Experiment 1 Overview

EXPERIMENT 1
Quantitative Determination of Lead
in a Contaminated Drinking Water Supply

PRE-LAB REQUIREMENTS

PRE-LAB REQUIREMENTS FOR EXPERIMENT 1 ARE…...

1. Read the entire experiment, contained in the following pages

2. Read the Online Material:

Work through the following Experiment 1 material in Canvas:

• Techniques and Standards for Recording Data:

• Weighing Objects
• Crucible Filtration
• Precision and Accuracy
• Errors
• Measured and Exact Numbers

• Virtual Lab:
• Complete the Virtual Lab Experiment 1 Tutorial on Gravimetric Analysis
• Bring the Feedback Form, for Evaluation Question(s) to the lab (printed
or screenshot)

3. Complete the Experimental Design Form (Pre-lab):

As you design your procedure and complete the EDF (in pen):
• Use the Experimental Overview and Virtual Lab Tutorial to assist with
designing your procedure
• As you read through the Experimental Overview, choose glassware,
equipment and chemicals for each step from the Laboratory Stockroom

4. Complete the Pre-Lab Quiz:

The pre-lab will be based on the following areas of this experiment:
• Techniques
• Calculations
• Experimental Overview
If you have prepared well for the experiment, the quiz should be straightforward

Do not attempt to leave all of the above work until the last minute.
You will be overwhelmed and poorly prepared for the lab if you do.
 Experiment 1 Overview

Rationale: This experiment demonstrates some standard techniques used in analytical chemistry, a
branch of chemistry that deals with the identification, measurement and quantification of small
amounts of components in a complex mixture. These techniques are also fundamental within the fields
of synthetic inorganic, organic and materials chemistry.

The paragraph below is adapted from the articles “Lead” and “Lead, Toxicology” from the Kirk-
Othmer Encyclopedia of Chemical Technology. The Kirk-Othmer Encyclopedia of Chemical Technology
is an online resource available through the UBC Library’s website. There are thousands of articles,
written by scientific experts, that cover every aspect of how chemistry is used within modern society.
As examples, there are articles on metals, metallurgy, chemical engineering, biochemical processes,
pharmaceuticals, artist’s dyes, paints and polymers as well as on specific topics such as sulfuric acid,
phosphate fertilizers, ammonia or sodium hydroxide. There are articles on the chemistry of candy,
chocolate, breakfast cereal, spirits, beer, paints, perfumes and fragrances, batteries and gasoline. The
Kirk-Othmer Encyclopedia of Chemical Technology (and Ullman’s Encyclopedia on Industrial
Chemistry, also available online through the UBC Library) should be the first place you consult
throughout your University career if you are looking for reputable information about chemistry or a
chemical that is used in modern society.

Background.
This element occurs naturally in the Earth’s crust, and was one of the first metals to be used by humans
thousands of years ago – probably because it was easy to find, extract and use. The primary use of lead
and its compounds today is within lead-acid batteries, such as standard car batteries.

Lead poisoning.
Humans have recognized the toxic effects of materials containing lead since the fourth century BCE.
Lead and its compounds are among the most well-studied environmental toxicants. Lead poisoning
disproportionally affects individuals in low-income or minority populations.

Lead exposure occurs mostly through inhalation of lead in air and dust, affecting those individuals
working in or living near industrial sources such as metal smelters, mines and coal-fired power plants.
The occupational exposure for workers in these industries is closely monitored.

The accidental ingestion of lead or its compounds is a second source of human exposure. Drinking water
rarely exceeds standards recommended by government agencies for lead before it flows into a system
of distribution pipes. But once water is distributed, it can flow through lead pipes, pipes with fittings
that contain lead solder, or fixtures that contain lead within homes. If the water is more acidic (pH 7.3 vs
pH 8-10) or a water utility does not control for corrosion, the protective film in the pipes can be
compromised, and lead can leach into drinking water. This type of pipe corrosion led to Flint, Michigan’s
drinking water contamination in 2014, and Washington, D.C.’s in the early 2000’s. For those interested,
more detailed, optional information is available at the end of this overview.

Generally, infants and children (those under 15) are much more susceptible than adults in absorbing
lead, in part because lead behaves similarly to calcium, a nutrient that children absorb at a higher rate
than adults. Childhood (0-3 years) is a particularly vulnerable period as there are distinct
neurodevelopments that occur in that development window.

In this experiment, you will act as a technician in an environmental analytical chemistry laboratory.
You are tasked with determining the lead content in a water sample.
 Experiment 1 Overview

EXPERIMENT 1
Quantitative Determination of Lead
in a Contaminated Drinking Water Supply

AIM
To master the principles of gravimetric quantitative analysis and to determine the lead content of a
sample using these techniques.

OBJECTIVES:
 Design and develop an experimental procedure for a gravimetric analysis.
 Determine appropriate glassware needed to perform the experiment.
 Describe the difference between qualitative and quantitative analysis.
 Precipitate lead ions as an insoluble lead salt.
 Master gravimetric quantitative analysis techniques.
 Quantitatively determine the lead content in an unknown sample.
 Assess the human health risk of the lead content in the water sample.

To achieve the objectives of this experiment, you should understand the following:

Chemical Concepts: Lab Techniques: Calculations:

• Quantitative • Weighing • Amount of sodium
analysis • Filtration sulfate required
• Gravimetric analysis • Drying • % of lead present
• Chemistry of lead • Heating • If % present will
• Cooling affect human health

Types of Analysis:
Quantitative analysis
• determines the amount of a specified element or substance in a sample
Qualitative analysis
• tells you what substances or elements are present in a sample, but little information on amounts is
gained
Gravimetric Analysis
• Gravimetric analysis means analysis by weighing. Three conditions must be met before using
gravimetric analysis:
o The substance being analyzed has to be separable from its contaminants or impurities.
o There needs to be 0.1 mg or more of the substance being analyzed.
o The separated substance must be in a form that can be weighed on an analytical balance.
When these conditions are met, the gravimetric technique is a simple, inexpensive and highly accurate
technique.
 Experiment 1 Overview

Central City Water Council

Request for Water Sample Testing
Source of Sample Snake River 0.5 km downstream from Robinson
Industries
Collected Sample Size 1000 L

Sample size to be tested 1g Original sample was boiled down to

Test sample for the presence
and quantity of:
Additional information on the
sample to be tested
Analysis to be Completed
give this sample size
Lead
This solid sample contains lead (Pb2+) in the form of a water-soluble salt.
Quantitative Gravimetric Analysis (see below for definitions)

Additional information on the Isolation technique

analysis to be completed
The water-soluble Pb2+ salt needs to be separated from the sample by
dissolving a precisely weighed amount of the sample in an acidic solution
and then precipitating the lead ion as water-insoluble salt PbSO4 of
known composition.
The insoluble salt can be filtered off, dried and weighed. From the mass
and known composition of the salt, the amount of the lead ion in the
original sample can be calculated.

Public Health Information
Exposures to lead by an individual can be obtained by the measurement
of the amount of lead in a blood sample. Small amounts of lead in the
blood represents relatively large amounts of lead elsewhere in the body:
lead accumulates in bones, kidneys, and liver, and a small fraction
circulates in the bloodstream.

Table 1. Human toxicity effects of lead, correlated to bloodstream lead content.

Symptoms Blood Lead Level in mg/L
Developmental toxicity (effects on IQ, hearing, growth) 0.050
Decrease in Vitamin D metabolism 0.150
Decrease in nerve conduction velocity 0.200
Decrease in hemoglobin synthesis 0.400
Abdominal pain/irritation 0.600
Increase in the breakdown of red blood cells 0.700
Kidney failure 0.800
Brain structure breakdown 0.900
Death 1.350
• Approximately 5% of ingested lead is absorbed into the bloodstream by adults (higher for children).
• A person has ~ 100 mL of blood / 1 kg body weight.
 Experiment 1 Overview

The Experiment
LAB PROJECT SUMMARY
Perform an experiment as follows:
1. Quantitatively obtain and dissolve an unknown lead sample.
2. Precipitate the lead ions as an insoluble lead salt.
3. Quantitatively isolate and dry the lead salt.
4. Weigh the mass of dried lead salt to four decimal places.
5. Calculate the mass % of Pb in the unknown lead sample.

REAGENTS AND APPARATUS

Choose the appropriate glassware, equipment and reagents needed for the experiment from the
Laboratory Stockroom. Remember to consider the accuracy needed in each step when choosing
glassware.

EXPERIMENTAL PROCEDURE
Dissolve
Weigh the the Weigh the
Precipitate Isolate Dry
sample sample product

While you read through the procedure, consider the general concepts in the left-hand column and think
about questions in purple text using your answers to help you develop your own experimental
procedure and improve your lab skills.

General Concepts Procedural Steps and Points to Consider

• Using a top-loading balance, weigh out
Weigh the
approximately 0.8 g of the sample into a
sample
weigh boat.
This experiment requires a high degree
of precision, 4 significant figures, as it is Q: Why do we pre-weigh on the top
a quantitative analysis. loading balance?
Q: What range of mass is acceptable in this step?
Technique: Weighing Objects
• Using an analytical balance, weigh this sample by
difference into a beaker.
Q: To how many significant figures do you need to read
the analytical balance?
 Experiment 1 Overview
General Concepts
Most lead compounds must be dissolved •
in hot water to form Pb2+ ions.
Lead is hydrolyzed by water:
Pb2+ + H2O → Pb(OH)+ + H+(solv.)
To prevent this side reaction from •
occurring, this part of the experiment
must be performed under acidic
conditions.
Q: How do acidic conditions prevent
hydrolysis of lead? • Cover the beaker with a watch glass and reheat to a gentle
Q: How do you ensure complete
dissolution of the solid sample?
The lead dissolved in the sample in the •
previous step now needs to form an
insoluble precipitate, ready for isolating •
in the next step.
The addition of sulfate ions to the
dissolved lead (II) will form an insoluble
precipitate, PbSO4. (Ksp at 25°C for PbSO4
is 1.6 x 10-8).
Pb2+(aq) + SO42-(aq) → PbSO4(s)
Q: Assuming that the entire unknown
was lead, how many mL of sulfate
solution would you need to completely
precipitate the lead ions?
Calculation Help: Experiment 1 Virtual
Lab - Gravimetric Analysis (step 2
Digestion
During digestion, small particles dissolve
and larger ones grow. It is an important
practical process in gravimetric analysis Important safety notes on heating the solution:
as it aids with filtration.
Procedural Steps and Points to Consider
Heat roughly 50 mL of deionized water Dissolve
on a hotplate set to 3. the
Q: Why does it have to be deionized sample
water?
Q: Why do you not have to measure the
water carefully?
Add ~5 mL of acetic acid to the beaker containing your
weighed unknown sample and then add the ~50 mL of the
boiled deionized water from the step above.
Q: Why do you only have to use an approximate amount
of acid and what glassware is a\most appropriate?
boil.
Q: Why should the beaker be covered with a watch glass?
Remove the beaker from the hotplate
and place on a ceramic tile. Precipitate
Slowly add the sulfate solution while
stirring with a stirring rod.
Q: How accurate does the amount of
sulfate solution have to be?
Q: Which piece of glassware is appropriate to measure it
out?
Q: Once you have stirred the solution, what should you
do with the stirring rod?
• Allow the precipitate to settle for a few minutes.
• Cover the beaker with a watch glass and sustain boiling
for 10 minutes. This process is called “digestion”
Q: Why should the beaker be covered with a watch glass?
Q: Why do you think digestion is important?
• Then cool the beaker, using a cool air gun, until it is cold
enough to handle (about the same temperature as a
warm cup of coffee)
If the solution gets too hot, “bumping” may occur and the
solution can start spitting out of the beaker. If this happens,
turn down the hotplate, carefully remove the watch glass and
place a stirring rod in the beaker. Replace the watch glass.
 Experiment 1 Overview

General Concepts Procedural Steps and Points to Consider

Once the lead has formed an insoluble The first 2 bullet points below can be
precipitate, a glass crucible is used to filter done at the start of the experiment. Isolate
and collect the precipitate quantitatively. • Collect a glass crucible from the
oven (it is kept there to ensure
Techniques: Using a sintered glass crucible complete dryness). Use an oven mitt as it is very hot!
• Place the crucible on a ceramic tile and cover it with
Two things to keep in mind when using a a foil lid. Cool the crucible to room temperature.
sintered glass crucible: Q: Why does it have to be cooled to room
1. You cannot touch it with bare hands due temperature?
to oils on your fingers effecting the mass. • Weigh the empty crucible.
Q: What can you use? Q: Why must you weigh it before you use it?
2. It must be at room temperature before Q: Which type of balance will you use to weigh the
you weigh it. crucible? Why?
• Set up the filtration apparatus.
• Quantitatively transfer all of the precipitate from the
beaker into the glass crucible. The beaker is rinsed
with deionized water until no precipitate is left.
Q: Should the watch glass and stirring rod also be
rinsed? Why?

• Dispense ~5 mL of ethanol onto

Anhydrous ethanol facilitates drying of the
solid by removing the water from the
collected precipitate into the filter flask.
Suction drying evaporates the residual
ethanol. The ethanol must evaporate
completely before the precipitate is placed in •
the oven!
your precipitate in the crucible, and Dry
leave it under suction for 2-3
minutes.
Q: What is the purpose of the
ethanol?
Place the crucible back in the small beaker and cover
the beaker with the foil lid.
Q: Why does there need to be a hole poked in the
foil?

The precipitate must be completely dry in • Final drying can be achieved by placing the glass
order to determine its mass. crucible in the oven for 30 minutes.

Precise weighing is achieved only when the •
crucible and precipitate have cooled to room
temperature. If a sample is still warm, it will
weigh less because of buoyancy due to
• Cool to room temperature.
upward circulation of hot air.
Double check that you are still meeting the
precision requirements of quantitative •
analysis.
Remove the crucible from the
oven. Use an oven mitt as it is very Weigh the
hot! product
Q: Why does the crucible have to
be cooled to room temperature?
Weigh using the same analytical balance as you used
to weigh the crucible the first time.
Q: Why use the same balance?
 Experiment 1 Overview

CLEAN UP
Glassware Rinse all glassware with tap water and return it to the
basket, following the clean-up instructions provided

Crucible LEAD CANNOT GO DOWN THE SINK

Your TA will point out where the waste
container and tubs for the
crucible/beaker/foil lid are, during the lab
Filter flask
Chemical disposal
Lead
All other chemicals used in the experiment
Scrape the lead sulphate in to the waste container
Remove any remaining small amounts of lead
sulphate with a wire brush and hot water
Place the cleaned crucible (plus the 100 mL beaker)
and the foil lid, in the appropriate tubs
Rinse with hot water and re-clamp the flask
LEAD CANNOT GO DOWN THE SINK
Scrape the lead sulphate in to the waste container
Pour down sink with plenty of water

PRE-LAB CHECKLIST
Make sure to do the following before you do the experiment:
 Read through all the components of the experiment
 Complete the Virtual Lab and bring the feedback form to lab (screenshot or printout)
Complete the pre-lab quiz. You can be tested on techniques, calculations and the experimental
 overview
Complete IN PEN the pre-lab part of the EDF, including glassware/equipment and chemicals
 needed, calculation for the amount of sodium sulfate needed and the procedure
The more you prepare for the wet lab the easier your experiment will seem. Familiarize yourself with:
• your own procedure so you are aware of the order the experimental steps are performed
• any techniques in the experiment
• calculations you will need to complete to analyze your data to gain results

SUBMISSION DEADLINES
Task
Prepare for lab:
• Read experimental overview
• Read online material
Complete EDF (Pre-lab)
Virtual Lab Tutorial
Complete the Pre-lab Quiz
Complete EDF (In-lab)
**No late submissions
Submit (where) Submit (when)
Before the start of your
Bring to lab
scheduled lab session**
Bring Feedback Form to lab Before the start of your
(screenshot or printout) scheduled lab session**
Before the start of your
In Canvas
scheduled lab session**
Before the end of your
In the lab
scheduled lab session
 Experiment 1 Overview

Extra Information:
Flint Water Crisis

In April 2014, the city of Flint, Michigan changed its water supply from Detroit (sourced from Lake
Huron) to the Flint River as a cost-saving measure. Soon after the switch, Flint residents became
concerned about the colour, taste, and odour of the drinking water. Residents soon had health
complaints. The drinking water had elevated levels of lead.

The lead in a water distribution system derives from a) the physical flaking of corrosion scale (a mix of
PbCO3, Pb3(CO3)2(OH)2, Pb10(CO3)6(OH)6O, PbO, and PbO2) and b) the dissolution of corrosion scale. Theis
scale forms on the inside of lead pipes. Both this corrosion scale and the exposed lead pipe can release
lead into the water.

A number of factors caused increased lead corrosion from the Flint Raver water system: 1) absence of
an orthophosphate corrosion inhibitor, 2) lower pH of the water, and 3) high chloride levels.

1) In the water from Detroit, orthophosphate was added in order to encourage the formation of a low-
solubility lead-phosphate complex inside lead pipes, protecting the pipes from corrosion.
Orthophosphate was not added to Flint River water and the protective layer dissolved, exposing the
bare metal pipe.

2) The pH of Flint River water was not controlled, changing from pH 8 in December 2014 to pH 7.3 in
August 2015. The solubility of lead corrosion scale increases as pH lowers. In fact, Boston, another city
with a lot of lead pipes, maintains a pH of 9.6 in its water in order to minimize lead corrosion.

3) High chloride levels, in particular high chloride-to-sulfate ratios, will lead to increased lead corrosion
because chloride will react with metals in the pipes. Flint River water naturally has much higher chloride
levels than Detroit water. To make matters worse, a series of water treatment actions further increased
the chloride levels. First, excess chlorine was added to combat E. coli contamination. This resulted in the
reaction of organic matter and chlorine to form toxic trihalomethanes, which was in turn addressed by
adding iron (III) chloride, further increasing the chloride levels.

Lead in drinking water disproportionately affects children and pregnant mothers. Children can absorb
40-50% of lead in water (compared to 3-10% for adults). The Centers for Disease Control and Prevention
(CDC) define blood lead level (BLL) to be elevated at above 0.05 mg/L. Hanna-Attisha et al. found that
the percentage of children with elevated BLL rose significantly: from 2.4% to 4.9% in some areas of Flint,
and from 4% to 10.6% in areas with the highest water lead levels.

The Flint Water Crisis became a political controversy that was widely covered in the media in late 2015
and early 2016. Class-action lawsuits have been filed against various government officials for gross
negligence leading to serious injuries from lead poisoning.

Hanna-Attisha, M.; LaChance, J.; Sadler, R. C.; Schnepp, A. C. Am. J. Public Health 2016, 106(2), 283-290.
Kim, E. J.; Herrara, J. E.; Huggins, D.; Braam, J.; Koshowski, S. Water Res. 2011, 45, 2763-2774.
Torrice, M. Chem. Eng. News 2016, 94(7), 26-29. http://cen.acs.org/articles/94/i7/Lead-Ended-Flints-
Tap-Water.html

Compiled by Emily Lai

Former Chem 121/123 Laboratory Technician