝑎𝑡𝑖𝑣𝑒 𝑒𝑟𝑟𝑜𝑟 = × 100 = × 100 = 1%
𝑚𝑎𝑔𝑛𝑖𝑡𝑢𝑑𝑒 𝑜𝑓 𝑚𝑒𝑎𝑠𝑢𝑟𝑒𝑚𝑒𝑛𝑡 3.96

Note that if the precision of the buret readings had been ±0.1 mL instead, the total error in the
volume delivered would be ±0.2 mL and the volume of liquid delivered would have to be rounded
off to the first decimal place as 4.0 ± 0.2 mL. The result of a calculation must be written with the
correct number of significant digits to convey the uncertainty in the result.

2. The relative error in a product or quotient of two measurements is the sum of the relative
errors of the two numbers that are multiplied or divided.

· 23 · Introduction
CHEM 12XX Laboratory Manual: Introduction and Appendices

Significant Digits in a Calculated Result

You are expected to use the following two rules regarding significant digits when performing
calculations for your lab reports. The use of significant digits is a useful approximation to the full
use of the above two rules for the propagation of errors. The fundamental rule is that the least
certain measurement sets the limit of certainty in the answer to the overall calculation.
1. In addition and subtraction, the answer must be written with the same number of decimal
places (same number of significant digits to the right of the decimal point) as there are in the
measurement with the fewest decimal places. The reason for this rule is that the precision of the
answer (i.e. the number of decimal places) is limited by the least certain number which has the
greatest absolute error. Example: 9.5 mL + 7.25 mL = 16.75 mL (properly rounded off to the
nearest ± 0.1 mL as 16.8 mL). Note that the answer (16.8 mL) contains three significant digits
even though the first measurement has only two significant digits.
2. In multiplication and division, the answer is generally written with the same number of
significant digits as there are in the measurement with the fewest significant digits (greatest relative
error). The more exact rule is that the final answer must have about the same relative uncertainty
(% error) as the measurement that has the greatest relative uncertainty.
Usually the significant-digit rule agrees with this exact rule but occasionally it results in incorrect
rounding. You will be expected to use the significant-digit rule.

Example:
If 10.0 mL of water at 22 ºC weighed 9.978 g, calculate its density at this temperature.

𝑚 9.978 𝑔
𝑑𝑒𝑛𝑠𝑖𝑡𝑦 = = = 0.998 𝑔 ⋅ 𝑚𝐿−1 (3 𝑠𝑖𝑔. 𝑑𝑖𝑔𝑖𝑡𝑠)
𝑉 10.0 𝑚𝐿

Tip: In a multi-step calculation, retain one or more insignificant digits until you have finished the
entire calculation, then round off the final answer to the correct number of significant digits.
However, when asked to report a result of any one step in the calculation you must also report it
properly rounded off with the correct number of significant digits.

e. Rejection of Suspect Data before Averaging

In some experiments you will be asked to report an average value of a result from two or more
determinations of the same quantity. Since the number of runs is too small to allow for valid

· 24 · Introduction
CHEM 12XX Laboratory Manual: Introduction and Appendices

statistical treatment of the data, you should use common sense in determining the best average to
report. Significantly different values of the same quantity should not be averaged. If you are aware
of a known determinate error for a particular run, reject that run before calculating the average.
Thus, if you make three determinations and observe that one of them is very different (≥ 5%) from
the other two which are more precise, the suspect value should be rejected before calculating the
average of the two remaining runs.

· 25 · Introduction
CHEM 12XX Laboratory Manual: Introduction and Appendices

V. APPENDICES
What follows on these pages are specific instructions on specific techniques and/or how to use
specific equipment in the laboratory.

I. WEIGHING TECHNIQUES AND USE OF AN ELECTRONIC BALANCE

INSTRUCTIONS FOR THE METTLER PE-360 ELECTRONIC BALANCE

The total mass of a container and its contents must not exceed the 360-g capacity of the
balance. Before weighing ensure that the pan compartment is clean and the door to the
compartment is closed. Check to see that the balance is level (bubble is in the center of the spirit
level) and if not, adjust the appropriate leveling leg.

A. Direct Weighing of a Solid Sample Into a Weighed Container

1. Turn on the digital display by depressing the control bar. Wait for the display to read 0.000.
Place the container to be weighed gently on the pan and close the door.
Never place chemicals directly on the pan; use a suitable container such as a beaker,
plastic weighing boat or weighing paper.
2. A green dot to the left of the display will go out when the reading has stabilized. Read and
record the mass to ±0.001 g.
Although the balance operates to a precision of ± 0.003 g, it is essential that the digital read-
out scale be read to ± 0.001 g. Thus if the reading is 9.750 g, the actual mass lies in the range
9.747 - 9.753 g.
3. Remove the container from the balance pan momentarily and with your spatula add the
approximate amount of sample required to the container. Return the container to the pan and

Weighing Techniques · 26 · Appendix I

CHEM 12XX Laboratory Manual: Introduction and Appendices

re weigh. Transfer chemicals outside the balance compartment to avoid spilling chemicals on
the pan and inside the balance compartment.
Any excess solid taken must be disposed of in the "solid waste" container on the balance
bench and must never be returned to the reagent bottle.
DO NOT TRANSFER CORROSIVE CHEMICALS TO OR FROM THE CONTAINER
WHILE THE CONTAINER IS ON THE BALANCE PAN.
If the sample mass is not in the acceptable range required,1 remove the container from the
balance again and use a spatula to add or subtract sample. Reweigh the container and contents.
4. Record all weighings directly into your lab data sheet in ink.
5. When finished, switch off the display by lifting the control bar briefly. Ensure that the
compartment is clean and the door is closed.

B. Weighing a Sample by Taring The Weight of the Container

When a sample is weighed into a container the weight of the container may be canceled out
(tared) as follows:
1. Turn on the digital display to get 0.000 g.
2. Place the container gently on the pan and close the door.
3. After the weight is displayed on the readout, briefly press the control bar. The display will
blank out momentarily, then read 0.000. The container weight is now tared.
4. Remove the container from the balance pan.2
5. Add the sample to the container, return the container to the balance pan, and read the mass of
the sample directly from the display.

CLEAN UP ANY SPILLS IMMEDIATELY.

1
When you are asked to weigh about 1 g of sample to ±0.001 g, you must know the sample mass accurately to ± 0.001
g, however, the mass does not have to be exactly 1.000 g. A range of sample masses (±5-10%) will suffice but you
must know the mass of sample taken accurately to ±0.001g. Do not spend time trying to obtain the exact amount
specified in the procedure.
2
IF THE SAMPLE IS NOT CORROSIVE, YOU ARE PERMITTED TO CAREFULLY ADD THE SAMPLE TO
THE CONTAINER WHILE IT IS ON THE BALANCE PAN AND MONITOR THE DISPLAY AS THE SAMPLE
IS BEING ADDED.

Weighing Techniques · 27 · Appendix I

CHEM 12XX Laboratory Manual: Introduction and Appendices

II. VOLUME MEASUREMENTS

A. GRADUATED CYLINDERS
Graduated cylinders are used for only approximate volume measurements and various sizes
are available. By use of the smallest size that will hold the volume being measured, an accuracy in
the range 1-5% can be attained. The precision of a 10-mL graduate cylinder is ±0.05 mL. A 100
mL graduate cylinder can be read with a precision of ±0.5 mL and has an accuracy of about +1%.
When reading the liquid level, the bottom of the meniscus should be read with the eye on the same
level as the bottom of meniscus to minimize parallax error.

B. USE OF THE BURET

Burets are designed to deliver precise but variable volumes of liquid, particularly for
titrations. A 50 mL buret has 0.1 mL graduations along its length and the meniscus level must be
read by interpolation to the nearest 0.01 mL. The precision is ±0.02 mL. Typical uncertainty in the
volume of liquid delivered is about +0.1%. Parallax errors in reading must be minimized as
described below. For reproducible delivery the tip must be free of chips and the buret must be
properly cleaned.

1. Cleaning a Buret. First use a detergent solution and a buret brush to remove any grease and
dirt from the buret. Rinse out the cleaning solution with tap water and then with distilled water
(drained through the stopcock). If a buret is properly cleaned, distilled water should drain
evenly down the walls leaving no clinging droplets.
2. Filling a Buret. To avoid diluting the solution to be used, rinse the cleaned buret two or three
times with 5 mL portions of the solution with which the buret is to be filled. Tilt the buret to
allow the entire inner surface to come in contact with the liquid. Drain the buret after each
rinsing then fill with the solution to above the graduations. Allow the solution to fill the buret
tip by slowly opening the stopcock. Expel air bubbles that form beneath the stopcock by
draining the buret with the stopcock wide open. Drain the buret to bring the meniscus below
the zero mark. Wait 30 seconds for drainage of liquid down the buret walls before taking a
reading.
3. Reading a Buret. Always read the bottom of a meniscus and the eye must be level with the
bottom of the meniscus to avoid parallax. Your eye will be level with the bottom of the

Volume Measurements · 28 · Appendix II

CHEM 12XX Laboratory Manual: Introduction and Appendices

meniscus if you cannot see the back-side of the encircling graduation nearest to the meniscus.
Since graduations on a 50-mL buret are 0.1 mL apart, a meniscus level between the marks
must be interpolated. In this estimation the width of the lines must be taken into account. The
thickness of a graduation line on a 50-mL buret corresponds to about 0.02 mL and thus takes
up one fifth of the distance from one mark to another. Read a given line value when the bottom
of the meniscus just touches the top of the line. When the bottom of the meniscus is at the
bottom of the mark, the reading is 0.02 mL greater than the reading when the meniscus just
touches the top of the line as illustrated in Figure 1.

Figure 1: Several meniscus levels in a 50-mL buret read to ±0.01 mL by interpolating the last
digit. The thickness of a line is about one-fifth of the distance between one division line and the
next and therefore is equal to about 0.02 mL. For clarity the vertical scale is exaggerated over the
horizontal.

Use a buret-reading card to locate the bottom of the transparent meniscus. Place the card
behind and against the buret so that the top edge of the black portion is at, or no more than a scale
division below, the bottom edge of the meniscus as shown in Figure 2. Reflection of the dark
portion of the card in the meniscus makes the bottom of meniscus stand out more clearly. For some
highly colored solutions, such as permanganate or iodine, there appear to be two meniscuses and
the bottom of the meniscus may be difficult to see; in such cases the top may be read. The important
point is to perform the readings reproducibly.

Volume Measurements · 29 · Appendix II

CHEM 12XX Laboratory Manual: Introduction and Appendices

Figure 2: Holding a buret-reading card in the correct position to sharpen the bottom of the
meniscus.

4. Titration. Hold the Erlenmeyer so that the buret tip is about 1-2 cm into the neck and
continuously swirl the flask with your right hand while manipulating the stopcock with your
left. (Use the opposite configuration if you are left-handed). This technique may seem
awkward at first but with practice it becomes automatic.

5. Endpoint. Near the endpoint of a titration, you should be adding titrant 1 drop at a time. When
the endpoint is close there is a local transient indicator color change when a drop from the
buret hits the solution. As the trail of color persists longer and longer make the additions
smaller. Since one drop from a buret is about 0.05 mL, better precision is achieved by adding
less than one drop of titrant when very near the end point. To deliver a partial drop, carefully
turn the stopcock until a part of a drop builds up on the buret tip, then touch the inner wall of
the flask to the buret tip and wash down the walls of the flask with a small amount of distilled
water from a wash bottle. The titration is complete at the first indication of a permanent
indicator color change.

C. USE OF THE TRANSFER PIPET

A transfer pipet is used to deliver a fixed volume of liquid (e.g. 1 mL, 5 mL, 10 mL, 25 mL,...)
called an aliquot. Since the volume of liquid actually delivered depends on how the pipet is used,
a reproducible technique must be employed. Typical uncertainties in the volume delivered are in
the range ±0.1-0.5%.

Volume Measurements · 30 · Appendix II

CHEM 12XX Laboratory Manual: Introduction and Appendices

a. With the tip of the pipet b. Remove the bulb and quickly c. Tilt the pipet slightly and wipe
immersed in the solution, apply place your forefinger over the the stem with a Kimwipe.
suction with a pipet bulb until the stem (a faintly moist forefinger
liquid level is somewhat above applies a better seal).
the graduation mark.

d. Touch the pipet tip to the wall e. Allow the pipet to drain freely f. When free flow of liquid stops,
of the waste beaker and partially into the receiving flask, keeping wait 10 seconds for proper
release the forefinger until the the pipet tip in contact with the drainage then withdraw the pipet
bottom of the meniscus is at the inner wall and the pipet is held with a rotating motion to remove
graduation mark (rotate the pipet vertically. any adhering drops. Do not blow
slightly to drop the meniscus out the last portion of liquid in
level slowly). the tip.
Figure 3: Procedure For Using a Transfer Pipet to Deliver an Aliquot

Volume Measurements · 31 · Appendix II

CHEM 12XX Laboratory Manual: Introduction and Appendices

1. Clean the pipet with water. If the pipet is very dirty, clean with a detergent solution followed
by 3 or 4 rinses with water. A clean pipet drains so that no droplets cling to the inside walls.
2. Rinse the interior by drawing into the pipet a 2-5 mL portion of the liquid to be pipetted with
the aid of a suction bulb, and then tilt and turn the pipet until all the surface has been wetted.
Discard this portion of the liquid and repeat this operation twice.
3. Use a rubber squeeze bulb to fill the pipet. Do not use your mouth. If you are right-handed,
hold the pipet with your right hand and control the rubber bulb with your left hand. The bulb
should rest easily over the open end of the pipet stem, it should not be forced onto it.
4. With the pipet tip near the bottom of the solution in the container, draw the solution well above
the calibration mark but not into the bulb.
5. Remove the bulb and quickly place the index finger over the stem end of the pipet. Do not
use your thumb to control the liquid level. If difficulty is experienced with a "leaky index
finger", moisten your finger slightly.
6. Withdraw the pipet from the solution and wipe off the excess liquid from the pipet stem with
a kimwipe.
7. With the pipet held vertically and with the tip touching the inside edge of the container (above
the solution), adjust the meniscus until the bottom of meniscus reaches the top edge of the
calibration mark.
8. Move the tip from the wall of the container (there should not be a drop clinging to the tip).
9. To deliver the solution, hold the pipet vertically and the receiving vessel at a slight angle.
Introduce the pipet tip into the receiving vessel and allow the pipet to drain freely, keeping
the pipet tip in contact with the wall of the container throughout.
10. Once free flow of the solution has stopped, wait 5-10 seconds for the interior of the pipet to
drain properly and rotate the pipet tip 360° while still in contact with the receiving vessel to
remove any drop clinging to the tip.
11. Remove the pipet. Do not blow out the small amount of liquid remaining in the tip.

D. USE OF A VOLUMETRIC FLASK: TECHNIQUE OF QUANTITATIVE TRANSFER

Volumetric flasks are calibrated to contain a specified volume of liquid and are used to prepare
solutions of a known concentration. Various sizes are available. A label of "TC 20 ºC" on the flask
means that the flask is calibrated to contain the indicated volume at 20 ºC. If used within +5 ºC of
this temperature, typical uncertainties are about + 0.1%. To prepare a solution of a known

Volume Measurements · 32 · Appendix II

CHEM 12XX Laboratory Manual: Introduction and Appendices

concentration, two methods are available: (1) dissolving a known weight of solid in sufficient
solvent to make a definite volume of solution, or (2) dilution of an aliquot of a more concentrated
solution.

Use of a Volumetric Flask

1. Dissolve a known mass of solid in a beaker with a minimum amount of water.
2. Fit a clean funnel into a previously cleaned volumetric flask and pour the concentrated solution
down the edge of a stirring rod into the flask, being careful not to lose a drop. The funnel may
have to be raised (by supporting it on a ring stand) to permit the solution to flow freely into
the flask.
3. Rinse the beaker with several small portions of distilled water from your wash bottle, each
time adding the washings down the stirring rod to the volumetric flask. Rinse the stirring rod
and the funnel with a spray of water from a wash bottle and let the washings drain into the
flask.
4. Remove the funnel, fill the flask about 3/4 full, and swirl the flask to mix and dissolve any
undissolved solute.
5. Set the flask on the bench top and add water from your wash bottle until the bottom of
meniscus is near the calibration mark. Next using an eyedropper or a disposable (Pasteur)
pipet, add water until the bottom of the meniscus is at the calibration mark.
6. Stopper the flask tightly, and with stopper held firmly in place, repeatedly invert the flask at
least 10 times to thoroughly mix the solution.

If a more concentrated solution is to be diluted in a volumetric flask, pipet an aliquot of the solution
directly into the flask, dilute to volume and mix as described above.

Volume Measurements · 33 · Appendix II

CHEM 12XX Laboratory Manual: Introduction and Appendices

III. USE OF A BUNSEN BURNER

The Bunsen burner is commonly used in the lab when an open flame poses no special fire
hazards. For general heating purposes, the burner flame should be non−luminous, about 10 cm
high with two zones as illustrated below.

Natural gas (mostly methane) and air are mixed in the barrel and burn as they emerge at the
top. The combustion mixture is varied by adjusting the gas control valve and/or the air control
collar (air vents).

To light a Bunsen burner, first close the gas valve completely, and then open it about one-half
turn. Open the air control collar to expose about one-third of the air slot area. Turn on the gas at
its source. Ignite the flame with a flint striker held at the top of the barrel.

If the flame appears yellow, which is caused by incomplete combustion (incandescent carbon
particles), insufficient air is being mixed with gas. This type of flame is called a luminous flame
and it will be cooler, sooty, and it will flicker. To correct this, either rotate the air collar to increase
the amount of air or close down the gas valve on the burner. As you increase the flow of air, the
flame will get smaller, change from yellow to blue and become very hot. If the flame has a
"roaring" sound or extinguishes itself, decrease the air supply and/or increase the gas flow with
the gas valve. If you cannot get the burner to light, turn off the gas and consult you lab instructor.

Never leave a lit burner unattended.

Use of a Bunsen Burner · 34 · Appendix III

CHEM 12XX Laboratory Manual: Introduction and Appendices

IV. FILTRATION TECHNIQUES

Filtration Techniques · 35 · Appendix IV

CHEM 12XX Laboratory Manual: Introduction and Appendices

V. USE OF THE pH METER

A pH meter consists of a pH probe connected to a voltmeter. The probe is composed of two
electrodes, a glass-membrane indicator electrode whose potential is linearly related to pH, and a
reference electrode whose potential is constant. The two electrodes act as an electrochemical cell
whose potential (voltage) depends upon the concentration of hydrogen ion in the solution in
contact with the glass indicator electrode. The glass electrode responds to pH because a potential
difference develops across the glass membrane due to the difference in [H+] inside as compared to
outside the membrane. The overall cell potential, Ecell = Eind. – Eref., is measured with a
millivoltmeter whose scale is calibrated in pH units.

Measurement Procedures

General

1. Plug the meter into 110 volt A/C outlet and allow 10 minutes for warm-up before use. The
probe is mounted on a bracket which can be raised or lowered on the mounting post. The
glass electrode is very fragile so be very careful when lowering the probe into a
beaker.

2. Carefully remove the rubber protector cap at the bottom of the probe. Rinse the end of the
probe with distilled water from your wash bottle between measurements.

3. All samples and buffers should be at the same temperature since electrode response and
solution pH are temperature dependent. The temperature control should be set to the
temperature of the buffer.

4. At the end of the lab replace the protective cap without applying pressure on the fragile glass
bulb and unplug the pH meter.

pH Meters · 36 · Appendix V
CHEM 12XX Laboratory Manual: Introduction and Appendices

Single-Buffer Calibration (Orion Model 301 pH Meter)

1. Place the pH probe in a buffer solution whose pH is within +1.5 pH units of the expected
pH of the sample.
2. Set the TEMP control to the temperature of the buffer.
3. Allow the buffer pH reading to stabilize, then adjust the CALIB control until the meter
needle points to the pH of the buffer.
4. Remove the probe from the buffer solution and rinse with distilled water.
5. Lower the probe into the sample solution and swirl the solution gently. Allow the reading
to stabilize and record the solution pH.

USE OF THE ORION MODEL 301 pH METER AS A MILLIVOLTMETER

1. Set the TEMP control to the "mv" mark (15 oC).

2. Plug the connectors of the shorting strap into the sensing and reference jacks on the rear
panel of the meter.

3. Turn the CALIB control until the needle points to "0" on the millivolt scale.

4. Remove the shorting strap and connect the electrode(s) to the meter.

5. Place the electrode(s) in the sample. If the needle comes to rest on-scale, record the
steady electrode reading.

If the needle comes to rest off-scale, disconnect the electrode(s) and reconnect the shorting
strap. Turn the CALIB control to bring the needle to full-scale at the OPPOSITE side of the
off-scale deflection. This rescales the meter so that it reads from 0 to 800 mv, if the needle
has been brought to full-scale right, or 0 to -800 mv, if the needle has been brought to full-
scale left. Reconnect the electrode(s), and record the reading, taking into account the
rescaled values.

pH Meters · 37 · Appendix V
CHEM 12XX Laboratory Manual: Introduction and Appendices

VI. PRODUCTS FORMED IN THE REACTION OF METAL CATIONS WITH

VARIOUS REAGENTS

CATION 0.3 M HCl 0.3 M H+, H2S Basic H2S NH3,NH4Cl NaOH excess NaOH

Ag+ AgCl Ag2S Ag2S Ag(NH3)2+ Ag2O Ag2O

white black black colorless br-black br-black

Pb2+ PbCl2 PbS PbS Pb(OH)2 Pb(OH)2 Pb(OH)2

white black black white white white

Hg22+ Hg2Cl2 HgS + Hg HgS + Hg Hg(NH3)2Cl HgO yellow HgO yellow

white black black white
+Hg black +Hg black +Hg black

Cu2+ N.R. CuS CuS Cu(NH3)42+ Cu(OH)2 Cu(OH)2

black black blue blue blue

Cd2+ N.R. CdS CdS Cd(NH3)42+ Cd(OH)2 Cd(OH)2

yellow yellow colorless white white

Bi3+ N.R. Bi2S3 Bi2S3 Bi(OH)3 Bi(OH)3 Bi(OH)3

brown brown white white white

Al3+ N.R. N.R. Al(OH)3 Al(OH)3 Al(OH)3 Al(OH)4–

white gel white gel white gel colorless

Cr3+ N.R. N.R. Cr(OH)3 Cr(OH)3 Cr(OH)3 Cr(OH)4–

grey-green grey-green grey-green light green

Zn2+ N.R. N.R. ZnS Zn(NH3)42+ Zn(OH)2 Zn(OH)42–

white colorless white colorless

Fe3+ N.R. Fe2+ + S FeS Fe(OH)3 Fe(OH)3 Fe(OH)3

milky white black rust-brown rust-brown rust-brown

Co2+ N.R. N.R. CoS Co(NH3)62+ Co(OH)2 Co(OH)2

black pink blue blue

Ni2+ N.R. N.R. NiS Ni(NH3)62+ Ni(OH)2 Ni(OH)2

black blue lt green lt green

Mn2+ N.R. N.R. MnS Mn(OH)2 Mn(OH)2 Mn(OH)2

pink white white white

Ca2+ N.R. N.R. N.R. N.R. Ca(OH)2 Ca(OH)2

white white

Ba2+ N.R. N.R. N.R. N.R. Ba(OH)2 Ba(OH)2

white white

Mg2+ N.R. N.R. N.R. Mg(OH)2 Mg(OH)2 Mg(OH)2

white white white

NH4+ N.R. N.R. N.R. N.R. NH3 (g) NH3 (g)

Metal Cation Reactions · 38 · Appendix VI

CHEM 12XX Laboratory Manual: Introduction and Appendices

VII. GENERALIZED RULES FOR THE SOLUBILITY OF SALTS IN WATER

1. All sodium, potassium and ammonium salts are soluble.

2. All metal nitrates are soluble.

3. All metal carbonates and phosphates are insoluble with the exception of sodium, potassium
and ammonium.

4. All chlorides, bromides and iodides are soluble except silver, lead (slightly soluble) and
mercury(I).

5. All sulfates are soluble except the sulfates of calcium, barium, strontium, lead and mercury(I).
The sulfate of silver is partly soluble.

Cations Which Form Amphoteric Hydroxides

Cation Soluble Anion Formed in Excess Base

Cr3+ Cr(OH)4–

Al3+ Al(OH)4–

Zn2+ Zn(OH)42–

Sn4+ Sn(OH)62–

Cations Which Form Ammonia Complex Ions

Cation Soluble Ammonia Complex Ion

Ag+ Ag(NH3)2+, colorless

Cu2+ Cu(NH3)42+, azure blue

Cd2+ Cd(NH3)42+, colorless

Zn2+ Zn(NH3)42+, colorless

Ni2+ Ni(NH3)62+, blue

Co2+ Co(NH3)42+, pink

Solubility Rules · 39 · Appendix VII