CMI533 Background Theory WN2017

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY
SCHOOL OF BIOLOGICAL SCIENCES AND APPLIED CHEMISTRY
CMI533: Background Theory to Lab Projects (WN2017)

Laboratory Project 1: Atomic Absorption Spectrophotometry
GOAL OF THIS EXPERIMENT:
Familiarize the student with:
a) flame/furnace atomic absorption spectrophotometry
b) a nebulizer system (common to Flame AAS, ICP, and flame photometry)
c) the idea that analytical sensitivity depends on the choice of absorption line
(the electronic transition)
d) quality control
Discussion : Atomic absorption Spectrophotometry is based on the fact that each element has
a unique electronic structure and will therefore absorb radiation characteristic of the energy
level difference between the ground electronic state and an excited electronic state.
In order to evaluate the atomic form of the element, flame atomic absorption involves
aspirating solutions of metal ions into a flame where heat and reducing conditions convert the
sample into a cloud of atoms. lf light corresponding to the resonance (excitation) wavelength
is passed through the cloud of atoms, some of the light will be absorbed. The extent of
absorption is measured by the detector.
Most atomic absorption spectrophotometers are single beam systems and have 4 main parts:
1. a source of characteristic radiation
a. A hollow cathode lamp which contains a cathode composed of the
same metal as we are trying to analyze in our samples (i.e. if we wish to analyze
copper in our samples, we choose a copper hollow cathode lamp) is used.
Monochromatic light is emitted by these lamps.
2. an atomizer
a. The atomizer provides a means of turning our liquid sample into a cloud of atoms.
Only if the sample is in atomic form can we guarantee that we are studying atomic
absorption and not some form of molecular absorption.
3. an analyzing device
a. We have a monochromator present to ensure that we only look at specific
wavelengths
4. a detector
a. We use a photomultiplier tube to detect changes in light intensity from the source
and then convert these changes into electrical signals.
This laboratory exercise will involve:
a) familiarizing the student with the setup and operation of a flame and furnace atomic
absorption spectrophotometer.
b) analyzing copper standards at the primary (lowest energy electronic transition) wavelength
and at the secondary (next highest energy electronic transition) wavelength, in order to
demonstrate the difference in analytical sensitivity at different wavelengths of analysis.
c) analyzing an unknown solution
d) analyzing 2 fertilizers in order to evaluate the manufacturer's claim of analysis
e) familiarize the student with a standardized procedure for decomposition and analysis of
pills containing chromium picolinate and manganese salts.
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CMI533: Background Theory to Lab Projects
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In the first week's lab, you will prepare standards and samples. ln the second week's lab you
will run all of Experiment 1 and Experiment 2.
AA Experiment 1: Beer-Lambert Calibration Curve Using the Buck 210 Spectrophotometer
All spectrophotometric work normally involves:
a) working at the wavelength of maximum absorption and
b) working in the linear range of the species (the region in which Beer's Law is obeyed i.e.
when absorbance is directly proportional to concentration)
As stated above, each element has a characteristic absorption spectrum. The strongest of the
absorption lines are generally used during analysis. For example, if you wished to determine the
concentration of copper in a sample of drinking water, you would use the 324.8 nm copper
absorption line.
In the following experiment, you will prepare a series of copper standards and analyze them at
324.8 nm. From this data you will determine the linear working range for copper at this
wavelength.
Preparation of Working Standards
1. 100 ppm intermediate copper standard: Prepare at least 200 mL of a 100 ppm copper
standard using the 1000 ppm copper stock solution. Dilute with 2% nitric acid. Mix
thoroughly and store in a clean plastic bottle.
2. Working Standards: Prepare 100 mL of each of the following copper standards from the
100 ppm intermediate and transfer to 60 ml plastic bottles : 0, 0.5, 1, 2, 4, 5, 8, 10, 15,
20, 30, 40 ppm copper. All dilutions are to be made with 2% nitric acid.
3. Higher Concentration Standards: Prepare 50 mL or less of the following standards: 100
(use some of your intermediate standard), 200, 300, 400 ppm copper. Use the 1000
ppm standard to prepare these, and use 2% nitric acid as the diluent. Store in plastic
bottles.
Preparation of Fertilizers
Assuming that the fertilizers contain about 0.05% copper, dissolve an appropriate
amount of each fertilizer in deionized water to produce a solution that 'should' contain
about 2.5 ppm of copper. Note: prepare a different fertilizer for each group member.
The person whose last name is first alphabetically is responsible for fertilizer number 1; the
second person for fertilizer number 2, etc.
Analysis of the Cu Unknown
We will determine the concentration of the unknown at 324.8 nm after you have diluted it
using the information which you obtained from the 249.2 nm line.
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AA Experiment 2 : Analysis of Pills Containing Chromium Picolinate

In the third week, we will move to the Varian Flame system (the SpectrAA 220FS). This
experiment will involve following the USP for analysis of for chromium picolinate.
Preparation of Working Standards
1. 100 ppm intermediate chromium standard : Prepare at least 200 ml of a 100 ppm chromium
standard using the 1000 ppm chromium stock solution. Dilute with 2% nitric acid. Mix thoroughly
and store in a clean plastic bottle.
2. Working Standards: Prepare 100 ml of each of the following chromium standards from
the 100 ppm intermediate and transfer to 60 mL plastic bottles: 0, 2, 4, 6, 8, 10, 20 ppm chromium.
All dilutions are to be made with 2% nitric acid. NOTE: Save some of
the 100 ppm standard.
3. Digestion of Pills Containing Chromium Picolinate
a) Accurately weigh each pill and place in separate 100 mL volumetric flasks.
b) Add approximately 5.0 mL of deionized water and approximately 5.0 mL of concentrated
nitric acid (do this in the fume hood). Do not shake or swirl these solutions; you will end
up with powder from the pill on the sides of the volumetric that will not be properly digested.
c) Remove the caps from the volumetric flasks. In the fume hood, place these volumetric
flasks onto a hot plate and allow to boil gently for 20 minutes (a setting of about 4 on the
newer hotplates). Make sure that someone is watching these solutions to ensure that they
do not boil violently. NOTE: not all of the pill will dissolve; there will be a slight white
residue. You are not affecting a complete dissolution of the pill, but a digestion. This
digestion does effectively solubilize the chromium.
d) Allow these solutions to cool and then dilute to the mark with deionized water.
e) Set up a funnel stand and place a slow filter paper into each funnel. Dampen each filter
paper with deionized water and then place waste beakers to collect the first few millilitres
of sample solution being filtered. Discard this initial solution and collect the rest of the
filtrate into separate 60 mL plastic bottles. Collect at least 50 mL of each sample.
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AA Experiment 3: Analysis of Nails Containing Manganese

In the fourth week, we will move from the Varian Flame system to the Varian furnace atomic
absorption spectrophotometer (the SpectrAA Zeeman 220).
1. 1.0 ppm intermediate manganese standard : Prepare 100 mL of a 1.0 ppm manganese
standard using the 1000 ppm manganese stock solution.
2. Working Standard: Prepare a 30 ppb Mn standard. Make this standard from the 1.0 ppm (1000
ppb) Mn standard using the ANALAR nitric acid for your dilution.
3. Digestion of Nails Containing Manganese
a) Obtain these nails from your instructor.
b) Accurately weigh each nail and place in a separate 100 mL beaker.
c) Cautiously add approximately 10.0 mL of concentrated hydrochloric acid to each beaker
(do this in the fume hood). Do not shake or swirl these solutions.
d) In the fume hood, place these beakers onto a hot plate at a setting of about 2 and heat
until the nail is completely dissolved (a setting of about 4 on the newer hotplates). Make
sure that someone is watching these solutions to ensure that they do not go dry or boil
vigorously. This dissolution of the nail will take about 20 minutes.
e) Now continue to heat these solutions until the first crystals of salt appear in the beaker there will be a few millilitres of acid left at this point. Do not allow the solution to go dry.
Carefully remove the beaker from the hot plate and allow it to cool in the fumehood for
about one minute.
f)
Cautiously add approximately 2.0 mL of concentrated nitric acid to each beaker. Do this
in the fumehood. You may see some brown nitrous oxide gas evolving from the beaker.
Do not breathe this gas.
g) Quantitatively transfer each solution to a 100 mL volumetric and fill to the mark with
deionized water. (By "Quantitatively transfer", l mean that you add a small amount of water
to the original beaker from step f. Carefully pour all of this solution into the volumetric. Now
add some more water to the beaker and pour this into the flask. Continue to do this until
you are sure that all of the original solution has been transferred to the flask.)
h) Set up a funnel stand and place a slow filter paper into each funnel. Dampen each filter
paper with deionized water and then place waste beakers to collect the first few (!)
millilitres of sample solution being filtered. Discard this solution and collect the rest of the
filtrate into separate 60 mL plastic bottles. Collect at least 50 mL of each sample.
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Concepts Involved ln Lab #1

We stated that each element has a unique electronic configuration. This means that, besides
variations in the number of electrons, the distances between the various energy levels varies
with the element.
Now consider the process of an atom absorbing energy. We said earlier that an atom can only
absorb energy if the electron is hit with just the right magnitude of energy, and if there is a
vacancy for this electron to move to. Since all inner electron shells are filled, only the outer
valence electrons are capable of moving to vacancies. Therefore we depict the atom absorbing
energy as follows:
In the case of copper, this energy corresponds to light having a wavelength of 324.8 nm.
However, we should realize that an electron could also absorb energy and move to a higher
electronic level. In fact, if copper atoms are hit with a higher energy (corresponding to light
having a wavelength of 249.2 nm), the electron will move to the second excited electronic
level.
However, since it is easier for electrons to move to the first excited electronic level than to the
second, one would expect more atoms would absorb the 324.8 nm radiation than would
absorb the 249.2 nm radiation. Since Atomic Absorption Spectrophotometry actually involves
counting the number of atoms that absorb at a given wavelength, one would expect a higher
absorbance value for a solution of copper at 324.8 nm than for the same solution at 249.2 nm.
Therefore the calibration curves at the two wavelengths will look something like:
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This is in fact what is seen. Also worth noting is the fact that because the curve at 324.8 nm rises
faster than the other curve (i.e. has a higher slope), it will begin to deviate from Beer-Lambert Law
faster than the curve at 249.2 nm. Therefore, while the sensitivity is poorer for the 249.2 nm line,
its response is linear over a wider range of concentrations.
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Laboratory Project 2: Atomic Emission Spectrophotometry

a) Inductively Coupled Plasma atomic (or optical) emission spectrophotometry (AES or OES)
b) a nebulizer system (common to Flame AAS, ICP, and flame photometry)
c) the idea that analytical sensitivity depends on the choice of absorption line
(the electronic transition)
d) quality control
Discussion: ICP-AES is an emission spectrophotometric technique, exploiting the fact that
excited electrons emit energy at a given wavelength as they return to ground state. The
fundamental characteristic of this process is that each element emits energy at specific
wavelengths peculiar to its chemical character.
Although each element emits energy at multiple wavelengths, in the ICP-AES technique it is most
common to select a single wavelength (or a limited few) for a given element. The intensity of the
energy emitted at the chosen wavelength is proportional to the amount (concentration) of that
element in the analyzed sample. Thus, by determining which wavelengths are emitted by a
sample and by determining their intensities, the analyst can quantify the elemental composition
of the given sample relative to a reference standard.
However, as elements have more than one characteristic emission wavelength, an analyst must
be careful that primary emission wavelengths (the lowest energy or most common transition)
selected for analysis do not overlap with secondary and tertiary emission wavelengths of other
elements present in the samples and standards.
ICP-AES analysis requires a sample to be in solution. Thus, water can be analyzed simply,
requiring only dilution in most cases. Igneous rocks, sedimentary rocks, and sediments,
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however, must be dissolved. One must take care that elements present in the standards and/or
sample do not have solubility or reactive incompatibilities with analytes of interest.
All ICP-AES systems consist of several components.
Source: Analytical Instruments Image By: Unknown
Sample Introduction system: The sample introduction system on the ICP-AES consists of a
peristaltic pump, Teflon tubing, a nebulizer, and a spray chamber. The fluid sample is pumped
into the nebulizer via the peristaltic pump. The nebulizer generates an aerosol mist and injects
humidified Ar gas into the chamber along with the sample. This mist accumulates in the spray
chamber, where the largest mist particles settle out as waste and the finest particles are
subsequently swept into the torch assembly. Approximately 1% of the total solution eventually
enters the torch as a mist, whereas the remainder is pumped away as waste.
Plasma Torch: The fine aerosol mist containing Ar gas and sample is injected vertically up the
length of the torch assembly into the plasma. The radio frequency-generated and maintained Ar
plasma, portions of which are as hot as 10,000 K, excites the electrons. When the electrons return
to ground state at a certain spatial position in the plasma, they emit energy at the specific
wavelengths peculiar to the sample's elemental composition.
Analyzing Device & Detector: The plasma is viewed horizontally by an optical channel. Light
emitted from the plasma is focused through a lens and passed through an entrance slit into the
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spectrometer.
There are two types of spectrometers used in ICP-AES analysis: sequential (monochromator)
and simultaneous (polychromator). Our instrument is a sequential ICP-AES. A sequential
spectrometer means that the diffraction grating in the spectrometer is analogous to a prism that
refracts visible light into its component colors. The detector (photomultiplier tube) is fixed in space
at the far end of the spectrometer. Rotation of the diffraction grating sequentially moves each
wavelength into the detector. The computer control ensures that the detector is synchronized with
the grating so that the intensity at the detector at any given time is correlated with the wavelength
being diffracted by the grating. The operator enters the wavelengths that he or she wishes to
detect into the computer, the grating sequentially moves to the specified wavelengths, and the
energy intensity at each wavelength is measured to provide a quantitative result that can be
compared to a reference standard. Using standard spectroscopic techniques (e.g., background
corrections), sequential ICP-OES can provide extremely flexible and rapid analysis of many
chemical elements.
Common ICP-AES Applications include:
Ores, Rocks & Minerals: Acid digestion (aqua regia) or fusion/flux preparation of soil, ore and rock
(geological, metallurgical and archaeological) samples to analyze base & noble metals
(specifically, in the case of ores, Au & Ag) and trace elements, provenance studies of geological
and archaeological siliceous materials
Water & Effluents: Analysis of drinking water/wastewater samples for trace and major elements
Environmental / Occupational Samples: Analysis of trace elements & metals in workplace air /
water samples as per NIOSH Manual of Analytical Methods)
This laboratory exercise will involve:
a)
familiarizing the student with the setup and operation of an ICP atomic emission
spectrophotometer.
b)
preparation and analysis of multi-element standards and an unknown solution
c)
familiarize the student with USP procedure for decomposition and analysis of multivitamin
pills in order to evaluate the manufacturer's claim of analysis
d)
understand and anticipate matrix interference effects
In the first week's lab, you will prepare your multi-element standards and samples and familiarize
yourself with the ICP software of you have time. ln the second week's lab you will analyze all your
prepared solutions, unknowns and spiked solutions.
Analysis of Various Metals and Minerals in a Multivitamin Pill
In the following experiment, you will prepare a series of multi-element standards and multivitamin
pill samples to determine the mass and concentrations of these elements in your pill. This is often
a requirement to meet Good Manufacturing Practices (GMP) guidelines.
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First, it is used to confirm and verify the amounts of minerals present and ensure the product is
properly labelled. It also confirms that the product complies with regulations related to its
manufacture and distributions. Lastly, it confirms that the product is safe for consumption and has
not been contaminated or tampered with. Inductively coupled plasma optical emission (ICP-OES)
spectroscopy provided a rapid way to analyze many minerals simultaneously in commercial
products at trace (ppb) levels.
Analysis of Multivitamin Pills
A.
Preparation of Working Standards and Digestion of Pills
You will be provided with 1000 ppm standards of the following: Mn, Cu and Ca. What were they
made from?
1.
1000 ppm sodium standard: Prepare at least 1000 mL of a 1000 ppm sodium standard
using solid NaCl. Weigh out the appropriate amount and dilute with 2% nitric acid. Mix
thoroughly and store in a clean plastic bottle. Be sure to calculate the actual concentration of
your solution based on what you actually weighed.
2.
1000 ppm potassium standard: Prepare at least 1000 mL of a 1000 ppm potassium
standard using solid KCl. Weigh out the appropriate amount and dilute with 2% nitric acid. Mix
thoroughly and store in a clean plastic bottle. Be sure to calculate the actual concentration of
your solution based on what you actually weighed.
3.
Preparation of Working Multi-Element ICP Standards: Prepare THREE mixed standards
of varying concentration (to be determined by you, the analyst). In terms of volume, make at
least 250mL of each, but the final volume is up to you. These standards must include some
amount of all of the above elements (Mn, Cu, Ca, Na & K) and are to be made up in 2% Nitric
Acid. The following are the maximum concentrations to be used:
Calcium: 250ppm max. concentration
Copper: 25ppm max. concentration
Manganese: 50ppm max. concentration
Potassium: 100ppm max. concentration
Sodium: 150ppm max. concentration
For example, you final ICP mixed working standard (STD 3), should contain these elemental
concentrations. You mixed working standards 1 & 2 will contain all of these elements in lesser
amounts (but not 0ppm!) to be determined by you. Stores these working standards in plastic
bottles.
4.
Digestion of Multivitamin Pills
Obtain pills from your instructor. Accurately weigh each pill (one per group member) and place
in separate 100mL beaker. EACH STUDENT IN THE GROUP WILL ANALYZE THEIR OWN
PILL.
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a) Cautiously add approximately 15.0 mL of concentrated hydrochloric acid to each beaker

(do this in the fume hood with gloves on!). Do not shake or swirl these solutions; you
will end up with powder from the pill on the sides of the volumetric that will not be properly
digested. In a fourth beaker (with no pill), add the same amount of concentrated HCl. This
will be your sample blank. Carry out the following steps with this sample blank alongside
your samples.
b) In the fume hood, place these beakers onto a hot plate at a setting of about 3 and heat
until the pill is completely dissolved (a setting of about 4 on the newer hot plates). Make
sure that someone is watching these solutions to ensure that they do not go dry or boil
vigorously. This dissolution of the pill will take at least 20 minutes, perhaps more. Note:
not all of the pill will dissolve; there will be a waxy yellow residue. You are not affecting
a complete dissolution of the pill, but a digestion. This digestion should effectively
solubilize the elements of interest.
NOTE: if you are using the DigiPREP digester, place your samples pills into the provided
disposable digestion tubes (no lid) and run the digestions sequence of 45 minutes at
105C. Make sure that someone is watching these solutions to ensure that they do not
go dry or boil vigorously.
c) Now continue to heat these solutions until there is approximately 1mL of solution left in
the beaker or tube. Do not allow the solution to go dry. Carefully remove the beaker
from the hot plate and allow it to cool in the fume hood for about one minute.
d) Cautiously add 2.0 mL of concentrated nitric acid to each beaker. Do this in the fume
hood. You will see some brown nitrous oxide gas evolving from the beaker or tube. Do
not breathe this gas.
e) When the digestion is complete, quantitatively transfer each solution to a 100 mL beaker
and fill to the 50mL mark with 2% nitric acid (provided). (By "Quantitatively transfer", I
mean that you add a small amount of 2% nitric acid to the original beaker from step 6).
Carefully pour all of this solution into the volumetric. Now add some more water to the
beaker and pour this into the flask. Continue to do this until you are sure that all of the
original solution has been transferred to the flask. Do you have any concerns?
f)
Set up a funnel stand and place a slow filter paper into each funnel. Dampen each filter
paper with 2% nitric acid and then place waste beakers to collect the first few (!) milliliters
of sample solution being filtered. Discard this solution and collect the rest of the filtrate
into a separate clean 100mL. When the collected solution has reached approximately
75mL, perform a quantitative transfer to a 100mL volumetric flask and dilute to the mark
with 2% nitric acid. Transfer the solution to 100 mL plastic bottles. Collect at least 50mL
of each sample.
g) Clean all glassware first with dH2O then with 1M NaOH if needed (provided) and again
with dH2O. NOTE: at the end of this process, you should have 100mL total volume of the
quantitatively transferred and filtered pill solution!
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h) Make diluted (1:100) working pill solutions (and sample blank!) by taking 10mL of your pill
solution and quantitatively transferring it solution to a 100 mL volumetric and fill to the
mark with 2% nitric acid (provided). Remember to do the same for your sample blank!
i)
Make spiked working pill solutions solutions (and sample blank!) by taking 10mL of your
original pill solution and quantitatively transferring it solution to a 100 mL volumetric. Add
the appropriate amount of your standards to add 5ppm of each element (except being
analyzed to your solutions. Fill to the mark with 2% nitric acid (provided). Remember to do
the same for your sample blank!
You should have 13 solutions to analyze now (if you are in a group of three). Three working
multi-element standards, three digested and diluted pill solutions, sample blank and three
spiked pill solutions and three diluted unknowns provided by your instructor.
5.
Emission Wavelength Selection Jan. 9, 2017
For the Winter 2017 Semester, use the following Emission Wavelengths:
Ca: 393.366nm
Cu: 327.396nm
Mn: 257.610nm
K: 766.491nm
Na: 589.592nm
Note the potential interferences and relative intensity of these selected emission lines
when developing your method. You will need this information when writing your lab
report!
To analyze your liquid unknown, make a 1:10 dilution of the provided unknown and
analyze alongside your pill samples.
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Laboratory Project 3: Fluoride Ion By Specific lon Electrode

a) the field of electroanalytical chemistry
b) the use of specific ion electrodes to determine fluoride ion in solution
c) the Nernst equation
d) Quality Control
Discussion: pH electrodes are specific for the determination of the hydrogen ion content of a
solution. Likewise, fluoride specific ion electrodes have been designed for the specific
determination of fluoride ions. READ the CONCEPTS section at the end of this experiment
before coming to the lab.
Unlike the various chloride compounds, most fluorides are sparingly soluble, and are therefore
present in most natural waters in only small amounts. Fluorides are also seldom found in large
quantities in industrial wastes, except as a result of spillage. The major use of fluorides is in the
area of insecticides, disinfectants and preservatives.
A fluoride concentration of approximately 1.0 mg/litre in drinking water is believed to be an
effective preventative of dental caries without harmful effects on health. In rare instances, the
fluoride concentration naturally occurring in drinking water may approach 10 mg/litre. Such
waters will cause discoloration in children's teeth and therefore the level of fluoride should be
reduced.
Among the many methods suggested for the determination of fluoride ion in water are the ion
selective electrode method and the zirconium-dye lake colorimetric method. The present
experiment will investigate the ion selective electrode method.
It is important to note that all solutions containing fluoride will be prepared in the presence of
a total ionic strength adjustment buffer (TISAB). This buffer has a number of functions
including:
1) maintaining a reasonably constant high ionic strength in all solutions
2) holding the pH of the solution to between 5.0 and 5.5
3) minimizing chemical interferences from sample matrix
Let us consider some of these issues further. Polyvalent cations such as Al(llI), Fe(lll) and Si(|V)
will complex fluoride ion. The extent to which complexing takes place depends on the pH of
the solution and the relative concentrations of the fluoride ion and the complexing species.
The citrate ion present in the buffer solution is actually intended to preferentially complex up
to 2 mg/L aluminum and release any bound fluoride as the free ion. ln acid solution, hydrogen
ion forms complexes with fluoride ion, but this complexing becomes negligible if the pH is
adjusted to above pH 5.0. In alkaline solution, the hydroxide ion also interferes with the
electrode response to fluoride ion whenever the concentration of hydroxide ion is greater than
1/10 of the concentration of fluoride ion present. However, at a pH of 8 or less, the hydroxide
concentration is 10-6 molar or less, and no interference with the fluoride ion by hydroxide has
been detected. Your TISAB buffer is therefore intended to deal with common interferences.
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Electrode Preparation: Make sure that the fluoride selective electrode is soaking in a solution of
50% deionized water, 50% TISAB buffer. Unacceptable drift in the readings will occur if the
electrodes have not been prepared in this way.
At the end of each lab make sure that you rinse out all bottles, glassware and beakers with
deionized water before putting them away.
Preparation of Solutions (Week 1)
1. Stock Fluoride Solution: 100 mg/mL fluoride (Note that this is NOT 100 mg/mL sodium
fluoride.): Dissolve the correct amount of anhydrous sodium fluoride (in deionized water and dilute
to 1 litre in a volumetric flask. Record your actual weight and the exact concentration. Transfer
this solution to a plastic bottle as soon as it is made.
Based on the actual mass of sodium fluoride that you used, calculate the exact concentration of
this stock solution, in ppm.
Note: Sodium fluoride is highly toxic. NaF is toxic in gram amounts if inhaled or ingested! Be
careful to wash your hands after this lab and before you eat. lf any sodium fluoride spills on your
hands, wash it off immediately.
2. Total Ionic Strength Adjustment Buffer: Prepare 2.0 litres of the TISAB buffer (prepare one litre
at a time) by mixing equal volumes of each of the following:
0.004 M sodium citrate
3 M sodium acetate
1 M acetic acid
Verify that the pH is between 5.0 and 6.0 using the supplied pH meter.
3. Working Standards: Using the 100 ppm fluoride standard, prepare the following standards:
0.5 ppm fluoride
1.0 ppm fluoride
2.0 ppm fluoride
3.0 ppm fluoride
5.0 ppm fluoride
10.0 ppm fluoride
14.0 ppm fluoride
16.0 ppm fluoride
20.0 ppm fluoride
Note: To prepare each solution, pipette the correct amount of one of the stock solutions into a
100 ml volumetric flask, add 50 ml of TISAB and dilute to the mark with deionized water. Shake
each solution and transfer each to a plastic bottle or directly into a plastic beaker. Record the
temperature of your TISAB.
Preparation of Mouthwash Samples (Week 2)
1. Record the brand of mouthwash that you are using. Also record its lot number.
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Preparation of Toothpaste Samples (Week 2)

1. Record the brand of toothpaste that you are using. Also record the lot number.
Concepts involved in Lab #3
The first issue to consider is: what exactly are we talking about when we say slope". When we
were dealing with spectroscopy we had the Beer-Lambert relationship:
A=bC
and we said that if we plotted absorbance versus concentration (A/C) the slope was b. After
we generated the calibration curve, we only had to measure the absorbance of our unknown
and we could read its concentration from the curve.
The idea is the same in electrochemistry except here we measure potential (voltage) instead of
absorbance. The law that we are now dealing with is the Nernst equation which gives us the
relationship between potential and concentration. At first it appears much more complex than the
Beer Lambert Law, but this equation can be simplified. According to the Nernst we can write:
E = E0 ((2.303 R T/nF) log (ion in reduced form)/(ion in oxidized form))
The E values represent the potentials (voltages) that we will be dealing with. T is temperature (in
degrees Kelvin), and R and F are constants (just as was). ln order to generate a calibration
curve, we will produce a set of standards and measure their potential, so lets re-write the equation
this way to see what the slope will be.
First, put the 2 values of potential on the same side of the equation.
E - E0 = -(2.303 R T)/(nF) log (ion in reduced form)/(ion in oxidized form)
Next, realize that fluoride ion, F-, in its oxidized form is F, which, by definition is given a value of
1 (all elements in their atomic form are given the value of 1, by definition). Therefore we can rewrite this equation, replacing E-E0 with the word 'potential' and replaced the 'concentration of
oxidized ion' with the number 1.
Therefore,
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Potential = -(2.303 RT)/(nF) Iog[F-]

Now, we want to plot 'Potential' versus 'Concentration', so that we can analyze our unknown. But
according to this equation, we should get a straight line if we plot log [concentration], instead of
just [concentration], this line should have a slope of:
Potential = slope = -(2.303 RT) log[F-]
nF
If we plug in values for the constants:
R = 8.314 volt coulomb K-1 mole-1
F = 96,487 coulombs mole-1
and lets assume for now that the temperature is 25C (= 298 K). If we do this, we end up with a
slope of -0.059. Therefore if the temperature of the lab is 25C and we analyze a series of fluoride
standards, we should get a slope of -0.059. (Always make sure that you use the actual
temperature, in Kelvin, when you use this equation.)
This is not quite as nice as our Beer-Lambert plot that started at 0 and increased with a positive
slope. This brings us to the reason why we do a slope check with the fluoride ion meter. At the
beginning of each day, you want to do some kind of fast check to see if you are doing everything
right. Therefore, you quickly make 2 standards and analyze them to see if the slope between them
is -0.059 (assuming 25C). If you get a value close to this, then you know that everything is going
as planned. If you do not get this value, then you quickly check to make sure that you are making
your standards correctly. You also check and make sure that the electrodes were plugged in
correctly. Of course, in order to check the slope you would have to plot the values on a graph and
then calculate the slope. This takes too much time (we have better things to do). We would prefer
that the instrument work out our slope for us. This is the reason for the rather strange procedure
we go through in the slope check.
CMI533 WN 2017
Page 16 of 32

Remember that:
slope = y2 - y1 = potential1 - potential2
x2 - x1 log [F-]1 - log[F-]2
Experimentally, the first thing you do is analyze a blank and end up with a large positive
number (+140 to +170). This represents the potential of the solution, but note that this
number is in millivolts, not volts, the way the Nernst equation is written. Now you check the
solution containing 1 ppm fluoride and end up with a potential around +10 to +40. This
represents the potential of your first standard (in millivolts). Therefore, for example
(potential)1 = +40
[F-], = 1 ppm, therefore log [1] = 0
At this point we force the potential to read 0.0 millivolts, which forces the curve to start at
(0,0), the same as a Beer-Lambert plot. Now, we analyze a 10 ppm standard and measure the
potential. Lets say we get -60.3 millivolts. Now, lets look at our slope:
slope = (0.0 (-60.3))
(0.0 - log[10 ppm])
and, log[10] = 1
Therefore our slope = -60.3, the potential of our second standard. Note that this is in millivolts
so if we converted this to volts (to satisfy the Nernst equation) by dividing by 1000, we end up
with a slope of -0.060. We can then say that this slope is close to the ideal value of -0.059,
with differences due to all of the experimental errors, including temperature, which may not
have been 25C. You should always recalculate what the ideal value should be, by substituting
the actual temperature (in Kelvin) into the Nernst equation.
This exercise can be seen below, if we plot the original values against the same line forced to
pass through 0.0. Note that the slope of both lines is the same (all parallel lines have the same
slope).
CMI533 WN 2017
Page 17 of 32

CMI533 WN 2017
Page 18 of 32

Laboratory Project 4: Measurement of Oxidation/Reduction Potentials Using a

Potentiometer
a) the field of electroanalytical chemistry
b) the idea of redox reactions (oxidation/reduction reactions)
c) the Nernst equation
d) the use of a redox electrode (an electrode capable of measuring redox potential)
e) the use of quinhydrone as a calibration standard
Discussion: The measurement of oxidation/reduction potentials is referred to as redox
measurement. Remember that oxidation involves the loss of electrons and reduction involves
the gain of electrons. Common examples are hydrogen peroxide as an oxidizing agent and
hydrogen sulfide as a reducing agent.
A redox measurement is, in fact, very similar to a pH measurement. A pH measurement gives
an indication of the acid/base status of a solution (hydrogen ion activity), whereas, a redox
measurement gives us a measure of the oxidation/reduction status (the electron activity).
lt is well known that the pH of a solution can be measured by immersing a pH-sensitive
electrode (e.g. a glass electrode), and a reference electrode (e.g. calomel electrode) into a
solution and then measuring the potential difference between them with a pH meter.
Similarly, it has been found that placing an "indifferent electrode" (e.g. platinum or gold
electrode) and a reference electrode into a solution, it is again possible to measure a potential
difference; this time this difference represents the strength of the solution with regard to its
ability to oxidize or reduce.
lt is also known from acid/base theory that an aqueous solution containing a strong acid will
contain OH- ions in addition to the H+ ions. Likewise, an aqueous solution containing a weak
acid will always contain the corresponding base. The pH of the solution actually represents the
ratio of acid to corresponding base.
This is also the case for redox systems. An aqueous solution containing a reducing agent will
invariably also contain the corresponding oxidation agent. The redox potential of the system
actually represents the ratio of reducing agent to oxidation agent. lt is because both species
are always present that we talk about the redox potential and not just its reduction potential
or its oxidation potential.
We usually speak of an acid base equilibrium as:
HA
acid
A- + H+
base hydrogen ion
Likewise we define a redox equilibrium as:

Ox + eCMI533 WN 2017
Red
Page 19 of 32

For example:
Fe+3 + e- = Fe+2
lf a platinum wire is placed in a solution containing such a redox system, the platinum will
develop a potential given by the Nernst equation
E = E0(Fe3+,Fe+2)
- RT ln [Fe+2]
nF
[Fe+3]
where:
E is the potential of the half-cell for the half-reaction, as written
E is the standard potential for the half-reaction
R is the Universal gas constant
T is the absolute temperature (Kelvin)
n is the moles of electrons which are transferred in the reaction
F is the Faraday constant (96,487)
ln is the log to the base e
[Fe+n] is the molar concentration of the ion
lf we assume a temperature of 25C and change the log to the base 10 we simplify to
E = E(Fe+3,Fe+2) - 0.059 log [Fe+2]
[Fe+3]
The above redox system, however, represents only a "half-cell" and it is not possible to
measure a single potential. (lt is like saying something is "high" without comparing its height to
something else.) In order to measure a potential difference, we must compare it to a
reference electrode (just as we compared a solutions "absorbance" to the absorbance of a
blank"). It would be best to use a hydrogen reference electrode since its potential is zero,
however, it is easier to use a calomel electrode which in fact has a potential of 0.246 V
compared to the hydrogen electrode.
In the following experiment, we are going to calibrate the millivolt scale of a "pH" meter using
a series of quinhydrone solutions which have a known redox potential. We will then prepare a
series of Fe3+ / Fe2+ solutions and measure their redox potentials. From these redox potentials,
we will use the Nernst Equation to calculate the standard electrode potential, E0, for the Fe3+ /
Fe2+ system.
CMI533 WN 2017
Page 20 of 32

Note 1:
The platinum electrode is very expensive and very delicate.

NEVER wipe this electrode.
NEVER let this electrode touch the bottom of a beaker.
NEVER let this electrode rest against any surface.
NEVER let the stir bar hit this electrode.
Note 2:
Only open the quinhydrone bottle long enough to take out small
samples. Keep this bottle closed at all other times. If you leave this
bottle open, even for short periods of time, the ratio of quinone to
hydroquinone will change and your readings will not be accurate.
Note 3:
In Experiment 2 you will prepare a ferrous iron solution. This solution mist not be
prepared until the day of the experiment since it will slowly change to ferric iron.
The ferric iron solution can be prepared in advance.
Experiment 1 :The Quinhydrone System

In order to calibrate a redox electrode, it may be immersed in a solution of known
oxidation/reduction potential. A quinhydrone solution is ideal for these purposes. This solution is
simply prepared by adding quinhydrone crystals to a suitable acid/base buffer solution until a state
of saturation is reached. The redox potential of this solution is only dependent on the pH and
temperature.
The electrode half-reaction for this compound can be written as:
OC6H4O + 2H+ + 2e- = HOC6H4OH
Quinone
hydroquinone
Quinone and hydroquinone unite in equimolecular proportions to form the compound
quinhydrone.
The Nernst equation for the above half-cell can be written as:
EQH = E + 0.0591 log [H+] - (0.0591 / 2) log [hydroquinone]
[quinone]
Assuming that we have 1:1 hydroquinone: quinone at equilibrium (= quinhydrone), then this
equation simplifies to
EQH = E + 0.0591 log [H+]
lf we are then taking a reading of the potential versus the standard calomel electrode (whose
potential is 0.246 V) we have
Eobserved= E - Ereference + 0.0591 log [H+]
= (0.6990) - (0.246) - 0.0591 pH
CMI533 WN 2017
Page 21 of 32

Therefore:
Eobserved = 0.453 (0.0591)(pH) at 25C
It is this equation we will be working with. For example, at 25C, the instrument should be reading
217 mV (0.217V). We will prepare pH buffer solutions, saturated with
quinhydrone, and measure their potential.
However, if your solution is not at 25C, you will have to determine the correct value that the
instrument should be reading at the existing temperature using the Nernst Equation. For example,
at a pH of 4.0, use the following equation:
0.453 - [2.303] RT pH = the potential (in volts)
nF
where
pH = 4.0
T = solution temperature in degrees Kelvin
n = number of moles of electrons involved = 1
F = 96, 487 coulombs mole-1
Your answer will be in the range of 200 to 250 mV. You now want to "offset" the
reading that is presently on the display, in order to read your calculated value.
NOTE: Quinhydrone is hazardous when in contact with the skin be sure to wear all PPE
(goggles / gloves) and dispense powder in the fumehood. Don not breath dusts!
CMI533 WN 2017
Page 22 of 32

Week 1 Procedure
1. You will prepare 5 buffer solutions, each containing 0.05 M acetic acid, citric acid and
phosphoric acid.
2. Place 10.0 ml of the 1M acetic acid, 10.0 ml of the 1M citric acid and 10.0 ml of the 1M
phosphoric acid into each beaker.
3. Add enough deionized water to bring the volume up to about 100 to 125 mL.
4. Using a magnetic stirrer, a pH meter and the 1 M sodium hydroxide/1 M sulphuric acid,
adjust the pH of the solutions to give you the following buffer solutions:
pH 3.0
pH 4.0
pH 5.0
pH 6.0
pH 7.0
5. You will also calibrate the potentiometer using hydroquinone. Note that in your lab project,
you must calibrate the instrument using your pH 4.0 solution. For example, at 25C, the
instrument should be reading 217mV (0.217 V). Based on the temperature of your
solution, determine the correct value that the instrument should be reading. To do this,
use the equation:
0.453 - [2.303] RT pH = the potential (in volts)
nF
where
pH = 4.0
Your answer will be in the range of 200 to 250 mV. You now want to "offset" the
reading that is presently on the display, in order to read your calculated value.
CMI533 WN 2017
Page 23 of 32

Week 2 - EXPERIMENT 2: Redox System

In this experiment you will determine the standard oxidiation potential of the Fe2+ / Fe3+ system
by preparing a series of ferrous and ferric solutions and measuring their redox potential.
The ferrous / ferric system could be written as:
Fe3+
e-
Fe2+
E0=____________ (HINT: look up this std. red. potential)
From the Nernst equation we can write:

E observed = E0 0.0591 log [Fe2+ ] / [Fe3+ ]
If we are then taking the reading of the potential versus the standard calomel electrode (standard
potential is 0.246V), then
E observed = E0 Ereference - 0.0591 log [Fe2+ ] / [Fe3+ ]
Therefore:
E observed = E0 (0.246) - 0.0591 log [Fe2+ ] / [Fe3+ ]
It is this equation we will be working with. Remember, though, this equation is only valid at 25C.
Should it not be at 25C, we will have to use the full Nernst Equation again to determine the
theoretical Eobserved. Use the Following equation:
E observed = E0 (Fe+3,Fe+2) (0.246) - [2.303] RT (log [Fe2+ ] / [Fe3+ ])
nF
where
E0 = the standard reduction potential of the reaction
E observed = the observed potential of the experimental ferrous / ferric system
[Fe+n] is the molar concentration of the ion
We will prepare mixed solutions of Fe2+ and Fe3+, measure their redox potential, and knowing their
concentration and the overall potential of the system, calculate the standard electrode potential,
E0, from experimental data.
CMI533 WN 2017
Page 24 of 32

Concepts involved in Lab #4 - This is for interest purposes only.
Source: SubsTech Image By: D.Kopeliovich
This figure shows a plot of the potential versus PH of the iron system. The axis marked E(V)
represents redox potentials. Any value above zero on the axis represents oxidizing conditions
and any value below zero represents reducing conditions (this is seen by the fact that metallic
iron, Fe0, is below zero, and the cations tend to be above zero). Each area in the diagram shows
which species is stable under those conditions. You will see the dividing line between Fe2+ and
Fe3+, which you just studied, marked as e-d. You can also see that under normal conditions at the
surface of the earth (potentials from 0 to +0.2 volts), metallic iron is not the stable form of iron. In
acidic conditions (pH less than 4), the ionic form is stable, and under neutral and alkaline
conditions, the oxides (rust) are the stable forms of iron. This explains why iron rusts; it is not
stable under atmospheric conditions at any pH. Note that pH is not a source of error when you
are doing the second half of lab 4 this diagram proves it.
CMI533 WN 2017
Page 25 of 32

Concepts involved in Lab 4

If we look at water (H2O) and hydrogen peroxide (H2O2), we know that they are similar, but that
hydrogen peroxide is an oxidizer, certainly a stronger oxidizer than water. Another way of saying
this is that water is a stronger reducing agent than hydrogen peroxide. Therefore, we are
measuring the difference between them. We can express this difference in terms of voltage (their
potential to oxidize or reduce).
This is the idea behind this lab. We will consider two related ions, Fe2+ and Fe3+, and determine
the potential generated when the two are placed in the same solution. This potential, of course,
should vary depending on how much of each is present at the same time.
We will measure the potential almost the same way we measure pH. However, instead of using
a pH electrode, we will use a platinum electrode, and instead of reading pH, we will read potential
(volts).
Note also that the ability of something to oxidize or reduce, depends on pH. In general, if we place
an oxidizing agent into solution, the more acidic the solution, the more powerful is the oxidizing
effect. This is why it is important that we never mix a bleach and an acid. Bleach solutions are
strong oxidizers prepared in an alkaline solution. However, if we make the solution more acidic,
its ability to oxidize increases rapidly and we can produce chlorine gas, a highly toxic species.
Therefore, the oxidizing ability of a solution depends on the concentration of the species present,
and the pH of the solution.
Next we must consider the calibration of the instrument. Before you can measure pH, you must
analyze a buffer solution and then adjust the pH meter to read the correct pH. Similarly, before
we can analyze the potential of a solution, we must analyze a solution whose potential we know,
and set the instrument to this reading. This is the function of the first weeks lab where you
calibrated the instrument using the potential generated by the pH 4.0 quinhydrone solution.
Redox measurements are widely used in a variety of environmental, industrial and
pharmaceutical/ biological applications. For example, iron will rust under oxidizing conditions.
Therefore, industry will monitor the redox potential of the water passing through their iron pipes
and attempt to keep this potential as reducing as possible. We also know that aquatic life forms
prefer the pH of their environment to be near 7.0. It is obvious that these life forms will also be
affected by redox conditions of their environment, when on considers the toxic effects of bleach
(an oxidizer) (note that bleach can exist at pH 7.0)
NOTE: PLEASE BE VERY CAREFUL WITH THE PLATUNUM ELECTRODE!!!
CMI533 WN 2017
Page 26 of 32

Mass and Concentration Calculations

1. State in words how you would prepare 100 mL of 0.6 M uranium, starting with a stock
solution containing 5.4 M uranium.
2. State in words how you would prepare 250 mL of 1.4 x l0-7 M thallium, starting with a stock
solution containing 2.5 x 10-6 M thallium.
3. I was given an unknown, I pipetted 0.5 mL of this solution into a 50 mL volumetric and
found that there was 23.6 ppm of dextrose. How much dextrose was in the original
unknown?
4. I was given an unknown. I pipetted 2.0 mL of this solution into a 250 mL volumetric and
found that there was 31.6 ug/mL of ascorbic acid. How much ascorbic acid was in the
original unknown?
5. State in words how you would prepare one 200 mL volumetric containing 5 ppm of silver,
8.6 ppm of gold and 14 ppm of nickel, starting with one solution containing 1000 ppm of
silver, one containing 500 ppm of gold and one containing 1000 ppm of nickel.
6. I was given a 100 mL solution of saccharin in water. I analyzed this solution and found
that it contained 0.5ppm of saccharin. How many micrograms of saccharin are present in
this solution?
7. a)
b)
c)
State how you would prepare one litre of a 1000 ppm solution of sodium chloride.
What is the molarity of this solution?
State how you would prepare one litre of a 1000 ppm solution of sodium, starting
with sodium chloride.
8. Colgate toothpaste contains 0.245 wt % NaF.

a)
How many grams of NaF are in 1.0 grams of this toothpaste?
b)
How many grams of fluoride are in one gram of toothpaste?
9. I dissolved 2.2 grams of Colgate toothpaste in 100 mL of water.
a)
What is the molarity of NaF?
b)
What is the molarity of fluoride?
c)
How many ppm of NaF are present?
d)
How many ppm of fluoride are present?
10. Kellogg's Special K cereal contains 2.5 grams of sugar in a 30 gram serving. What is the
weight percent sugar?
11. Carnation milk contains 4.9 grams of protein per 65 mL serving. What is the %
weight/volume of protein in the milk?
CMI533 WN 2017
Page 27 of 32

12. The label on Oral B mouthwash states that it contains 0.5% NaF.
a)
State this concentration as ppm.
b)
How much mouthwash should I place in a 100 mL volumetric flask in order to obtain
a 2 ppm solution of NaF.
13. A bottle of Montclair spring water contains 35 ppm calcium. I read somewhere that my
body requires at least one gram of calcium per day. How many litres of Montclair water
would I have to drink in order to obtain the one gram of calcium that I need?
14. A solution contains 25 ppm chlorophyll. What is the weight percent of chlorophyll?
15. How would I prepare one 2.0 bottle containing 1000 ppm cobalt and 2000 ppm dextrose?
16. Prepare 1.0 L of 1000 ppm bismuth, starting with bismuth fluoride (BiF3). We are given the
following atomic weights: bismuth 209.0; fluorine l9.00.3.
17. Prepare 1.0 L of 1000 ppm fluoride, starting with bismuth fluoride (BiF3). We are given the
following atomic weights: bismuth 209.0; fluorine 19.00.
Points to remember:
1. ppm = parts per million
= 1/106
therefore, ppm = ug/g
only for water can we say that ppm = ug /mL or mg/L. This assumes the density of water
is 1.0 g/mL (this is only true at 40C)
2. weight % (or %w/w) = g of species/100g of sample
3. %w/v = g of species/100mL of sample
4. volume % (%v/v) = mL of species/100mL of sample
EXAMPLE QUESTIONS
1.
C1 V1 = C2 V2
stock = final
(5.4 M)(V1) = (0.6 M)(l00 mL)
V1 = 11.1 mL
Place 11.1 mL of the 5.4 M uranium standard into a I00 mL volumetric flask and dilute to
the mark.
2.
C1 V1 = C2 V2
(2.5 X 10-6 M)(v1) = (1.4 X 10-7 1v1)(250 mL)
v1= l4 mL
Place 14.0 mL of the 2.5 x 10 M thallium standard into a 250 mL volumetric flask and
dilute to the mark
3.
C1 V1 = C2 V2
(C1)(0.5 mL) = (23.6 ppm)(50 mL)
Cr = 2360 ppm.
The unknown contains 2.36 x I03 ppm dextrose.
4.
C1 V1 = C2 V2
(C1)(2.0 ml) = (31.6 g/mL)(250 ml.)
C1 = 3950 g/ml
CMI533 WN 2017
Page 28 of 32

5.
The unknown contains 3.95 x I03 mg/mL of ascorbic acid.

Silver
C1 V1 = C2 V2
(1000 ppm)(V1) = (5 ppm)(200 mL)
V1 = 1.0 mL
Gold
C1 V1 = C2 V2
(500 ppm)(V1) = (8.6 ppm)(200 mL)
V1 = 3.44 mL
Nickel
C1 V1 = C2 V2
(1000 ppm)(V1) = (14 ppm)(200 mL)
V1 = 2.8 mL
Carefully pipette 1.0 mL of the 1000 ppm silver standard, 3.44 mL of the 500 ppm gold standard
and 2.8mL of the 1000 ppm nickel standard into a 200 mL volumetric flask and dilute to the mark
6.
0.5 ppm = 0.5 g/mL

1.0 mL contains 0.5 g of saccharin
100 mL contains (0.5)(100) = 50 g of saccharin
7.
a) 1000 ppm = 1000 g /mL

= 106 g/L
= 1.0 grams of NaCl/L
Therefore dissolve 1.0 grams of sodium chloride in a volumetric flask and dilute to the mark
b) Moles = grams NaCl =

1.0
=
MW NaCl
58.44
Therefore molarity = moles/L = 1.7 x 10-2M.
c) 1000 ppm Na = 1.0 g
L
Na
moles Na =
0.0435
1
22.99
1.7*10-2 MOLES
1.0 moles of Na is in 1.0 moles of NaCl

Therefore 0.0435 moles of Na is in 0.0435 moles of NaCl
Therefore grams NaCl
= (00435 moles)(MW NaCl)
= (0.0435)(5 8.44)
= 2.54
Therefore, dissolve 2.54 grams of NaC| in 1.0 litre.
8.
a) 0.245% =
0.245 g NaF
100 g toothpaste
100 g of toothpaste has 0.245 g of NaF
Therefore 1 g of toothpaste has
(0.245) = 2.45 X 10-3 g NaF
100
b) Change to moles NaF = 2.45 x 10-3
= 5.83 x 10-5 moles NaF
CMI533 WN 2017
Page 29 of 32

41.99
= 5.83 x 10-5 moles F
= (5.83 x 10 moles F)(19.00)
= 1.1 1 x 10-3 grams of fluoride
-5
Therefore grams NaF
9a).
First find the grams of NaF.

100 g of toothpaste has 0.245 g NaF
2.2 g of toothpaste has (0.245)(2.2)/100 = 5.39 x 10-3g NaF
moles NaF = (5.39 x 10-3 g)(41.99 MW of NaF) = 1.28 X 10-4 moles NaF
molarity = moles/litre
100 mL has 1.28 x 10-4 moles
1000 mL has (1.28 X 10-4 moles)(1000)/100 = 1.28 X 10-3 M
b)
1 mole NaF has 1 mole F

Therefore the molarities are equal
c)
ppm = g /mL
We have 5.39 x 10-3 g NaF in 100 mL
Therefore in one mL we have (5.39 x 10-3 g NaF)/100 = 53.9 ppm
d)
1.28 x 10-4 moles F are in 100 mL

grams F = (1.28 x 10-4 moles)(19.00) = 2.43 x 10-3 grams F
Therefore in 100 mL we have (2.43 x 10-3 grams F)(106) g /(100 mL) = 24.3 g/mL
= 24.3 ppm
10.
wt% = grams sugar/100 g cereal

30 g of cereal has 2.5 g of sugar
100 g of cereal has (2.5)(100)/(30) = 8.3 wt %
11.
%w/v= g protein/100mL milk

65 mL has 4.9 g of protein
100 mL has (4.9)(100)/(65) = 7.54% w/v
12a)
change 0.5% to g /mL

0.5% = 0.5 g NaF/100 mL of mouthwash
= (0.5)(106) g /100 mL of mouthwash
= 5 x 103 ppm
b)
C1 V1= C2 V2
(5 X 103ppm)(V1) = (2 ppm)(100mL)
V1 = 0.04 mL into a 100 mL flask
13.
35 ppm = 35 g Ca/mL of water

I want 1 gram of Ca = l06g of Ca
35 g of Ca are in 1.0 mL of water
106g of Ca are in (106)(1.0)/(35) = 2.86 x 104mL of water = 28.6 L of water
14.
25 ppm = 25 g /mL
CMI533 WN 2017
Page 30 of 32

weight % = g/100 mL
Therefore, 25 ppm is 2500 g /100 mL = 0.0025 wt%
15.
1000 ppm =1.0 g/L

Therefore, cobalt: 2g/2L
Therefore dextrose: 1000 ppm is 2 grams of dextrose in 2 litres
2000 ppm is 4 grams of dextrose in 2 litres
Therefore place 2 g of Co and 4 g of dextrose into a 2 L volumetric flask
16.
1000 ppm Bi = 1 g of Bi per litre

= (1.0 g Bi)/(209) = 0.00478 moles Bi
1.0 moles of Bi are in 1.0 moles BiF3
0.00478 moles of Bi are in (1.0)(0.00478)
= 0.00478 moles of BiF3

= (0.00478 moles of BiF3) (266)
= 1.27 grams BiF3
Therefore, place 1.27 grams BiF3 into a 1.0 L volumetric flask and fill to the mark.
17.
1000 ppm F
= 1 g of F per litre
= (1.0 g F)/ (19) = 0.0526 moles Bi
3.0 moles of F are in 1.0 moles BiF3

0.0526 moles of F are in (1.0) (0.0526)/(3.0)
= 0.0175 moles of BiF3;
= (0.0175 moles ofBiF3)(266)
= 4.655 grams BiF3
Therefore, place 4.655 grams BiF3 into a 1.0 L volumetric flask and fill to the mark.
Mass Concentration Units

1 ppm = 1 microgram/gram = 1 g/g = microgram/mL (for water only) = 1 g /mL
1ppb = 1 nanogram/gram = 1 ng/g = nanogram/mL (for water only) = 1 ng/mL
Mass Versus Concentration Calculations
You are accustomed to working with solution concentrations and commonly use C1 V1= C2 V2 to
do all your calculations. However, you must become very familiar with using mass calculations,
and converting between concentration and mass calculations.
Example 1: If I give you 2 apples and you hold one in each hand, the concentration of apples
can be reported as 1.0 apples/hand, but the mass of apples (the total) is 2.0 apples.
Example 2: If I place 1 gram of salt into a 100 mL flask, it's concentration is reported as
0.01g/mL. Note that this is 0.01 grams of salt in 1.0 mL, but I have 100 of these 1.0 mL volumes
CMI533 WN 2017
Page 31 of 32

(it is a 100 mL flask), therefore the total salt is (100 mL)(0.01 g/mL) = 1.0 grams of salt, it's
mass.
Example 3 : I was given 5 grams of soil and I dissolved it into 100 mL of acid. I then analyzed
this solution and found that it contained 1 ppm of gold. a) What was the total quantity (mass) of
gold in the soil sample? b) How many ppm of gold are in the soil sample?
Answer:
a) 1.0 ppm of gold in solution is 1.0 micrograms of gold/mL. But I actually had 100 mL of this
solution (it was in a 100 mL flask). Therefore the total gold is (1.0 g /mL)(100 mL) = 100
micrograms of gold.
b) If I now asked you how many ppm of gold are in the soil sample, l am asking you how many
g of gold are contained in 1.0 grams of soil. The answer is then (100 micrograms gold)/(5
grams of soil) = 20 micrograms gold/gram soil = 20 ppm
Note that the gold concentration in the solution is not the same as the gold concentration in the
soil!!!!!!
CMI533 WN 2017
Page 32 of 32

CMI533 Background Theory WN2017

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SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

SCHOOL OF BIOLOGICAL SCIENCES AND APPLIED CHEMISTRY

CMI533: Background Theory to Lab Projects (WN2017)

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

AA Experiment 2 : Analysis of Pills Containing Chromium Picolinate

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

AA Experiment 3: Analysis of Nails Containing Manganese

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

Concepts Involved ln Lab #1

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

Laboratory Project 2: Atomic Emission Spectrophotometry

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

Source: Analytical Instruments Image By: Unknown

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

Preparation of Working Standards and Digestion of Pills

Digestion of Multivitamin Pills

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

a) Cautiously add approximately 15.0 mL of concentrated hydrochloric acid to each beaker

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

Emission Wavelength Selection Jan. 9, 2017

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

Laboratory Project 3: Fluoride Ion By Specific lon Electrode

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

Preparation of Toothpaste Samples (Week 2)

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

Potential = -(2.303 RT)/(nF) Iog[F-]

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

Laboratory Project 4: Measurement of Oxidation/Reduction Potentials Using a

Likewise we define a redox equilibrium as:

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

The platinum electrode is very expensive and very delicate.

Experiment 1 :The Quinhydrone System

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

CMI533: Background Theory to Lab Projects

SENECA COLLEGE OF APPLIED ARTS AND TECHNOLOGY

CMI533: Background Theory to Lab Projects