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Redox Titration of Bleach - Concentration of Sodium Hypochlorite

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Table of Contents
1.0 Research Question ........................................................................................................................... 4

2.0 Rationale ...................................................................................................................................... 4-5

3.0 Methodology ................................................................................................................................... 6

3.1 Original Experiment ............................................................................................................................... 6

3.2 Modifications ........................................................................................................................................ 6
4.0 Risk Management ........................................................................................................................... 6

5.0 Results ............................................................................................................................................ 7

5.1 Qualitative observations ....................................................................................................................... 7

5.2 Raw Data ............................................................................................................................................... 7
5.3 Processing Data .................................................................................................................................. 8-9
5.4 Error Propagation ............................................................................................................................. 9-10
5.5 Results with considered error ............................................................................................................ 10
5.6 Graphical Representation .................................................................................................................. 11
6.0 Analysis of Data ............................................................................................................................. 12

6.1 Identification of limitations and uncertainty in data ......................................................................... 12

6.2 Interpretation and analysis of evidence.............................................................................................. 12
7.0 Evaluation ...................................................................................................................................... 13

7.1 Suggestions for improvements .................................................................................................. 13

7.2 Experiment could be extended by .............................................................................................. 13
8.0 Conclusion ..................................................................................................................................... 13

9.0 References .................................................................................................................................... 14

10.0 Appendix ..................................................................................................................................... 15

10.1 Original Experiment Procedure ................................................................................................ 15

10.2 Risk Assessment .................................................................................................................16-18

1
Abstract

2
1. Research Question
What is the accuracy of the advertised concentration of hypochlorite in commercial household bleach
compared to that determined by volumetric analysis?

Independent variable: Bleach solution type

Dependent variable: Concentration of sodium hypochlorite

2. Rationale
According to the Brønsted-Lowry model, acid is a chemical species capable of donating hydrogen ions (H+),
or more specifically protons. A Brønsted-Lowry base is any species acting as an acceptor of protons donated
by the acid. Facilitation is via a lone electron pair on the base (Jessie A. Key, n.d). Exchanging of protons is
formally known as, acid-base reaction (Ronald Bell, 2019). In Brønsted‐Lowry neutralisation, acids donate
protons to a base:
Acid + Base → Conjugate Acid + Conjugate Base

Titration is a quantitative analytical technique used to determine unknown concentrations of a solution by

precisely neutralising it with acid/base solutions of known concentration (Kelly Cox, 2019). This point of
neutralisation is the exact equivalence point, where equal amounts of reactants and products have reacted
together. Indicator is added to solution of unknown concentration to assist with identification of the
equivalence point.

Figure 1: Standard titration setup

The original in-class experiment was conducted to determine the concentration of ethanoic acid (CH3COOH)
in various white vinegar samples. During a reaction of CH3COOH with NaOH base, neutralisation occurred.
CH3COOH (aq) + NaOH(aq) → CH3COONa(aq) + H2O(l)
The experimental findings were used in calculating moles of base used (Eq. 1), and in turn concentration for
the unknown acid in solution (Eq. 2).

This experimental design was modified to determine basic sodium hypochlorite (NaClO) concentrations in
household bleach. NaClO is the primary bleaching agent used in household chlorine-based bleach solutions.
NaClO is highly unstable due its desired breakdown into chloride ions (Cl-) (Purva Shah, 2015). A strong
oxidising agent; NaClO is able to oxidise other substances by accepting electrons via a reduction process.

3
Bleaching is a process where molecules of staining substances (chromophores) are chemically modified to no
longer reflect visible light (M.S Vela Gurovic, 2016). This occurs through redox reactions of hypochlorite ions,
ClO-, which form from NaClO dissociation, with chromophore bonds (Melissa Sandoval, n.d). When placed in
contact with a stain, ClO reduction occurs as it oxidises the chemical bonds within chromophores that reflect
coloured light by accepting electrons donated by this bond. Chromophores undergo oxidation as electrons
are donated, this transfer of electrons is a reduction-oxidation (redox) reaction.
Sodium hypochlorite is also used to remove bacteria and disinfect pools and similar moist environments.
NaClO is a liquid form of chlorine (Cl), containing 5% available Cl (USNM, 2019). When added to water,
NaClO rapidly reacts to form different chemicals. Primarily the disinfecting agent of hypochlorous acid
(HOCl). Dependent on the solution’s pH, hypochlorous almost immediately disassociates, forming less
microbicidal hypochlorite ions (ClO-) (Barcin Ozturk, 2019). Greater H+ concentrations result in lower pH, and
greater OH- concentrations result in higher pH. The disinfecting efficacy of chlorine decreases as pH
increases, demonstrated by a greater conversion rate of HOCl to ClO− at higher pH’s (Laurence McKeen,
2012). The pH of standard (5% (w:v)) bleach solutions is 11. Due to its strong basicity, over application of
NaClO (bleach) to moist environments increases environmental pH, decreasing disinfecting efficacy
(Cleanroom Technology, 2013).

Figure 2: Relationship between HOCl and ClO- (OCl-) at Various pH Values (Susan Delia Freese, n.d)

For the purpose of this task, ‘Power Force’ toilet bleach and ‘White King’ laundry bleach were identified as
solutions where the concentration of NaClO could be experimentally calculated.
These modifications redirected the original experiment towards determining concentrations of NaClO in two
bleach samples and verifying this with theoretical and expected values.
To achieve this, Redox titration using potassium iodate solution, bleach sample, starch indicator and sodium
thiosulfate, was undertaken.

Two individual redox reactions occurred during the process of this experiment:
1) As iodide ion (of potassium iodate) is added to ClO- (of bleach solution), oxidising iodide to iodine.
2) As the iodine formed is titrated with sodium thiosulfate (Na2S2O3) to reduce iodine back to iodide.

It is expected results will match concentrations labelled on each bleach solution. As stated, a lower
concentration of sodium hypochlorite in toilet bleach compared to laundry bleach is hypothesised. This is
because NaClO forms HOCl when reacted with water. If over-addition of NaClO occurred, efficacy of the
disinfecting agent would be compromised and be no more effective than a smaller concentration. Since
more disease is present in a toilet than a washing machine, it requires greater disinfecting efficacy.
4
3. Methodology
3.1 Original Experiment:
The original experiment aimed to determine the concentration of ethanoic acid (CH3COOH) in samples of
white vinegar using a standard solution as reference. This was achieved by neutralising the vinegar with a
sodium hydroxide (NaOH) base of known concentration (CH3COOH).
A greater average titre of NaOH used indicated more ethanoic acid present in the vinegar. Using the average
titre, mole ratios and chemical calculations for the completed titrations, the concentration of CH3COOH was
calculated. This was found to be 0.805 mol L-1 in undiluted vinegar solution.
3.2 Modifications
To ensure the collection of sufficient and relevant data, the original experiment was:
Extended by:
a) Using 2 samples of household bleach to determine the concentration of sodium hypochlorite
(NaClO) – (independent variable). This experimental value was then compared to the theoretical to
determine the reliability and safety of the product.
Refined by:
a) Completing 4 trials of each titration to uncover inaccuracies and thus eliminate them from averages
calculations (controlled variable)
b) Identical samples of solutions (ie. sodium thiosulfate, potassium iodate, diluted bleach) were used
for each titration to ensure results were not skewed or inaccurate given the potential for differing
sample quality (controlled variable).

4. Risk Management
In reference to MSDS sheets (10.1.2), NaClO (bleach) may cause severe skin burns, rashes and wheezing.
Na2S2O3 and Iodine (I) when in contact with the eye and skin may cause severe irritation. All waste products
were disposed of down a dedicated chemical drain immediately after use. Any chemical solution that
contacts the skin will be washed off instantly. Personal protective equipment such as safety glasses and
gloves will be worn when dealing with chemicals to reduce the aforementioned risks. Thus, ensuring
contamination, contact or inhalation of chemicals is minimised. All waste products will be disposed of down
a dedicated ‘waste’ drain immediately after use.

5
5. Results
5.1 Qualitative Observations:
During the redox reaction of bleach solution, addition of potassium iodide (KI) caused a reaction to occur
between I (iodine) and ClO- resulting in a brown-coloured solution, Figure 4 (a).
As Na2S2O3 from the burette was added, the colour changed to a straw yellow.
Starch was then added, turning the solution a dark blue, see Figure 4 (b), and further addition of Na2S2O3
eventually turned the solution colourless, indicating the end of the titration, as shown in Figure 4 (c).

Figure 4: Left (a): solution colour after addition of Iodine, Middle (b): solution after addition of
starch indication, Right (c): solution after addition of final sodium thiosulfate.

5.2 Raw Data:

Toilet Bleach – (Power Force Brand)
Experimental Results: Titration of Iodine in Diluted Bleach solution
Titration
Initial burette reading (mL) Final burette reading (mL) Titre (mL)
No.
Error ± 0.05 ± 0.05 ± 0.10
1 29.48 20.50
2 29.69 20.30
50
3 29.21 20.80
4 28.60 21.40

Household Laundry Bleach – (White King Brand)

Experimental Results: Titration of Iodine in Diluted Bleach solution
Titration
Initial burette reading (mL) Final burette reading (mL) Titre (mL)
No.
Error ± 0.05 ± 0.05 ± 0.10
1 28.80 21.20
2 28.90 21.10
50
3 29.00 21.00
4 29.50 20.50
Table 1: Raw Data – experimental results

* Note: Only concordant titres were used in calculating average titre.

6
5.3 Processing Data:
Raw data shown in Table 1 was processed to determine the concentration of hypochlorite. Systematic errors
were propagated to determine the precision and reliability of the experimentation. The investigation’s
accuracy and validity were established through comparison of theoretical and experimental values. 4
significant figures (SF) are carried through calculations.
The known constants and values for the following calculations are:

- Molar Mass (mm) of KIO3 = 214.0 g mol-1 - Molar Mass (mm) of NaCIO = 74.44 g mol-1

Concentration of NaS2O3:
0.1 mol L-1 solution of sodium thiosulafate was provided.

Toilet Bleach (Power Force Brand) - Concentration of hypochlorite ions (ClO-):

7
 Household Laundry Bleach (White King Brand) - Concentration of hypochlorite ions (ClO-):
Using the identical calculation process shown above, the percentage of hypochlorite in 1L of undiluted
household laundry bleach was calculated.

5.4 Error Propagation:

Error calculations were used to confirm accuracy and/or inaccuracy of data.

Table 2: Error – Toilet Bleach Titration (4 SF)

Table 3: Error – Laundry Bleach Titration (4 SF)

The titre’s mean error, (excluding non-concordant trial) was calculated based on table 1 data:

Table 4: Absolute & Percentage Error from mean titre

8
 Toilet Bleach - experimental relative to theoretical:
‘Power Force’ bleach = Sodium hypochlorite (2.18% (w/v)) equating to 2.18g/100mL of solution.

Household Laundry Bleach - experimental relative to theoretical:

‘White King’ bleach = Sodium hypochlorite (4.2% (w/v)) equating to 4.2g/100mL of solution

5.5 Results with absolute error:

*Note calculated uncertainty was used for error bars on constructed graphs (5.6).
Table 5: Results w/ absolute error

9
5.6 Graphical Representation:

The processed experimental data above for concentration of sodium hypochlorite was graphically
represented using the determined error for error bars (Figure 5):

Due to minimal errors associated with results and low visibility of error bars, enlarged Figure 6 and 7
provide analysis:

Comparison of actual theoretical concentration of NaClO in ‘Power Force’ toilet bleach and ‘White King’
laundry bleach (Figure 8):

Theoretical Concentration of NaClO in Bleach Solution

0.6

0.5
(Concentation (mol L-1)

0.4

0.3

0.2

0.1

0
1 2
Type of Bleach Solution

Figure 8: Theoretical concentration of NaClO in Toilet and Laundry Bleach solution

10
6. Data Analysis
6.1 Identification of limitations and uncertainty in data
Table 4 Indicates that the titre of Na2S2O3 used for the titration of toilet and laundry bleach were extremely
precise relative to each other, with variances of ± 1.22% for toilet bleach and ± 0.47% for laundry bleach from the
mean. The systematic error calculated for the sodium hypochlorite concentration in each bleach solution is
minimal and shows no extreme shortfall in calculations due to the accuracy of titration equipment. Comparison of
the experimental and theoretical concentration of sodium hypochlorite allowed the accuracy and validity of the
investigation to be assessed. The experimental calculations proved inaccurate, with the concentration of sodium
hypochlorite in toilet bleach possessing a 41.59% error, and laundry bleach a 24.64% error. However, the
experimental concentration still aligns with the outcome defined in the original hypothesis and can be supported
by scientific theory.

6.2 Interpretation and analysis of evidence:

Data represented in figure 5 and 8 confirms the hypothesis of a lower sodium hypochlorite concentration
present in toilet bleach compared to laundry bleach. Despite the error mentioned in section 6.1,
experimental concentrations align to the desired general trend.
For the titration of laundry bleach, a slightly greater average titre of NaS2O3 (21.10 mL) was required to reach
the end point compared to toilet bleach (20.53 mL). Iodometry is a volumetric analysis technique where the
presence of I2 is used to determine the end point of a redox reaction (University of Illinois, n.d). An excess
amount of iodine was added to the oxidising agent NaClO. This resulted in a conversion of ClO- ions to
chloride ions and an oxidation of iodide ions to brown iodine molecules (Richard Walding, 2018).
The addition of the titre, S2O32- to yellow I2 (aq) solution caused a gradual decrease in colour strength to a pale
yellow. This signified a decrease in I2 concentration. At this point, starch indicator was added to assist in end
point determination. The solution turned dark blue in colour, before additional NaS2O3 was reacted until
colourless solution appeared. This signified the reactions end point with titrated NaS2O3 where no more I2
was present in solution (Cornell University, n.d).
Starch is a polysaccharide consisting of amylose and amylopectin molecules, of which the amylose is
responsible for the dark-blue colour formation in the presence of I2 (Matthew Cherian, 2016). This dark-blue
complex allowed identification of the end point so used titre could be noted. A transfer of charge between
Iodine and starch resulted in altercations of the energy level spacings in the helix shaped starch-iodide
complex (Eric Bertoft, 2017). This new arrangement assists in selectively absorbing near all visible light and
thus appearing dark blue in colour (M. Hassan, 2016).
The more NaS2O3 required to balance I2, the larger the concentration of NaClO in solution according to the
theory that moles produced of I2 is equal to moles present of ClO- in bleach solution. This supports the
hypothesis given that greater titre was required for household laundry bleach.
The calculated concentration of NaClO was found to be 0.4220  1.507  10-3 mol L-1 in household laundry
bleach and 0.4106  1.478  10-3 mol L-1 in toilet bleach. Given that the toilet bleach is strongly basic and is
applied to moist environments, its efficacy as a bleaching agent would be compromised if a large
concentration of basic NaClO reacted with water (H2O). Bleach dissociates into the strong bleaching agent,
HOCl, when reacted with H2O. However, as pH rises with the increased addition of strongly basic NaClO,
more ClO- becomes available than HOCl which is 80 times less powerful as a bleaching agent. This conversion
is represented as: HOCl ⇌ ClO− + H+. Once a solution’s pH rises above 6.0, HOCl declines from near 100% of
the portion to 0 at pH 9 (See Figure 2). Hence, this theory supports the experimental findings of a lower
NaClO concentration in toilet bleach.

11
7. Evaluation
Suggestions for improvements:
A great quantity of uncontrollable error was present in this experiment. For example, the concentration of sodium
thiosulfate solution provided may not have exactly corresponded to its label. This may have impacted on the
accuracy of experimental concentrations relative to theoretical concentrations. Sodium Thiosulfate could be self-
standardised in future for this error to be limited.

Aged or impure samples of potassium iodide may have been utilised in this experimental process. Iodide oxidises
slowly with air when in storage for large periods of time, meaning more iodine than iodide may have been
present during testing. As such, a larger amount of sodium thiosulfate would be required to turn the solution
brown. Hence, calculations would show a greater concentration of NaClO than expected, as occurred in this
experiment. This could be improved by sourcing fresh chemicals and ensuring storage is in a suitable place.

The experiment could be extended by:

Initial research indicated that an alternative, safer bleach product made from sodium peroxide exists (biome,
2019). A future experiment could aim to investigate and compare the effectiveness of sodium peroxide and other
brands of sodium hypochlorite bleach. This would be in terms of the bleaching agent released when reacted with
water and disinfecting efficacy. Coherently, the general acceptance of chlorine-based bleach could be questioned
and potentially launch a shift toward the use of safer, oxygen bleach.

8. Conclusion
The investigation found the concentration of NaClO to be 0.4220  1.507  10-3 mol L-1 in household laundry
bleach (White King) and 0.4106  1.478  10-3 mol L-1 in toilet bleach (Power Force). It was established that
this was due to the varying dissociation rate of HOCl in different pH’s when NaClO was applied to moist
environments, and the poor disinfecting efficacy of ClO- in solutions of high pH.

Despite error likely resulting from discrepancies in quality of the provided chemicals and reactions occurring
prematurely, the experimental data reflected the hypothesis and desired theoretical relationship for
concentration of NaClO in two different bleach samples.

The stated improvements will assist in controlling errors for future experimental processes.

12
9. References
Bertoft, E. (2017, July). Understanding Starch Structure. Agronomy - Gamla Sampasvägen.
Clarke, C. W. (2017). Effectiveness of sodium hypochlorite as a disinfestation treatment. Retrieved from:
https://vinehealth.com.au/wp-content/uploads/2017/12/Clarke_et_al-2017-
Australian_Journal_of_Grape_and_Wine_Research.pdf
Crampton, L. (2013, August 17). How Bleach Works: Disinfection, Stain Removal, and Dangers. Owlcation.
Retrieved from:
https://owlcation.com/stem/How-Bleach-Works-Disinfection-and-Stain-Removal
Department of Physical Sciences Kingsborough Community College The City University of New York. (2010). The
Determination of Hypochlorite in Bleach. Retrieved from:
https://www.kbcc.cuny.edu/academicDepartments/PHYSCI/PL/chm11/Documents/Bleach.pdf. https://www.uwo.ca/animal
-research/doc/bleach-sop.pdf
Determining the Percent Sodium Hypochlorite in Commercial Bleach. (n.d.). Retrieved from:
https://web.lemoyne.edu/giunta/chm151L/bleach.html

Fabiano Barbieri Gonzaga. (n.d.). Precise determination of hypochlorite in commercial bleaches with established
traceability using automatic potentiometric titration.
Hydro Instruments. (n.d.). Basic Chemistry of chlorination. Retrieved from:
http://www.hydroinstruments.com/files/Basic%20Chemistry%20of%20Chlorination.pdf
Hypochlorite - ClO- Structure, Molecular Weight, Properties, Uses. (2019, April 17). Retrieved from:
https://byjus.com/chemistry/hypochlorite/

Hypochlorite. (n.d.). ScienceDirect.com | Science, health and medical journals, full text articles and books.
Retrieved from:
https://www.sciencedirect.com/topics/chemistry/hypochlorite
Hypochlorous Acid. (n.d.). ScienceDirect.com | Science, health and medical journals, full text articles and books.
Retrieved from:
https://www.sciencedirect.com/topics/pharmacology-toxicology-and-pharmaceutical-science/hypochlorous-acid
Sodium Hypochlorite (NaOCl). (n.d.). Chemical Blending, Dilution, Production, Handling (Sodium Hypochlorite,
Chlorine, Sulfur Dioxide, and More. Retrieved from:
https://www.powellfab.com/technical_information/preview/general_info_about_sodium_hypo.aspx
Sodium hypochlorite as a disinfectant. (n.d.). Water Treatment and Purification - Lenntech. Retrieved from:
https://www.lenntech.com/processes/disinfection/chemical/disinfectants-sodium-hypochlorite.htm
Starch and Iodine. (2019, June 5). Chemistry LibreTexts. Retrieved from:
https://chem.libretexts.org/Bookshelves/Biological_Chemistry/Supplemental_Modules_(Biological_Chemistry)/Carbohydr
ates/Case_Studies/Starch_and_Iodine
The structure of the blue starch-iodine complex. (n.d.). The Science of Nature. Retrieved from:
https://link.springer.com/article/10.1007%2FBF00365977
Titration of a Weak Base with a Strong Acid. (2019, June 5). Chemistry LibreTexts. Retrieved from:
https://chem.libretexts.org/Bookshelves/Ancillary_Materials/Demos%2C_Techniques%2C_and_Experiments/General_Lab
_Techniques/Titration/Titration_of_a_Weak_Base_with_a_Strong_Acid
Why Does Iodine Turn Starch Blue? Education :: ChemistryViews. (n.d.). ChemistryViews. Retrieved from:
https://www.chemistryviews.org/details/education/10128441/Why_Does_Iodine_Turn_Starch_Blue.html

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10. Appendix

14
 10.1.2 Material Safety Data Sheet

Sodium Thiosulfate

Retrieved from: (Chem Supply PTY LTD, 2018)

15
Sodium Hypochlorite:

Retrieved from: (Chem Supply PTY LTD, 2018)

16
 Iodine:

Retrieved from: (Chem Supply PTY LTD, 2018)

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