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1
INTRODUCTION TO CHEMICAL TECHNIQUES
Fall 2008
Course
Content: An introductory laboratory course in basic chemistry techniques.
Goals/
Objectives: Discovery of basic chemical principles and an introduction to basic chemical
techniques through experimentation. Introduction to data collection, recording,
analysis, evaluation and reporting.
Webpage: http://chem.qc.cuny.edu/~introchemlab/CHEM113/home.html
Required
Text: Queens College Chemistry 113.1 Laboratory Manual.
SECTION 2. POLICIES/RULES
Pre-laboratory
quizzes: All pre-laboratory quizzes will be 30 minutes in length and will be given at the
beginning of the laboratory period. Additional time will not be given to students
who are tardy. These quizzes will consist of three questions, which may contain
multiple parts:
Question 1. A post-laboratory question from the previous experiment.
Question 2. A safety question about the current experiment.
Question 3. A pre-laboratory question from the current experiment.
Laboratory
project: A complete laboratory project consists of the following documents, which should
be stapled together in the order listed:
1. Hard copy of the laboratory report
2. The pre-laboratory questions
3. The laboratory report sheet
4. The post laboratory questions
In addition to this package, an electronic version of the laboratory report should also
be submitted to Blackboard. The completed project (i.e., Items 1-4) must be
submitted at the beginning of the laboratory period on the date due (see the
schedule). An electronic version (i.e., Word or WordPerfect) of the laboratory report
must be submitted to Blackboard on the date due. Electronic versions of
laboratory reports will be submitted to Turn-it-in software and checked for
plagiarism. Turn-it-in checks both internet sources and previously submitted
reports. Failure to submit an electronic version of the report will result in a zero on
the laboratory report.
Laboratory
worksheets: Some laboratories do not have projects associated with them. For these laboratories,
the worksheet that accompanies the laboratory must be submitted at the end of the
laboratory in question.
Laboratory
reports: A style guide for the laboratory reports is attached to this document and can also be
found on the course website. Unless specified by the laboratory instructor, laboratory
reports are limited in length to 6 pages, excluding Figures and Tables.
Academic
dishonesty: While it is natural to discuss experiments among each other, copying and/or
plagiarism will NOT be tolerated on any assignment and will be treated in
accordance with university policy. This policy can be found at:
http://www1.cuny.edu/portal_ur/content/2004/policies/image/policy.pdf
Electronic versions of laboratory reports will be submitted to Turn-it-in
software and checked for plagiarism. Turn-it-in checks both internet sources
and previously submitted reports. We should note here that copying and
downloading graphs from the internet, without express permission of the instructor,
constitutes plagiarism (even if referenced). An originality score $ 30% (indicating
that # 70% of the work is original) from a single reference will result in a grade
of zero on the laboratory report in question.
SECTION 3. GRADING
Course
grading: Pre-laboratory quizzes (12 @ 10 pts) 120 pts
Laboratory Projects (12 @ 20 pts) 240 pts
Laboratory practical 60 pts
Total: 420 pts
Grading for
Project: 1. Laboratory report* 7 pt
a. Style guide formatting (0.5 pt)
b. Introduction and Experiment (1.5 pt)
d. Results and Discussion (2 pts)
2. Pre-laboratory questions 4 pt
3. Report sheet 3 pt
4. Post laboratory questions 4 pt
Safety and laboratory technique 2 pt
*
Failure to submit an electronic version of the laboratory report will result in the loss of these 7
points.
Laboratory Schedule
Lab Pre-Lab (60 min) Lab Work (120 min) Projects due
1 Syllabus and safety. Check-in.
Safety exam. Laboratory techniques.
2 Pre-laboratory quiz Finish laboratory techniques. Laboratory Techniques
Density and graphing. Project.
Density
3 Pre-laboratory quiz Law of definite proportions. Density Project
Chemical formulas.
4 Pre-laboratory quiz Stoichiometry. Law of definite
Moles. proportions project.
5 Pre-laboratory quiz Copper reactions Stoichiometry project.
Chemical reactions.
6 Pre-laboratory quiz Acid/base titrations with an Copper reaction project.
Acid/base chemistry indicator
7 Pre-laboratory quiz Potentiometric analysis. Acid/base project 1.
Acid/base chemistry
8 Pre-laboratory quiz Heat of reactions. Acid/base project 2.
Energy in chemistry.
9 Pre-laboratory quiz Activity of metals. Heat of reaction project.
Metal reactivity.
10 Pre-laboratory quiz Emission and Beer’s Law. Activity of metal project.
Electronic spectroscopy
11 Pre-laboratory quiz Redox titration of bleach Beer’s Law Project
Redox Chemistry
12 Chemical kinetics Kinetics of bleaching Redox Titration Project
(60 min lecture)
13 Pre-laboratory quiz
Finish Kinetics of bleaching experiment
Kinetics data analysis using computers (in recitation room)
14 Laboratory check-out and Kinetics Project.
LABORATORY PRACTICAL (60 pts).
Laboratory Drawer Combination:
Chemistry 113.1.
Introduction to Chemical Techniques
Laboratory Manual
ii
QC Chemistry Laboratory Manual
Version 1.0, 2008
Introduction
SECTION 1
General Rules
1.1. Attendance
Attendance in laboratory is mandatory. An unexcused absence results in the loss of all
points associated with that laboratory (i.e., pre-laboratory quiz, laboratory project grade).
If you have a university excused absence (such as illness, etc), you have one week to show the
excuse to the course instructor (not teaching assistant) or the absence will not be excused.
If you will miss a laboratory due to religious observance, you must inform the
course instructor (not teaching assistant) the week BEFORE the absence, or
the absence will not be excused. If you will miss two sequential weeks due to
religious observance, you must inform the instructor (not teaching assistant)
that you will be missing two laboratory periods BEFORE the absences, or the
absences will not be excused. If the absence is excused by the course instructor, the
course instructor will make arrangements with the teaching assistants for the laboratory to
be made-up during a separate laboratory section.
1.2. Laboratories
There are 14 laboratories, including the check-in/introductory laboratory and the check-
out/laboratory practical meeting. Grades will be determined from pre-laboratory quizzes,
laboratory technique and safety, laboratory reports, laboratory related questions, and the
laboratory practical.
1.3. Tardiness
It is your responsibility to attend class and to be punctual. Pre-laboratory quizzes will be
given at the beginning of class. Tardiness will not result in additional time being allotted
for pre-laboratory quizzes.
1.4. Safety
An open book safety examination, worth 5 points, will be given during the first pre-
laboratory period. Students must score a 3/5 on this examination. Failure to do so will
result in the student being barred from the laboratory, until such time as a 3/5 is achieved.
(Laboratories that are missed due to failure of the safety examination cannot be made-up.)
Moreover, all students will be required to sign the Laboratory Safety Agreement given
at the end of Section 3. Failure to do so will result in removal from the laboratory.
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1.9. Grading
Course grading:
• Safety examination and Pre-laboratory quizzes: 20% of grade
• Laboratory assignments: 60% of grade
• Laboratory practical: 20% of grade
Any student missing a laboratory with an university excused absence will be given a make-
up laboratory during the fourteenth week.
Grade distribution:
A+ 95.5 - 100 % C+ 70.5 - 75.4 %
A 87.5 - 95.4 % C 63.5 - 70.4 %
B+ 82.5 - 87.4 % D 49.5 - 63.4 %
B 75.5 - 82.4 % F < 49.5 %
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Introduction
SECTION 2
Schedule
Date Session Pre-laboratory (60 min) Laboratory (120 min) Projects due
1 Syllabus and safety Experiment 1: Basic
laboratory techniques
2 Safety exam. Significant Experiment 2: Density. Experiment 1
figures and error analysis. Project.
3 Pre-laboratory quiz. Experiment 3: Law of Experiment 2
Chemical Formulas. definite proportions. Project.
4 Pre-laboratory quiz. Experiment 4: Stoi- Experiment 3
Formulas and reactions. chiometry. Project.
5 Pre-laboratory quiz. Experiment 5: Prepara- Experiment 4
Chemical reactions. tion of a simple salt Project.
6 Aqueous chemistry. Experiment 6: Reac- Experiment 5
tions in Solution. Project.
7 Pre-laboratory quiz. Experiment 6: Reac-
Aqueous chemistry. tions in Solution.
8 Pre-laboratory quiz. Experiment 6: Reac- Experiment
Aqueous chemistry. tions in Solution. 6 Project:
Knowns.
9 Pre-laboratory quiz. Experiment 7: Experiment 6
Acid/base chemistry Acid/base titrations Project: Un-
knowns.
10 Pre-laboratory quiz. Experiment 8: Potentio- Experiment 7
Acid/base chemistry. metric titrations Project.
11 Pre-laboratory quiz. Experiment 9: Heat of Experiment 8
Heat and heat capacity. reaction. Project.
12 Pre-laboratory quiz. Experiment 10: Emis- Experiment 9
Electron spectroscopy. sion and Beer’s Law. Project.
13 Pre-laboratory quiz. Experiment 11: Activity Experiment 10
Metal reactivity and of metals Project.
perfect gases
14 LABORATORY PRACTICAL. Check- Experiment 11
out. Make-up laboratory (examination and Project.
laboratory).
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Introduction
SECTION 3
Laboratory Safety
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• Wash your hands after handling chemical and/or reagent bottles. ALWAYS wash
your hands with soap and water before leaving the laboratory at the end of the
period.
• Cell phones are a distraction. Therefore, cell phones must be turned off dur-
ing the laboratory period. If a cell phone rings, this phone will be confiscated
by the laboratory instructor for the duration of the laboratory.
• Assemble your laboratory apparatus at least 8 inches from the edge of the labora-
tory bench.
• Maintain a clean and orderly laboratory desk and drawer. Keep drawers or cabinets
closed and aisles free of obstructions. Do not place book bags, athletic equipment
or other items on the floor near the laboratory bench.
• Be aware of the actions of your neighbor as well as yourself. You could be the
victim of a mistake made by a neighbor. Therefore, advise them of improper
technique or unsafe practices. If necessary report them to the instructor.
3.5. Cleanliness
It is important to keep the laboratory as clean as possible, for safety reasons as well as
aesthetic reasons. Each pair of students is responsible for their immediate desk area. Before
leaving the laboratory, students should make sure that the area of the laboratory bench near
their assigned drawer is clean and dry, that Bunsen burners and other shared equipment
are put away in the appropriate space, and that the trough to the sink is free of any solid
material. Laboratory instructors will check work areas before approving completion of
the experiment. Pairs of students will be assigned dates for which they are responsible
for cleaning the reagent shelves, balances and balance tables in the weighing room, and
surfaces under the hoods. This duty will be rotated so that each pair of students will be
responsible for general laboratory cleanliness at least once during the semester.
General tips:
• Place broken glassware in the broken glassware box.
• Keep drawers and cabinets closed to avoid physical hazards.
• Never place materials or chemical bottles on the floor.
Because few laboratory chemicals are without hazards, general precautions for handling all
laboratory chemicals should be adopted.
• It is prudent to minimize all chemical exposures. Precautions should be taken to
avoid exposure by the principal routes of entry, that is, contact with skin and eyes,
inhalation and ingestion.
Personal hazards of chemicals fall into two major groups: Health Hazards and Physical
Hazards.
you must wear contact lenses for medical reasons, then safety glasses with side
shields or tight-fitting safety goggles must be worn over the contact lenses.
Reference:
FIRE EMERGENCY
MEDICAL EMERGENCY
This plan was designed to reduce the potential for overexposure to hazardous chemicals in
the event of a chemical spill. Proper spill containment and cleanup procedures are ordinarily
obtained from material safety data sheets (MSDS’s). However, you should not take it upon
yourself to contain or clean up a chemical spill if you:
• Are not familiar with the chemical involved and with the potential hazards asso-
ciated with the chemical.
• Do not have the proper personal protective equipment (PPE).
• Cannot reasonably be expected to handle the incident.
We should note that you are responsible for familiarizing yourself with the
chemicals (including potential hazards and the required PPE) used for a given
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laboratory procedure. If you are unable to address the clean up of a chemical spill based
upon the criteria listed above, then
(1) Evacuate the area.
(2) If the spill occurred within a laboratory, notify the instructor or principal investi-
gator.
(3) During normal business hours (8:00 am to 4:00 pm), also notify the Environmental
Safety and Health Officer (ESHO) and/or the Laboratory Safety Officer (LSO).
During normal business hours, the ESHO and LSO can be reached at:
• ESHO: William Graffeo, (718) 997-2881
• LSO: Parmanand Panday, (718) 997-4108 or (718) 997-4171
• Assistant LSO: Rick Sherrick, (718) 997-4177
(4) During off-hours, notify the Public Safety Desk Officer at (718) 997-5911 or (718)
997-5912. The Public Safety Officer will make sure that the instructor (or principal
investigator), the ESHO and the LSO are informed of the spill.
(5) Let both your instructor (or principal investigator) and Safety Officer (or the
Public Safety Desk Officer) know the following:
• The existence of a spill incident.
• Specific location of the incident (building, floor, room, etc.).
• Type of material spilled, if known.
• Any other information that you deem pertinent for the spill clean up.
Once the spill is reported, the ESHO, LSO or Campus Patrol Officer will respond to the
scene. The room will be evacuated and the affected area will be cordoned off. This area may
include rooms adjacent to the area where the spill has occurred. If an injury has occurred as
a result of the spill, the person reporting the spill and/or the Safety Officer will immediately
notify the New York City Emergency Medical Service (see Medical Emergency above). If
occupants are trapped within the affected area, or if the ESHO, LSO or instructor/principal
investigator cannot be reached, then the Public Safety desk will contact the New York Fire
Department to respond to the scene. For a large chemical spill, an incident report must be
completed and submitted to the ESHO and the LSO. Thus, the Safety Officer will attempt
to gather as much information as possible from the individuals present at the site at the
time of the spill. Therefore, do not leave the temporary headquarters until you have talked
to the Safety Officer.
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Queens College faculty, staff, students, contractors, and other parties that handle or gen-
erate hazardous wastes are required to properly handle, store and label hazardous wastes
and to comply with applicable federal, state and local regulations. As a student, your
responsibilities are:
(1) Follow the Queens College Hazardous Waste Program requirements of
• Do not dispose of hazardous waste down sink drains.
• Do not dispose of hazardous waste in the normal trash.
• Do not dispose of hazardous waste by evaporation in fume hood.
• Do not dispose of hazardous waste in broken glass container.
• Hazardous waste must be collected in a compatible container which is in good
condition.
• All containers of hazardous waste MUST be labeled with the word Hazardous
Waste and with other words identifying contents and hazards present.
• All hazardous waste containers must be kept tightly capped except when
adding or removing waste.
• Do not mix incompatible chemicals together in the same waste container.
• Do not store waste containers next to other bottles holding incompatible
chemicals.
• Separate incompatible chemicals into separate secondary containment trays.
• Store hazardous waste containers at or near point of generation and under
the control of generator.
(2) Review Material Safety Data Sheets prior to working with chemicals.
(3) Use appropriate personal protective equipment when working with chemicals.
(4) Report any accident to laboratory instructor.
(5) Report any emergency to Public Safety (Ext. 7-5911).
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I, the undersigned, have read and understand the safety instructions given in this lab-
oratory manual. I agree to abide by these rules. I also understand that failure to obey the
safety rules given above or to follow my instructors advise while in the laboratory can lead
to my dismissal from the laboratory for one or more class periods, with a grade of zero for
the missed experiment(s).
As part of the safety lecture during the first laboratory period, an overview of chemical
disposal and general laboratory safety was discussed. In particular, the items in Section
3.9 were reviewed.
All laboratory experiments in this manual have been checked for safety when performed
according to directions. I, the undersigned, understand that I am responsible for reading
all safety precautions required for performing each experiment. Because this is a chemistry
laboratory, I understand that there is the potential for serious accidents if these safety
precautions are not followed and acknowledge that the fundamental responsibility for safety
lies with myself.
Introduction
SECTION 4
Freshman Chemistry Style Guide
4.1. Margins
The margins should be standard paper margins, namely
Top 1” Bottom 0.5”
Left 1” Right 1”
The page number should be located 0.5” from the bottom of the page and centered hori-
zontally (cf. Figs. 4.1 - 4.7). The text should be 1” from the bottom of the page.
4.3. Font
Times New Roman (or Times Roman or Roman) or Helvetica (or Courier or Arial). 12
point type size. Reports written in different fonts will not be accepted.
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4.4. Layout
Section headings should be preceded by a roman numeral and a period, be left justified, use
all capital letters and be bold. The body of the text should use full paragraph justification.
There should be two lines between each section. Widows (i.e., the last line of a paragraph
that is carried over to a following page) and orphans (i.e., the first line of a paragraph
appearing alone at the bottom of a page) will not be tolerated.
4.5. Tables
Tables should be placed at the end of the text after the references in consecutive order.
Tables should be numbered sequentially and consecutively from the first table using roman
numerals (i.e., I, II, etc.). The table caption should be located at the top of the table. Pay
attention to significant figures when making tables. No table should be wrapped so
that it exists on two pages. If a table will not fit on a single page, consult your instructor
for how to format long tables. Fig. 4.6 gives an example of a page of tables for a laboratory
report. Notice that the table is separated from the table caption by a double line and is
ended by a double line. Also notice that the table headings are separated from the values
by a single line. You should copy this format when typing tables.
4.6. Figures
Figures should be placed after the tables with one figure/page in consecutive order. Fig-
ures should be numbered sequentially and consecutively from the first figure using arabic
numerals. If a figure is composed of multiple parts, each sub-part should be identified with
a letter of the alphabet in sequential order from top to bottom. Do not use color on figures
unless required. The figure caption should be placed below the figure.
If data are obtained by scanning a parameter (such as temperature or energy), then the
data should be graphed as a line. If, however, the data are obtained by analyzing different
objects, then the data should be graphed as markers. If data are presented as markers
and a line is drawn through the markers, you should indicate if the line is the result of a
regression or is drawn as a help to the reader. Fig. 4.7 gives an example of a line drawn
as a regression, while Fig. 4.8 shows an example of a line drawn to help the reader. Note
how the figure captions indicate each type of line.
Figures should not have color backgrounds. The fonts for axis markers and labels should
match the font used in writing the report and should be at least 18 points in size. Figures
When a figure is pasted into a word processors (such as Microsoft Word),
4.7. Referencing
References should be placed at the end of the document before the tables and figures. The
references should be numbered sequentially and consecutively from the first time of use in
the document. Citing references in the text should use on-line numerals in square brackets
(i.e., [1]) which are spaced away from the preceding word or symbol and are placed inside
punctuation. Examples are given below.
• Journal article
A. A. Author, B. B. Author and C. C. Author, “Article title,” Journal Abbr. Vol,
start page (year).
23
• Web site
A. A. Author (if any), Title of document, year. Title of site. http://url.of.site
(accessed Month day, year).
• Book
A. A. Author, Title of book (Publisher, location, year), start page (if any).
• Edited volume
Title of book, E. E. Editor, eds. (Publisher, location, year).
John X. Smith
ABSTRACT
The density, defined as mass per unit volume, of a set of regular shaped objects was obtained from
the slope of a graph of mass (measured with an electronic balance) as a function of volume. The
density of 1.16 g/mL indicates that the objects were either polyamide or acrylic. The density of
silver/pink irregular cylinders was determined using Archimede’s principle to be 9.84 g/mL,
indicating that the unknown sample is probably bismuth. Finally, the density of water and
water/ethanol mixtures was obtained. These data were plotted as a function of ethanol concentration
in order to generate a calibration curve. This calibration curve was used to determine that the
I. INTRODUCTION
The identification of a substance is often performed using intensive properties, which are
properties that do not depend on the quantity of the substance. Examples of these properties include
color, odor, melting point, boiling point and density. The density of a substance is the mass m of
=m/V, (1)
with standard units of kg/m3 (although it is more commonly reported in units of g/cm3 or g/mL).
Density is independent of the quantity of the substance, since both the mass and the volume are
proportional to one another at a fixed temperature. As the temperature changes, the volume of the
substance changes which, in turn, changes the density. In this experiment, we determine the density
II. EXPERIMENTAL
In the first procedure, we obtained a set composed of four regular shaped objects from the
instructor and recorded the code number. We then used a metric ruler to determine the dimensions
of each object with a precision of 0.01 cm. For the cubic object, we calculated the volume V from
V=l×w×h, (2)
where l is the length in cm, w is the width in cm and h is the height in cm. The volume of cylindrical
V = × r2 × h , (3)
where r is the radius of the cylinder. To obtain the error in the our volume, we remeasured the
dimensions and recalculated the volume. The mass of the block was determined using an electronic
balance. The balance pan was cleaned, a piece of weighing paper was added to the balance, and then
the balance was tared to ensure an accurate measurement of the mass. Each block was individually
placed on the center of the pan (re-zeroing the balance after each measurement) and the mass was
Irregular shaped metal objects (or metal powders) cannot be physically measured in order to
obtain the volume of the sample. However, we were able to determine the volume of the objects by
observing the volume of water displaced by the object. In this procedure, we filled a graduate
metal (after recording the code number) and weighed it. After determining the mass, we slowly
added this sample to the water. We tapped the cylinder to dislodge any air bubbles from the metal
sample, and then determined the new water volume. The difference in water volume is equivalent
to the volume of the metal. The density was then calculated using eq. (1) and the identity of the
The density of the liquid samples in Part C was evaluated by weighing a 10 mL graduate
cylinder and then adding a volume of the liquid to this cylinder. The mass of the liquid was
determined by the difference in the weight of the graduate cylinder before and after the addition of
the sample. The density was then calculated from eq. (1). The temperature was measured using a
standard alcohol thermometer that was calibrated for the range of 0 – 100 C during Experiment 1.
The set obtained from the instructor for Part A consisted of one cubic and three cylinders of red
plastic with code number 2A02. Table I presents the dimensions used in eqs. (2) and (3) to
determine the volume as well as the mass of each objected obtained from the electronic balance.
Fig. 4.3: Continuation of the example experimental section and beginning of the results
and discussion section of a laboratory report.
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m= V. (4)
indicates that a graph of the mass as a function of volume should yield a straight line with an
intercept of zero and with a slope that is equivalent to the density of the objects. Thus, Fig. 1
presents the mass of the red plastic cube and cylinders versus the volume of the objects. A linear
regression of these data gives a density of 1.16 ± 0.01 g/cm3. Using standard densities provided in
[1], we determined that the unknown plastic blocks and cylinders are either acrylic or polyamide.
Distinguishing between acrylic or polyamide would require additional physical or chemical tests.
In Part B, we were given metallic pellets (Code 2B05) that had a slight pinkish tint. The mass
of our sample was 8.451 g, while the volume of displaced water was 0.87 ± 0.01 mL. Substitution
of these data into eq. (1) yields a density of 9.7 ± 0.1 g/mL, or 9.7 ± 0.1 g cm-3 (since 1 mL = 1 cm3).
Comparison of this result to standard densities in [1] indicates that the metallic pellets are bismuth.
Since bismuth has a silver pink color [2], the color of our sample gives additional evidence for our
Table II gives the volume and mass of ethanol/water mixtures at various concentrations, along
with the density determined using eq. (1). This density is plotted as a function of ethanol
concentration in Fig. 2 to generate a calibration curve for ethanol/water density. A volume of 6.20
mL of the unknown sample 2C03 had a mass of 5.756 g, while a volume of 6.80 mL had a mass of
6.348 g. Thus, the unknown sample 2C03 has a density of 0.931 ± 0.003 g/mL. The calibration
curve in Fig. 2 indicates that a density of 0.931 g/mL corresponds to an ethanol concentration of 38
In this experiment, we determined the density of various regular shaped objects by direct
determination of the volume (using a ruler to measure the dimensions) and mass (using an electronic
balance). From our data set, we obtained a density of 1.16 ± 0.01 g/cm3, indicating that the objects
Fig. 4.4: Continuation of the example results and discussion section of a laboratory report.
28
were made of either acrylic or polyamide. We also obtained the density of an unknown metal
sample by indirectly measuring the volume (using water displacement) and directly measuring the
mass. Our density of 9.7 ± 0.1 g/mL indicates that the unknown pinkish metal is probably bismuth.
ethanol/water mixtures. This calibration curve allowed us to determine that the unknown sample
References
Fig. 4.5: Continuation of the example results and discussion section and references of a
laboratory report.
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Table I. The dimensions, volume V [calculated using eqs. (2) and (3)], and mass m of the four red
plastic objects in package 2A02. The dimensions for the cubic object are given as length × width
× height. The dimensions for the cylindrical objects are given as radius × height.
Object Dimensions (cm) Volume (cm3) Mass (g)
1 2.01 ± 0.01 × 2.00 ± 0.01 × 2.02 ± 0.01 8.12 ± 0.12 9.419
2 1.27 ± 0.02 × 3.01 ± 0.02 15.3 ± 0.6 17.748
3 1.27 ± 0.01 × 6.00 ± 0.01 30.4 ± 0.5 35.26
4 1.27 ± 0.02 × 9.00 ± 0.02 45.6 ± 1.5 52.90
Table II. The volume Vi and mass mi [where i = A, B for the measurements obtained by myself and
my laboratory partner, respectively] for various ethanol (EtOH) concentrations (% by volume). The
density i (i = A, B) for each measurement was determined using eq. (1). The temperature for all
measurements was 23.4 C.
% EtOH VA (mL) mA (g) VB (mL) mB (g) A (g/mL) B (g/mL)
0 5.60 5.548 7.22 7.182 0.991 0.995
18 6.42 6.193 7.60 7.350 0.965 0.967
36 5.70 5.343 7.80 7.318 0.937 0.938
54 6.42 5.831 7.60 6.848 0.901 0.904
72 6.38 5.447 8.50 7.350 0.865 0.860
90 6.59 5.435 7.40 6.207 0.839 0.832
60
50
40
m (g) 30
20
10
0
0 10 20 30 40 50 60
3
V (cm )
Fig. 1. The mass m (g) of various red plastic objects plotted as a function of the volume V (cm3) of
the object. The solid line represents a linear least square analysis of the experimental data with a
regression equation of m = 1.16 ± 0.01 g cm-3 × V.
1.00
0.95
(g/mL)
0.90
0.85
0.80
0 20 40 60 80 100
% EtOH (by volume)
Fig. 2. The density (g/mL) plotted as a function of ethanol concentration (% by volume) for
various ethanol/water mixtures. The solid markers are the data obtained for the stock solutions. The
open marker indicates the density and volume position for unknown sample 2C03. The solid line
is provided as a visual aid.
Introduction
SECTION 5
Instructions for Turn-it-in Assignments
All laboratory reports must be submitted both in hard copy to the instructor and as
an electronic version to Blackboard. The electronic version will be checked for instances of
academic dishonesty using Turn-it-in software. To submit the electronic version,
(1) Go to http://www.cuny.edu and log-in to the CUNY portal.
(2) Go to the Blackboard website and to the Chemistry 113 course site for your section.
(3) Select the Lab Reports folder under the Assignment link (cf. Fig. 5.1).
(4) Within the Lab Reports folder (cf. Fig. 5.2), select View/Complete under the lab
report that needs to be submitted.
(5) Type your first and last name in the appropriate forms (cf. Fig. 5.3).
(6) Type the title of the laboratory report in the appropriate form (cf. Fig. 5.3).
(7) Click on the Browse button (cf. Fig. 5.3) to load the dialog that will allow
you to select the file to be uploaded. Although the website lists several file
formats that are acceptable, only Word or Wordperfect files are valid
submissions for this course.
(8) Select the file to be uploaded and then click okay. This will return you to the
Blackboard site with the path for the file placed in the file form.
(9) Click the Submit button (cf. Fig. 5.3) to submit the paper.
(10) Once the paper is successfully uploaded (cf. Fig. 5.4), click the OK button to
return to the Lab Reports folder (cf. Fig. 5.2) on the Blackboard Chemistry 113
site.
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33
34
Fig. 5.1: The Assignments section of the Blackboard Chemistry 113 site.
Fig. 5.2: The Lab Reports folder within the Assignments section of the Blackboard Chem-
istry 113 site.
35
Fig. 5.4: The page that appears after successful submission of an electronic laboratory
report.
36
Introduction
SECTION 6
Useful information
c
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37
38
Experiments
EXPERIMENT 1
Check-in and Basic Laboratory Techniques
1.1. Safety
During Check-in, you may encounter broken or chipped glassware. This glassware should
be handled with care to prevent injury. Broken and/or chipped glassware should be placed
in the broken glassware box. Bunsen burners, hot glassware, metal ring stands, and boiling
water can cause painful and serious burns to skin. Hot glassware does not glow and,
therefore, looks identical to glassware at room temperature. Thus, be careful when handling
hot glassware.
1.2. Check-in
You will be assigned a laboratory bench and drawer containing your laboratory kit. You
will be responsible for all items in this kit. Check-in allows you to confirm that your kit has
all required glassware and to replace glassware that is broken or too dirty to clean. This is
the only day when missing or broken items are replaced free of charge. Thus, you should
report all items that are missing, scratched, corroded or otherwise unfit for use. You should
also use this time to clean all of the glassware in the kit, since this will save time in the
future. The condition and cleanliness of all items will be spot checked during the semester.
At the end of the semester, check-out will be performed to ensure that all items in the
laboratory kit are still in good shape and clean. Illustrations of the items that should be
in the laboratory kit are given in Figs. 1.1 and 1.2. General rules about the laboratory kit
are:
• This kit is your responsibility. Missing items are replaced free of charge only on
the day of check-in.
• If you drop the course, you must report to room 214 to check-out immediately.
• Students completing the course must check out with their regularly scheduled last
lab class. There will be no late check-out.
• At Check-out, missing or broken items are billed to the student. Other items must
be clean, dry and flawless to be accepted for check-out.
• After the last scheduled day of classes, students who have not checked-
out will be charged a $50 fee in addition to the fee from missing, broken
and dirty items.
c
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39
40
These experiments are meant to provide your first experience in the laboratory. If you
have prior laboratory experience, these exercises constitute a good review. Your instructor
will give you the rotation order for the experiment. Submit all results on the Worksheet
provided.
1.4. Weighing
You must learn how to use laboratory balances. As always, the limit of readable precision
of the scale should be recorded. When approaching the balance you will need the following:
(1) The substance to be weighed;
(2) A container or holder for the sample while on the balance;
(3) A sample handling device such as a spatula; and
(4) Your report sheet and a pencil or pen to record your measurement.
Balances in this laboratory have a semi-automatic tare (an allowance for mass of the con-
tainer or holder). On an electronic balance, ”tare equals zero” is set by depressing the bar,
which is also the on/off switch: up for off, down for on, down again to tare. These balances
have an automatic range selector that will change the readout precision automatically to
0.01 g when the gross mass on the pan is over 35 g. The measurement precision for small
masses is best if very light containers are used, such as the glassine weighing paper for dry
solid samples. The precision for samples less than 30 g gross mass is 0.001 g.
Stick a test tube into the flame briefly. You should observe
a deposit of carbon black on the tube. When hydrocarbons such
as methane [CH4 (natural gas)] burn in too little air (oxygen), the
reaction is
CH4 (gas) + O2 (gas) → C (sol) + 2 H2 O (liq) .
With a bit more air, the flame becomes hotter and blue, but carbon
monoxide is formed:
2 CH4 (gas) + 3 O2 (gas) → 2 CO (gas) + 4 H2 O (liq) .
Now adjust the air supply – you may also have to adjust the gas
with the burner valve – until the flame resembles the schematic to
the right. This is the hottest flame and is characterized by a blue
inverted cone shape within the flame that is the so-called reducing
flame. A little above the apex of the cone is the hottest area in the
flame, reaching temperatures around 1500◦ C.
Towards the top of the flame, conditions are oxidizing (high tem-
peratures, excess O2 ). The well-adjusted flame completely converts Schematic of a
methane and oxygen to carbon dioxide and water: bunsen burner
CH4 (gas) + 2 O2 (gas) → CO2 (gas) + 2 H2 O (liq) . flame when the
flame is the
To turn off the Bunsen burner, execute the lighting procedure in
hottest.
reverse. Shut the gas valve at the base of the burner, then close the
close the bench gas cock.
Name: Student ID #:
Check In:
Student Signature: Date:
Check Out:
Student Signature: Date:
Name: Section:
Partner: Date:
Results
Fill out all tables and answer all questions below. All values must have appropriate
significant figures and units. Show these data to your instructor before leaving class.
Table B.I. The cumulative mass of the sample, obtained by adding each penny to the col-
lection of pennies on the balance, and the mass of each penny (determined by directly
weighing the individual pennies).
2st penny
3st penny
4th penny
5th penny
1st penny:
2nd penny:
3rd penny:
4th penny:
5th penny:
50
Table C.I. The length of a wood splint provided by the instructor measured in inches and
in centimeters by myself (Measurement A) and my laboratory partner (Measurement B).
Determine the average length for the sample.
Measurement A in cm
Measurement B in cm
Average in cm
Write your name in the center of the wood splint and give to your instructor.
Table E.I. Measurement of the melting point and boiling point of water by myself (Mea-
surement A) and my laboratory partner (Measurement B).
Measurement A Measurement B
Observed melting point (Tm ) of ice
Barometric pressure (P )
Actual Tb of water at P
Table F.I. The volume of water as determined using the graduations in the glassware (Row
1) and the graduated cylinder (Row 2). The error in volume (i.e., |Row 1 - Row 2|) should
be given in Row 3.
Volume (mL)
using gradu-
ated cylinder
Error in vol-
ume of glass-
ware
52
Calculations
Fill out all tables and answer all questions below. All values must have appropriate
significant figures and units. To receive full credit all details for all calculations must
be shown.
Table B.II. The mass of each penny determined by the difference using the cumulative mass
in Table B.I and the mass of each penny determined by direct weighing. From these two
measurements, calculate the average mass of each penny. Then, using the space below,
determine the mean [i.e., eq. (1.1)] and the deviation from mean [i.e., eq. (1.2)].
2st penny
3st penny
4th penny
5th penny
Mean NAN
53
(1) What is the deviation from mean in inches for the values given in Table C.I? in
centimeters?
(2) Convert the average length in inches to centimeters using the factor 2.54 cm/in.
(3) Convert the average length in centimeters to inches using the factor 2.54 cm/in.
(1) When the bunsen burner had a yellow, luminous flame, what was deposited on the
test tube? How is this deposit related to the yellow flame color?
(2) When the flame was set to a two zone flame, in which zone did the wooden splint
burn first? Why?
54
Plot the average for the two temperatures recorded with your thermometer in ◦ C as a
function of the theoretical values on the graph below. Be sure to label all axis of the graph
and to use the appropriate number of significant figures when labeling the graph. Use this
graph and the space provided below to determine the calibration line for your thermometer.
This calibration line will be used for all temperatures measured during this semester and,
therefore, should be recorded in Section 6.
55
(1) Ethanol has a boiling point of 78.4◦ C and a melting point of -114.3◦ C. If your
thermometer was placed into boiling ethanol, what temperature would it read? If
the ethanol was freezing, what temperature would your thermometer give?
Name: Section:
Partner: Date:
(1) A student used a graduated cylinder having volume markings every 1 mL to care-
fully measure 100 mL of water for an experiment. A fellow student said that by
reporting the volume as “100” mL in her lab notebook, she was only entitled to
one significant figure. She disagreed. Why did her fellow student say the reported
volume had only one significant figure? Considering the circumstances, how many
significant figures are in her measured volume? Justify your answers.
(2) A healthy dog has a temperature ranging from 37.2 to 39.2◦ C. Is a dog with a
temperature of 103.5◦ F within normal range?
(3) Natural gas is mostly methane, a substance that boils at a temperature of 111 K.
What is its boiling point in ◦ C and in ◦ F?
58
Experiments
EXPERIMENT 2
Density
2.1. Safety
Certain metals, such as lead, can be toxic when ingested. Wash your hands after handling
all samples. Laboratory ethanol has trace impurities of methanol and toluene. Therefore,
laboratory ethanol should not be ingested. Ethanol and ethanol/water mixtures are also
flammable and, therefore, should be kept away from open flames.
2.2. Introduction
Density ρ is defined as the ratio of the mass m of a sample to its volume V , or
m
ρ= . (2.1)
V
Mass and volume are extensive properties of matter – properties that depend on the
quantities of substances. Such properties are not of themselves useful in characterizing sub-
stances. Intensive properties, on the other hand, are useful in characterizing substances.
Intensive properties are often determined by ratioing two extensive properties measured at
constant temperature T and pressure P . Density is an example of this kind of intensive
property. When measured under known conditions of T and P , density can be used to
characterize substances. Of course, two or more substances may have the same density,
but for a given substance there is only one density (at constant T and P ). Thus, if you
determine that a colorless liquid has a density of 1.00 g/mL at 4◦ C and 1 atm, this does
not prove the liquid is water. This fact is simply one piece of evidence that the substance
may be water.
59
60
(3) Determine the mass of each object and record this on the Report Sheet.
(4) From these data, calculate the volume.
(5) Graph the mass as a function of volume.
(6) Determine the density of the material from the slope of this graph.
(7) Then, identify the material (cf. Table 2.1 for density of some common materials).
References
1. Buoyancy, 2008. Wikipedia. http://en.wikipedia.org/wiki/Buoyancy (accessed
August 13, 2008).
62
Partner: Date:
(3) When chemicals are weighed on a balance, how is the pan protected?
(6) To correctly determine the volume in a graduated cylinder, where should your eyes
be in relation to the rules on the cylinder and the meniscus of the sample?
64
Partner: Date:
Results
Fill out all tables and answer all questions below. All values must have appropriate signif-
icant figures and units. The details for all calculations must be shown for full credit to be
obtained.
Sample code:
Table A.I. The height, area, volume and mass of each object determined by myself.
Table A.II. The height, area, volume and mass of each object determined by my labora-
tory partner.
D
66
Object A
Table B.I. The mass m of the object, the initial volume [i.e., Vi (H2 O)] of water in the
graduated cylinder, the final volume [i.e., Vf (H2 O)] of water in the graduate cylinder, and
the volume V of the object [i.e., V = Vf (H2 O) - Vi (H2 O)] determined by myself.
m:
Vi (H2 O):
Vf (H2 O):
V:
Object B
Table B.II. The mass m of the object, the initial volume [i.e., Vi (H2 O)] of water in the
graduated cylinder, the final volume [i.e., Vf (H2 O)] of water in the graduate cylinder, and
the volume V of the object [i.e., V = Vf (H2 O) - Vi (H2 O)] determined by my laboratory
partner.
m:
Vi (H2 O):
Vf (H2 O):
V:
67
Table C.I. The volume VEtOH of 95% ethanol, total volume V and mass m for each of the
ethanol/water mixtures determined by myself.
Sample VEtOH V m
1
Unknown
Table C.II. The volume VEtOH of 95% ethanol, total volume V and mass m for each of the
ethanol/water mixtures determined by my laboratory partner.
Sample VEtOH V m
1
Unknown
68
Calculations
Table A.III. The volumes VA and VB , calculated from the dimensions given in Table A.I
and A.II, respectively, the average volume Vavg and the average mass mavg for each object
measured. The details for all of the calculations are given below the table.
D
69
Experiment 2A (continued)
Figure A.1. Plot the average mass mavg as a function of the average volume Vavg on the
grid provided below. (Remember to label all axes and to use the appropriate significant
figures.)
(1) Perform a linear regression on the data in Table A.III and Fig. A.1. What is the
final regression equation?
(2) What is the density of the material, as determined from this regression equation?
Object A
(1) From the data in Table B.I, the density was determined to be:
Object B
(1) From the data in Table B.II, the density was determined to be:
Table C.III. The % concentration (by volume) of ethanol CA and CB and the densities ρA
and ρB for myself (A) and my laboratory partner (B). The details of the the calculations
are given below this table.
Sample CA ρA CB ρB
1
5
72
Experiment 2C (continued)
What is the density of the unknown sample for both measurements (yourself and your
laboratory partner) as determined from the data in Tables C.I and C.II and the average
density.
Figure C.1. Graph the average densities ρx for Samples 1 - 5 as functions of the % ethanol
(by volume) on the grid provided below. (Remember to label all axes and to use the appro-
priate significant figures.)
(1) What is the concentration of the unknown sample, as determined from Fig. C.1?
73
Partner: Date:
(1) A miner discovered some yellow nuggets. They weighted 0.0560 kg and had a
volume of 2.91 mL at 20◦ C. Were the nuggets gold or pyrite (otherwise known as
fool’s gold)? Note: The density of gold is 19.3 g/cm3 and that of pyrite is 5.0
g/cm3 at 20◦ C.
(3) The density of solid sand (without air spaces) is 2.84 g/mL. The density of gold is
19.3 g/mL. If a 1.00 kg sample of sand containing some gold has a density of 3.10
g/mL (without air spaces), what is the percentage of gold in the sample?
74
Experiments
EXPERIMENT 3
The Law of Definite Proportions
3.1. Safety
Copper sulfate pentahydrate and barium chloride dihydrate are harmful if swallowed and
can cause irritation to skin, eyes and respiratory tract. At high concentrations, these
compound can affect the liver and kidneys. The anhydrous compounds are also harmful
if swallowed. (We should note that 1 gr is the estimated lethal dose for a human.) Thus,
gloves should be worn when handling the compounds of this experiment. If any of these
compounds come in contact with the skin or the eyes, flush with plenty of water for at
least 15 minutes. Bunsen burners, hot glassware, and metal ring stands can cause painful
and serious burns to skin. Hot glassware does not glow and, therefore, looks identical to
glassware at room temperature. Thus, be careful when handling hot glassware.
3.2. Introduction
The law of definite proportions states that when two or more elements combine to form
a given compound, they do so in fixed proportions by mass. This is the same as saying
the composition of a compound is fixed. For example, sodium chloride contains 39.3%
by mass sodium and 60.7% by mass chlorine. In these experiments, the law of definite
proportions will be used to determine the empirical formulas of hydrated ionic salts. (An
empirical formula expresses the simplest whole number ratio of atoms for each element in
a compound.)
The previous two experiments have introduced basic laboratory techniques that will be
used throughout the semester. This experiment represents the first laboratory involving ba-
sic chemical principles and reactions. However, before these principles can be investigated,
an understanding of chemical formulas and nomenclature must first be developed.
75
76
mass for elemental chemistry, namely the atomic mass unit (amu or dalton) is defined as 1
1
amu ≡ 12 the mass of an atom of 12 C = 1.6605 × 10−24 g. Thus,
1 C atom
1 mole = 12 g C atoms × = 6.022 × 1023 C atoms .
19.926 × 10−24 g C atom
The constant 6.022 × 1023 atoms (or molecules)/mole is known as Avogadro’s number .
Since the mole and the atomic mass unit are defined using the same scale, 1 amu = 1
g/mole. Thus, the masses given on the periodic table can also be expressed as the number
of grams of the element per mole of element. The molar mass M of a compound (sometimes
known as molecular weight) is obtained by summing the mass of all of the elements in a
compound and, therefore, has units of g/mol. Moreover, the definition of a mole when
combined with the law of definite proportions implies that a sample of H2 O will have 2
moles of atomic hydrogen for every 1 mole of atomic oxygen.
3.4.3. Cations
(1) Cations from periodic table groups I, II and III have charges of +1, +2 and +3,
respectively. Since the charge cannot vary for stable compounds with these cations,
the unmodified metal name is used for the ion.
(2) Silver, zinc and cadmium only form +1 cations and, therefore, are named using
the unmodified metal name.
(3) Mercury(I) ion is not stable and, therefore, always forms the cation Hg2+2 in ionic
compounds.
(4) All other metal cations are named by adding a roman numeral in parentheses after
the metal name to indicate the charge on the ion (known as the Stock system of
nomenclature). For example, Fe3+ is iron(III), while Pb2+ is lead(II). Some of these
metal compounds have an older nomenclature, which you will see on some of the
reagent bottles in the laboratory. Table 3.2 gives the older system in comparison
to the Stock system for metals that are important in freshman chemistry.
(5) NH+ 4 , known as the ammonium ion, behaves as a Group I metal ion although it
does not contain a metallic element. Thus, the ammonium ion can act as a cation
in an ionic compound.
Table 3.2: Metal cation nomenclature: The Stock system in comparison to the older
system.
3.4.4. Anions
(1) Monoatomic anions formed from non-metal elements with sufficient extra electrons
to have a rare gas configuration have names that end in -ide. Thus O2− , which has
an electron configuration similar to the rare gas Ne, is named oxide. Similarly, P3−
(having an electron configuration similar to the rare gas Ar) is named phosphide.
(2) Table 3.3 lists the common polyatomic ions that are important in freshman chem-
istry. It is important to known the names and formulas of these anions
and, therefore, this table should be memorized.
(3) Polyatomic anions with names ending in -ite are related to the -ate anions in
Table 3.3 but have one less oxygen atom. The standard -ite anions are also given
in Table 3.3.
(4) Anions with names having the form Per-ate are related to the -ate anions in Table
3.3, but contain one additional oxygen atom. Thus, ClO− 4 is the perchlorate
anion.
(5) Anions with names of the form Hypo-ite are related to the -ite anions in Table
3.3, but have one less oxygen atom. Thus, ClO− is the hypochlorite anion.
(6) Anions that are formed from the combination of an anion with a charge > −1
and an H+ unit are named hydrogen - ion. Thus, HS− is hydrogen sulfide ion,
HPO2− −
4 is hydrogen phosphate ion, and H2 PO4 is dihydrogen phosphate ion.
3.4.5. Hydrates
Hydrates are substances formed when water combines chemically in definite proportions
with an ionic salt, thereby giving a constant ratio of water molecules to the ions of the salt.
Hydrates are not mixtures, since the water is coordinatively bound to either the cation
or anion or both in the salt. In CuSO4 • 5 H2 O, for example, the bonding involves four
water molecules coordinatively bound to the Cu2+ ion in a square planar structure and one
molecule of water bound to the sulfate ion by hydrogen bonds [cf. Fig. 3.2]. The anhydrous
(without water) form of a hydrated salt is produced when all the water of hydration is lost.
Some examples of hydrates are listed below:
Formula Chemical name Common name
(CaSO4 )2 • H2 O calcium sulfate hemihydrate plaster of paris
CaSO4 • 2 H2 O calcium sulfate dihydrate gypsum
CuSO4 • 5 H2 O copper (II) sulfate pentahydrate blue vitriol
MgSO4 • 7 H2 O magnesium sulfate heptahydrate epsom salt
Na2 CO3 • 10 H2 O sodium carbonate decahydrate washing soda
79
Notice that hydrates are named by first naming the ionic salt and then adding x-hydrate,
where x− is the appropriate Greek prefix (cf. Section 3.4.1) to indicate the number of
water molecules associated with salt. The • in the formula indicates a kind of chemical
bond that usually can be easily broken. For example, magnesium sulfate heptahydrate can
be converted to anhydrous magnesium sulfate by heating:
MgSO4 • 7H2 O (s) → MgSO4 (s) + 7H2 O (g) . (3.1)
3.4.6. Acids
Acids are covalent compounds formed from the hydrogen cation and any of the anions.
Although these compounds are covalent, the hydrogen cation can be easily removed when
the acid is in solution. Thus, acids also have some properties of ionic compounds. Because
of this uniqueness, acids have a different nomenclature standard with the rules:
(1) Acids formed with -ide anions are named hydro-ic acid. Thus, HCl (which
contains a chloride anion) is hydrochloric acid.
(2) Acids formed with -ate anions (including per-ates) are named -ic acid. As an
example, H2 SO4 is sulfuric acid and HClO4 is perchloric acid.
(3) Acids formed with -ite anions (including hypo-ites) are named -ous acid. Thus,
HNO2 is nitrous acid, while HClO is hypochlorous acid.
Fig. 3.2: Schematic picture of the CuSO4 • 5 H2 O compound with the Cu2+ ion forming
a square planar structure involving four water molecules, while the fifth water molecule is
hydrogen bonded to the sulfate counter ion [i.e., SO2−
4 ].
80
See Section 3.3.4, Item (6) for the nomenclature of acidic anions (i.e., anions formed
from the loss of a single H+ from an acid that has more than one hydrogen cation available).
Partner: Date:
(1) What should you do if any of the solid compounds come in contact with your skin?
(2) Heptahydrate implies how many water molecules are complexed to a salt?
(3) Name the following: (a) (NH4 )2 S, (b) H2 CO3 , (c) I2 , and (d) AlCl3 • 6 H2 O.
(4) Write the chemical formula for the following: (a) barium chloride, (b) ferrous
sulfate, (c) disulfur dichloride, and (d) sodium hydrogen carbonate.
(5) If 3.5 g of CuSO4 • 5 H2 O (s) undergoes dehydration, what is the mass of the
gaseous water produced?
84
Partner: Date:
Results
Fill out all tables and answer all questions below. All values must have appropriate
significant figures and units.
Table A.I. The information on the reactants obtained during the performance of Experi-
ment 3A.
washing soda
lithium chloride
(3) Explain why one sample gained water and why one lost water.
86
Table B.I. The information, obtain during the performance of Experiment 3B, on the hy-
drates given to me.
Hydrate 1 Hydrate 2
Name of salt in hydrate:
Mass of hydrate:
Mass of anhydride:
*The mass after heating should only be entered after the crucible and contents have
reached constants mass. Use the table below to monitor the mass of the crucible during the
heat/cool/weigh cycles for your hydrates. (Please note that all of the cycles listed below
may not be necessary.)
Mass of dish after heating
Hydrate 1 Hydrate 2
Cycle 1
Cycle 2
Cycle 3
Cycle 4
Cycle 5
Cycle 6
87
Table B.II. The information, obtain during the performance of Experiment 3B, on the
hydrates given to my laboratory partner.
Hydrate 1 Hydrate 2
Name of salt in hydrate:
Mass of hydrate:
Mass of anhydride:
*The mass after heating should only be entered after the crucible and contents have
reached constants mass.
88
Use the information in Tables B.I and B.II to answer the following questions for the hy-
drates studied by both you and your laboratory partner. All values must have appropriate
significant figures and units.
(1) What evidence of a chemical change did you observe when the hydrated sample
was heated?
(2) What evidence of a chemical change did you observe when water was added to the
anhydrous sample?
(3) What is the mass mH2 O of the water in the hydrate (determine by subtracting the
mass man of the anhydride from the mass mhy of the hydrate) for (a) Hydrate 1
and (b) Hydrate 2?
89
(4) What is the percentage of water in the hydrate for (a) Hydrate 1 and (b) Hydrate
2? The percentage of water can be determined by
mH2 O
%H2 O = × 100 ,
mhy
where mH2 O is the mass of water in the hydrate and mhy is the mass of the hydrate.
(5) How many moles of water were in the sample from (a) Hydrate 1 and (b) Hydrate
2? The number of moles nH2 O of water in the sample can be obtained using
mH2 O
nH2 O = ,
MH2 O
where MH2 O is the molar mass of water.
90
(6) How many moles of anhydride were created in (a) Hydrate 1 and (b) Hydrate 2?
The number of moles nan of the anhydride in the sample can be obtained using
man
nan = ,
Man
where Man is the molar mass of the anhydride.
(7) How many moles of water are associated with a single mole of anhydride in (a)
Hydrate 1 and (b) Hydrate 2? [Determine this by dividing the moles nH2 O of water
by the moles nan of anhydride.]
(8) What is the formula for the hydrate [i.e., anhydride • x H2 O, where x is the ratio
in question (7)] that was thermally decomposed in (a) Hydrate 1 and (b) Hydrate
2?
91
Partner: Date:
(1) Rochelle salt is the tetrahydrate of the ionic salt KNaC4 H4 O6 . Write the formula
for Rochelle salt.
(2) Describe (a) the three situations in which Greek prefixes are used and (b) when
Roman numerals are used in naming chemical compounds.
(4) If 5.051 g of magnesium sulfate heptahydrate is heated to remove all water, what
is the mass of the anhydride formed?
92
Experiments
EXPERIMENT 4
Stoichiometry of a Reaction
4.1. Safety
Copper sulfate pentahydrate is harmful if swallowed and can cause irritation to skin, eyes
and respiratory tract. At high concentrations, this compound can affect the liver and
kidneys. If any of this compound comes in contact with the skin or the eyes, flush with
plenty of water for at least 15 minutes. Methanol is flammable and should be heated with
care. Bunsen burners, hot glassware, and metal ring stands can cause painful and serious
burns to skin. Hot glassware does not glow and, therefore, looks identical to glassware at
room temperature. Thus, be careful when handling hot glassware.
4.2. Introduction
A very common and useful type of reaction is the displacement reaction, which occurs when
a metal displaces another metal in a solution with a single ionic salt. Displacement reactions
between metals occur when one metal is more active than another metal and usually involve
the oxidation of one metal and the reduction of the other metal. Oxidation refers to the
process in which an atom, ion, or molecule loses electrons, while reduction implies that an
atom, ion, or molecule gains electrons. A useful mnemonic device to remember this is OIL
RIG, or Oxidation Is Loss (of electrons) and Reduction Is Gain (of electrons). In this
experiment, we will use stoichiometric principles to determine the oxidation state of iron
ions (i.e., Fe2+ or Fe3+ ) formed during the reaction of copper sulfate (i.e, CuSO4 ) with
solid iron (i.e., Fe0 ).
93
94
of solvent), normality (equivalents of solute/liter of solution) and parts per million (ppm)]
will be introduced later. Below, we have shown two examples that illustrate how molarity
is calculated and how molarity is used in solution chemistry.
µ ¶
0.499 mol NH3 1000 mL
molarity NH3 = = 1.0 mol NH3 /L = 1.0 M
500 mL 1L
4.3.2. Molarity in solution chemistry
If you wanted to make 750 mL (3 significant figures) of a 0.200 M aqueous solution of
sodium chloride, one would calculate the number of grams of sodium chloride (s) by the
following steps:
(1) Determine the number of moles of NaCl needed to prepare the solution.
(2) Determine the molar mass of NaCl.
(3) Multiply the number of moles of NaCl needed by the molar mass of NaCl.
These steps are illustrated below.
µ ¶ µ ¶
0.200moles NaCl 1000 mL
moles NaCl = 750 mL solution
1 L solution 1L
= 0.1500 moles NaCl
µ ¶ µ ¶
1mole Na 1mole Cl
molar mass NaCl = 23.00 g/mol of Na + 35.45 g/mol of Cl
1mole NaCl 1mole NaCl
= 58.45 g/molNaCl
grams NaCl = 0.1500 moles NaCl × 58.45 g/mol of NaCl = 8.767 g NaCl
= 8.77 g NaCl
reaction [i.e., eq. (4.1) or (4.2)] is consistent with experiment. Therefore, we will add an
excess of copper sulfate solution to a known amount of elemental iron and will weight the
product obtained from the chemical reaction. If eq. (4.1) is dominate, the number of moles
of copper produced will equal the number of moles of iron reacted. If, however, eq. (4.2)
is dominate, the number of moles of copper produced will larger than the number of moles
of iron that reacted. The procedure for this study is as follows:
(1) Weigh 1.0 g of iron filings.
(2) Transfer the iron filings to a clean, dry, weighed 150 mL beaker.
(3) Reweigh the 150 mL beaker containing the iron filings to verify the mass of iron.
(4) In Question 1 of the Pre-laboratory questions, you were asked to calculate the
amount of a 1.0 M copper(II) sulfate solution needed for the reaction given in eq.
(4.2) to go to completion for a 1.0 g mass of iron. Show this calculation to your
laboratory instructor for approval.
(5) Add the volume of copper(II) sulfate obtained in (3) plus a 5% excess to a clean,
dry Erlenmeyer flask.
(6) Heat the copper sulfate solution to almost boiling.
(7) Slowly add the hot copper sulfate solution to the beaker containing the iron filings.
(If the addition is performed quickly, the solution will froth and material will be
lost during the reaction.)
(8) When the reaction has ceased, allow the copper product to settle. Then carefully
decant the liquid from above the product.
(9) Add approximately 10 mL of distilled water to the product and swirl the beaker
to mix. Again, allow the product to settle and decant. This washes the product
to remove trace amounts of iron cations. Repeat with a second 10 mL portion of
distilled water.
(10) Added 5 mL of methanol and swirl. Allow the product to settle and decant.
Repeat with a second 5 mL portion of methanol.
(11) Heat the beaker in a hot water bath to remove any remaining methanol. If nec-
essary, carefully break up any clumps of copper with the spatula tip. (Check the
spatula to ensure that you are not removing any copper from the beaker.)
(12) When the product is thoroughly dry, dry the outside of the beaker and weigh the
beaker to determine the mass of the product.
(13) Transfer the product to a clean, dry, labeled vial for use in Experiment 5.
(14) Repeat the entire procedure one more time and added this product to the labeled
vial.
Partner: Date:
(1) What is the minimum volume needed to react all of 1.000 g of iron with a 1.0
M aqueous solution of copper(II) sulfate for the reaction in eq. (4.2). Hint: The
chemical reaction equation for an aqueous solution of copper(II) sulfate is
CuSO4 (aq) → Cu2+ (aq) + SO2− 4 (aq) .
(2) In eq. (4.1) which compound is (a) oxidized and (b) reduced?
(3) If copper foil is added to a (colorless) solution of silver nitrate, the solution turns
blue, while the foil turns silvery. (a) What is happening? (b) Which is the more
active metal: silver or copper?
98
Partner: Date:
Results
Fill out all tables and answer all questions below. All values must have appropriate
significant figures and units.
Table B.I. The data obtain during the performance of Experiment 4 by myself.
Trial 1 Trial 2
Mass of empty 150 mL beaker:
Mass of product:
Table B.II. The data obtain during the performance of Experiment 4 by my laboratory
partner.
Trial 3 Trial 4
Mass of empty 150 mL beaker:
Mass of product:
100
Calculations
(1) For each trial, calculate the number of moles of iron used. (The calculation for
each trial should be clearly indicated to receive credit.)
(2) For each trial, calculate the number of moles of copper formed.
(3) Write the balanced chemical equation that is indicative of these experimental data?
101
(5) What would happen if copper metal is added to iron sulfate solution? Why?
(6) Extra credit (2 pts): What is the molarity of the iron solution created during
this reaction?
(7) Extra credit (2 pts): If the water was evaporated from the aqueous iron solution
after the reaction, what ionic salt would be left as the residue?
102
Partner: Date:
(1) Write the balanced chemical reaction equations for the following: (a) iron reacts
with molecular oxygen to yield iron(III) oxide, (b) silver nitrate and calcium chlo-
ride react to form calcium nitrate and silver chloride, and (c) ethane reacts with
oxygen to form carbon dioxide and water.
(2) The following reaction is used to extract silver impurities from gold:
Au (l) + Ag (l) + Cl2 (g) → Au (l) + AgCl (s) .
(b) How many grams of Cl2 gas would be required to remove the silver impurity in
250 grams of 95% (by mass) pure gold? (Assume that silver is the only impurity.)
104
Experiments
EXPERIMENT 5
Copper reactions
5.1. Safety
Aqueous nitric acid and aqueous sulfuric acid are hazardous. They produce severe burns
on the skin and the vapor is a lung irritant. These compounds should be handled in a
fume hood while wearing safety glasses and gloves. Rinse your hands with water for 5
minutes after handling the acid bottles. The gases produced during these reactions are
toxic and must be avoided. Thus, when the experiment states that a procedure should be
performed in the fume hood, DO so. Aqueous sodium hydroxide is also corrosive to the
skin and is especially dangerous if splashed into eyes. Again, handle this compound with
gloves. Copper sulfate pentahydrate is harmful if swallowed and can cause irritation to
skin, eyes and respiratory tract. At high concentrations, this compound can affect the liver
and kidneys. If any of this compound comes in contact with the skin or the eyes, flush with
plenty of water for at least 15 minutes. Methanol is flammable and should be heated with
care. Bunsen burners, hot glassware, and metal ring stands can cause painful and serious
burns to skin. Hot glassware does not glow and, therefore, looks identical to glassware at
room temperature. Thus, be careful when handling hot glassware.
5.2. Introduction
Chemical reactions are classified into three broad categories: (i) precipitation reactions, (ii)
acid/base reactions, (iii) oxidation/reduction reactions and (iv) decomposition reactions.
In precipitation reactions (or double displacement reactions) the ions of two soluble salts
react to form an insoluble neutral compound and a different soluble salt. A good example of
this type of reaction is the reaction of aqueous sodium chloride with aqueous silver nitrate
to yield aqueous sodium nitrate and solid silver chloride, or
NaCl (aq) + AgNO3 (aq) → NaNO3 (aq) + AgCl (s) .
Acid/base reactions involve the reaction of an acid with a base to form a salt and (usually)
water. These reactions will be covered in more detail during Experiments 7 and 8. Redox
reactions, such as the reaction investigated in Experiment 4, involve the transfer of electrons
from one atom to another. Decomposition reactions occur when a compound breaks down
to form simpler substances, such as when calcium carbonate decomposes into calcium oxide
and carbon dioxide under high temperatures. In this experiment, various chemical reactions
involving copper and copper salts will be investigated.
c
°2008 QC Chemistry and Biochemistry
105
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5.3. Solubility
The reactions that will be investigated below will rely on the precipitation of insoluble
salts from aqueous solutions. The formation of a precipitate can be predicted using the
solubility rules, which are important rules that guide inorganic chemical reactions. Thus,
the solubility rules in Table 5.3 should be committed to memory.
Fig. 5.1: Schematics of (a) an vacuum filtration setup and (b) a hot water bath setup.
108
(2) Place a piece of filter paper having the correct diameter on the flat area in the
Buchner funnel and moisten the filter paper with the solvent in use.
(3) Check the moist filter paper for creases.
(4) Make sure that the vacuum line is attached, then turn on the vacuum.
(5) Slowly pour the solution to be filtered into the Buchner funnel. Try to keep the
solution in the center of the filter paper, which ensure that all of the precipitate
is centered in the middle of the funnel.
(6) Once the solution has been filtered, rinse the container with a small amount of the
solvent to ensure that all of the precipitate was collected.
(7) Use solvents to help dry the precipitate as specified in the experimental procedures.
At this point, if clumps are forming a spatula can be used to separate the clumps.
(8) Break the vacuum at the flask or the vacuum line.
(9) Turn off the vacuum.
Partner: Date:
Write the balanced reaction equation for the following reactions. (Remember that a bal-
anced reaction equation includes the physical information about the compounds and is
charge and mass balanced.)
(1) reaction of solid copper with aqueous nitric acid and molecular oxygen to produce
gaseous nitrogen dioxide and copper(II) nitrate.
(2) Write the balanced reaction equation for the reaction of copper(II) nitrate with
aqueous sodium hydroxide.
(3) Write the balanced reaction equation for the decomposition of copper(II) hydroxide
to copper(II) oxide.
(4) Write the balanced reaction equation for the reaction of copper(II) oxide with
aqueous sulfuric acid.
110
Partner: Date:
Results
Fill out all tables and answer all questions below. All values must have appropriate
significant figures and units.
Calculations
(1) What is the molarity of the copper(II) nitrate solution after the addition of distilled
water in Reaction 1?
(2) How many moles of hydroxide ion (OH− ) are in the 30 mL of 3.0 M aqueous
sodium hydroxide solution used in Reaction 2?
(3) The limiting reactant is the reactant that controls the extent of reaction, because it
is present in the smallest molar quantity. What is the limiting reactant in Reaction
2?
(4) Using the moles of the limiting reactant, determine the mass of copper(II) hydrox-
ide created during Reaction 2.
114
(5) Using the mass of copper(II) hydroxide calculated above, determine the theoretical
yield of copper(II) oxide in Reaction 3. (The theoretical yield is the mass of
copper(II) oxide predicted if all reactions proceed at 100% efficiency.)
(7) What steps in the reaction introduced error which, in turn, lowered the percent
yield?
115
(1) What is the percent yield for this reaction? Show all necessary calculations below.
116
Partner: Date:
Describe whether the error introduced by each of the following problems would result in a
high or low value for the preparation of copper oxide, or would not affect the results.
(1) Some of the copper nitrate solution is splashed out of the beaker before the addition
of sodium hydroxide.
(3) The solution bumps during the heating of copper(II) hydroxide to produce cop-
per(II) oxide.
(5) The washings with water and methanol are insufficient to remove all of the solution
residues from the copper(II) oxide.
(6) The copper(II) oxide crystals are still damp when weighed.