Unit 2: Practical scientific procedures and techniques

Introduction:

I am a newly appointed technical assistant at a large chemical plant, Terra's solutions

chemical group. As a part of my induction period and to progress in my role, i must
demonstrate skills in a range of practical procedures and techniques. Part of my role is to
ensure equipment is calibrated and equipment and chemicals are safety checked. Titration is
slowly adding one solution of a known concentration to a known volume of an unknown
concentration until a colour change and colorimetry is a technique used to find the
concentration of a solution based on the intensity of light it scatters or absorbs A positive of
titration is that it produces quick results a negative of titration is that volumes can be misread.
A positive for colorimetry is it's also low cost but a negative it that . An aim of my job will be
making and testing standard solutions using titration and colorimetry procedures. I must
demonstrate my ability to carry out these techniques precisely, safely, accurately and
efficiently.

Lab report 1 = Titration

Lab report 2 = Colorimetry

Lab report 1(Titration of the sodium hydroxide (NaOH) solution of unknown concentration
with the standardised HCl)

Calibration of PH probe, balance, volumetric flask, pipette and burette

Before beginning the titration, I firstly needed to calibrate some of the equipment. Calibration
is done to ensure that the instrument being used will yield correct results and it also means
that you don't change the equipment to ensure the results are precise; it is crucial since the
particle's results would not be impacted if the equipment were not calibrated.

To calibrate the PH probe, I set up 7 buffer solutions in separate beakers (PH 4 – 10) and a
beaker filled with distilled water. I first rinsed the PH probe in the distilled water then placed
the PH probe into PH 4, make sure it is levitating in the water, after getting the result I
recorded it then rinsed the PH probe again and repeated this trying different all the other PH’s
to get the actual reading that the PH probe got so our results are accurate below are my results
for the PH probe calibration. Now we know the readings of the PH probe
PH 4 5 6 7 8 9 10
PH probe 3.98 4.97 6.01 6.98 8.01 9.03 9.99
reading
For calibration of the balanced I pressed down on a button shown as ‘Cal’ which calibrated
the reading on the scale to 0.00 so I set the balance aside for later.
For the calibration of the pipette take distilled water in a beaker and place a thermometer
leave it until it reaches room temperature which is around 20degrees

Calibration of volumetric flask:

The volumetric flask was calibrated by placing it on a calibrated scale, recording its weight,
and then filling it with 250 cm³ of water. Because the weight of a calibrated volumetric flask
must be as close to its maximum value as feasible, I took the weight of the flask with water
and subtracted it from the original weight to ensure the result was as close to 250g as possible

Calibration of pipette:
In order to get precise results from our experiments, I'm calibrating the pipette.
Equipment
• 25cm3 Pipette
• Pipette Filler
• Water
• Balancing Scales
• 100 ml Beaker
Turn on the balance then press 0 to make it read 0.00 then place an empty 100ml beaker onto
the balance then press 0 again to make the reading 0.00 with the beaker on the scale. Next
you fill a pipette up to the 25cm3 line with water then empty it into the beaker on the scale
For me the reading on the balance was 24.71cm3.

Calibration of balance:

To calibrate a balance i had weights of 20, 50 and 100 grams to measure onto the balance
here are the results:

Mass provided(g) Reading on balance to 2 d.p(g)

20 19.98
50 51.00
100 99.98

Risk Assessment for standardising solution:

 Hazard Risk level How to minimise Dangers
risk
Broken glassware low Place any glass Can cut skin and
items away from the bleed allowing
table edge bacteria or
chemicals to infect
the cut
HCl Medium to high By wearing Coughing/ short of
corrosive proof breath and eye
gloves, safety contact can cause
goggles and avoid blindness
inhaling
Sodium carbonate Medium to high risk Corrosive proof Coughing/ short of
gloves safety breath and eye
goggles and avoid contact can cause
inhaling eye problems

I was able to create a standardised solution in the titration experiment by first

dissolving a known mass of solute and then diluting the solution. I had to dissolve the
solute, sodium carbonate, in distilled water.

How to carry out standard solution:

Equipment list:

• Sodium carbonate
• Beaker
• Volumetric flask (250cm3)
• Distilled water
• Spatula
• Funnel
• Glass rod
• pipette
• Weighing boat
• Balance

Method
1. The first step to perform standardising solution is that you would turn on the weighing
scale and then place the weighing boat onto the weighing scale and write the weight
of the weighing boat onto the results table (this was 0.5g)
2. After that you would add approximately 2.5-3.5g of sodium carbonate however, mine
was 1.36g of sodium carbonate and you would add this by using a spatula
3. Next time you would transfer the sodium carbonate from your weighing boat to the
volumetric flask making sure you do not spill any otherwise it would affect the results
4. After that you would pour distilled water into the weighing boat to get the excess
sodium carbonate into the volumetric flask this is to ensure that the results are
accurate
5. Then you would reweigh the weighing boat and record it on your results table
 6. After that you would pour approximately 100cm3 of distilled water into the
volumetric flask this is to leave room to pour water around the beaker to make sure
there’s no sodium carbonate stuck on the side
7. Then stir the mixture thoroughly until the sodium carbonate is completely dissolved
8. After that add the 100cm3 of distilled water to the sides that would affect the results
9. Then for the final cm3 of the distilled water use a pipette until you reach the meniscus
line to ensure complete accuracy
10. After that you would mix the solution for 60s by shaking the liquid

A solution is prepared by weighing a solid, which is the first step being done
accurately The next step is dissolving the weighed solid into a solvent namely
distilled water making a solution with a known concentration. If you measure the
correct mass, the solid is placed into the vessel and is then dissolved in the solvent, be
it in a beaker or a volumetric flask. Preventing the formation of precipitates, the
solution is then mixed until fully dissolved.

Evaluation
The standardisation we had to complete today was quite simple. Although I believe
my standardisation went well, I could have set up and prepped for further titrations
during this time. We combined sodium carbonate and distilled water to create sodium
hydroxide.

Calculation for the concentration and moles of the standard solution

Moles=mass/Mr
Mr of Na2CO3=106.0000g/mol
Moles of Na2CO3= 1.3600/106.0000=0.0128 x4
=0/0128mol/250L
Con=0.05120mol/L

Risk assessment for titration:

Hazard Risk level How to minimise Dangers

risk
Methyl orange Medium to high Avoid using near lit Burn you or your
flame clothes

Sodium hydroxide Medium to high Handle it cautiously If in eye can cause

and wear eye blindness and can
protection. irritate skin
Burette tap left open Low to medium Make sure tap is Spillages people can
closed slip

Using sodium carbonate to standardise HCl

Equipment list
1. funnel
2. graduated pipette
3. burette
4.clonical flask
5. 3 beakers
6. indicator(methyl orange)
7. clamp stand
8. pipette filler
9. distilled water

Method:
1. Using two beakers, place one with a solution of sodium carbonate and the other
with hydrochloric acid (HCl) on a clamp stand.
2. To rinse the inside of the burette, keep the tap open and rinse it first with distilled
water and then with a sodium carbonate solution.
3. Apply hydrochloric acid to the pipette to rinse it.
4. To prevent more solution dripping, fill the burette with 50 cm³ of HCl and take
out the funnel.
5. Using a pipette, transfer 25 cm³ of sodium carbonate into a conical flask. Next,
add a few drops of methyl orange indicator.
6. Note the HCl's initial volume in the burette which was 50cm3.
 7. As you slowly add HCl while swirling the conical flask, watch for a hue shift from
clear to dark orange.
8. Reduce the flow of HCl as soon as a colour shift is noticed.
9. Determine the titre (difference between start and end volumes) by recording the
burette's ultimate volume.
10. After every titration, rinse every piece of equipment with distilled water.
11. Determine the molar ratio of HCl to Na2CO3, compute moles of sodium
carbonate, balance the chemical equation, and calculate the concentration using
volumes.

Yellow > orange > red

(Alkali) > (endpoint) > (acid)

Results for finding concentration of acid titration

Volume of HCl added /cm3 pH reading
0.00 13.20
1.00 13.20
2.00 13.20
3.00 13.20
4.00 13.20
5.00 13.20
6.00 13.19
7.00 13.16
8.00 13.15
9.00 13.15
10.00 13.10
11.00 13.10
12.00 13.10
13.00 13.08
14.00 13.06
15.00 13.03
16.00 13.00
17.00 12.96
18.00 12.93
 19.00 12.87
20.00 12.83
21.00 12.79
22.00 12.71
23.00 12.64
24.00 12.55
25.00 12.27
26.00 12.08
27.00 10.80
28.00 8.32
29.00 2.85
30.00 2.16
Results:

Volume = 28cm3

Number of moles of HCl used to neutralise NaOH

Moles = concentration x volume0.0907 X 28 = 2.5396

0.0907 X 28 = 2.5396

Rough 1st 2nd 3rd

Final volume 29.5 28.5 28 28.1
Initial burette 0 0 0 0
reading
 Volume of 29.5 28.3 28 28.1
HCL used
ffcm3

Average volume of HCl used = 28.3+28+28.1 = 85.6/3 = 28.3

Calculating the moles and concentration of HCl

Equation is 2HCl(aq) + Na2CO3(aq)→ 2NaCl(aq) + H2O(l) +CO2(g)

Reacting ratio 2 : 1 2 : 1 : 1

C (moldm-3) : 0.0513

V(dm3) 0.0283 : 0.025

N(mol) 0.0256 <-- x2 0.0128

C = n/v

C=0.0256/0.0283= 0.0907mol/dm3

A standard sodium hydroxide (NaOH) solution was used to determine the concentration of
the unknown hydrochloric acid (HCl) solution via titration. Volume of HCl was measured
into a conical flask, and NaOH was carefully added from a burette until neutralisation was
reached, determined using an indicator methyl orange. The concentration of the unknown
HCl was then determined by dividing the amount of NaOH used by the known concentration
of NaOH used in the bulk volume. The endpoint of the titration was identified by the first
permanent colour change, which marked the point of neutralisation.

titration of HCl and NaOH using a pH probe:

Equipment:
- PH
probe
- Pipette
- White tile
- Burette
- Distilled water
- Conical flask
- HCl solution
- NaOH solution
 Method:
• Calibrate the pipette youll be using
• Carefully and accurately transfer 25cm3 of sodium hydroxide solution
(unknown concentration) into a small beaker
• Calibrate the PH meter
• Place the PH meter into the beaker of sodium hydroxide
• Clean and fill a burette with the standardised solution of HCl
• Add the HCl from the burette to the sodium hydroxide solution in 1cm3
portions until all the acid has been added. Measure the PH reading on the PH
meter every 1cm3 of HCl added

• Accurately and precisely record all burette and pH measurements in a table.

• Plot a graph of pH against volume of acid added

Graph of amount added and PH

At 30cm3 is ph7

Moles of HCl used

N=c*v
0.0907*0.0283 = 0.00256

Mols and concentration of NaOH:

Equation is HCl(aq) + NaOH(aq)→ NaCl(aq) + H2O(l)

Reacting ratio 1 : 1 : 1 : 1
C (moldm-3). 0.0907 :

V(dm3) 0.028 : 0.025

N(mol) 0.00256. : 0.00256

N=c*v
C = n/v

0.00256/0.025 = 0.1024mol/dm-3
Results table of ph after every cm3

Changes to the method

• Stir solution continuously during titration - Stirring the solution as titration proceeds
ensures that the sodium hydroxide and hydrochloric acid are well mixed together to
give uniform concentration and contributes to accurate pH measurement. We can
improve accuracy and repeatability by ensuring the reactants are well mixed and
similar in concentrations across the entire reaction volume, rather than in some
locations of the reaction volume, where the reaction would misrepresent therefore
skews the results

• Make sure solution is at a constant temperature- Temperature can influence the rate of
reaction as well as the pH readings. Using standard solution of sodium hydroxide and
hydrochloric acid at the same temperature (room temperature) also helps to minimize
variations.

Equipment

• smaller changes in acid increment, constant stirring, and multiple trials) maximize
accuracy, precision, reliability, and repeatability by being a more accurate
measurement and better mixing. more accurate titrator
• (e.g., burette, pH meter, magnetic stirrer, pipette from a calibrated pipette stand) yield
better results by lowering systematic error and making the experiment less reliant on
the reaction intermediate features

Comparing results

I compared my results to normal values for volume of Hydrochloric Acid (HCl) used,
and concentration of Sodium Hydroxide (NaOH) calculated, in my titration
experiment. The average volume of HCl used to neutralizing the NaOH was 28.3
cm3which in a reasonable range of expected values as a average volume will range
between 25 to 30cm3 for similar titration. The NaOH concentration thus calculated
was 0.1026 mol/dm3 which is also relatively reasonable for a typical titration setup.

Risk assessment for making a standard solution of CuSO

 Hazard Risk level How to minimise Dangers
risk
Copper sulphate medium Avoid inhalation an Can cut skin and
wear gloves and bleed allowing
goggles bacteria or
chemicals to infect
the cut
Spilled solution Medium to high Clean up spillage Skin irritation
immediately and
wear gloves
Hot distilled water medium Handle with care Burns in the
skin

Colorimetry

A method called colorimetry uses the intensity of light (of a particular wavelength) that a
solution absorbs or scatters to determine its concentration. It is possible to determine how
much light is absorbed by a sample by measuring the amount of light that goes through it.

Method to make standard solution of CuSO4

Calibrate the weighing balance that you will be using.

First weigh 2.60g of hydrated copper (II) sulphate (CuSO4.5H2O) andCarefully transfer the
hydrated copper(II) sulphate to a beaker, accurately and precisely recording measurements to
determine the exact mass transferred. Next, add 25cm3 of hot distilled water to the beaker,
stir and completely dissolve the hydrated copper (II) sulphate. Carefully and accurately
transfer all the solution to a 100cm3 volumetric flask and make up the solution to 100cm3
with more distilled water. You have made a stock copper(II) sulphate solution of
approximately 0.1M. Calculate the precise concentration and label the volumetric flask.
Using some of the stock copper(II) sulphate solution you have made, dilute so that you have
four other solutions of approximately 0.08M, 0.06M, 0.04M and 0.02M. Calculate the precise
concentration of each solution that you make. Select an appropriate colour filter and calibrate
the colorimeter (or visible spectrometer) that you will be using with the stock solution and
distilled water, according to the manufacturer’s instructions. Measure and record the
absorbance (or transmission) of each copper(II) sulphate solution (approximately 0.1M,
0.08M, 0.06M, 0.04M, 0.02M) and for distilled water (0.00M) using the calibrated
colorimeter (or visible spectrometer). Plot a calibration curve of absorbance (or transmission)
against the concentration of copper(II) sulphate. Measure and record the absorbance (or
transmission) of Sample A and Sample B (the unknown concentrations of copper(II) sulphate
solution) Using the calibration curve, determine the concentrations of Sample A and B.

moles and concentration of CuSO4

Molar mass of CuSO₄ 5H₂O = 249.7 g/mol

Volume of solution prepared = 100 cm³ = 0.100 L
N= m/mr

2.60/249.7 = 0.0104mol

C = n/v

0.0104/0.100= 0.104

Concentration of copper sulphate = 0.0104mol/dm3

Balance Calibration

To calibrate the balances so that mass is measured correctly. This allows the balance to
display the accurate mass.

Steps:

Once you have cleaned the balance, make sure to place it on a level surface.

Tare the balance to zero before putting any calibration weights on the platform.

Put certified scales with known mass on the balance and look for mismatches.

Also, if necessary, balance the balance to the manufacturer's instructions, if not to do so, the
margin of error.

Colorimetry:

• prepare calibration – pick a range of known coloured solution concentrations you will
subsequently measure. These are your standard solutions, which will enable to make a
calibration curve. Prepare the solutions with a pipette and volumetric flasks, and
assure these are homogeneous.
• Prepare the equipment- Clean the colorimeter or spectrometer to remove any residue
from the previous use. Switch on the gadget and give it time to warm up as per the
instructions (usually enough 10-15 minutes for accurate readings). Wavelength that
will be measured for the colored solution. If you are not sure, check the t absorbance
spectrum of the solution itself and look for the wavelength of maximal absorbance
(which is usually at the peak of the solution’s color).
• zero the equipment- Put the blank solution (a colored solvent, such as water or the
solvent used in your sample) into the colorimeter or spectrometer. This will establish
the zero absorbance or transmission for the instrument.
• Set the instrument to read zero absorbance
• Measure the standards - Individually introduce each of the standard solutions into the
colorimeter or spectrometer. Measure the absorbance (or transmittance) values of
each solution at the desired wavelength. Make sure that the cuvette(s) or sample
holders are clean (free of fingerprints / contaminants)..
 • Plot a calibration curve −Plot the absorbance (y-axis) vs the concentration (x-axis) of
the standard solutions. If Beer-Lambert law applies, the relationship should be linear.
If the plot does not look linear, you need to check your standard preparation, or either
select another wavelength.

Using the colorimeter to determine concentration:

• Prepare the coloured solution whose concentration you are interested in determining.
Take care to avoid air bubble and particulate contamination by mixing the solution
properly. Dilute the sample, if needed, so that the absorbance of your sample appears
within the scope of your calibration curve.
• Measure- .put the sample onto the colorimeter and measure how much is being
absorbed at the wavelength used for the calibration standards make sure that the
sample is put with the same side facing the light path
• Find concentration- use the graph curve to find out the concentration of the coloured
solution

Colorimetry results:

A=ϵ⋅c⋅l

The beer-lambert law states that the absorbance is directly proportional to the concentration
and since the calibration curve is a straight line it shows that this law is true.
To find the concentration of the unknown solution (in this case its copper sulphate) you’d
measure the absorbance and find the corresponding concentration.

Unknown Absorbance 1 Absorbance 2 Average Unknown

Sample (nm) (nm) absorbance (nm) concentration

(mol dm-3)

Sample A 0.13 0.12 0.13 0.03

Sample B 0.31 0.30 0.31 0.07

Copper sulphate Absorbance 1 Absorbance 2 Absorbance 2 Average (nm)

conc. (mol/dm3) (nm) (nm) (nm)

0.10 0.44 0.43 0.44 0.44

0.08 0.43 0.36 0.36 0.38

0.06 0.34 0.31 0.31 0.32

 0.04 0.19 0.16 0.17 0.17

0.02 0.12 0.10 0.10 0.13

0.00 0.00 0.00 0.00 0.00

Distilled water

The concentration of the unknown copper sulphate (CuSO₄) solution was figured out using
colorimetry. The known concentrations of CuSO₄ was prepared and their absorbance was
measured using a colorimeter with the wavelength of 600 nm. Absorbance readings were
plotted to create a calibration curve. The unknown solution ,CuSO₄,was then tested, and its
absorbance was compared to the calibration curve to find the concentration, following the
beer lambert law. This method provided a quantitative measure of the concentration of the
unknown solution based on the intensity of the colour.

Investigating the concentration of unknown solution using titration and

colorimetry
Acid-base titration involves the gradual addition of an acid to a base (or vice versa) until
neutralisation occurs, as indicated by a suitable pH indicator. Colorimetry, on the other hand,
measures the absorbance of a coloured solution at a specific wavelength to determine its
concentration based on the Beer-Lambert law.

Equipment

Burette

Pipette
Conical flask

Beakers

Standard solutions

pH indicator (phenolphthalein/methyl orange)

Colorimeter

Cuvettes

Unknown solutions
Method for titration
Rinse the burette with standard solution to fill burette and remove air bubbles from the tip.

Use a pipette to add a known volume of the unknown solution to a conical flask.
Pour several drops of the specific indicator into the flask.

Use the burette to slowly add the standard solution, swirling the flask constantly as you do so.

When the indicator changes colour, signalling the end point, stop adding the standard
solution.

Note the volume of the standard solution used.

Repeat the titration to record concordant results and calculate the average titre.
Volume of 0.1mol NaOH in beaker = 25.0cm3

Method for colorimetry

Collect or prepare a series of standard solutions of a known concentration.

This requires measuring the absorbance of each of the standard solutions at the relevant
wavelength on the colorimeter.

Plot a calibration curve of absorbance against concentration.

Then measure the absorbance of the unknown solution

Find the concentration of the unknown solution using the calibration curve. Before
measuring the unknown solution, make sure the colorimeter is blanked using distilled water
that does not absorb at the specific wavelength. This is so that any reading you take is due to
the analyte in the solution and its not contamination or any impurities in the cuvette.To test
the unknown fill the cuvette with the unknown solution then insert it into the colorimeter and
record the absorbance reading. Take at least 2 more measurements and calculate an average
so the accuracy of your result is improved

Results
The concentration of the unknown copper sulphate (CuSO₄) solution was determined using
colorimetry. Known concentrations of CuSO₄ were prepared and their absorbance was
measured using a colorimeter at a wavelength of 600 nm. The absorbance readings were
plotted to create a calibration curve. The unknown CuSO₄ solution was then tested, and its
absorbance was compared to the calibration curve to determine its concentration, following
the principles of Beer's Law. This method provided a quantitative measure of the
concentration of the unknown solution based on its colour intensity.

Reference list: titration: https://studymind.co.uk/notes/titrations: titration ph meter:

employees/Oneota.edu calorimetry: https://mmerevise.co.uk/a-level-chemistry-
revision/enthalpy-changes-and-calorimetry/ chem.libretexts.org www.chemistrystudent.com