CHM 327 Name: ______________________

LABORATORY MANUAL

ANALYTICAL CHEMISTRY I

CHM 327

Fall 2024

for

T836

Chemical Laboratory Technology

Instructor: Dr. Meghan Doster

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CHM 327 Name: ______________________

St. Clair College of Applied Arts and Technology

CHM 327 Analytical Chemistry I
Introduction
The experiments performed in Analytical Chemistry I will introduce you to
analytical techniques that are widely used by chemists in industry. For many of the
experiments, the composition of the samples will be known. Thus, you will be able to
judge how well you are mastering these basic techniques.
Safety in the Analytical laboratory
You must consider safety in the laboratory as your number one priority. In
addition to always remembering your Safety Pledge, you must read and understand all the
information found in Fundamentals of Analytical Chemistry, 10th ed., Section 36J (or 2J
in the 9th edition) SAFETY IN THE LABORATORY and the booklet Laboratory Health
and Safety Guidelines, 4th edition (available in the stock room). Be prepared throughout
the semester to answer questions related to the information outlined in these safety-
related information sources. Remember, a positive assessment of your skills in the
laboratory is directly related to your ability to work safely using Good Laboratory
Practice.

Preparing to Work in the Analytical Laboratory

Your chances of success in the laboratory will greatly improve when you take
time before you enter the laboratory to read carefully and understand each step in the
method and to develop a plan for how and when you will perform each step. In fact, a
complete flow chart is considered to be a safety related concern, so production of a Flow
Chart that briefly outlines the experiment’s major steps and shows how reagents
will be produced is mandatory before you can perform the experiment. The prelab
including the Flow Chart is worth 2 marks. Before you start an analysis, you should
understand the significance of each step in the procedure to avoid the pitfalls and
potential sources of error that are inherent in all analytical methods. Information about
these steps can be found in (1) Experiment Overview and Procedure sections, (2)
classroom discussions, and (3) the procedure detailed in a relevant standardized method.

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CHM 327 Name: ______________________
If, after reading this information you still do not understand the reason for doing one or
more of the steps in the method, consult your instructor before you begin your laboratory
work.
Accuracy of Your Measurements
In looking over any analytical procedure, you should decide which measurements
must be made with maximum precision, and thus with greatest care, as opposed to those
that can be carried out rapidly with little concern for precision. Generally, measurements
that appear in the equation used to compute the results must be performed with maximum
precision. The remaining measurements can and should be made less carefully to
conserve time. The words “about” and “approximately” are frequently used to indicate
that a measurement does not have to be done carefully. For example, you should not
waste time and effort to measure a volume to 0.02 mL when an uncertainty of 0.5 mL or
even 5 mL will have no discernible effect on the results.
In some procedures, a statement such as “weigh three 0.5 g samples to the nearest
0.1 mg” is encountered. Here, samples of perhaps 0.4 to 0.6 g are acceptable, but their
masses must be known to the nearest 0.1 mg. The number of significant figures in the
specification of a volume or a mass is also a guide to the care that should be taken in
making a measurement. For example, the statement “add 10.00 mL of a solution to the
beaker” indicates that you should measure the volume carefully with a buret or a pipet,
with the aim of limiting the uncertainty to perhaps 0.02 mL. In contrast, if the directions
read “add 50 mL,” the measurement can be made with a graduated cylinder or even with
the graduations on a beaker.
Marks associated with accuracy will be awarded based on how close the student’s
reported value comes to the actual amount of target compound in unknowns or in
laboratory fabricated spikes of known concentrations. In the case of unknowns, the
difference between the actual amount of target present will be calculated as a percentage
and marks will be awarded depending on how close the reported amount is to the actual
amount. In the case of fabricated samples, marks will be based on proximity to 100 %
recovery of target compound. Accuracy marks will also be dedicated to precision
(indicated by standard deviation) and precise calibration lines (indicated by the
correlation coefficient). The calculation of accuracy marks will be discussed when the
laboratory reports are returned.

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CHM 327 Name: ______________________
Time Utilization
You should study carefully the time requirements involved in an analysis before
work is started. This study will reveal operations that require considerable elapsed, or
clock time but little or no operator time. Examples of such operations include drying a
sample in an oven, cooling a sample in a desiccator, or evaporating liquid on a hot plate.
Efficient workers use such periods to perform other operations or perhaps to begin a new
analysis. Some people find it worthwhile to prepare a written time schedule for each
laboratory period to avoid dead time. Time planning is also needed to identify places
where an analysis can be interrupted for overnight or longer, as well as those operations
that must be completed without a break.
The following schedule will be followed as closely as possible for CHM 327.
Some laboratories (such as the ISE labs) will have to be run simultaneously. This is
subject to time depending on time and resources available.
Method Name Method Source Week #
Check In Stock Room 1
th
Standardization/Production of Common Desk Reagents Skoog (9 ed.) 1&2

Standardization/Production of Common Desk Reagents Standard Methods 3

Acidity/Alkalinity Standard Methods 4

Determination of Hardness of Water Skoog (9th ed.) 5
th
Chloride by Argentometric Titration using Fluorescein Skoog (9 ed.) 6
Chloride by Precipitation Reaction + Scale Calibration Skoog (9th ed.) 7&8
Chloride in Surface Waters by ISE Standard Methods 9
Fluoride in Toothpaste by ISE Standard Methods 10
Titrations with Iodine and Sodium Thiosulfate Skoog (9th ed.) 11
Vitamin C by Iodide Titration Standard Methods 12
Optimization of Coagulation & Flocculation Parameters for
Standard Methods 13
the Jar Test
Check out Stock Room 14

Lab Reports
Lab reports are written using MS Word and MS Excel. All raw data from each
experiment (charts) and the prelab must be submitted along with your report originals or
a scan of the corresponding pages from your laboratory notebook to receive accuracy
marks. Written lab reports that are due and not submitted before the next lab session
begins result in the loss of 10 % of the total possible marks associated with the lab report.
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CHM 327 Name: ______________________
Another 10 % is lost for each additional day late. Experiments not performed and written
lab reports not submitted after one week get an automatic grade of 0. Labs must be
performed on the day specified in the time allotted (usually 2 hours 50 minutes); working
overtime results in a loss of 10% of the possible marks for the first 10 min over and
an additional 5 % for every additional 5 min, unless stated otherwise by the instructor.
Marks will be lost if instructions for creating a Flow Chart/ Prelab (before lab begins) are
not followed, assigned scale, lab bench, equipment, or instruments are not clean (5
% deduction), if you show up late to lab (5 % will be deducted for every 5 minutes
that you are late) if your original data sheets are not attached (results/accuracy will not
be marked) and if the minimum write up information is not included in the submitted lab
report. NOTE: All information used in your lab report (even if written in your own
words, you learned it somewhere) must be properly sourced and the full reference must
be included in the reference section of your lab report. You are NOT allowed to copy AI
generated information directly into your lab report, all information must be written in
your own words, and all information must be properly cited in ACS format, with real
references!!

The Lab Report will contain the following sections:

• Title Page
• Purpose
• Theory
• Results and Calculations
• Discussion
• Conclusion
• Questions (If applicable)
• References
• NOTE: For full marks you must include your prelab and all data sheets.

All students are responsible for writing their own unique lab report written in
their own words using their own data and observations gathered during the performance
of their practical laboratory work. Any unauthorized copying or unreferenced work will
be considered to be plagiarism, which could result in a warning, marks deducted, a mark
of 0, or a failing grade in the course. NOTE: All instances of plagiarism will be
entered into St. Clair College’s database for academic misconduct and further
consequences will be determined by the chair if necessary.

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CHM 327 Name: ______________________

Lab 1&2
Standardization of Common Desk Reagents
Method References: Fund. of Anal. Chem., 8th edition, Method 37 C (pp 1066 – 1072)
Standard Methods 2310

Safety: This laboratory involves the production and use of extremely corrosive
substances. The use of local exhaust (fume hood) and personal protective equipment
such as gloves, lab coat and approved safety glasses is necessary. Concentrated solutions
such as acids should be dispensed under local exhaust conditions. Follow instructions
regarding waste handling and disposal.

Method Summary: The production of standard solutions containing HCl and NaOH is
common practice for most analytical laboratories. Standard acid and base solutions are
made to an exact (four significant figure) accuracy by using volumetric glassware and
primary standards. For standard sodium hydroxide solutions, potassium acid phthalate
(KHP) is used as the primary standard and phenolphthalein indicates the titration point.
For standard hydrochloric acid solutions, sodium carbonate is used as the primary
standard and bromocresol green indicates the titration point. For this laboratory, the
primary standard will be weighed into conical flasks and then titrated with the solution to
be standardized. The solutions manufactured and/or standardized during Lab 1&2 will be
used for Lab 3 and Lab 4.

Apparatus and Reagents

ACS grade potassium acid phthalate (previously dried for 2 h at 103oC)
ACS grade sodium carbonate (previously dried for 2 h at 103oC)
Conc HCl
ACS grade sodium hydroxide
0.05 M NaCl
Phenolphthalein indicator
Bromocresol green indicator
250 mL conical flasks
Beakers to hold solutions
50 mL burette
5, 10, 15, 20, 25 mL volumetric pipettes
100.0 mL volumetric flasks
Hot plates
Glass and/or plastic storage bottles (2)

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CHM 327 Name: ______________________
Procedure: Standardization of 0.1 M NaOH
1) Calculate the target mass of NaOH pellets (MW = 40.00 g/mol) to produce a 0.1
M NaOH solution (prepare in a 1 L storage bottle):
Target Mass: ______________(g)

2) Obtain a 1 L storage bottle and use a graduated cylinder to mark the 1 L

graduation on your bottle (NOTE: some bottles are smaller than 1 L; in this case,
fill your bottle to just below the neck with water; mark water level with marker;
determine correct volume of bottle by dumping into a graduated cylinder).

3) Half-fill your labeled storage bottle with deionized water and then add the
calculated mass of NaOH pellets. When the pellets have dissolved, dilute the
solution to the predetermined 1 L mark with deionized water. Place the solution
in a buret.

4) Calculate the target mass of KHP (MW = 204.22 g/mol) for a 15 mL 0.1 M
NaOH titration. Place the target mass in Table 1.
Target Mass: ______________(g)

5) Place the calculated amount of primary standard (KHP), weighed by difference, to

the nearest 0.1 mg into four separate labeled 250 mL capacity conical flasks (at
least four titrations will be required). Record all observations in Table 1. Hand in
Table 1 to the instructor when you have finished this laboratory to be signed off.

6) Dilute the primary standard to 50 mL with deionized water (NOTE: estimate this
volume using the graduations on the conical flask, DO NOT use graduated
cylinder).

7) Prepare a conical flask with 50 mL of deionized water for a blank titration.

8) Add the required amount of phenolphthalein indicator to each flask (~3 drops).

9) Titrate the contents of each conical flask until the titration point (faint pink colour
that persists for a least 1 min) is reached, remember to record all data in Table 1.

Procedure: Standardization of 0.1 M HCl

1) Calculate the target volume (mL) conc HCl (M = 12 mol/L) to produce a 0.1
mol/L solution in a 1 L container.
Target Volume conc HCl:_____________(mL)

2) Obtain a 1 L storage bottle and use a graduated cylinder to mark the 1 L

graduation on your bottle. (NOTE: some bottles are smaller than 1 L; in this case,
fill your bottle to just below the neck with water; mark water level with marker;
determine correct volume of bottle by dumping into a graduated cylinder).

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CHM 327 Name: ______________________
3) Half-fill your labeled storage bottle with deionized water. In the fume hood, using
a 10 mL graduated cylinder and Pasteur pipette, add the calculated volume of
concentrated HCl into the half-filled labeled storage bottle. Gently swirl the
solution, and then dilute the solution to the predetermined 1 L mark with
deionized water. Place the solution in a buret.

4) Calculate the target mass (g) Na2CO3 (MW = 105.989 g/mol) for a 25 mL 0.1 M
HCl titration. Record target mass in Table 2.
Target Mass: ______________(g)

5) Place the calculated amount of primary standard (Na2CO3) weighed to the nearest
0.1 mg into four separate labeled 250 mL capacity conical flasks (at least four
titrations will be required). Record all observations in Table 2. Hand in Table 2
when you have finished this laboratory for your instructor to sign off.

6) Dilute the primary standard to 50 mL with deionized water (estimate this volume
using the graduations on the conical flask).

7) Prepare a conical flask with 50 mL of 0.05 M NaCl for a blank titration.

8) Add the required amount of bromocresol green indicator to each flask. Titrate the
solution just until the colour begins to change from blue to green. Boil the
solution for one minute (solution should turn blue again, if not it was over
titrated) then cool the solution in an ice-cold water bath for 5 minutes so that it
can be handled safely.

9) Finish the titration of the contents of each conical flask remembering to record all
observations in Table 2 (NOTE: indicator should turn from blue to green/yellow).

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CHM 327 Name: ______________________
Lab 1 & 2 - Raw Data sheet must be signed by instructor & handed in with Report.

Table 1. Observations for the Standardization of 0.1 M NaOH for Lab 1&2
Actual mass NaOH added: _______________ g
Volume marked on Storage Bottle: _________ L
Expected M NaOH:_______________ (use actual mass added and volume of bottle)

# Mass Vi NaOH Vf NaOH Vt NaOH Vt NaOH MNaOH

KHP (g) (mL) (mL) (mL) (mL) corr (mol/L)
B Avg MNaOH s CV
(mol/L) (mol/L) %
1
2
3
4
5
6

% difference _____________________(%)

Table 2. Observations for the Standardization of 0.1 M HCl for Lab1&2

V conc HCl added:______________(mL)
Volume marked on Storage Bottle: _________ L
Expected M HCl:____________(M) (use actual mass added and volume of bottle)

Before Boiling After Boiling

# Mass Vi1 HCl Vf1 HCl Vi2 HCl Vf2 HCl Vt HCl Vt HCl MHCl
Na2CO3 (g) (mL) (mL) (mL) (mL) (mL) (mL) corr (mol/L)
B
1
2
3
4
5
6

Average MHCl: _______________(mol/L). s: _________________(mol/L).

CV: ______________(%) %difference: _______________(%)

Workstation/scales clean: _________________________________________

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CHM 327 Name: ______________________
Supplemental Lab Question: (1 mark) NAME: ___________________________.
(Note you can answer this question directly on this sheet of paper and hand in with your
lab report).

1. What molarity of KHP is required if 15.00 mL of the KHP solution will

use 18 mL of 0.1 M NaOH solution?

2. What approximate mass (g) of KHP (MW = 204.22 g/mol) is required to

manufacture the solution mentioned in the previous question in a 250.0
mL volumetric flask?

3. What Na2CO3 molarity is required if 10.00 mL of the solution will use 13

mL of 0.10 M HCl?

4. What approximate mass (g) of Na2CO3 (MW = 105.989 g/mol) is required

to manufacture the solution mentioned in the previous question in a 250.0
mL flask?

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CHM 327 Name: ______________________
Lab 1&2 Prelab and Flow Chart
Standardization of Common Desk Reagents
Obtain a Blueline A91 Notebook from the bookstore or chemistry stockroom. UPC
069775460075 St Clair Bookstore: MMS024416179/0,

For your pre-lab, please prepare in your laboratory notebook. (See notebook rules on
Blackboard).
1) Enter your Name, Program, Course No., Lab Period (section #), and date (Fall
2021) on the cover.
2) Enter your Name and Contact information on the inside page in the space allotted.
3) The back of the cover page is page 1, and the first lined-page is page 2. Using a
pen (blue or black), enter the page numbers on all the top left corners for odd
pages, and the top right corners for even pages, and continue to the end of the lab
notebook.
4) Reserve pages 2-7 for Table of contents. Print “Table of Contents” on the top of
Page 2, and leave pages 3-7 blank.
5) Your first experiment will begin on page 8.

Lab 1&2 - Prelab to be completed in Laboratory Notebook before Lab begins:

1) Purpose: Briefly state the purpose of the experiment.

2) Materials/Chemicals: In this section, list any specific equipment that is required,
or chemical information that is important for the lab. (ie. Chemical name, CAS#,
MW, molecular formula, bp, mp, etc. ) Be sure to state the source of your
information.
3) Safety Hazards and Precautions: In this section, list any safety hazards that might
arise in the lab, including from chemicals or equipment. (hint: most of this
information is found in the chemical SDS.)
4) Balanced Equations: In this section include balanced equation for all reactions
involved in the experiment. For experiment #1 this includes (NaOH and KHP)
and (HCl and Na2CO3).
5) Calculations: In this section include all calculations for standards and reagents
required to begin the experiment. Be sure to show all work! For experiment #1
complete the following calculations:
A) Calculate the target mass of NaOH pellets (MW = 40.00 g/mol) to produce
a 0.1 M NaOH solution (prepare in a 1 L storage bottle).
B) Calculate the target mass of KHP (MW = 204.22 g/mol) for a 15 mL 0.1
M NaOH titration. Place the target mass in Table 1.
C) Calculate the target volume (mL) conc HCl (M = 12 mol/L) to produce a
0.1 mol/L solution in a 1 L container.
D) Calculate the target mass (g) Na2CO3 (MW = 105.989 g/mol) for a 25 mL
0.1 M HCl titration. Record target mass in Table 2.
E) Calculate the target mass (g) of NaCl required to make 50 mL of 0.05 M
NaCl solution for the blank.
6) Flowchart: Construct a flowchart for the lab. This should NOT be a reproduction
of the manual, but instead a graphical summary of the major steps. (NOTE: Do
not rewrite procedure word for word.)

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CHM 327 Name: ______________________
Lab 1&2 - Standardization of Common Desk Reagents

Lab 1&2 Report Requirements: (Total 20 marks Report)

NOTE: Original data must be submitted with your lab report!!!!!

Lab Report Format (2 marks)

- Title Page: Title of the experiment (center of page); At the bottom right: Your name,
course and section, date of experiment.
- Headings: Each section is clearly defined with the heading that is bolded or
underlined. (Purpose, Theory, Results, Discussion, etc..)
- Figures and Tables: Must be formatted in ACS style. Each table must have a # and
title at the top, and each figure will have a #, title and legend at the bottom. Include
references if they are not your own work.
- Spelling & Grammar: Text must be written in sentence format with proper spelling
and grammar.
- References: Cite all information throughout report with a superscripted number
corresponding to the source included in the reference section, in ACS format.
Purpose (0.5 marks)
- State the solutions to be standardized and the method(s) referenced.
Theory (4 marks):
- Give all reaction equations and describe the type of titration being performed.
- State 4 properties associated with good primary standards.
- Provide the structures of the two indicators used and describe how they work.
- Describe the Q-test and what it is used for.
Reference all information!
Results and Calculations (6 marks):
Reproduce Table 1 and 2 in your report (include all data from titrations, molarities,
average, s and CV for both NaOH and HCl solutions).

Give sample calculations for the following (typed or handwritten in results and
calculation section of lab report):
-Expected MNaOH and MHCl from mass weighed out and volume of container.
-MNaOH and MHCl for the first titration for each solution.
- Average MNaOH.
- s for MNaOH .
- CV for MNaOH.
- Q-test to check for any potential outliers (must show even if no outliers!)
- % difference between expected MNaOH from actual mass weighed out and
volume of bottle and the average MNaOH calculated from the experimental data.

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CHM 327 Name: ______________________
Discussion (4 marks):
- Describe the two typical determinate (systematic) and two indeterminate
(random) errors that affect neutralization titrations and how you attempted to
overcome or prevent these errors from occurring.
- Discuss the indication of precision associated with the experiment (state s and
CV and explain what these values mean).
- Discuss the differences between titration point and equivalence point.
- Discuss the % percent difference for the M expected (from your mass and
volume) to M observed (from titration data) for NaOH and HCl and explain 2
reasons why they are not the same.
Conclusion (0.5 marks)
- State the average molarities of the standard solutions and the value of s for
each.
Supplemental Lab Question (1 mark)
Notebook: Prelab and Flow Chart (2 marks)

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CHM 327 Name: ______________________
Lab #3
Standardization of Common Desk Reagents
Method References: Fund. of Anal. Chem., 9th edition, Method 37 C
Standard Method 2310

Safety: This laboratory involves the production and use of extremely corrosive
substances. The use of local exhaust (fume hood) and personal protective equipment
such as gloves, coat and safety glasses are necessary. Concentrated solutions such as
acids should be dispensed under local exhaust conditions. Follow instructions regarding
waste handling and disposal.

Method Summary: The production of standard solutions containing HCl and NaOH is
common practice for most analytical laboratories. Standard acid and base solutions are
made to an exact (four significant figure) accuracy by using volumetric glassware and
primary standards. For standard sodium hydroxide solutions, potassium acid phthalate
(KHP) is used as the primary standard and phenolphthalein indicates the titration point.
For standard hydrochloric acid solutions, sodium carbonate is used as the primary
standard and bromocresol green indicates the titration point. For this laboratory, the
primary standard will be diluted in a volumetric flask and aliquots of primary standard
will be placed into conical flasks and then titrated with the solution to be standardized.
The solutions manufactured and/or standardized during Lab #3 will be used for Lab #4.

Apparatus and Reagents

ACS grade potassium acid phthalate (previously dried for 2 h at 103oC)
ACS grade sodium carbonate (previously dried for 2 h at 103oC)
Conc HCl
ACS grade sodium hydroxide
Phenolphthalein indicator and bromocresol green indicator
10 mL graduated cylinder
250 mL conical flasks
Beakers to hold standard solutions and deionized water.
50 mL burette
5, 10, 15, 20, 25 mL volumetric pipettes
100.0 mL volumetric flasks
Glass and/or plastic storage bottles (2)

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CHM 327 Name: ______________________
Procedure: Standardization of 0.1 M NaOH
1) NOTE: ONLY MAKE IF NECESSARY. If you have enough proceed to step 3.
Calculate target mass (g) of NaOH (MW = 40.00 g/mol) to produce a 0.1 mol/L
solution.
Calculated mass = _____________g.

2) If the manufacture of 0.1 M NaOH solution is necessary, add the calculated mass
of NaOH pellets into a labeled storage bottle that is half-filled with deionized
water. When the pellets have dissolved, dilute the solution to a predetermined 1 L
mark with deionized water.

3) Calculate the target mass (g) of KHP (MW = 204.22 g/mol) to produce a 100.0
mL solution which 10.00 mL aliquot requires ~15 mL volume of 0.1 M NaOH.
Calculated mass = _____________g.

4) Pipette 10.00 mL of primary standard (KHP) into four separate labeled conical
flasks (at least four titrations will be required). Record all observations in Table 1.
Hand in Table 1 to the instructor when you have finished this laboratory.

5) Dilute the primary standard to 50 mL with deionized water (estimate this volume
using the graduations on the conical flask). Prepare blank with 50 mL deionized
water.

6) Add the required amount of phenolphthalein indicator to each flask (2-3 drops).

7) Titrate the contents of each conical flask until the titration point is reached
remembering to record all observations in Table 1.

Procedure: Standardization of 0.1 M HCl

1) NOTE: ONLY MAKE IF NECESSARY. If you have enough proceed to step 3.
Calculate volume (mL) conc HCl (M = 12 mol/L) to produce a 0.1 mol/L
solution.
Calculated volume = _____________mL.

2) If making the 0.1 M HCl solution is necessary, in the fume hood, using a 10 mL
graduated cylinder add the calculated volume of concentrated HCl into a labeled
storage bottle that is half-filled with deionized water. Gently swirl the solution,
then dilute the solution to a predetermined 1 L mark with deionized water.

3) Calculate the target mass (g) of Na2CO3 (MW = 105.989 g/mol) to produce a
100.0 mL solution which 10.00 mL aliquot requires ~15 mL volume of 0.1 M
HCl.
Calculated mass = _____________g.

4) Pipette 10.00 mL of primary standard (Na2CO3) into four separate labeled conical
flasks (at least four titrations will be required). Record all observations in Table
2.

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CHM 327 Name: ______________________

5) Dilute the primary standard to 50 mL with deionized water (estimate this volume
using the graduations on the conical flask). Prepare a blank with 50 mL of 0.05
M NaCl.

6) Add the required amount of bromocresol green indicator to each flask. Titrate the
solution just until the colour begins to change from blue to green. Boil the
solution for one minute (solution should turn blue again, if not it was over
titrated) then cool the solution in an ice-cold water bath for 5 minutes so that it
can be handled safely.

7) Finish the titration of the contents of each conical flask remembering to record all
observations in Table 2. (NOTE: indicator should turn from blue to
green/yellow.)

NOTE: Get Table 1 and Table 2 initialed by the instructor before leaving the lab today.
Attach initialed Tables 1 and 2 to the back of your submitted Lab #3 report.

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CHM 327 Name: ______________________
Lab 3 - Raw Data sheet must be signed by instructor & handed in with Report.

Table 1. Observations for the Standardization of 0.1 M NaOH for Lab #3

Actual mass NaOH added:_______________g (if you skipped this use lab 1&2 values)
Volume marked on Storage Bottle: _________ L (if you skipped this use lab 1&2 values)
Expected M NaOH:___________M (if you skipped this use lab 1&2 values)
Purity of KHP:_______________%
Actual KHP mass in 100.0 mL:_______g Corrected mass KHP in 100 mL __________g
Molarity of KHP = _______________M

# V KHP Vi NaOH Vf NaOH Vt NaOH Vt NaOH MNaOH

(mL) (mL) (mL) (mL) (mL) corr (mol/L)
B 0 Avg MNaOH s CV
(mol/L) (mol/L) (%)
1 10.00
2 10.00
3 10.00
4 10.00
5 10.00
6 10.00

Table 2. Observations for the Standardization of 0.1 M HCl for Lab #3

Actual volume HCl added:_______________mL (if you skipped this use lab 1&2 values)
Volume marked on Storage Bottle: _________ L (if you skipped this use lab 1&2 values)
Expected M HCl:___________M (if you skipped this use lab 1&2 values)
Purity of Na2CO3:_______________%
Actual Na2CO3 mass in 100.0 mL:_______g
Corrected mass Na2CO3 in 100 mL __________g
Molarity of Na2CO3 = _______________M

Before Boiling After Boiling

# V Na2CO3 Vi1 HCl Vf1 HCl Vi2 HCl Vf2 HCl Vt HCl Vt HCl MHCl
(mL) (mL) (mL) (mL) (mL) (mL) (mL) corr (mol/L)
B NaCl
1 10.00
2 10.00
3 10.00
4 10.00
5 10.00
6 10.00

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CHM 327 Name: ______________________

Average MHCl: _______________(mol/L).

s: _________________(mol/L).
CV: ______________(%)

Workstation/scales clean: _________________________________________

Supplemental Lab Questions: (2 marks) NAME: ___________________________.

(Note you can answer these questions directly on this sheet of paper and submit scanned
PDF with your lab report). Show all work to determine the correct values.

1) Determine the volumes (mL and µL) of a 1.00 M solution of NaOH (MW= 40.00
g/mol) that are required to create the following masses of NaOH.

a) 1 mg

b) 2 mg

c) 5 mg

2) Describe how to manufacture a 1.00 M solution of NaOH in a 100.0 mL volumetric

flask.

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CHM 327 Name: ______________________
Lab #3 Prelab and Flow Chart
Standardization of Common Desk Reagents
To be completed in Lab Notebook:
NOTE: Any information found in a previous experiment ex. Materials or chemicals
please reference the page where this information can be found and include scan with
report of referenced pages.
1) Purpose: Briefly state the purpose of the experiment.
2) Materials/Chemicals: In this section, list any specific equipment that is required,
or chemical information that is important for the lab. (ie. Chemical name, CAS#,
MW, molecular formula, bp, mp, etc. ) Be sure to state the source of your
information.
3) Safety Hazards and Precautions: In this section, list any safety hazards that might
arise in the lab, including from chemicals or equipment. (hint: most of this
information is found in the chemical SDS.)
4) Balanced Equations: In this section include balanced equation for all reactions
involved in the experiment. For lab 3 this includes (NaOH and KHP) and (HCl
and Na2CO3).
5) Required Values from Lab 2: In this section include the target mass of NaOH in
(g) and target volume of HCl in (mL).
6) Calculations: In this section include all calculations for standards and reagents
required to begin the experiment. Be sure to show all work! For lab 3 complete
the following calculations:
A) Calculate the target mass (g) of KHP (MW = 204.22 g/mol) to produce a
100.0 mL solution which 10.00 mL aliquot requires ~15 mL volume of 0.1
M NaOH.
B) Calculate the target mass (g) of Na2CO3 (MW = 105.989 g/mol) to
produce a 100.0 mL solution which 10.00 mL aliquot requires ~15 mL
volume of 0.1 M HCl.
7) Flowchart: Construct a flowchart for the lab. This should NOT be a reproduction
of the manual, but instead a graphical summary of the major steps. (NOTE: Do
not rewrite procedure word for word.)

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CHM 327 Name: ______________________
Lab #3 - Standardization of Common Desk Reagents

Laboratory Report Requirements (Total 20 marks for Report)

NOTE: Original data must be submitted with your lab report!!!!!

Lab Report Format (2 marks)

- Title Page: Title of the experiment (center of page); At the bottom right: Your name,
course and section, date of experiment.
- Headings: Each section is clearly defined with the heading that is bolded or
underlined. (Purpose, Theory, Results, Discussion, etc..)
- Figures and Tables: Must be formatted in ACS style. Each table must have a # and
title at the top, and each figure will have a #, title and legend at the bottom. Include
references if they are not your own work.
- Spelling & Grammar: Text must be written in sentence format with proper spelling
and grammar.
- References: Cite all information throughout report with a superscripted number
corresponding to the source included in the reference section, in ACS format.

Purpose (0.5 marks)

- State the solutions to be standardized and the method(s) referenced.

Theory (3 marks)
- Give all reaction equations and explain the reactions in words as well.
- Compare the standardization procedures employed for Lab #2 to Lab #3 (how
are the procedures different, advantages, disadvantages).
- Describe a t-test for comparison of two experimental means and its application
to this experiment. (See 5B-2 in textbook and example 5-6).
- Reference all work!

Results (6 marks)
- Reproduce Tables 1 and 2 that were filled in during the experiment (include all
data from titrations, molarities, avg., s and CV for both NaOH and HCl solutions).
- Produce Table 3 to contrast and compare results from Lab 1&2 and Lab #3 (mean
concentrations, values for s and CV). Include results of the t-test in Table 3.

- Give calculations for:

o MNaOH and MHCl from titration 1.
o Average MNaOH.
o s for MNaOH .
o CV for MNaOH.
o Q-test of potential outliers.
o T-test for data from Lab #1&2 and Lab #3 for both standard solutions.

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CHM 327 Name: ______________________
Discussion (4 marks)
- Discuss the indication of precision associated with Lab 1&2 and compare to the
precision observed for Lab #3 (s and CV), which method was more precise and
why? State actual values of s and CV and discuss what these values mean.
- Discuss the results of the t-test of Lab 1&2 and Lab #3 data, what do the results
tell you, state actual t-values and tcrit for each.
- Discuss at least 3 possible sources of error that could account for any differences
in your results from Lab 1&2 and Lab #3. What improvements could you make to
the procedure to help minimize these errors?
- List an application for each of the standard solutions prepared during this
experiment.

Conclusion (0.5 marks)

- State the average molarities and s values of the standard solutions found after
performing Lab #3.

Questions (2 marks)

Notebook: Prelab and Flow Chart (2 marks)

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CHM 327 Name: ______________________
Lab #4
Determination of Acidity and Alkalinity in a Water Sample

Method References: Standard Methods 2310B and 2320B

Safety: This laboratory involves the production and use of extremely corrosive
substances. The use of personal protective equipment including gloves, lab coat, proper
footwear and safety glasses is necessary.

Method Summary: The production and use of HCl and NaOH standard solutions is a
common practice for most analytical laboratories. This laboratory uses solutions made in
Lab 1&2 and Lab #3 to determine the acidity and alkalinity in water samples. The HCl
and NaOH standard solutions are re-standardized before titrating the unknown samples
for acidity and alkalinity. As in the Standard Methods, alkalinity and acidity is expressed
in terms of mg/L CaCO3.

Apparatus and Reagents

Standard HCl, NaOH, KHP and Na2CO3 primary standard solutions from Lab #2 and #3.
Phenolphthalein indicator and bromocresol green indicator
250 mL conical flasks.
Beakers to hold standard solutions, waste and deionized water
Wash Bottle (containing H2OD)
Glass storage bottles (2) for samples
50 mL burette
10 and 15 mL volumetric pipettes, Pasteur pipettes
Unknown water samples

Part A: Only complete if necessary!!

(Ex. You have to make a new 0.1 M NaOH solution if you ran out from Lab 1&2 and Lab 3 or
if t-test failed and you need to confirm which concentration is correct)

Procedure: Standardization of 0.1 M NaOH

1. Produce a 0.15 M KHP (MW = 204.22 g/mol) solution diluted to 100.0 mL with H2OD
(weigh KHP to nearest 0.1 mg).
2. Pipette 10.00 mL of primary standard KHP into three separate labeled conical flasks (do a
blank). Record all observations in Table 1.
3. Dilute the primary standard solution to 50 mL with deionized water.
4. Add the required amount of phenolphthalein indicator to each flask (2-3 drops).
5. Titrate the contents of each conical flask until titration point is reached remembering to
record all observations in Table 1. Get all Tables initialed by the instructor.

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CHM 327 Name: ______________________
Part B: Only complete if necessary!!
(Ex. You have to make a new 0.1 M HCl solution if you ran out from Lab 1&2 and Lab 3 or if
t-test failed and you need to confirm correct concentration)
Procedure: Standardization of 0.1 M HCl
1. Produce a 0.075 M Na2CO3 (MW = 105.989 g/mol) solution diluted to 100.0 mL with H2OD
(weigh Na2CO3 to nearest 0.1 mg).
2. Pipette 10.00 mL of primary standard Na2CO3 into three separate labeled conical flasks (do
a blank). Record all observations in Table 2.
3. Dilute the primary standard to 50 mL with deionized water (gauge this volume using the
graduations on the conical flask).
4. Add the required amount of bromocresol green indicator to each flask (8-10 drops).
5. Titrate of the contents of each conical flask until titration point is reached remembering to
record all observations in Table 2.

Part C: Determination of Alkalinity in unknown sample! You must complete this part!
Procedure: Determination of Alkalinity with standardized 0.1 M HCl
1. Obtain 100 mL of unknown alkalinity sample in a labeled storage bottle. Record your
unknown number.
2. Pipette 15.00 mL of your unknown sample into four separate labeled conical flasks (at least
four titrations will be required).
3. Dilute each sample aliquot to 50 mL with deionized water (estimate this volume using the
graduations on the conical flask).
4. Prepare a blank using 50 mL of 0.05 M NaCl.
5. Add the required amount of bromocresol green indicator to each flask (3-4 drops).
6. Titrate the solution with your standardized 0.1 M HCl just until the colour begins to change
from blue to green. Boil the solution for one minute (solution should turn blue again, if not
past end-point) then cool the solution in an ice cold water bath for 5 minutes so that it can
be handled safely.
7. Finish the titration of the contents of each conical flask remembering to record all
observations in Table 3. (Indicator should change from blue to green/yellow).

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CHM 327 Name: ______________________
Part D: Determination of Acidity in unknown sample! You must complete this part!
Procedure: Determination of Acidity with standardized 0.1 M NaOH
Obtain 100 mL of unknown acidity sample in a labeled storage bottle. Record unknown #.
1. Pipette 15.00 mL of sample into four separate labeled conical flasks (at least four titrations
will be required). Record all observations in Table 4.
2. Dilute the sample aliquot to 50 mL with deionized water (estimate this volume using the
graduations on the conical flask).
3. Prepare Blank with H2OD.
4. Add the required amount of phenolphthalein indicator to each flask.
5. Titrate the contents of each conical flask with your standardized 0.1 M NaOH. Record all
observations in Table 4.

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CHM 327 Name: ______________________

Lab 4 - Raw Data sheet must be signed by instructor & handed in with Report.

**Only fill in Table 1 if you had to re-standardize your NaOH solution ****

Table 1. Observations for the Re-standardization of 0.1 M NaOH for Lab #4

MNaOH (Lab #3): ________ Purity KHP = ___________
KHP mass (g) in 100.0 mL (Lab #4):_____________ MKHP = _______________

Vt
Vi Vf Vt
V KHP NaOH MNaOH
# NaOH NaOH NaOH
(mL) (mL) (mol/L)
(mL) (mL) (mL)
corr
Avg MNaOH s CV
B 0 (mol/L) (mol/L) (%)
1 10.00
2 10.00
3 10.00
4 10.00

**Only fill in Table 2 if you had to re-standardize your HCl solution ****
Table 2. Observations for the Re-standardization of 0.1 M HCl for Lab #4

MHCl (Lab #3): ____________ Purity Na2CO3 =

__________
Na2CO3 mass (g) in 100.0 mL (Lab #4):______________ MNa2CO3 = ____________

Vt
V Vi1 Vf1 Vi2 Vf2 Vt
HCl MHCl
# Na2CO3 HCl HCl HCl HCl HCl
(mL) (mol/L)
(mL) (mL) (mL) (mL) (mL) (mL)
corr
Avg MHCl s CV
B 0 (mol/L) (mol/L) (%)
1 10.00
2 10.00
3 10.00
4 10.00

**You must fill in Table 3 for your unknown Alkaline sample ****

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CHM 327 Name: ______________________

Lab 4 - Raw Data sheet must be signed by instructor & handed in with Report.

Table 3. Determination of Alkalinity (expressed as ppm (mg/L) of CaCO3) in a

Water Sample using 0.1 M HCl and Bromocresol Green Indicator.
Unknown #: _________. MHCl: _____________.

Vt Mass
Vi1 Vf1 Vi2 Vf2 Vt
Sample V HCl as [CaCO3]
# HCl HCl HCl HCl HCl
(mL) (mL) CaCO3 (mg/L)
(mL) (mL) (mL) (mL) (mL)
corr (mg)
Avg s CV
B [CaCO3] [CaCO3] [CaCO3]
(mg/L) (mg/L) (%)
1
2
3
4
5
6

Sample Calculations:
#moles CaCO3 = MHCl x VHCl x 1 mole CaCO3/2 moles HCl
wt(mg) CaCO3 = molesCaCO3 x MWCaCO3 x 1000 mg/1g
Alkalinity (as CaCO3) = wt(mg) CaCO3 / sample volume (L)

**You must fill in Table 4 for your unknown Acidity sample ****

Table 4. Determination of Acidity (expressed as ppm of CaCO3) in a Water Sample

using 0.1 M NaOH and Phenolphthalein Indicator.
Unknown #: _________. MNaOH: _____________.

Vt Mass
Sample Vi1 Vf1 Vt
NaOH as [CaCO3]
# V NaOH NaOH NaOH
(mL) CaCO3 (mg/L)
(mL) (mL) (mL) (mL)
corr (mg)
Avg s CV
B [CaCO3] [CaCO3] [CaCO3]
(mg/L) (mg/L) (%)
1
2
3
4
5
6
Sample Calculations:
# moles CaCO3 = MNaOH x VNaOH x 1molCaCO3 / 2molNaOH
Wt(mg) CaCO3 = # moles CaCO3 x MW CaCO3
[CaCO3] mg/L = wt(mg) CaCO3/ sample volume (L)

Workstation/scales clean: _________________________________________

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CHM 327 Name: ______________________

Lab #4 Prelab and Flow Chart

Determination of Acidity and Alkalinity in a Water Sample
To be completed in Lab Notebook:
NOTE: Any information found in a previous experiment ex. Materials or chemicals
please reference the page where this information can be found and include scan with
report of referenced pages.
1) Purpose: Briefly state the purpose of the experiment.
2) Materials/Chemicals: In this section, list any specific equipment that is required,
or chemical information that is important for the lab. (ie. Chemical name, CAS#,
MW, molecular formula, bp, mp, etc.) Be sure to state the source of your
information.
3) Safety Hazards and Precautions: In this section, list any safety hazards that might
arise in the lab, including from chemicals or equipment. (Hint: most of this
information is found in the chemical SDS.)
4) Balanced Equations: In this section include balanced equation for all reactions
involved in the experiment. For lab 4 this includes (NaOH and H2CO3) and (HCl
and CaCO3).
5) Calculations: In this section include all calculations for standards and reagents
required to begin the experiment. Be sure to show all work! For lab 4 complete
the following calculations:
A) Mass of KHP to produce a 0.15 M KHP (MW = 204.22 g/mol) solution
diluted to 100.0 mL with H2OD.
B) Mass of Na2CO3 to produce a 0.075 M Na2CO3 (MW = 105.989 g/mol)
solution diluted to 100.0 mL with H2OD .
6) Flowchart: Construct a flowchart for the lab. This should NOT be a reproduction
of the manual, but instead a graphical summary of the major steps. (NOTE: Do
not rewrite procedure word for word.)

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CHM 327 Name: ______________________

Lab #4
Determination of Acidity and Alkalinity in a Water Sample

Laboratory Report Requirements (Total 26 marks → 16 for Report and 10 for Accuracy)

Lab Report Format (2 marks)

- Title Page: Title of the experiment (center of page); At the bottom right: Your name,
course and section, date of experiment.
- Headings: Each section is clearly defined with the heading that is bolded or
underlined. (Purpose, Theory, Results, Discussion, etc..)
- Figures and Tables: Must be formatted in ACS style. Each table must have a # and
title at the top, and each figure will have a #, title and legend at the bottom. Include
references if they are not your own work.
- Spelling & Grammar: Text must be written in sentence format with proper spelling
and grammar.
- References: Cite all information throughout report with a superscripted number
corresponding to the source included in the reference section, in ACS format.

Purpose (0.5 marks)

• State the analytical targets, unknown numbers and the methods referenced.

Theory (3 marks)
• Give all reaction equations, explain what is happening in words.
• Explain why acidity and alkalinity are important measurements in environmental samples.
• Describe the sources of alkalinity and acidity in surface waters.
• Reference all work!

Results (4 marks)
• Reproduce Tables 3 and 4 (and 1 and 2 if applicable).
• Give sample calculations for:
o Q-test of potential outlier (must show example of one).
o Alkalinity from titration 1 (Table 3) (all calculations to determine [CaCO3])
o Acidity from titration 1 (Table 4) (all calculations to determine [CaCO3])
o Avg alkalinity [CaCO3].

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CHM 327 Name: ______________________

Discussion (4 marks)
• State your results (Avg CaCO3 +/- s for each water sample and CV), discuss what
these results mean (s and CV) and possible sources of error that could contribute
to potential error in your unknown mass for alkalinity and acidity.
• Suggest 2 improvements that could be made to the experiment to improve your results.
• Discuss what the limit of detection means and explain how it could be calculated for the
standard solutions.
• Compare the acidity and alkalinity concentrations found in the samples to the
acidity and alkalinity found in other common waters such as drinking water and
surface waters like the Great Lakes, Detroit River, etc. (cite references).

Conclusion (0.5 marks)

• State unknown numbers, acidity and alkalinity concentrations in terms of CaCO3
mg/L +/- s.

Notebook: Flow Chart and Prelab (2 marks)

NOTE: All initialed tables and your flow chart must be stapled to the back of your lab.

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CHM 327 Name: ______________________

Lab #5
Hardness of Water by Complexometric (EDTA) Titration
Method References: Standard Method 2340 C
Fund. of Anal. Chem., 9th edition, Method 38 E

Safety: This laboratory involves the production and use of extremely corrosive
substances. The use of local exhaust (fume hood) and personal protective equipment
such as gloves, lab coat and safety glasses is necessary. Buffer and concentrated
solutions such as hydrochloric acid and ammonium hydroxide must be dispensed under
local exhaust conditions.

Method Summary: The need to determine water hardness is very common where water
boiling takes place in large industrial scale. This method uses a standard 0.01 M EDTA
solution to chelate calcium in aqueous solution that has been buffered to pH 10. The
indication of titration point is accomplished by using Eriochrome Black T indicator.
Water hardness is reported in terms of milligrams CaCO3 per liter of sample.

Apparatus and Reagents:

Conc ammonium hydroxide (15.4 M NH4OH) ,ACS ammonium chloride (NH4Cl)
Buffer solution – make 100 mL (add 5.7 mL NH4OH and 0.7 g NH4Cl to 0.1 L H2OD)
10 mL graduated cylinder and Pasteur pipette to distribute 2.0 mL of buffer
ACS grade disodiumethylenediaminetetraacetic acid dehydrate (Na2H2Y.2H2O or EDTA)
Conc HCl (12 M HCl) and Pasteur pipette to distribute drops of acid
1 M NaOH and Pasteur pipette to distribute drops of reagent
ACS grade calcium carbonate (CaCO3) Purity CaCO3 = _______ %
Eriochrome Black T indicator (in ethanolamine and absolute ethanol) prepare FRESH
Beakers to contain standard solutions, H2OD, waste, conc HCl, buffer and samples
250 mL conical flasks (four are required)
50.00 mL burette, 10.00 mL and 15.00 mL volumetric pipettes
100 mL graduate cylinder to measure sample (tap water and unknown) volumes
250.0 mL capacity volumetric flasks (two are required) and 60o funnels to prepare the
EDTA and CaCO3 solutions in H2OD from solid reagent.

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CHM 327 Name: ______________________

Preparation of 0.01 M EDTA Solution:

1) Create this solution by weighing the required amount of ACS grade EDTA
(weighed by difference) to the nearest 0.1 mg into a 250.0 mL volumetric flask.
Record the actual mass into Table 1.

Target Mass: (EDTA) Na2H2Y.2H2O:_____________ g

(MW = 372.240 g/mol)

2) Half-fill the flask with H2OD.

3) To aid in getting the EDTA solid into aqueous solution only if necessary, add,
dropwise, 1 M NaOH into the continuously swirled volumetric flask contents until
all of the EDTA has dissolved.

4) Make to volume with H2OD.

Preparation of Standard Calcium Carbonate Solution:

5) Calculate the required molarity of CaCO3 if 15 mL of CaCO3 requires 15 mL of
0.01 M Na2H2Y.2H2O to reach the end point.
Required M:___________M CaCO3 (MW = 100.087 g/mol)

6) Using the molarity calculated in step 1, calculate the mass of CaCO3 that would
be required to make a 250.0 mL solution. Weigh out the required mass by
difference to the nearest 0.1 mg. Enter mass into Table 1.
Target Mass: _________g CaCO3 required to make standard solution in a 250.0
mL volumetric flask.

To produce a standard solution of calcium carbonate in 250.0 mL, carbonate must first be
expelled from the solution. Perform this task as follows:
7) Place the calculated mass of CaCO3 required in a 250.0 mL volumetric flask.

8) Half-fill the 250.0 mL the volumetric flask with H2OD.

9) Add 2 drops of conc HCl (carefully!) and swirl. Continue to add conc HCl
(carefully!) with swirling until all of the CaCO3 has dissolved.

10) Make to volume with H2OD.

Procedure: Standardization of 0.01 M EDTA

1. Place 0.01 M EDTA solution in a 50.00 mL burette.

2. Pipette 15.00 mL of standard CaCO3 into four separate labeled conical flasks (at
least four titrations will be required). Record all observations in Table 1.

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CHM 327 Name: ______________________
3. Dilute the primary standard aliquot to 100 mL with deionized water (gauge this
volume using the graduations on the conical flask).

4. Complete steps 5-7 within 5 minutes on each flask individually.

(Do one flask at a time!!!)

5. Starting with E-flask 1, use a Pasteur pipette to transfer 2.0 mL of buffer solution
(use a 10 mL graduated cylinder to measure).

6. Add the required amount of Eriochrome Black T indicator to E-flask 1.

7. Titrate the contents of E-flask 1 until titration point is reached (stop when solution
is a light blue with no traces of red or purple).

8. Perform steps 5-7 on the next flask. Enter all values in Table 1.

9. Do a blank (blank = 100 mL H2OD, 2.0 mL buffer and indicator).

Procedure: Determination of Hardness of Water by EDTA Titration

1. Place standard 0.01 M EDTA in the burette. Assay solutions include tap water
and an unknown (record your unknown # at the top of Table 2). Record all
observations in Table 2.

2. Using a 100 mL graduated cylinder transfer 100.0 mL of tap water (NOT H2OD)
into four separate labeled conical flasks (titration of at least four replicates will be
required). Solutions should be at room temperature when volume is measured.

Complete the next 3 steps within 5 minutes on each flask individually.

3. Use a Pasteur pipette to transfer 2.0 mL (use a 10 mL graduated cylinder to
measure) of buffer solution to the E-flask.

4. Add the required amount of Eriochrome Black indicator to the E- flask.

5. Titrate the contents of the E-flask with 0.01 M EDTA until titration point is
reached. Record all observations in Table 2.

6. Continue steps 3-5 on each E-flask until all titrations are complete.

7. Using a 25.0 mL graduated cylinder transfer 25.0 mL of your unknown into four
separate labeled conical flasks. Add enough H2OD (NOT tap water) to make total
volume 100 mL gauging volume of flask.

8. Repeat steps 3-5 on each Flask until all titrations are complete.

9. Get Tables 1 and 2 initialed before you leave the laboratory.

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CHM 327 Name: ______________________

Lab 5 - Raw Data sheet must be signed by instructor & handed in with Report.

Table 1. Observations for the Standardization of 0.01 M EDTA for Lab #5

Purity EDTA: ___________% Purity CaCO3:________%
Actual Mass EDTA:___________ g Mass CaCO3:____________g
Corrected Mass EDTA:__________ g Corrected Mass CaCO3:_________ g
Expected M EDTA_____________M Molarity CaCO3: ____________ M

V Vi Vf Vt Vt EDTA M
CaCO3 EDTA EDTA EDTA (mL) corr EDTA
(mL) (mL) (mL) (mL) (mol/L)
#
B 0 Avg M EDTA s CV
(mol/L) (mol/L) (%)
1 15.00
2 15.00
3 15.00
4 15.00
5 15.00
6 15.00

Table 2. Observations for Hardness of Water in Tap Water and Unknown #_____
NOTE: RECORD ALL OBSERVARTIONS IN INK PEN
Sample # Vs Vi Vf Vt Vt Mass [CaCO3] Avg s CV
and ID (mL) EDTA EDTA EDTA EDTA CaCO3 (mg/L) [CaCO3] (mg/ (%)
(mL) (mL) (mL) (mL) (mg) (mg/L) L)
corr
1 TW 100
2 TW 100
3 TW 100
4 TW 100
5 TW 100
1 Unk 25.0
2 Unk 25.0
3 Unk 25.0
4 Unk 25.0
5 Unk 25.0
MEDTA (from Table 1):________________

Workstation/scales clean: _________________________________________

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CHM 327 Name: ______________________

Supplemental Lab Questions:

1) Calculate the volume of 0.0700 M EDTA solution needed to completely react with the
Ca2+ (MW = 40.078 g/mol) in 0.1890 g of CaCO3 (MW = 100.087).

2) An EDTA solution was prepared by dissolving 17.990 g of Na2H2EDTA.2H2O (MW =

372.240 g/mol) in 1.000 L of deionized water. What was the expected molarity of the
EDTA solution?

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CHM 327 Name: ______________________

Lab #5 Prelab and Flow Chart

Hardness of Water by Complexometric (EDTA) Titration
To be completed in Lab Notebook:
1) Purpose: Briefly state the purpose of the experiment.
2) Materials/Chemicals: In this section, list any specific equipment that is required,
or chemical information that is important for the lab. (ie. Chemical name, CAS#,
MW, molecular formula, bp, mp, etc. ) Be sure to state the source of your
information.
3) Safety Hazards and Precautions: In this section, list any safety hazards that might
arise in the lab, including from chemicals or equipment. (hint: most of this
information is found in the chemical SDS.)
4) Balanced Equations: In this section include balanced equation for all reactions
involved in the experiment. For lab 5 this includes (Ca2+ and EDTA).
5) Calculations: In this section include all calculations for standards and reagents
required to begin the experiment. Be sure to show all work! For lab 5 complete
the following calculations:
A) Calculate the required amount of ACS grade EDTA (weighed by
difference) to prepare a 0.01 M EDTA solution in a 250.0 mL volumetric
flask.
B) Calculate the required molarity of CaCO3 if 15 mL of CaCO3 requires 15
mL of 0.01 M Na2H2Y.2H2O to reach the end point.
C) Using the molarity calculated in question 2, calculate the mass of CaCO3
that would be required to make a 250.0 mL solution.
6) Flowchart: Construct a flowchart for the lab. This should NOT be a reproduction
of the manual, but instead a graphical summary of the major steps. (NOTE: Do
not rewrite procedure word for word.)

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CHM 327 Name: ______________________

Lab #5 - Hardness of Water by Complexometric (EDTA) Titration

Laboratory Report Requirements (Total 30 marks; 20 for Report + 10 for Accuracy)

Lab Report Format (2 marks)

- Title Page: Title of the experiment (center of page); At the bottom right: Your name,
course and section, date of experiment.
- Headings: Each section is clearly defined with the heading that is bolded or
underlined. (Purpose, Theory, Results, Discussion, etc..)
- Figures and Tables: Must be formatted in ACS style. Each table must have a # and
title at the top, and each figure will have a #, title and legend at the bottom. Include
references if they are not your own work.
- Spelling & Grammar: Text must be written in sentence format with proper spelling
and grammar.
- References: Cite all information throughout report with a superscripted number
corresponding to the source included in the reference section, in ACS format.

Purpose (0.5 marks)

• State the analytical targets, unknown numbers and the methods referenced.

Theory (5 marks)
• Explain what hard water is, how it is caused and the minerals that may be
present.
• Explain the difference between temporary and permanent hardness.
• Describe how water is softened by ion exchange.
• Explain what complexometric titrations are and why EDTA is used as the titrant.
• Use structures to show the reaction equation that occurs during this experiment
(between Ca2+ and EDTA).
• Reference all work!

Results (4 marks)
• Reproduce Tables 1 and 2.
• Give sample calculations for:
o Determine the limit of detection (LOD) (as mg CaCO3.) Assume 1 drop is
smallest volume that can be delivered (0.05 mL).
o Calculate MCaCO3 standard and theoretical MEDTA from actual mass.
o MEDTA from Titration #1 in Table 1.
o % difference between theoretical MEDTA (calculate from the mass you
weighed out and volume – show work) and experimental average MEDTA
(from titration data).
o Mass (mg) CaCO3 from first titration in Table 2 (show all work to get to
this value).
o CaCO3 concentration (mg/L) for first titration for each sample type (water
and unknown) in Table 2.
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CHM 327 Name: ______________________
Discussion (4 marks) (** For full marks you must state actual values from lab***)
• Comment and explain any differences observed between the expected
(calculated) and the observed molar concentration found for the EDTA solution,
provide possible sources of error.
• Explain how the indicator works, why a blank correction is necessary, and why
we have to add buffer to the solution.
• Discuss the indication of precision (s value and CV) associated with Lab #5.
Compare CV associated with the average molarity found for the standard
solution in Lab #5 (EDTA) to CV observed for NaOH and HCl standardizations (Lab
#2 & 3). (Which standardization is the most/least precise? Explain why)
• Comment on the hardness value found for tap water. What are some common
hardness values? Compare the expected hardness value for Essex County tap
water (cite references) to the hardness found in the tap water and unknown.

Conclusion (0.5 marks)

• State the unknown(s) identity, the molarity of the EDTA solution +/- s, the water
hardness as mg CaCO3/L +/- s in tap water and in the unknown.

Notebook: Flow Chart and Prelab (2 marks)

Supplemental Lab Questions (2 marks)

NOTE: All initialed and rough data sheets (tables), flow chart and questions must be
submitted with your lab.

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CHM 327 Name: ______________________
Lab #6
Fajans Chloride
Method References: Fund. of Anal. Chem., 9th edition, Method 37 B

Safety: This laboratory involves the production and use of corrosive substances. The use
of personal protective equipment such as gloves, lab coat and safety glasses are
necessary. Follow instructions regarding waste handling and disposal.

Method Summary: The determination of chloride can easily be determined by

precipitating it with silver nitrate standard solution on a finely divided solid such as
dextrin. Typically, a 0.1 M solution of silver nitrate solution is standardized with ACS
grade NaCl standard solution and then is employed to precipitate chloride in an aqueous
solution containing dextrin. After reacting all chloride ion with standard AgNO3, titration
end-point is reached when one drop of excess Ag+ reacts with fluorescein indicator.
Concentration of chloride in a water-soluble powder is expressed in percent +/- s.

Apparatus and Reagents

Dichlorofluorescein indicator
ACS silver nitrate (AgNO3)
ACS NaCl
Dextrin
50 mL burette, burette clamp and retort stand
250 mL Erlenmeyer flasks
Beakers to hold solutions and deionized water
10.00 mL volumetric pipette 100.0 mL volumetric flask 250.0 mL volumetric flask

Preparation of 0.1 M AgNO3 Solution

Create this solution by weighing ACS grade AgNO3 (MW = 169.873 g/mol) to the
nearest 0.1 mg and transferring it into an appropriately sized volumetric flask (make this
solution in a 250.0 mL volumetric flask and store it if necessary in an amber bottle).
Target Mass (g) AgNO3:________________________

Preparation of 0.1 M Sodium Chloride Standard Solution for AgNO3

Standardization

Create the solution by weighing ACS grade NaCl (MW = 58.443 g/mol) to the nearest
0.1 mg and transferring it into 100.0 mL volumetric flask.
Target Mass (g) NaCl: ______________ for a 100.0 mL capacity volumetric flask

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CHM 327 Name: ______________________
Preparation of Unknown Sample Solution for Percent Chloride Determination
Create the solution by weighing the water-soluble powder to the nearest 0.1 mg and
transferring it into a 100.0 mL volumetric flask. Sample target mass (g) is the same as
pure NaCl mass (g) used for standardization.
Target Mass (g) Sample: ______________ for a 100.0 mL capacity volumetric flask

Procedure: Standardization of 0.1 M AgNO3

1. Place the AgNO3 solution to be standardized into a 50 mL burette.
2. Pipette into labeled 250 mL Erlenmeyer flasks 10.00 mL of NaCl standard
solution (NOTE: ~10 mL of a 0.1 M AgNO3 solution should be required to reach
titration point). At least six titrations will be required.
3. Dilute the standard NaCl solution in each flask to the 100 mL mark on the E-flask
using deionized water.
4. One flask at a time, add 4 drops of the indicator solution (dichlorofluorescein)
and roughly 0.1 g of dextrin to the NaCl solution (no need to weigh the dextrin-
estimate 0.1 g on the end of a spatula). NOTE: Do not add indicator or dextrin to
next flask until previous titration complete!!)
5. Immediately titrate the contents with the 0.1 M AgNO3 solution until the first
permanent appearance of the pink color of the indicator.
6. Read the buret volume to 0.01 mL. Record all observations in Table 1. Have
Table 1 initialed by the instructor at the end of the lab.
7. Repeat steps 4-6 five more times for a total of six titrations.
8. Prepare a Blank (100 mL H2OD, ~0.1 g Dextrin do not weight, 4 drops of
indicator), titrate with AgNO3.
9. If time permits, calculate the average AgNO3 molarity and standard deviation.

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CHM 327 Name: ______________________
Procedure: Determination of Soluble Chloride in an Unknown
1. Place standard AgNO3 into a 50 mL buret.
2. Pipette into labeled 250 mL Erlenmeyer flasks 10.00 mL of Unknown Sample
solution. At least six titrations will be required.
3. Make the solution up to the 100 mL graduation on the E-flask using H2OD.
4. One flask at a time, add 4 drops of the indicator solution (dichlorofluorescein) and
roughly 0.1 g of dextrin (no need to weigh the dextrin) to the NaCl solution.
5. Immediately titrate the contents with the 0.1 M AgNO3 solution until the first
permanent appearance of the pink color of the indicator.
6. Read the buret volume to 0.01 mL. Record all observations in Table2. Hand in
Table 2 to the instructor at the end of the lab.
7. Repeat steps 4-6 five more times for a total of six titrations.
8. If time permits, calculate the average % Cl- in the powder +/- s or [NaCl] in
solution (mg/L).

Time saving Tip:

Start preparing crucibles for Lab 7&8 if time permits.
(see page 45 Part A of Lab 7&8).

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 CHM 327 Name: ______________________
Lab 6 - Raw Data sheet must be signed by instructor & handed in with Report.

Table 1. Standardization of 0.1 M AgNO3

Mass AgNO3:_______________g Expected MAgNO3:_____________M
% Purity NaCl _________________%
NaCl mass in 100.0 mL: ______________g Corrected Mass NaCl:___________g
MNaCl = _______________M

VNaCl Vi AgNO3 Vf AgNO3 Vt AgNO3 Vt AgNO3 MAgNO3

#
(mL) (mL) (mL) (mL) (mL) corr (mol/L)

B 0 Avg MAgNO3 CV
s (mol/L)
(mol/L) (%)
1 10.00
2 10.00
3 10.00
4 10.00
5 10.00
6 10.00

Calculated MAgNO3:____________ MAgNO3 = MNaCl x 10.00 / Vt(mL corr)

Table 2. Titration of Soluble Chloride

Unknown sample mass (g) in 100.0 mL:____________g
Calculate unknown sample mass (g) in 10.00 mL = ____________g

# Vsample Vi AgNO3 Vf AgNO3 VtAgNO3 Vt AgNO3 Chloride Chloride Avg Cl- +/- S CV
(mL) (mL) (mL) (mL) (mL) corr Mass(g) (%) (%) (%) (%)
B 0
1 10.00
2 10.00
3 10.00
4 10.00
5 10.00
6 10.00

Average MAgNO3:_________________ (from Table 1 standardization data)

Chloride Mass (g) = MAgNO3 x Vt(L corr) x 35.453 g/mol Cl- % = Chloride Mass (g) / Sample mass (g) in 10.00 mL x 100 %

Workstation/scales clean: _________________________________________

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CHM 327 Name: ______________________
Supplemental Lab Questions:
1. Calculate the concentration of KCl (MW = 74.551g/mol) so that 17.00 mL
of this solution would require 18.22 mL of 0.10 M AgNO3 to reach
titration point. What mass of KCl was required to produce 250.0 mL of
this solution?

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CHM 327 Name: ______________________
Lab #6 Prelab and Flow Chart
Fajans Chloride
To be completed in Lab Notebook:
1) Purpose: Briefly state the purpose of the experiment.
2) Materials/Chemicals: In this section, list any specific equipment that is required,
or chemical information that is important for the lab. (ie. Chemical name, CAS#,
MW, molecular formula, bp, mp, etc. ) Be sure to state the source of your
information.
3) Safety Hazards and Precautions: In this section, list any safety hazards that might
arise in the lab, including from chemicals or equipment. (hint: most of this
information is found in the chemical SDS.)
4) Balanced Equations: In this section include balanced equation for all reactions
involved in the experiment. For lab 8 this includes (AgNO3 and NaCl).
5) Calculations: In this section include all calculations for standards and reagents
required to begin the experiment. Be sure to show all work! For lab 8 complete
the following calculations:
A) Calculate the mass of AgNO3 (MW = 169.873 g/mol) required to produce
a 0.1 M AgNO3 solution in a 250.0 mL volumetric flask.
B) Calculate the mass of NaCl (MW = 58.443 g/mol) required to produce a
0.1 M NaCl standard solution in a 100.0 mL volumetric flask.
6) Flowchart: Construct a flowchart for the lab. This should NOT be a reproduction
of the manual, but instead a graphical summary of the major steps. (NOTE: Do
not rewrite procedure word for word.)

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CHM 327 Name: ______________________
Lab #6 - Fajans Chloride

Laboratory Report Requirements (Total 25 marks; 20 for Report + 5 Accuracy Marks)

Lab Report Format (2 marks)

- Title Page: Title of the experiment (center of page); At the bottom right: Your name,
course and section, date of experiment.
- Headings: Each section is clearly defined with the heading that is bolded or
underlined. (Purpose, Theory, Results, Discussion, etc..)
- Figures and Tables: Must be formatted in ACS style. Each table must have a # and
title at the top, and each figure will have a #, title and legend at the bottom. Include
references if they are not your own work.
- Spelling & Grammar: Text must be written in sentence format with proper spelling
and grammar.
- References: Cite all information throughout report with a superscripted number
corresponding to the source included in the reference section, in ACS format.

Purpose (0.5 marks)

• State the target (chloride), unknown number, and the method(s) referenced.

Theory (4 marks)
• Describe the Fajans chloride method.
• Explain the purpose of adding dextrin to your samples before titrating.
• With the aid of an illustration, describe how an adsorption indicator works and
relate it to how dichlorofluorescein works in this experiment.
• Explain what adsorption and occlusion coprecipitation is, how can they be
avoided and the types of errors that can occur. Provide an example of how each
may occur during precipitation in the Fajans chloride method.
• Include all references.

Results (5 marks)
Reproduce Table 1 and Table 2.
• Give sample calculations for:
o Expected MAgNO3 from corrected mass.
o MNaCl standard solution from mass weighed out.
o MAgNO3 from first titration of 10.00 mL pure NaCl aliquot.
o % Difference between experimental and expected M AgNO3.
o Mass (g) chloride from first titration of 10.00 mL unknown aliquot.
o Sample mass (g) in 10.00 mL aliquot of unknown solution.
o Percent chloride from first titration of 10.00 mL unknown aliquot.

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CHM 327 Name: ______________________
Discussion (4 marks)
• Describe two advantages and two disadvantages for the Fajans method for
chloride determination.
• Discuss two possible reasons for the % difference observed between the
calculated and observed MAgNO3 (State value of your % difference calculated).
• Discuss the indication of precision of % Cl- associated with Lab #6 and compare
to the CV of another titration lab you have completed (be specific state and
compare the s and CV values that you observed). Which method was more
precise? Why do you think this was?
• State the value of %Cl obtained and two possible sources of error.

Conclusion (0.5 marks)

• State the unknown number, the MAgNO3 average/s value as well the % Cl-
average/s value found for the unknown.

Questions (2 marks)

Notebook: Flow Chart and Prelab (2 marks)

You must submit all initialed data sheets, questions and flow with lab report, or you
will lose marks!!!

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CHM 327 Name: ______________________
Lab #7&8
Chloride by Gravimetric Analysis
Method References: Fund. of Anal. Chem., 9th edition, Method 38 B

Safety: This laboratory involves the production and use of extremely corrosive
substances as well as objects that are extremely hot. The use of local exhaust (fume
hood) and personal protective equipment such as gloves, lab coat and safety glasses are
necessary. Use oven m

itt(s) and/or extended tongs for hot objects. Place crucibles on the bench top to cool to
room temperature before weighing. Concentrated solutions such as ammonium
hydroxide and nitric acid should be dispensed under local exhaust conditions. Follow
instructions regarding waste handling and disposal. Take special care to use the proper
vacuum flask and crucible holder. Always break vacuum (slowly) at its source before
removing crucibles from the holder.

Method Summary: The determination of percent chloride in a water-soluble solid can

easily be determined by gravimetric analysis. The procedure involves using an excess of
0.2 M silver nitrate solution to precipitate chloride ion in an acidic aqueous medium and
heating to boiling for 60 minutes. After filtering the solution through a medium porosity
sintered glass crucible, the captured silver chloride precipitate is washed thoroughly,
dried and weighed. The chloride mass found in a sample can be corrected by dividing it
by the recovery of chloride observed from Laboratory Fabricated Blank (LFB) solutions
that contain a known mass of chloride. Chloride in aqueous samples can be reported as a
mass or in terms of a concentration in milligrams of chloride per liter of water. The
soluble salt concentration can be expressed in terms of % chloride or in % sodium
chloride.

Apparatus and Reagents

6 M HNO3 (prepared by stock room)
6 M NH4OH (prepared by stock room)
0.2 M AgNO3
ACS NaCl (purity = _______%)
400 mL beakers for digestion (6 total required)
1 L beakers for holding crucibles
6 glass stirring rods
Hot plate
500 mL vacuum flask with vacuum hose, retort stand, clamp for flask, rubber vac ring
6 medium porosity sintered glass crucibles and crucible holder
Hot air oven capable of heating to 110oC
Two 250.0 mL volumetric flasks with two 60o funnels
Two weigh bottles to contain pure NaCl and unknown (store in desiccator)

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CHM 327 Name: ______________________
Part A: Preparation of Sintered Glass Crucibles (Week 1)

1. Place a labeled medium porosity sintered glass crucible on a crucible holder that
is fitted on a filter flask. (Label crucible with a lab marker if necessary. Do not
use masking tape. Remove any masking tape if present.

2. Alternately place ~5 mL of nitric acid rinse reagent and ~ 5mL NH4OH rinse
reagent in the crucible (do not add next wash reagent until all the previous wash
reagent has filtered through and you switch to the correct filter flask). Do this
procedure three times. Use separate filter flasks – one marked ACID the other
labeled BASE. Do this procedure in a fume hood if there is room to do so.

3. Rinse each the crucible three times with ~5 mL tap water.

4. Repeat steps 2 and 3 until all crucibles have been rinsed. (6 in total)

5. Place the crucibles in a staggered fashion in a labeled 1 L capacity beaker and dry
for one hour at 110oC.

6. Proceed to Part B, C and D while waiting for crucibles to dry!

7. After the crucibles have cooled to room temperature, weigh them to the nearest
0.1 mg or place them in a desiccator until they can be weighed later.

Part B: Preparation of 0.2 M AgNO3 Solution (Week 1)

Create this solution by weighing ACS grade AgNO3 (MW = 169.873 g/mol) to the
nearest 0.01 g and transferring it into an appropriately sized beaker for dilution (measure
volume using graduations on the side of the beaker). You will need ~ 200 mL of 0.2 M
AgNO3.
Target Mass AgNO3:________________________g
Mass AgNO3:_______________g
Calculated M AgNO3:_______________M

Part C: Preparation of 1.0 mg/mL Chloride (MW = 35.453 g/mol) Standard Solution
for Laboratory Fabricated Blank (LFB) (Week 1)
Create the solution by weighing ACS grade NaCl (MW = 58.443 g/mol) to the nearest
0.1 mg and transferring it into an appropriately sized volumetric flask (250.0 mL) for
dilution.
Target Mass (g) NaCl: _____________ g.
Purity NaCl = _________%
Weighed mass NaCl (g) in 250.0 mL:__________g
Purity corrected mass Cl- (g) in 250.0 mL:__________g

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CHM 327 Name: ______________________
Part D: Determination of Soluble Chloride (Week 1)

1. Preparation of 3 identical unknown sample solutions (SMP1, SMP2 and SMP 3).
a. If your unknown is in a powdered form, create ~ 1 mg/mL chloride
solution in a 250.0 mL volumetric flask, assume unknown chloride sample
is 100 % NaCl. Using a graduated cylinder add 50.0 mL of unknown stock
solution to a 400 mL beaker. Create 3 identical (replicate) samples in total
labelled SMP1, SMP2 and SMP3.
i. Target mass unknown in stock SMP: __________________g.
ii. Actual mass unknown in stock SMP: ______________g.
iii. ~ mass chloride in SMP1, SMP2 and SMP3: ___________mg.

b. If your unknown is a liquid, accurately deliver a calculated volume to

provide ~50 mg chloride into a 400 mL capacity beaker (assume unknown
~ 1 mg/mL chloride). Create 3 identical (replicate) samples labeled
SMP1, SMP2 and SMP3.
i. Target and actual V added to SMP1, SMP 2 and SMP3:______mL.

2. Place a calculated sample mass/volume or volume of your standard chloride

solution (~50 mg chloride) into a properly labeled 400 mL capacity beaker.
Create 3 identical replicate solutions labelled LFB1, LFB2 and LFB3.
a. Target and actual V added to LFB1, LFB2 and LFB3:_____________mL.
b. Expected mass of chloride in LFB1, LFB2 and LFB3._____________ mg.

3. If the solution volumes are not 100 mL, make the solution volume up to the 100
mL graduation on the 6 beakers using deionized water.

4. Add 2 mL of 6 M HNO3 to the contents of each beaker using a 10 mL graduated

cylinder and Pasteur pipette to measure volume (add reagent to 6 beakers total).

5. Slowly, with good stirring using a glass rod, add 5 mL of 0.2 M AgNO3 to each
solution over a 5 minute period until the total volume for complete chloride
precipitation is added. REMEMBER: Complete this step over a time period of about 5
minutes.

6. Add an additional 3 mL of 0.2 M AgNO3 to each solution all at once and stir.

7. Heat solutions to near boiling (~110 °C) to digest solids for at least 10 minutes
(No Stirring).

8. Add a few drops of 0.2 M AgNO3 to each digestate to check for complete
precipitation. If more precipitate forms in a solution, add an additional 3 mL 0.2
M AgNO3 and repeat steps 6 and 7. If precipitation does not occur in the solution,
go to step 9.

9. Heat all four solutions to near boiling for 50 min (or for as long as time permits).
(Finish Preparing 6 medium porosity sintered glass crucibles during this step.)

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CHM 327 Name: ______________________
10. After heating, cool the solutions and cover each beaker with a watch glass. Store
the solutions in the dark until the next lab period, or for a time specified by the
instructor.

Part E: Continuation of Determination of Soluble Chloride (Week 2)

1. Place a tared and properly labeled sintered glass crucible (prepared during
Lab #6 or week 1 of Lab7&8) in a crucible holder on a vacuum filter flask.

2. One solution at a time, decant the supernatant through the labeled crucible (label
must match label on solution). Rinse the precipitate in the bottom of the beaker
with H2OD and filter the rinses through the crucible. Rinse the precipitate from the
beaker into the crucible two more times with H2OD.

3. If necessary, rinse the precipitate that has collected in the crucible with a small
amount of 6 M HNO3.

4. Break vacuum carefully at its source. Remove the crucible from its holder and set
it aside. Discard the filtrate into a waste container if necessary. Reassemble the
filtration apparatus and repeat steps 2 and 3 until all the solutions are filtered.

5. Place all six crucibles in a labeled 1 L capacity beaker. Dry the precipitate at
110oC for one hour. **Complete scale calibration (see Part F) and fill in Table
2 during this time. ***

6. After heating, use beaker tongs to remove the beaker containing the crucibles
from the oven and place the beaker next to the oven. Place the crucibles on the
bench using crucible tongs. After the crucibles have cooled to room temperature,
weigh them to the nearest 0.1 mg or place them in a desiccator until they can be
weighed later.

7. Place crucibles back in the oven for an additional 20 min to ensure all moisture
has been removed. Allow crucibles to cool to room temperature and obtain final
weight. If masses are not constant heat for an additional 10 min if time permits
and obtain final mass.

8. Record all data in Table 1. If time permits, calculate the average recovery
observed in the LFBs, mass chloride, corrected mass sodium chloride, and
corrected % chloride in the sample.

**Clean out crucibles before leaving**. Scrape all AgCl into designated waste
container. Wash each crucible with Sparkling and water. Set up filter flask and rinse each
crucible with the nitric acid rinse solution, to prevent clogging, pull through with
vacuum. Finally, rinse the crucibles with H2OD and pull through with vacuum. Place back
in lockers to dry**

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CHM 327 Name: ______________________
Part F: Analytical Balance Calibration
1. Ensure scale is level (check that bubble in level is in the center if not feet on scale
made need to be adjusted, check with instructor).

2. Ensure balance is clean, use brush to clean inside of scale and pan.

3. Tare balance and ensure that it reads 0.0000 g.

4. Wearing gloves use tweezers to remove 100 mg weight and place in the center of
the balance, close the doors on the balance. Once the balance is stabilized record
all digits in Table 2. (NOTE: Do not touch with your fingers or you will transfer
oils etc. to the weight, and change its mass).

5. Using tweezers remove the mass from the scale, close the doors, and ensure the
balance returns to 0.0000 g, if not Tare balance again.

6. Using tweezers place the 100 mg mass on again, close the doors and when stable
record the mass in Table 2. (Record all digits)

7. Repeat steps 5 and 6, one additional time for the 100 mg weight.

8. Repeat the same process for the 500 mg and 1g masses (three times each).

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CHM 327 Name: ______________________
Lab 7/8 - Raw Data sheet must be signed by instructor & handed in with Report.

Table 1. Observations for Chloride by Gravimetric Analysis - Lab #7/8

1st Dried 2nd Dried corr

Dried
ppt + ppt + Mass
Crucible Mass Mass Recov Avg and s Avg and
Sample crucible crucible chlor % CV
Tare AgCl chloride from recov from s%
ID Mass Mass ide chloride
Mass (g) (g) (g) LFB LFB chloride
(g) (g) (g)
LFB
1
LFB
2
LFB
3
SMP
1
SMP
2
SMP
3

Mass (g) of NaCl in 250.0 mL:______________ Expected Mass (g) Cl- in 50.0 mL LFBs:___________

Mass (g) of sample in 250.0 mL:____________ Mass (g) sample in 50.0 mLs:___________

Table 2: Calibration of Analytical Balance # __________

Standard Observed Average Standard Coefficient % difference

Mass Mass observed deviation of (%)
(g) (g) mass (g) observed Variance
mass (g) (%)

0.1000

0.5000

1.0000

Workstation/scales clean: _________________________________________

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CHM 327 Name: ______________________

This page is left intentionally blank.

- 52 -
CHM 327 Name: ______________________

Lab #7 & 8 Prelab and Flow Chart

Chloride by Gravimetric Analysis
To be completed in Lab Notebook:
1) Purpose: Briefly state the purpose of the experiment.
2) Materials/Chemicals: In this section, list any specific equipment that is required,
or chemical information that is important for the lab. (ie. Chemical name, CAS#,
MW, molecular formula, bp, mp, etc. ) Be sure to state the source of your
information.
3) Safety Hazards and Precautions: In this section, list any safety hazards that might
arise in the lab, including from chemicals or equipment. (hint: most of this
information is found in the chemical SDS.)
4) Balanced Equations: In this section include balanced equation for all reactions
involved in the experiment. For lab 6&7 this includes (AgNO3 and NaCl).
5) Calculations: In this section include all calculations for standards and reagents
required to begin the experiment. Be sure to show all work! For lab 6&7 complete
the following calculations:
A) Calculate the mass of AgNO3 (MW = 169.873 g/mol) required to produce
200 mL of a 0.2 M AgNO3 solution.
B) Calculate the mass of NaCl (MW = 58.443 g/mol) required to produce 1.0
mg/mL chloride (MW = 35.453 g/mol) standard solution in a 250.0 mL
volumetric flask.
C) Calculate the mass of unknown required to create a ~ 1 mg/mL chloride
solution in a 250.0 mL volumetric flask, assuming the unknown chloride
sample is 100 % NaCl.
D) Calculate the volume of unknown solution required to provide ~ 50 mg of
chloride to a 400 mL beaker, assuming the unknown is ~1 mg/mL
chloride.
E) Calculate the volume of stock chloride solution required to provide ~ 50
mg of chloride to a 400 mL beaker, assuming the stock chloride solution is
~1 mg/mL chloride.
6) Flowchart: Construct a flowchart for the lab. This should NOT be a reproduction
of the manual, but instead a graphical summary of the major steps. (NOTE: Do
not rewrite procedure word for word.)

- 53 -
CHM 327 Name: ______________________
Lab #7&8
Chloride by Gravimetric Analysis

Laboratory Report Requirements (Total 30 marks; 20 for Report + 10 for Accuracy)

Lab Report Format (2 marks)

- Title Page: Title of the experiment (center of page); At the bottom right: Your name,
course and section, date of experiment.
- Headings: Each section is clearly defined with the heading that is bolded or
underlined. (Purpose, Theory, Results, Discussion, etc..)
- Figures and Tables: Must be formatted in ACS style. Each table must have a # and
title at the top, and each figure will have a #, title and legend at the bottom. Include
references if they are not your own work.
- Spelling & Grammar: Text must be written in sentence format with proper spelling
and grammar.
- References: Cite all information throughout report with a superscripted number
corresponding to the source included in the reference section, in ACS format.

Purpose (0.5 marks)

• State the target, unknown identity, and the method referenced.

Theory (4 marks)
• Describe the steps involved in a gravimetric precipitation reaction. In general terms,
compare the method to the Fajans chloride method (Lab 6).
• Describe why AgNO3 is a good precipitating reagent for Chloride.
• Describe why it is important to control particle growth. Explain how particle size during
precipitation reactions can be controlled?
• Why is chloride considered to be an important target for analysis? What are some
typical concentrations of chloride in surface waters in Ontario?
• Include all references.

Results (6 marks)
• Reproduce Table 1 and 2.
• Produce Table 3 showing results of the t-test.
• Give sample calculations for:
o Mass of chloride in LFB1 from mass of AgCl.
o Expected mass of chloride in LFB1.
o Recovery of chloride in LFB1.
o Expected unknown sample mass in SMP1.
o Corrected experimental chloride mass (g) in SMP1.
o % chloride in SMP1 using corrected chloride mass. (don’t forget your dilution
factors)
o % difference for 10 mg standard mass.
o Conduct t-test to compare data observed during Lab #6 and Lab #7&8 for % Cl-
in unknown samples. Show all work if doing by hand or excel table generated
by excel if you are using excel to calculate the t-value as Table 3.

- 54 -
CHM 327 Name: ______________________
Discussion (5 marks)
• Discuss the importance of your LFB, what recovery did you obtain, and what does this
tell you about the mass of chloride that you obtained? (State your actual data and
discuss).
• Discuss the indication of precision of % Cl- associated with Lab #6 and Lab #7/8
(be specific state and compare s and CV values that you observed). Which
method was more precise? Why do you think this was?
• Discuss why we washed the solution with HNO3? What errors can be introduced when
washing?
• Describe the clarity of the filtrate (solution left after filtering) that you observed. What
does turbidity in the filtrate indicate? How can the filtrate be checked for the presence
of chloride?
• Discuss the results you found for the calibration of each standard mass. If an acceptable
limit of error in wet chemistry is a CV of 0.5 %, would the values you obtained be
acceptable or should the scales be recalibrated? Explain.

Conclusion (0.5 marks)

• State the average recovery and s values associated with the LFB, and % Cl and s value for
the unknown.
• State the average mass, standard deviation, and CV for each standard mass.

Notebook: Flow Chart and Prelab (2 marks)

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CHM 327 Name: ______________________
Lab #9
Chloride by Ion Selective Electrode
Method References: Fund. of Anal. Chem., 9th edition, Method 38 J
Standard Method 4500-Cl- D

Safety: This laboratory involves the production and use of corrosive substances. The use
of local exhaust (fume hood) and personal protective equipment such as gloves, lab coat
and safety glasses are necessary. Concentrated solutions such as nitric acid should be
dispensed under local exhaust conditions. Follow instructions regarding waste handling
and disposal.

Method Summary: The determination of chloride is done routinely because it is one of

the most commonly found inorganic ions in the environment and above average chloride
concentrations can indicate pollution in air, water and soil. The method employed here
uses an Ion Selective Electrode (ISE) technique to determine the activity (and thus
concentration) of chloride ion in aqueous solution. The source of the chloride ion is a
water-soluble powder; pure sodium chloride provides known chloride masses. An Excel-
generated trend line for chloride is produced by relating potentiometer response to log
chloride concentration and from this trend line the chloride concentration (%) in an
unknown sample can be forecasted from a measured potential.

Apparatus and Reagents:

Potentiometer (mV mode) and Chloride ISE (Combination or Electrode Pair)
Stir pad, stir bar magnet, and stir bar magnet fetcher
ACS sodium chloride solid reagent and unknown [Cl-] in water-soluble powder
Purity NaCl: ______ %
Ionic Strength Adjustment (ISA) solution:
To 500 mL of deionized water, add 15.1 g sodium bromate and 75 mL conc nitric
acid. Dilute to 1 L in a 1.5 L beaker (or, make 50 mL of this buffer). Use 2.0 mL
of ISA for each 100 mL of sample to be analyzed.
250 mL beakers (or similar capacity) to hold solutions for analysis (8 required)
10 mL and 100 mL graduated cylinders
1, 5, 10, 15, 20, 25 mL volumetric pipettes
100.0 mL volumetric flask

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CHM 327 Name: ______________________
Preparation of Chloride Stock Solutions and Calibration Standards Containing
Known Chloride Concentrations:

1. Create a 1,000 ug/mL stock solution of Cl- by weighing ACS grade NaCl (MW =
58.443 g/mol) to the nearest 0.1 mg into a 100.0 mL volumetric flask and dilute to the
mark with H2OD. MWCl- = 35.453 g/mol
Target Mass NaCl:_______________g.

2. Make an Intermediate Stock Solution (ISS) by pipetting 10.00 mL of the Stock

Solution into a 100.0 mL volumetric flask and dilute to the mark with H2OD.
(NOTE: target ~ 100 ug/mL Cl- for the ISS).

3. Prepare 5 calibration standards of known [Cl-] from your ISS solution by pipetting the
required volume stated below into a 250 mL beaker and making the volume up to 100
mL with the required amount of H2OD using a 100 mL graduated cylinder. Calculate
[Cl-] (ug/mL) in each calibration standards from the calculated concentration of your
ISS and place below, as well as in Table 1.

Std1: 1.00 mL ISS → _______ ug/mL Cl- when diluted with 99.0 mL H2OD
Std2: 5.00 mL ISS → _______ ug/mL Cl- when diluted with 95.0 mL H2OD
Std3:10.00 mL ISS → _______ ug/mL Cl- when diluted with 90.0 mL H2OD
Std4: 15.00 mL ISS → ______ ug/mL Cl- when diluted with 85.0 mL H2OD
Std5: 25.00 mL ISS → ______ ug/mL Cl- when diluted with 75.0 mL H2OD

Preparation of Sample Solution:

4. Use the same target mass as that used for pure NaCl and create a Sample Solution by
weighing your unknown sample to the nearest 0.1 mg into a 100.0 mL volumetric flask,
and diluting to the mark with H2OD. (Unknown #: _______________).
Target Mass NaCl:_______________g.

5. Make an Intermediate Sample Solution by pipetting 10.00 mL of Sample Solution into

a 100.0 mL volumetric flask and dilute to mark with H2OD.

6. Make three replicate samples (SMP1, SMP2 and SMP3) by pipetting 10.00 mL
aliquots of Intermediate Sample Solution into 250 mL beakers followed by 90.0 mL of
H2OD using a 100.0 mL graduated cylinder.

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CHM 327 Name: ______________________
Procedure: Determination of percent chloride in unknown ________ for Lab #9
1. Just before analysis, add 2.0 mL ISA to all 8 of the solutions to be analyzed using a
Pasteur pipette and 10 mL graduated cylinder. After completion of this step, all
solutions must now contain 102 mL total volume: 8 solutions = 5 standards and 3
sample replicates.

2. Line up all 8 solutions to be analyzed next to the potentiometer. NOTE: All standards
must be analyzed together first, lowest concentration to highest, and then the three
replicate samples must be immediately analyzed next. Ensure potentiometer instrument
is on mV mode. Raise the electrode(s) out of the storage solution, rinse off and gently
pat dry the electrode(s) with a Kim wipe before initial use.

3. Add a rinsed stir bar to the beaker containing the lowest standard and place the beaker
on the stir pad. Mix at a moderate speed and then submerge the electrode(s) to a depth
of at least 1 cm above the stir bar. (NOTE: Ensure a vortex does not form).

4. Record the mV potential in Table 1 after the mV potential reading has stabilized. Wait
no longer than 30 seconds to take a reading.

5. Immerse the electrode(s) in the next solution to be analyzed remembering to measure

the solutions from lowest to highest concentration for the standards first followed
immediately by the three replicate samples. Rinse and gently dry the electrode(s)
between the last standard and first sample only. (NOTE: Ensure standards and sample
data makes sense, sample data must fall within range of standards!)

6. After all solutions are analyzed, submerge electrode(s) in storage solution

(1 ug/mL Cl-). If time permits, calculate the % Cl in the soluble powder.

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 CHM 327 Name: ______________________
Lab 9 - Raw Data sheet must be signed by instructor & handed in with Report.

Table 1. Observations for Percent Chloride in Unknown ___ by ISE for Lab #9
Unknown # ________
Purity NaCl = ______ %
Actual Mass NaCl:_______________g.
Purity Corrected Mass of NaCl in Stock Solution: ____________g.
Calculated [Cl-] in Stock Solution:______________µg/mL.
Calculated [Cl-] in ISS: ___________ µg/mL.
Sample Mass in stock solution: __________g
Sample mass in ISS:____________g
Sample mass in 10.00 mL aliquot: __________g
Sample mass in 10.00 mL aliquot: __________ug

VISS /
Forecast Forecast Avg s CV
Vdilsmp
Std/Smp [Cl-] log [Cl-] Potential log [Cl-] [Cl-] Mass Cl- [Cl-] [Cl-] [Cl-] [Cl-]
in 100 mL
(ug/mL) (log ug/mL) (mV) (log ug/mL) (ug/mL) (ug) (%) (%) (%) (%)
(mL)

Std 1 1.00

Std 2 5.00

Std 3 10.00

Std 4 15.00

Std 5 25.00

Smp 1 10.00

Smp 2 10.00

Smp 3 10.00

Workstation/scales clean: _________________________________________

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CHM 327 Name: ______________________

This page is left intentionally blank.

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CHM 327 Name: ______________________

Lab #9 Prelab and Flow Chart

Chloride by Ion Selective Electrodes
To be completed in Lab Notebook:
1) Purpose: Briefly state the purpose of the experiment.
2) Materials/Chemicals: In this section, list any specific equipment that is required,
or chemical information that is important for the lab. (ie. Chemical name, CAS#,
MW, molecular formula, bp, mp, etc. ) Be sure to state the source of your
information.
3) Safety Hazards and Precautions: In this section, list any safety hazards that might
arise in the lab, including from chemicals or equipment. (hint: most of this
information is found in the chemical SDS.)
4) Balanced Equations: In this section include balanced equation for all reactions
involved in the experiment. For lab 9 this includes (NaCl dissolved in water).
5) Calculations: In this section include all calculations for standards and reagents
required to begin the experiment. Be sure to show all work! For lab 9 complete
the following calculations:
A) Calculate the mass of sodium chloride (MWNaCl = 58.443 g/mol) required
to produce a 1000 µg/mL stock solution of chloride MWCl- = 35.453 g/mol
(Cl- not NaCl) in a 100.0 mL volumetric flask.
B) Calculate the [Cl-] in the intermediate stock solution (ISS) if 10.00 mL of
the 1000 µg/mL stock solution is diluted to 100.0 mL.
C) Calculate the [Cl-] in each standard if the following volumes of ISS
(concentration calculated in question 2) are diluted to 100.0 mL. (NOTE:
Dilutions, C1V1 = C2V2).
a. [Cl-] in STD 1 if 1 mL of ISS is diluted to 100 mL.
b. [Cl-] in STD 2 if 5 mL of ISS is diluted to 100 mL.
c. [Cl-] in STD 3 if 10 mL of ISS is diluted to 100 mL.
d. [Cl-] in STD 4 if 15 mL of ISS is diluted to 100 mL.
e. [Cl-] in STD 5 if 25 mL of ISS is diluted to 100 mL.
6) Flowchart: Construct a flowchart for the lab. This should NOT be a reproduction
of the manual, but instead a graphical summary of the major steps. (NOTE: Do
not rewrite procedure word for word.)

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CHM 327 Name: ______________________
Lab #9 - Chloride by Ion Selective Electrode
Laboratory Report Requirements (Total 30 marks; 20 for Report + 10 for Accuracy)

Lab Report Format (2 marks)

- Title Page: Title of the experiment (center of page); At the bottom right: Your name,
course and section, date of experiment.
- Headings: Each section is clearly defined with the heading that is bolded or
underlined. (Purpose, Theory, Results, Discussion, etc..)
- Figures and Tables: Must be formatted in ACS style. Each table must have a # and
title at the top, and each figure will have a #, title and legend at the bottom. Include
references if they are not your own work.
- Spelling & Grammar: Text must be written in sentence format with proper spelling
and grammar.
- References: Cite all information throughout report with a superscripted number
corresponding to the source included in the reference section, in ACS format.

Purpose (0.5 marks)

• State the target (chloride), unknown number, and the method(s) referenced.

Theory (4 marks)
• Describe what ion selective electrodes are, how they work, and what they are
used for.
• Provide 2 specific examples of applications that utilize ISEs and what they are
used to determine.
• Compare the differences in how the % of chloride is determined by ISE, Fajans
method and gravimetric determinations.
• Describe at least two general concerns associated with the measurements by
ISE.
• Include all references.

Results (7 marks)
• Reproduce Table 1 that was filled in during the experiment.
• Give sample calculations for:
o Purity corrected mass NaCl (g) in 1,000 ug/mL Stock Solution of Cl-.
o [Cl]- (ug/mL) in Intermediate Sock Solution (ISS) (ISS is made by taking a
10.00 mL aliquot of Stock and diluting to 100.0 mL with H2OD).
o [Cl-] (ug/mL) in Std 1.
o Log [Cl-] (log ug/mL) in Std 1.
o [Cl-] (log ug/mL) found for Smp 1 from trend line equation.
o [Cl-] (ug/mL) for Smp 1.
o Mass (ug) Cl- for Smp 1.
o % Cl in Smp 1

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CHM 327 Name: ______________________
**NOTE: You only need to do 1 of the following to determine to see if there is a
difference between your Chloride results from the 3 different methods (3 separate T-
Tests or a Single-Factor ANOVA)***
o T-test Lab #6 vs Lab #7/8, #7/8 vs Lab #9 and Lab #6 vs Lab #9 or you can
do a Single-Factor ANOVA to determine if there is a significant difference
between the mean % Cl found in Lab #6, Lab #7/8, and Lab #9. Which
results differed? (Can use excel ANOVA command under data analysis to
generate table with all data, if you remember from computer class).
• Graph your observed millivolt potential (mV) vs. log concentration (log ug/mL)
using Excel. Be sure to use your data for the standard [Cl-] values!! Place the
regression line equation and value for r2 on the plot. (NOTE: Concentration x-
axis; potential y-axis.) NOTE: All graphs must have both a title on graph and
heading labelled Graph 1 with a caption explain exactly what is shown in the
graph.

Discussion (4 marks)
• Discuss the precision observed for your tread line, state the actual value and
what your R2 value means.
• State your ANOVA results or perform three T-Tests (Lab 6 vs 7/8, 6 vs 9 and 7/8
vs 9) for your comparison of the means for the determination of Cl by 3 different
methods covered in Labs 6, 7/8 and 9. Discuss what these results mean. If the
means are considered significantly different which methods if any can be
considered the same and which differ significantly? (Use variances to determine
if range overlaps or not if it fails if you used an ANOVA).
• For Lab 6, 7/8 and 9, compare the ease of analysis, amount of sample required,
and the precision (from s and CV values) obtained for % chloride (state actual
values), and discuss which method provided the most precise results for the
determination of % Cl. Which one would you recommend to your boss if he asks
you to complete an analysis for % Cl in wastewater?
• Discuss two possible sources of error that were present for lab 9.

Conclusion (0.5 marks)

State the unknown identity and % chloride with s value found in the unknown powder
by ISE.

Notebook: Flow Chart and Prelab (2 marks)

You must attach all initialed data sheets, questions and flow chart with lab report or
marks will be deducted!!!

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CHM 327 Name: ______________________

Lab #10
Fluoride by Ion Selective Electrode
Method References: Fund. of Anal. Chem., 9th edition, Method 38 J
Standard Method 4500-F

Safety: This laboratory involves the production and use of corrosive substances. The use
of local exhaust (fume hood) and personal protective equipment such as gloves, lab coat
and safety glasses are necessary. Concentrated solutions should be dispensed under local
exhaust conditions. Compounds and solutions containing fluoride must be handled with
gloved hands. Follow instructions regarding waste handling and disposal.

Method Summary: The determination of fluoride is routine because it is commonly

found in drinking water and toothpaste. The method uses an Ion Selective Electrode
(ISE) technique to determine the activity (and thus concentration) of fluoride ion in
aqueous solution and a buffer (TISAB) which is necessary to liberate fluoride ion. A
calibration line for fluoride is generated by relating potentiometer response to fluoride
concentration and from the linear calibration line (found using Excel), the fluoride
concentration in an unknown sample is forecasted from a measured potential. Fluoride
concentration in solution is determined in terms of mg/L (ppm on a w/v basis) for
drinking water and a mg/L concentration can easily be translated to a ug/g and % NaF
w/w basis provided the mass of the soluble sample (e.g. toothpaste) and volume of
sample (e.g. drinking water) is known.

Apparatus and Reagents:

Potentiometer and Fluoride Combination Electrode
Stir pad, cork pad or other suitable protection from heat, magnet and magnet fetcher
Hot plate
ACS sodium fluoride
Total Ionic Strength Adjustment Buffer (TISAB) solution:
Make 1 L of this solution and use 50 mL for each sample to be analyzed. To 500
mL in a 1.5 L beaker add:
57 mL glacial acetic acid
58 g NaCl
4.0 g cyclohexylenediaminetetraacetic acid (CDTA)
Add 6 N NaOH (about 125 mL will be required) with stirring in an ice bath until
pH is between 5.3 and 5.5
Make to 1.000 L in a volumetric flask with deionized water
250 mL beakers (or similar capacity) to hold solutions for analysis
10 mL and 100 mL graduated cylinders
1, 5, 10, 15, 20, 25 mL volumetric pipettes
100.0 mL volumetric flasks

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CHM 327 Name: ______________________
Procedure: Determination of Fluoride in Toothpaste
1. Preparation of Sample Solutions:
Place a labeled 250 mL capacity beaker on a top loading balance and tare. Dab a
pea sized bead of toothpaste (TP) on the bottom of the beaker and place the
beaker back on the balance. Add a small amount more or remove a small amount
with a clean microspatula so that the mass is near 0.20 g. Produce three samples.
Enter the sample mass to the nearest 0.01 g below and in Table 1.
Mass (g) sample TP1 to nearest 0.01 g in 100 mL solution: ____________
Mass (g) sample TP2 to nearest 0.01 g in 100 mL solution: ____________
Mass (g) sample TP3 to nearest 0.01 g in 100 mL solution: ____________

2. To each beaker containing toothpaste (TP), add 50.0 mL of TISAB (measure

using a graduated cylinder) and with stirring (glass rod), bring the solutions to a
boil. Boil the solutions gently for 2 minutes with good mixing but avoid frothing.

3. Cool the solutions on the bench. Dilute to 100 mL with H2OD using beaker
graduation (100 mL mark).

4. Prepare fluoride Stock solution, Intermediate Stock Solution (ISS) and standard
solutions during sample heating and cooling.

5. Preparation of Fluoride Stock Solutions and Calibration Standards:

After first preparing tooth paste samples, prepare five calibration standards
containing known fluoride amounts (masses) using ACS grade sodium fluoride
(MW = 42.00 g/mol). Start by creating a 1,000 mg/L Stock solution of fluoride
(MW = 19.00 g/mol) by weighing ACS grade NaF to the nearest 0.1 mg into a
100.0 mL volumetric flask and dilute to the mark with H2OD.
Target Mass NaF:_______________g. Purity NaF = ______ %
Actual Mass NaF:_______________g.
Purity Corrected Mass of NaF in Stock Solution: ____________g.
Calculated [F-] in Stock Solution:______________ µg/mL. (4 sig figs)

6. Make an Intermediate Stock Solution (ISS) of fluoride by transferring 1.00 mL

aliquot of the Stock solution to a second 100.0 mL volumetric flask and diluting
to 100.0 mL with H2OD.
Calculated [F-] (ug/mL) ISS:___________ (to 4 sig. figs)

7. Produce the following concentrations of fluoride in labeled beakers. Make sure

to add 50.0 mL of TISAB to the beakers first, then transfer the ISS or stock
aliquot, and finally dilute with H2OD (measure H2OD volume with a graduated
cylinder): (NOTE: Final volume for all solutions is 100 mL).

Std1: 5.00 mL ISS → _______ ug/mL F- when diluted with 45.0 mL H2OD
Std2: 10.00 mL ISS → _______ ug/mL F- when diluted with 40.0 mL H2OD
Std3:15.00 mL ISS → _______ ug/mL F- when diluted with 35.0 mL H2OD
Std4: 25.00 mL ISS → ______ ug/mL F- when diluted with 25.0 mL H2OD
Std5: 1.00 mL Stock → ______ ug/mL F- when diluted with 49.0 mL H2OD

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CHM 327 Name: ______________________
8. Place all eight solutions to be analyzed as close as possible to the potentiometer
for easy access. All standards and samples must be analyzed one at a time, lowest
standard concentration first. Record all observations in Table 1. Retrieve the stir
bar from the storage beaker, rinse it off and dry it with a Kim wipe. Start reading
the mV potentials of the solutions with the lowest standard. Rinse and gently dry
the electrode(s) between the last standard and first sample only.

9. Add the stir bar to the solution, mix at a moderate speed and submerge the
electrode(s) to a depth of at least 1 cm above the stir bar. (Ensure no vortex is
formed).

10. Record the mV potential in Table 1 after the mV potential reading has stabilized
(should take no longer than 60 seconds to take a reading).

11. Immerse the electrode(s) in the next solution to be analyzed remembering to

measure the solutions from lowest to highest concentration for the standards first
followed immediately by the three TP samples. (NOTE: Ensure data makes sense
for standards and that samples actually fall within the range of your standard data)

12. After measuring the potential of the last solution, submerge electrode(s) in storage
solution (1 ug/mL F-) for storage. If time permits, calculate % recovery F- in TP.

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 CHM 327 Name: ______________________

Lab 10 - Raw Data sheet must be signed by instructor & handed in with Report.

Table 1. Observations for Percent Fluoride in Toothpaste

Mass (g) NaF in 100.0 mL: ________ Purity NaF (%): ________

Purity Corrected [F-] in Stock solution (ug/mL): ______ [F-] in ISS (ug/mL): _______

According to manufacturer, Fluoride Mass (g/g) in TP: ________

TP Mass in TP1 (g) in 100 mL: _____ Calc F- Mass in TP1 (ug) in 100 mL: _____

TP Mass in TP2 (g) in 100 mL: _____ Calc F- Mass in TP2 (ug) in 100 mL: _____

TP Mass in TP3 (g) in 100 mL: _____ Calc F- Mass in TP3 (ug) in 100 mL: _____

VISS Forecast Avg s CV

Forecast Experimental Calculated Recovery*
/ VSTOCK log [F-] log [F-] Recovery (%) (%)
Std/Smp [F-] Potential [F-] Mass F- Mass F- F-
in 100 mL (log (log F-
(ug/mL) (mV) (ug/mL) (ug) (ug) (%)
(mL) ug/mL) ug/mL) (%)

Std 1 5.00

Std 2 10.00

Std 3 15.00

Std 4 25.00

Std 5 1.00

TP 1

TP 2

TP 3
MW NaF = 42.00 g/mol MW F- = 19.00 g/mol

*Recovery = Experimental mass F- (g) / Calculated mass F- x 100 % (3 sig figs above 100)

Workstation/scales clean: _________________________________________

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CHM 327 Name: ______________________

This page is left intentionally blank.

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CHM 327 Name: ______________________
Lab #10 Prelab and Flow Chart
Fluoride by Ion Selective Electrodes
To be completed in Lab Notebook:
1) Purpose: Briefly state the purpose of the experiment.
2) Materials/Chemicals: In this section, list any specific equipment that is required,
or chemical information that is important for the lab. (ie. Chemical name, CAS#,
MW, molecular formula, bp, mp, etc. ) Be sure to state the source of your
information.
3) Safety Hazards and Precautions: In this section, list any safety hazards that might
arise in the lab, including from chemicals or equipment. (hint: most of this
information is found in the chemical SDS.)
4) Balanced Equations: In this section include balanced equation for all reactions
involved in the experiment. For lab 10 this includes (NaF dissolved in water).
5) Calculations: In this section include all calculations for standards and reagents
required to begin the experiment. Be sure to show all work! For lab 10 complete
the following calculations:
A) Calculate the mass of sodium fluoride (MWNaF = 42.00 g/mol) required to
produce a 1000 mg/L stock solution of fluoride MWF- = 19.00 g/mol (F-
not NaF) in a 100.0 mL volumetric flask.
B) Calculate the [F-] (ug/mL) in the intermediate stock solution (ISS) if 1.00
mL of the 1000 mg/L stock solution is diluted to 100.0 mL. (NOTE: ppm
= µg/mL = mg/L *all equivalent*).
C) Calculate the [F-] in each standard if the following volumes of ISS
(concentration calculated in question 2) or the original stock are diluted to
100.0 mL. (NOTE: Dilutions, C1V1 = C2V2).
a. [F-] in STD 1 if 5 mL of ISS is diluted to 100 mL.
b. [F-] in STD 2 if 10 mL of ISS is diluted to 100 mL.
c. [F-] in STD 3 if 15 mL of ISS is diluted to 100 mL.
d. [F-] in STD 4 if 25 mL of ISS is diluted to 100 mL.
e. [F-] in STD 5 if 1 mL of original stock (1000 mg/L) is diluted to
100 mL.
6) Flowchart: Construct a flowchart for the lab. This should NOT be a reproduction
of the manual, but instead a graphical summary of the major steps. (NOTE: Do
not rewrite procedure word for word.)

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CHM 327 Name: ______________________
Lab #10 Fluoride by Ion Selective Electrode

Laboratory Report Requirements (Total 30 marks; 20 for Report + 10 for Accuracy)

Lab Report Format (2 marks)

- Title Page: Title of the experiment (center of page); At the bottom right: Your name,
course and section, date of experiment.
- Headings: Each section is clearly defined with the heading that is bolded or
underlined. (Purpose, Theory, Results, Discussion, etc..)
- Figures and Tables: Must be formatted in ACS style. Each table must have a # and
title at the top, and each figure will have a #, title and legend at the bottom. Include
references if they are not your own work.
- Spelling & Grammar: Text must be written in sentence format with proper spelling
and grammar.
- References: Cite all information throughout report with a superscripted number
corresponding to the source included in the reference section, in ACS format.
Purpose (0.5 marks)
• State the target, unknown identity, and the method referenced.
Theory (4 marks)
• Describe at least four general concerns associated with the measurements by ISE and two
concerns specific to the measurement of fluoride in solution. (See attached document
under Lab # 10).
• Compare and discuss the expected fluoride electrode response to the chloride electrode
response from Lab #9. Discuss sensitivity of methods (indicated by slope of standards).
• Illustrate and explain a plot of mV potential vs log fluoride concentration from a
reliable source (electrode manual ex. From Thermo Fischer or citable internet
site). Cite your source.
• Describe 2 applications for the determination of fluoride in a sample.
• Include all references.

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CHM 327 Name: ______________________
Results (6 marks)
• Reproduce Table 1 that was filled in during the experiment. Include in your table
places for recovery information.
• Give sample calculations for:
o Purity corrected mass NaF (g) in 1,000 ug/mL Stock Solution of F -.
o [F-] ( ug/mL) in Intermediate Sock Solution (ISS) (ISS is made by taking a
1.00 mL aliquot of Stock and diluting to 100.0 mL with H2OD).
o [F-] (ug/mL) in Std 1.
o Log [F-] (log ug/mL) in Std 1.
o [F-] (log ug/mL) found for Smp 1 using trend line equation.
o [F-] (ug/mL) for Smp 1.
o Mass (ug) F- for Smp 1.
o Sample mass (ug) in TP1 solution.
o % F- in TP 1.
o % F- in TP (if not given on package).
o Recovery (%) for TP1.
• Graph your observed millivolt potential (mV) vs. fluoride concentration (ug/mL) and
graph your observed millivolt potential (mV) vs. log fluoride concentration (log ug/mL)
using Excel. Make a copy of these plots and attach them to the back of your Lab #10
submission. Be sure to use your data for the [F-] values!! Place the regression line
equation and value for r2 on the log plot.

Discussion (5 marks)
• Compare your experimental observations (two graphs in the Results section) to
those shown in a plot of mV potential vs log concentration from a reliable source
(graph of log plot in Theory section) and comment on all similarities and
differences that you observe.
• Discuss your R2 (state actual value), what does it indicate about your standards.
• Discuss the observed recovery value. (State actual values) Does it indicate good
technique? Why/why not.
• Discuss your precision for the experiment (s and CV). How did it compare to
precision (s and CV) for Lab #9 for the Cl- ISE lab?
• What are 3 possible sources of error for this experiment?

Conclusion (0.5 marks)

• Give toothpaste brand and stated % fluoride content and state your finding of %
fluoride with s value in the toothpaste by ISE.

Notebook: Flow Chart and Prelab (2 marks)

You must attach all initialed data sheets, questions and flow chart with lab report or
marks will be deducted!!!

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CHM 327 Name: ______________________
Lab #11
Standardization of Iodine and Thiosulfate

Method References: Fund. of Anal. Chem., Method 38 G, H

Standard Method 4500-O

Safety: This laboratory involves the production and use of extremely corrosive
substances. The use of local exhaust (fume hood) and personal protective equipment
such as gloves, coat and safety glasses are necessary. Concentrated solutions such as
acids should be dispensed under local exhaust conditions. Follow instructions regarding
waste handling and disposal.

Method Summary: The production of standard solutions containing 0.01 M sodium

thiosulfate and 0.005 M iodine is common practice for most analytical laboratories.
Standard oxidants and reductants are made to an exact (four significant figure) molarity
by using volumetric glassware and pure primary standards. For standard iodine solutions,
a standard solution of sodium thiosulfate (thiosulfate) is used to determine molarity and
starch indicates titration point. For standard sodium thiosulfate solutions, potassium
iodate is used as primary standard, and starch indicates titration point.

Apparatus and Reagents

ACS grade potassium iodate (previously dried for 2 h at 103oC)
ACS grade Na2S2O3.5H2O
ACS grade iodine ACS grade potassium iodide
conc HCl Conc H2SO4 Starch indicator beakers for solutions
250 mL conical flasks 50 mL burette 10 and 15 mL volumetric pipettes
250.0 mL and 100.0 mL volumetric flasks Amber glass and/or plastic storage bottles (2)

Production of 0.005 M I2 Solution

Dissolve 6 g KI in 20 mL of deionized water in a 150 mL capacity beaker and completely
dissolve the KI. Add the calculated mass of iodine crystals to the beaker (do not weigh
on an analytical balance, iodine is corrosive!). Gently swirl the solution for at least 20
minutes. Premark 600 mL on a 1 L brown glass storage bottle. Add the solution to the
brown storage bottle and dilute to the 600 mL mark with deionized water. Ensure all I2 is
dissolved before diluting.

Target mass (g) I2 (MW = 253.81 g/mol) to produce 1 L of a 0.005 mol/L

solution:_______________g

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CHM 327 Name: ______________________
Production of 0.01 M Sodium Thiosulfate Solution
Target mass (g) Na2S2O3.5H2O (MW = 248.184 g/mol) to produce 0.5 L of a
0.01 mol/L solution:___________________________g.

Add the calculated mass of Na2S2O3.5H2O pellets into a labeled 0.5 L storage bottle that
is half-filled with deionized water. When the pellets have dissolved, dilute the solution in
a storage bottle to a predetermined 0.5 L mark with deionized water.

Production of Standard Potassium Iodate Solution

Target mass (g) to produce 250.0 mL of a KIO3 (MW = 214.001 g/mol) solution from
which a 10.00 mL aliquot requires ~15 mL volume of 0.01 M sodium thiosulfate. (Hint:
molar ratio is 1KIO3 : 6 Na2S2O3). Enter exact mass (to 0.1 mg) and molarity values in
Table 1.

Target Mass KIO3 (g):____________________

Add the calculated mass of KIO3 into 250.0 mL volumetric flask, half fill with H2OD and
swirl until completely dissolved, dilute to mark.

Procedure: Standardization of 0.01 M Sodium Thiosulfate

1. Pipette 10.00 mL of primary standard (KIO3) into four separate labeled conical
flasks (at least four titrations will be required).
2. Dilute the primary standard solution to 50 mL with deionized water (gauge this
volume using the graduations on the conical flask).
TREAT EACH FLASK SEPARATELY FROM THIS STEP
3. Dissolve approximately 2 g KI (measure first portion to nearest 0.01g, estimate
other portions) into the solution that is to be titrated.
4. Add 2 mL of 6 M HCl (NOTE: you will need to make enough 6 M HCl for all
titrations, conc HCl is ~ 12 M) into the solution that is to be titrated.
5. Begin titrating with standard thiosulfate and add starch indicator when a pale
straw color is reached and complete the titration until the blue color first
disappears (solution becomes clear). Record all observations in Table 1. Get
Table 1 initialed when you have finished this laboratory.

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CHM 327 Name: ______________________
Procedure: Standardization of 0.005 M I2
1. Pipette 15.00 mL of iodine solution into four separate labeled conical flasks (at
least four titrations will be required). Perform a blank titration using 50 mL of
deionized water and acid.
2. Dilute the iodine solution to 50 mL with deionized water (gauge this volume
using the graduations on the conical flask).
TREAT EACH FLASK SEPARATELY FROM THIS STEP
3. Add 1 mL of 3 M sulfuric acid (NOTE: you will need to make enough 3 M
H2SO4 for all titrations, conc H2SO4 is ~ 18 M) and titrate immediately.
4. Begin titrating the solution with standardized sodium thiosulfate just until the
colour begins to fade to a “straw” pale yellow colour. Add the required amount of
starch solution.
5. Finish the titration of the contents of each conical flask (until blue/black solution
becomes clear) remembering to record all observations in Table 2. Get Table 2
initialed when you have finished this laboratory.

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CHM 327 Name: ______________________
Lab 11 - Raw Data sheet must be signed by instructor & handed in with Report.

Table 1. Standardization of 0.01 M Na2S2O3 for Lab #11

Actual Mass I2:______________g Estimated Molarity I2: ____________M
Mass thiosulfate:_____________g Expected M thiosulfate:___________M
Purity KIO3 (g): ___________ %
Actual KIO3 mass (g) in 250.0 mL:________________g
Purity corrected mass KIO3: _____________________g
Molarity of KIO3 = _______________M

Vi Vf Vt Vt Avg
V KIO3 MNa2S2O3 s CV
# Na2S2O3 Na2S2O3 Na2S2O3 Na2S2O3 MNa2S2O3
(mL) (mol/L) (mol/L) (%)
(mL) (mL) (mL) (mL) corr (mol/L)
B 0
1 10.00
2 10.00
3 10.00
4 10.00
5 10.00
6 10.00

Table 2. Standardization of 0.005 M I2 for Lab #11

M thio = _______________ Mass (g) I2 = _________ Expected M I2 = _______

# V I2 Vi Na2S2O3 Vf Na2S2O3 Vt Na2S2O3 Vt Na2S2O3 MI2 Avg MI2 s CV

(mL) (mL) (mL) (mL) (mL) corr (mol/L) (mol/L) (mol/L) (%)

B 0
1
2
3
4
5
6

Workstation/scales clean: _________________________________________

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CHM 327 Name: ______________________

This page is left intentionally blank.

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CHM 327 Name: ______________________

Lab #11 Prelab and Flow Chart

Standardization of Iodine and Thiosulfate
To be completed in Lab Notebook:
1) Purpose: Briefly state the purpose of the experiment.
2) Materials/Chemicals: In this section, list any specific equipment that is required,
or chemical information that is important for the lab. (ie. Chemical name, CAS#,
MW, molecular formula, bp, mp, etc. ) Be sure to state the source of your
information.
3) Safety Hazards and Precautions: In this section, list any safety hazards that might
arise in the lab, including from chemicals or equipment. (hint: most of this
information is found in the chemical SDS.)
4) Balanced Equations: In this section include balanced equation for all reactions
involved in the experiment. For lab 11 this includes (I2 + I-), (IO3- + I- + H+)
and (I2 + S2O32-).
5) Calculations: In this section include all calculations for standards and reagents
required to begin the experiment. Be sure to show all work! For lab 11 complete
the following calculations:
A) Calculate the mass of iodine (MW = 253.81 g/mol) crystals required to
produce 600 mL of a 0.005 M I2 solution.
B) Calculate the mass of Na2S2O3.5H2O (MW = 248.184 g/mol) to produce
0.5 L of a 0.01 mol/L NaS2O3 solution.
C) Calculate the mass of KIO3 (MW = 214.001 g/mol) to produce a 250.0 mL
solution from which a 10.00 mL aliquot requires ~15 mL volume of 0.01
M sodium thiosulfate solution to reach the end-point. (Hint: molar ratio is
1 KIO3 : 6 Na2S2O3).
D) Describe how to prepare 50 mL of 6 M HCl from conc. HCl.
E) Describe how to prepare 25 mL of 3 M H2SO4 from conc. H2SO4.
6) Flowchart: Construct a flowchart for the lab. This should NOT be a reproduction
of the manual, but instead a graphical summary of the major steps. (NOTE: Do
not rewrite procedure word for word.)

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CHM 327 Name: ______________________

Lab #11
Standardization of Iodine and Thiosulfate

Laboratory Report Requirements (Total 20 marks for Report)

Lab Report Format (2 marks)

- Title Page: Title of the experiment (center of page); At the bottom right: Your name,
course and section, date of experiment.
- Headings: Each section is clearly defined with the heading that is bolded or
underlined. (Purpose, Theory, Results, Discussion, etc..)
- Figures and Tables: Must be formatted in ACS style. Each table must have a # and
title at the top, and each figure will have a #, title and legend at the bottom. Include
references if they are not your own work.
- Spelling & Grammar: Text must be written in sentence format with proper spelling
and grammar.
- References: Cite all information throughout report with a superscripted number
corresponding to the source included in the reference section, in ACS format.

Purpose (0.5 marks)

• State the solutions to be standardized and the method(s) referenced.

Theory (4 marks)
• Give all reaction equations for both titrations and explain them in words. Explain why
the stoichiometric ratio for KIO3 and NaS2O3 is 1:6.
• Explain the purpose of adding KI to the I2 solution.
• Describe how the starch indicator is supposed to work.
• Describe the interferences that can influence results.
• Include all references.

Results (6 marks)
• Reproduce Tables 1 and 2 that were filled in during the experiment.
• Give sample calculations for:
o Expected MNa2S2O3 from mass weighed out.
o Mthio from first titration.
o % Difference between expected and actual MNa2S2O3 values obtained.
o Expected molarity of I2 from mass weighed out.
o MI2 from first titration.
o % Difference between expected and actual MI2 values obtained.
o Q-test of any potential outlier (must show even if no outliers appear).

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CHM 327 Name: ______________________
Discussion (5 marks)
• Describe the indication of precision associated with the molarities of thiosulfate and
iodine. Compare the CV values obtained for the solutions manufactured for Lab #11 to
the CV values observed for the two solutions (standard acid and base) manufactured for
Lab # 3 and Lab #5. (State actual values, which standardization indicates better
precision?)
• Describe the attempts made to overcome interferences for both standardization
procedures.
• Describe in general terms two applications for the standard solutions made during Lab
#11.
• Compare expected molarity of the solutions to the molarity actually found and
comment on why differences were observed (refer to calculated % differences).
• State 2 possible sources of error.

Conclusion (0.5 marks)

• State the average molarities and s values of the standard solutions found after
performing Lab #11.

Notebook: Flow Chart and Prelab (2 marks)

You must attach all initialed data sheets, questions and flow chart with lab report or
marks will be deducted!!!

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CHM 327 Name: ______________________
Lab #12
Analysis of Vitamin C in Juice
Method References: Fund. of Anal. Chem., Method 38 G, H
Standard Method 4500-O

Safety: This laboratory involves the production and use of extremely corrosive
substances. The use of local exhaust (fume hood) and personal protective equipment
such as gloves, coat and safety glasses are necessary. Concentrated solutions such as
acids should be dispensed under local exhaust conditions. Follow instructions regarding
waste handling and disposal.

Method Summary: The analysis of Vitamin C (ascorbic acid) by redox titration with
iodine and a starch indicator is common practice in most analytical laboratories. Adding
your standardized I2 solution from Lab # 11 to your ascorbic acid sample will oxidize the
ascorbic acid to dehydroascorbic acid, while the iodine is reduced to iodide ions. Once all
the ascorbic acid has reacted, the free I2 is now free to react with the starch indicator,
forming blue-black iodine complex.
ascorbic acid + I2 → 2 I− + dehydroascorbic acid

Apparatus and Reagents

Pure ascorbic acid
ACS grade potassium iodate (previously dried for 2 h at 103oC)
ACS grade Na2S2O3.5H2O
ACS grade iodine
ACS grade potassium iodide
Conc HCl
Conc H2SO4
Starch indicator (made fresh).
beakers for solutions
250 mL conical flasks
50 mL burette
10 and 15 mL volumetric pipettes
250.0 mL and 100.0 mL volumetric flasks
Amber glass and/or plastic storage bottles (2)
2 kinds of pulp-free colourless or lightly coloured fruit juices that contain vitamin C
(~250 mL of each juice per student).
Cheese cloth.

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CHM 327 Name: ______________________
Procedure:
Prepare 1 mg/mL pure ascorbic acid (AA) stock solution to manufacture
Laboratory Fabricated Blank (LFB) Solutions:
Calculate the mass (g) of pure ascorbic acid (MM = 176.12 g/mol) required to
manufacture a 1 mg/mL ascorbic acid solution in 100.0 mL: __________________.
Weigh the ascorbic acid to the nearest 0.1 mg. Place the actual mass (g) weighed out in
Table 1.

Measurement of ascorbic acid in Juice:

1. Place the 0.005 M standard iodine solution in the 50.00 mL buret.
2. Obtain 250 mL of 2 different juice samples, (if necessary, strain juice through
cheese cloth if there is a lot of pulp), measure 50.0 mL of juice into a labeled 250
mL Erlenmeyer flask. Make four juice replicates of the 2 different juices each
containing 50.0 mL of juice. Dilute the four replicates of each juice to 100 mL
with deionized water. (Record the total volume of juice on the bottle).
3. Place 15.00 mL of 1 mg/mL ascorbic acid solution into a labeled 250 mL
Erlenmeyer flask. Make four LFB solutions. Dilute each solution to 100 mL with
deionized water.
4. Add the required amount of starch solution to each flask (up to 5 drops).
5. Titrate all solutions with standard 0.005 M iodine solution just until the iodine-
starch colour appears (for at least one minute). Record all data in Table 1.
6. Do a blank titration with water and starch indicator. Subtract Vblank from all VI2
final volumes.

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 CHM 327 Name: ______________________
Lab 12 - Raw Data sheet must be signed by instructor & handed in with Report.

Table 1 – Results of Vitamin C Analysis of Juice

M I2 _________ (from Lab #11) Vblank = _____________ mL
Name of Juice 1: ___________________________
VJuice1 Bottle __________mL
Name of Juice 2: ___________________________
VJuice2 Bottle = __________mL
True Mass AA in Juice 1 is ______ mg / _____ mL.
True Mass AA in Juice 2 is ______ mg / _____ mL.
Purity AA ________ % Mass (g) AA in 100.0 mL: _________________
Purity Corrected Mass (mg) AA in 100.0 mL: _________________

Aliquot True corr Exp % s and Corr % Avg s and

Smp from Mass VI2 VI2 VI2 VI2 Mass % recovery CV Mass Diff. % Diff CV
ID S or J AA init final total total AA recovery Avg (%) AA (True (%)
(mL) (mg) (mL) (mL) (mL) (mL) (mg) (mg) &
From Expt)
Bottle
Blank
LFB1 15.00 s=

LFB2 15.00 CV =

LFB3 15.00

LFB4 15.00

Juice 1 50.0 s=
Rep1
Juice 1 50.0 CV =
Rep2
Juice 1 50.0
Rep3
Juice 1 50.0
Rep4
Juice 2 50.0 s=
Rep1
Juice 2 50.0 CV =
Rep 2
Juice 2 50.0
Rep3
Juice 2 50.0
Rep 4

Calculations are to be completed before leaving the lab.

Workstation/scales clean: _________________________________________

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CHM 327 Name: ______________________

Lab #12 Prelab and Flow Chart

Analysis of Vitamin C in Juice
To be completed in Lab Notebook:
1) Purpose: Briefly state the purpose of the experiment.
2) Materials/Chemicals: In this section, list any specific equipment that is required,
or chemical information that is important for the lab. (ie. Chemical name, CAS#,
MW, molecular formula, bp, mp, etc. ) Be sure to state the source of your
information.
3) Safety Hazards and Precautions: In this section, list any safety hazards that might
arise in the lab, including from chemicals or equipment. (hint: most of this
information is found in the chemical SDS.)
4) Balanced Equations: In this section include balanced equation for all reactions
involved in the experiment. For lab 12 this includes (ascorbic acid + I2).
5) Calculations: In this section include all calculations for standards and reagents
required to begin the experiment. Be sure to show all work! For lab 12 complete
the following calculations:
A) Calculate the mass of ascorbic acid (MW = 176.12 g/mol) required to
manufacture 100.0 mL of a 1 mg/mL ascorbic acid solution.
6) Flowchart: Construct a flowchart for the lab. This should NOT be a reproduction
of the manual, but instead a graphical summary of the major steps. (NOTE: Do
not rewrite procedure word for word.)

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CHM 327 Name: ______________________

CHM 327 Lab #12

Analysis of Vitamin C in Juice

Laboratory Report Requirements (Total 30 marks; 20 for Report + 10 for Accuracy)

Lab Report Format (2 marks)

- Title Page: Title of the experiment (center of page); At the bottom right: Your name,
course and section, date of experiment.
- Headings: Each section is clearly defined with the heading that is bolded or
underlined. (Purpose, Theory, Results, Discussion, etc..)
- Figures and Tables: Must be formatted in ACS style. Each table must have a # and
title at the top, and each figure will have a #, title and legend at the bottom. Include
references if they are not your own work.
- Spelling & Grammar: Text must be written in sentence format with proper spelling
and grammar.
- References: Cite all information throughout report with a superscripted number
corresponding to the source included in the reference section, in ACS format.

Purpose (0.5 marks)

• State the analytical target and the method of analysis, the name brands of each juice
and the vitamin C content of each.

Theory (5 marks)
• Provide the structure of ascorbic acid and give a description of the importance of
vitamin C in the body.
• Give reaction equation for ascorbic acid with I2 and explain reaction in words.
• Describe what a redox titration is and how it relates to the analysis of vitamin C with
iodine.
• Describe how the starch indicator works to indicate the presence of iodide.
• Provide 3 applications that require the determination of Vitamin C.
• Include all references.

Results (5 marks)
• Reproduce Tables 1 that was filled in during the experiment.
• Give sample calculations for:
o Purity corrected mass for AA.
o True mass of AA in LFB1.
o Experimental mass AA in LFB 1.
o % Recovery LFB1.
o True mass of AA in Juice1 Rep1.
o Experimental mass AA in Juice1 Rep1.
o Corrected mass of AA in Juice1 Rep1.
o % difference for true mass of AA and experimental mass of AA in Juice1 Rep1.

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CHM 327 Name: ______________________

Discussion (5 marks)
• Discuss the % recovery obtained for the LFB (state actual value) and what this value
means.
• Discuss what happened during the titration as iodine was added both the reactions that
occurred and why the solution eventually turned blue-black.
• Discuss the vitamin C results for each juice (state actual values), what was the %
difference from the value stated on the bottle.
• Discuss the precision observed with this method for the LFB and the two juice samples
(s and CV).
• Discuss 3 possible sources of error why your % recovery for you LFB was not exactly 100
% and why your % difference for your juice sample may have been greater than 0.

Conclusion (0.5 marks)

• State the results, (% recovery) of the vitamin C in your LFB and your two juice samples.

Notebook: Flow Chart and Prelab (2 marks)

You must attach all initialed data sheets, questions and flow chart with lab report or
marks will be deducted!!!

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CHM 327 Name: ______________________
Lab #13
Optimization of Coagulation and Flocculation Parameters
for the Jar Test

Method References: ASTM D 2035-08

Safety: This laboratory involves the use of extremely corrosive substances. The use of
personal protective equipment such as gloves, coat and safety glasses are necessary.
Solutions such as concentrated acids should be dispensed from a designated area (such as
a fume hood). Follow instructions regarding waste handling and disposal.

Method Summary: The jar test optimizes the concentrations of the agents employed to
treat water through coagulation and flocculation processes in order to separate the
suspended solids portion from the water.

Apparatus and Reagents

Jar Test 6-position speed-controlled lighted base mixer with (6) 1.5 L capacity beakers.
ACS grade aluminum sulfate and calcium oxide
Ten (10) 10 mL graduated cylinders for reagent dispensing (150 mL beakers (6))
100 mL graduated cylinder
Disposable plastic pipettes.
Diatomaceous earth (clay) or Bentonite Solution (0.1 g/L)
Ferric Chloride.
1N Sulfuric Acid
1N NaOH
Turbidity Meter and Measurement Vials
pH Meters (6)

Part 1: Preparation of Reagents and Material for Coagulation and Flocculation

1. Put 2.00 g Ferric Chloride (FeCl3·6H20) into 1 L of aqueous solution. This
solution delivers 2.00 mg ferric chloride per mL.
Part 2: Procedure for the determination of the optimum dosing of FeCl3. (Work in
groups of 2 or 3 to prepare two beakers for the Jar test).

1) Finely grind some clay using a mortar and pestle and weigh 0.20 g of the clay for
each beaker into a weigh boat (on top loader balance).
2) Using a graduated cylinder, pour 1 L of tap water (not DI) into a 1.5 L beaker.
Once all groups are ready, we will put all 6 beakers under the stirrer.
3) While the stirrer is set for rapid mixing (~150 rpm), add the 0.2 g of clay to each
beaker and allow mixture to spin for about 1 min to ensure the clay is completely
dispersed. This is the reference. If the clay settles to the bottom, it was not ground
finely enough.
4) Measure the initial pH in all 6 beakers. Adjust the pH to pH 7.00 +/- 0.05. Record
final pH’s for all solutions in table 1 for reference.

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CHM 327 Name: ______________________
5) Place all beakers under the paddle machine. Turn on the stirrers to (~ 150 RPM)
for 1 min to resuspend any clay that settled. While still stirring, take a sample
from each beaker and measure the turbidity of all 6 beakers as a reference and
record values in Table 1.
6) Decrease the stirrers to (~100 RPM). Beaker 1 will be the reference do not add
any solution to this beaker. While stirring, add increasing amounts of the prepared
coagulation/flocculation solutions to the remaining 5 beakers. Have all solutions
ready and add at the same time if possible. (5 mL, 10 mL, 25 mL, 50 mL and 100
mL of 2mg/mL FeCl3 solution).
7) After dosing each beaker stir for 30 sec at 100 RPM to simulate the static mixer in
a water treatment plant. (Record observation in Table 1).
8) After 30 sec reduce speed to match conditions for flocculator in water treatment
plant for 15 min (~25-30 RPM). (Record observation in Table 1). (Comment on
rate of formation of flock, flock size, amount of flock, rate of settling of flock,
turbidity etc.)
9) After flocculation stage complete, remove stirrers and allow sediment to settle for
20 min.
10) After sedimentation complete, check the turbidity in each jar to determine the
optimal concentration of coagulant and record your value and all observation in
Table 1.
11) Determine what the optimum dose of coagulant solution was from Part 1 to be
used in part 2. (Which FeCl3 dose provided the lowest turbidity reading?)

Part 3: Procedure for the determination of the optimum pH with the optimum dose
of FeCl3 determined in Part 2. (Work in groups of 2 or 3 to prepare two beakers for
the Jar test).

1) Finely grind some clay using a mortar and pestle and weigh 0.20 g of the clay for
each beaker into a weigh boat (on top loader balance).
2) Using a graduated cylinder, pour 1 L of tap water (DI water) into a 1.5 L beaker.
Once all groups are ready, we will put all 6 beakers under the stirrer.
3) While the stirrer is set for rapid mixing (~150 rpm), add the 0.2 g of clay to each
beaker and allow mixture to spin for about 1 min to ensure the clay is completely
dispersed. This is the reference. If the clay settles to the bottom, it was not ground
finely enough.
4) Adjust the pH in 1 beaker to pH 7.00 +/- 0.05. Record final pH’s for all solutions
in table 1 for reference.
5) Adjust the pH of 3 beakers using 1N Sulfur acid to pH 4.00, pH 5.00 and pH 6.00
+/- 0.05. Record final pH’s for the 3 beakers in Table 2 for reference.
6) Adjust the pH of 2 beakers using 1N NaOH to pH 8.00, and pH 9.00 +/- 0.05.
Record final pH’s for the 2 beakers in Table 2 for reference.

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CHM 327 Name: ______________________
7) Place all beakers under the paddle machine. Turn on the stirrers to (~ 150 RPM)
for 1 min. Measure the turbidity of all 6 beakers as a reference and record values
in Table 2.
8) Decrease the stirrers to ~100 RPM and while stirring, add optimum dose of
coagulation/flocculation solutions from Part 2 to all 6 beakers. Have all solutions
ready and add at the same time, if possible.
9) After dosing each beaker stir for 30 sec at 100 RPM to simulate the static mixer in
a water treatment plant. (Record observation in Table 2).
10) After 30 sec reduce speed to match conditions for flocculator in water treatment
plant for 15 min (~25-30 RPM). (Record observation in Table 2). (Comment on
rate of flock formation, flock size, amount of flock, rate of settling of flock,
turbidity etc.)
11) After flocculation stage complete, remove stirrers and allow sediment to settle for
20 min.
12) After sedimentation complete check the turbidity in each jar to determine the
affect of pH on the formation of floc and record your value and all observation for
how pH affected flocculation and settling in Table 2.
13) Determine what the optimum pH for coagulation and flocculation with ferric
chloride is given the optimum dose. (Which pH provided the lowest turbidity
reading?)

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CHM 327 Name: ______________________

Lab 13 - Raw Data sheet must be signed by instructor & handed in with Report.

Table 1. Observations and Turbidity Data Using Ferric Chloride for Coagulation
and Fluctuation of Wastewater.

Jar Mass of Initial Initial Observations during Final Observation of final

# FeCl3 added pH Turbidity Jar Test Turbidity solutions
per L of water
(mg)
1

Optimum FeCl3 dose: ________________________(mg/L).

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CHM 327 Name: ______________________
Lab 13 - Raw Data sheet must be signed by instructor & handed in with Report.

Table 2. Observations and Turbidity Data Optimum pH for coagulation and

flocculation using Optimum FeCl3 dose.

Optimum FeCl3 dose from Part 2: ___________________________.

Jar Mass of FeCl3 pH Initial Observations during Final Observation of final

# added to 1 L Turbidity Jar Test Turbidity solutions
of water
(mg)
1

Optimum pH for FeCl3 as coagulant: ________________________.

Workstation/scales clean: _________________________________________

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CHM 327 Name: ______________________

Lab #13 Prelab and Flow Chart

Jar Test for Treatment of Water
To be completed in Lab Notebook:
1) Purpose: Briefly state the purpose of the experiment.
2) Materials/Chemicals: In this section, list any specific equipment that is required,
or chemical information that is important for the lab. (ie. Chemical name, CAS#,
MW, molecular formula, bp, mp, etc. ) Be sure to state the source of your
information.
3) Safety Hazards and Precautions: In this section, list any safety hazards that might
arise in the lab, including from chemicals or equipment. (hint: most of this
information is found in the chemical SDS.)
4) Flowchart: Construct a flowchart for the lab. This should NOT be a reproduction
of the manual, but instead a graphical summary of the major steps. (NOTE: Do
not rewrite procedure word for word.)

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CHM 327 Name: ______________________

CHM 327 Lab #13

Optimization of Coagulation and Flocculation Parameters for the Jar Test
Laboratory Report Requirements (Total 20 marks for Report)

Lab Report Format (2 marks)

- Title Page: Title of the experiment (center of page); At the bottom right: Your name,
course and section, date of experiment.
- Headings: Each section is clearly defined with the heading that is bolded or
underlined. (Purpose, Theory, Results, Discussion, etc..)
- Figures and Tables: Must be formatted in ACS style. Each table must have a # and
title at the top, and each figure will have a #, title and legend at the bottom. Include
references if they are not your own work.
- Spelling & Grammar: Text must be written in sentence format with proper spelling
and grammar.
- References: Cite all information throughout report with a superscripted number
corresponding to the source included in the reference section, in ACS format.

Purpose (0.5 marks)

• State the purpose of lab and the method of analysis.

Theory (5 marks)
• Explain what coagulation and Flocculation are.
• Describe what the jar test is and what it is used for.
• What are two common problems that water treatments plants may use a jar test to
solve for.
• Discuss two common reagents that may be added to help coagulate/flocculate
wastewater.
• Explain how a turbidity meter work.
• Include all references.

Results (4 marks)
• Reproduce Table 1 and 2 that were filled in during the experiment, include all
observations.

Discussion (6 marks)
• What was the purpose of adding ferric chloride solution? How does it work?
• How did pH affect your results? Explain.
• Discuss the trends you noticed in your observations (comment on amount of floc, floc
size, rate of settling, clarity of water for each test etc.). How did your final solutions
compare to the reference beaker?
• Discuss how the turbidity of the water changed from the initial value to final value for
each beaker and coagulation/fluctuation solution used.
• Which FeCl3 dose and pH provided the most economical results, explain why?
• Discuss an additional reagent that could have been added and explain what it does?

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CHM 327 Name: ______________________

Conclusion (0.5 marks)

• State which FeCl3 dose and pH would be the most economical choice for a wastewater
treatment plant to use on this type of water sample.

Notebook: Flow Chart and Prelab (2 marks)

You must attach all initialed data sheets, questions and flow chart with lab report or
marks will be deducted!!!

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