6030 Lab Ex 3 Druk

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MARITIME UNIVERSITY OF SZCZECIN

Institute of Mathematics, Physics and Chemistry


Department of Chemistry

EXERCISE INSTRUCTION

Laboratory Exercise 3
pH of solutions
Hydrolysis of salts

dr inż. Andrzej Kozłowski


dr inż. Agnieszka Kalbarczyk-Jedynak
dr Magdalena Ślączka-Wilk
Prepared by:
dr inż. Konrad Ćwirko
mgr inż. Czesław Wiznerowicz
Grażyna Gorzycka
Teacher in Charge: dr Magdalena Ślączka-Wilk
Approved by: dr inż. Agnieszka Kalbarczyk-Jedynak
Effective from: 01.10.2023
EXERCISE SHEET
1 Relation to subjects: ESO/25, 27 DiRMiUO/25, 27 EOUNiE/25, 27
Learning outcomes
Specialty/Subject Detailed learning outcomes for the
for the subject
subject
ESO/26 Chemistry EKP3 SEKP3 – Water quality indicators;
of water, fuels and K_U014, K_U015, SEKP6 – Performing determinations of
lubricants K_U016. selected indicators of technical water
quality;
DiRMiUO/26 EKP3 SEKP3 – Water quality indicators;
Chemistry of water, K_U014, K_U015, SEKP6 – Performing determinations of
fuels and lubricants K_U016. selected indicators of technical water
quality;
EOUNiE/26 EKP3 SEKP3 – Water quality indicators;
Chemistry of water, K_U014, K_U015, SEKP6 – Performing determinations of
fuels and lubricants K_U016. selected indicators of technical water
quality;
2 Purpose of the exercise:
mastering basic chemical concepts related to solutions of acids, bases and salts as well
as acquiring practical skills in the field:
− determination of pH and measuring the pH of solutions,
− calculating the pH of solutions of strong and weak acids and bases,
− determining the reaction of individual types of salts after hydrolysis on the basis of
the reaction,
− calculating the pH of specific salt solutions and buffer mixtures.
3 Prerequisites:
general knowledge of pH, solution reaction, hydrolysis obtained from high school,
knowledge of the key issues of ion dissociation acquired during the previous exercise,
knowledge of the principles of work in a chemical laboratory
4 Description of the laboratory workplace:
a set of laboratory glassware, a set of reagents and indicators for testing pH and
hydrolysis,
5 Risk assessment:
the likelihood of chemical burns from exposure to 0.2 M sulphuric acid is very small,
and the effects are minor,
Final assessment – VERY SMALL THREAT
Security measures required:
1. Lab coats, gloves and safety glasses.
2. Health and safety cleaning products, paper towels.
6 The course of the exercise:
1. Getting to know the workplace manual (appendix 1).
2. Carrying out the experiments provided for in the manual.
7 Exercise report:
1. Develop an exercise in accordance with the instructions contained in the
workplace manual.
2. Solve the given task and/or answer the questions included in the set of tasks and
questions to be completed by the student.

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8 Archiving of research results:
report on exercises – prepared in accordance with the rules applicable in the laboratory
– should be submitted in writing to the academic teacher during the next classes.
9 Assessment method and criteria:
a) EKP1, EKP2 – checking the knowledge of basic chemical concepts of pH and
hydrolysis in class,
b) SEKP4 – the detailed learning outcome for an individual student will be assessed
on the basis of the solutions to tasks and problems presented in the report, given
for independent solution/development:
− mark 2,0 – the student has a general knowledge of pH and salt hydrolysis, but
is not able to use it in practice to solve basic problems,
− mark 3,0 – has basic chemical knowledge of pH and salt hydrolysis and is able
to use it to a small extent to solve potential problems in his specialty,
− mark 3,5 – 4,0 – has extensive chemical knowledge in the field of pH, salt
hydrolysis and is able to use it to a basic extent to determine the pH and
calculate the pH of various electrolyte solutions and to solve problems on the
ship,
− mark 4,5 – 5,0 – has complete chemical knowledge in the field of pH and salt
hydrolysis and is able to use in practice complex chemical knowledge to
determine and calculate the pH of individual acid, alkali, salt and buffer
solutions and to solve complex problems,
10 References:
1. https://assets.openstax.org/oscms-prodcms/media/documents/Chemistry2e-
WEB.pdf (accessed 15.07.22).
2. A. Kozłowski, A. Kalbarczyk-Jedynak, M. Ślączka-Wilk, K. Ćwirko, C.
Wiznerowicz, G. Gorzycka, Instrukcje stanowiskowe do ćwiczeń
laboratoryjnych: pH roztworów. Reakcje soli z wodą, AM Szczecin 2022 (in
Polish).
3. J. E. McMurry, R. C. Fay, J. K. Robinson, Chemistry, 7th edition, global edition,
publisher: Pearson, 2016.
4. A. Blackman, S. Bottle, S. Schmid, M. Mocerino, U. Wille, Chemistry, 2nd
edition, publisher: John Wiley&Sons, 2012.
5. G. Curran, Chemistry, publisher: The Career Press, 2011.
6. J. T. Moore, Chemistry for Dummies, publisher: Wiley Publishing, 2015.
7. D. Kealy, P.J. Haines, Analytical Chemistry, publisher: BIOS Scientific
Publishers Limited, 2002.
8. Sparkcharts Chemistry, 2002 Spark Publishing, A Division of Barnes & Noble,
Canada 2014.
9. M. D. Jackson, Chemistry, 2015 BarCharts, Inc. (Quickstudy.com).
10. M. Charmas, English for Students of Chemistry, Maria Curie-Skłodowska
University Press, Lublin 2012.
11. Stundis H., Trześniowski W., Żmijewska S.: Ćwiczenia laboratoryjne z chemii
nieorganicznej. WSM, Szczecin 1995 (in Polish).
12. M. Wesołowski, K. Szefer, D. Zimna, Zbiór zadań z analizy chemicznej,
Wydawnictwa Naukowo – Techniczne, Warszawa 1997 (in Polish).
11 Notes

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1. THEORY
KEYWORDS:

− pH,
− salt hydrolysis.

pH
Water dissociation constant (Kw):

H2O(l) + H2O(l) H3O+(aq) + OH–(aq) or simplified version:

H2 O H+ + OH– (self-ionization of water)

K = [H3O+] · [OH–] / [H2O] = 1,8 · 10–16 at 25°C; molar concentration of water [H2O] has
a constant value: 55.5 mol/dm3:

[H3O+] · [OH–] / 55.5 = 1.8 · 10–16

[H3O+] · [OH–] = Kw (The Kw value is constant!) = 1.0 · 10–14 in pure water

[H3O+] = [OH–] = 1.0 · 10–7

The Kw value allows to convert from [H3O+] to [OH–] and vice versa in any aqueous
solution not just pure water.
The pH is a measure of the acidity of the solution, the acidity is related to the
concentration of the hydronium ion [H3O+] in the solution. The more acidic the solution the
larger concentration of the hydronium ion.
The pH scale is based on the molar concentration of the hydronium ion [H3O+] in the
solution and ranges from 0 to 14 for most of the practical applications. There are values that
are lower than 0 (very acidic solution) and higher than 14 (concentrated aqueous bases).

The pH is defined as the negative logarithm (log) of the [H3O+]:

pH = –log [H3O+]; [H3O+] = 10–pH

pOH = –log [OH–]; [OH–] = 10–pOH

pH + pOH = 14

The pH of pure water equals 7 (pH=7): [H3O+] = [OH–] = 1.0 · 10–7.


Acidic solution has a pH value lower than 7 (pH < 7); Basic solution has a pH value
higher than 7 (pH >7).

pH indicators are substances that change the color in the presence of a base or an acid.
Examples of pH indicators:

− litmus paper (when the solution is acidic litmus turns red; when the solution is basic
litmus turns blue),

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− phenolphthalein (clear and colorless when the solution is acidic, pink in a basic
solution),
− methyl orange (red in acidic solution, yellow in basic solution),
− universal indicator (the colors from yellow to red indicate an acidic solution; the colors
from blue to violet indicate a basic solution, green color indicates the neutral solution).

Buffer solutions (buffers) – prevent a change in pH that is caused by the addition of


acid or base. Buffer must contain something that reacts with an acid – a base and also something
that reacts with a base – an acid. Buffer is a solution of a weak acid and a salt of its conjugate
base and a solution of a weak base and a salt of its conjugate acid.
In other words, an acidic buffer (for example acetic acid and sodium acetate) solution is
made from a weak acid and one of its salts – usually a sodium salt. An alkaline buffer (for
example ammonia plus chloride solution) solution is made from a weak base and one of its
salts.

pH calculation of a buffer of weak acid and conjugate base (weak acid plus one of its salts):

[H3O+] = Ka x Molarity of a weak acid / Molarity of its salt


pH = –log [H3O+]

Example: Determine the pH of a buffer of 0.5 M of an acetic acid (HAc) and 0.3 M
of sodium acetate (Ac–). Given: Ka = 1.7 · 10 –5.
[H3O+] = 1.7 · 10 –5 · 0.5 / 0,3 = 2.8 · 10 –5mol/dm3
pH = –log [0.000028] = 4.55
Henderson – Hassellbach Approximation can be also used for calculation pH
of an acid – salt buffer:
pH = pKa + log ([A–] / [HA])
pH = 4.77 + log (0.3 / 0,5) = 4.55

pH calculation of a buffer of weak base and conjugate acid (weak base plus one of
its salts):
[H3O+] = 10–14 · Molarity of a salt / Kb x Molarity of a weak base
pH = –log [H3O+]

Hydrolysis of salts
Hydrolysis reaction is the reverse reaction to neutralization reaction, salts react with
water to give back an acid and a base – a simplified definition.
In other words hydrolysis of salts is the reaction between water and aqueous ion, yields
to a basic or acidic solution by forming H3O+ (or simplified version H+) or OH– ions.

A– + H2O ↔ HA + OH– (basic solution) salts formed from strong bases and weak acids
M+ + H2O↔ MOH + H+ (acidic solution) salts formed from strong acids and weak bases

Salts formed from strong acids and strong bases do not hydrolyze!
Salts formed from strong acids and weak bases, weak acids and strong bases and finally
weak acids and weak bases hydrolyze!

Example 1 (A worked example): write a hydrolysis reaction of MgCl2 (a salt formed from
a strong acid and a weak base):

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Solution:
a) the first step: write a dissociation reaction of a given salt: MgCl2→Mg2+ + 2Cl–
b) the second step: pick an ion that is a weak part of the given salt: Mg2+
c) write a hydrolysis reaction: Mg2+ + 2H2O↔ Mg(OH)2 + 2H+ acidic solution

Example 2 (A worked example): write a hydrolysis reaction of Na2CO3 (a salt formed from
a weak acid and a strong base):

Solution:
a) the first step: write a dissociation reaction of a given salt:
Na2CO3→2Na+ + CO32–
b) the second step: pick an ion that is a weak part of the given salt: CO32-
c) write a hydrolysis reaction: CO32– + 2H2O↔ H2CO3 + 2OH– basic solution

Example 3 (A worked example): write a hydrolysis reaction of MgCO3 (a salt formed from
a weak acid and a weak base):

Solution:
a) the first step: write a dissociation reaction of a given salt:
MgCO3→Mg2+ + CO32–
b) the second step: pick an ion that is a weak part of the given salt: CO32–; Mg2+
c) write a hydrolysis reaction: CO32- + 2H2O ↔ H2CO3 + 2OH–
Mg2+ + 2H2O ↔ Mg(OH)2 + 2H+

Examples of selected calculations related to concentration of [H3O+], [OH–] and pH


(with a solution)

Example 1 What are the [H3O+] and [OH–] of a solution with pH of 4?

pH = 4 [H3O+] = 10–4 mol/dm3


pOH = 14 – 4 = 10 [OH–] = 10–10 mol/dm3
Example 2 What are the pH and pOH of a solution with a [OH–] of 4.5 · 10–2 mol/dm3?

pOH = –log [4.5 · 10–2] = 1.35


pH = 14 – 1.35 = 12.65
Example 3 Determine the pH of a 0.1 mol/dm3 solution of HCl, a strong acid.
HCl H+ + Cl–
+
Strong acid: [H3O ] = Given concentration of strong acid solution

[H3O+] = 0.1 mol/dm3


pH = –log [0.1] = 1
Example 4 Determine the pH of a 0.01 mol/dm3 solution of NaOH and Ba(OH)2, strong bases.
Strong base: [OH–] = coefficient in front of the hydroxide ion (OH–) x given concentration of
strong base solution

NaOH Na+ + OH– [OH–] = 1 · 0.01 mol/dm3 = 0.01 mol/dm3 pOH = –log[0.01] = 2;
pH = 14 – 2 = 12
Ba(OH)2 Ba + 2OH [OH–] = 2 · 0.01 mol/dm3 = 0.02 mol/dm3
2+ –

pOH = –log[0.02] = 1.70; pH = 14 – 1.70 = 12.3

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Example 5 Determine the pH of a solution of CH3COOH (acetic acid), weak acid. Given: molar
concentration of acetic acid (c; M) = 0.4 mol/dm3; Ka = 1.8 · 10–5

c/K = 0.4/0.000018 = 22222 simplified version of law of dilution:


K= c · α2 α = (K/c)0.5 = 0.0067
α = the molar concentration of dissociated electrolyte / the total molar concentration of
electrolyte [mol/dm3; mol/l].
0.0067 = x / 0.4 mol/dm x = 0.00268 mol/dm3 pH = – log [x] = – log [0.00268] = 2.57
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Tasks and questions to be performed by the student:

1. What are the [H3O+] and [OH–] of a solution with pH of 6? Answer: [H3O+]=10–6mol/dm3;
[OH–]=10–8mol/dm3
2. What are the pH and pOH of a solution with a [H3O+] of 2.1 · 10–2 mol/dm3? Answer:
pH=1,7; pOH=12,3
3. What are the pH and pOH of a solution with a [OH–] of 5.5 · 10–5 mol/dm3? Answer:
pH=9,74; pOH=4,26
4. Determine the pH of a 0.005 mol/dm3 solution of HClO4. Answer: pH=2,30
5. Determine the pH of a 0.01 mol/dm3 solution of KOH. Answer: pH=12,0
6. Determine the pH of a 0.01 mol/dm3 solution of Sr(OH)2. Answer: pH=12,3
7. Determine the pH of a 0.01 mol/dm3 solution of CH3COOH; Ka = 1.8 · 10–5. Answer:
pH=3,37
8. Determine the pH of a 0.01 mol/dm3 solution of NH4OH; Kb = 1.8 · 10–5. Answer:
pH=10,63
9. Write a hydrolysis reaction of BaCO3 and state whether a salt solution is acidic, basic or
neutral.
10. Write a hydrolysis reaction of K2S and ZnSO4 and state whether salt solutions are acidic,
basic or neutral.

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2. INSTRUCTION 3 – LABORATORY EXERCISE 3
Experiment 1 – Acid / Base indicators (Identifying acids and bases with indicators)

Materials and reagents:

Glass test tube set, measuring cylinder, acetic acid solution (0.1M CH3COOH),
ammonium hydroxide solution (0.1M NH4OH), pH indicators: methyl orange, methyl red,
litmus, phenolphthalein, universal indicator.

Experimental procedure:

Pour 4 cm3 of acetic acid solution (0.1M CH3COOH) to each of five test tubes, into the
next five test tubes pour 4 cm3 of ammonium hydroxide solution (0.1M NH4OH). Test tubes
with the ammonium hydroxide solution should be placed behind the test tubes with acetic acid
solution on the test tube rack. Add to each pair of test tubes (acid and base) 3 drops of indicator
given in the table.

The colour of the


The colour of the acetic
Test ammonium hydroxide pH ranges of pH
pH indicator acid solution
tube solution indicators
(0.1M CH3COOH)
(0.1M NH4OH)
1. Methyl orange
2. Methyl red
3. Litmus
4. Phenolphthalein
5. Universal

Data analysis (after the experiment):

1. Fill in the given table for the pH indicators.


2. Calculate the pH of acetic acid solution. Given: K = 1.8 · 10–5; [CH3COOH] = 0.01 M.
3. Calculate the pH of ammonium hydroxide solution. Given: K = 1.8 · 10–5;
[NH4OH] = 0.01 M.

Experiment 2 – pH of salt solutions

Materials and reagents:

Glass test tube set, measuring cylinder, micro spatula, pH indicators: universal,
phenolphthalein, selected salt solutions: sodium sulfide (2M Na2S), zinc chloride (2M ZnCl2),
solids: copper (II) sulfate (CuSO4), sodium carbonate (Na2CO3), potassium nitrate (KNO3),
sodium sulfate (Na2SO4), sodium acetate (CH3COONa), ammonium chloride (NH4Cl).

Experimental procedure:

Pour 4 cm3 of distilled water to each of nine test tubes. Add to each of the test tube 5
drops of the universal indicator solution. The first test tube treat as a control sample and add to
the rest of the test tubes small amount of salts listed in the given table. Do not mix it. Record
the color change of the universal indicator. Repeat the procedure using phenolphthalein as a pH
indicator.
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Acidic/Basic/neutral
The colour
pH value solution The colour
Test Salts plus control change of the
(see the table (state whether change of the
tube sample universal
below) solution is acidic, phenolphthalein
indicator
basic or neutral)
1. Control sample
2. Copper (II) sulfate (CuSO4)
3. Sodium carbonate (Na2CO3)
4. Potassium nitrate (KNO3)
5. Sodium sulfide (2M Na2S)
6. Zinc chloride (2M ZnCl2)
7. Sodium sulfate (Na2SO4)
8. Sodium acetate
(CH3COONa)
9. Ammonium chloride
(NH4Cl)

The colour of the universal indicator


pH value
(according to Yamada – based on pH value)
4.0 Red
5.0 Orange
6.0 Yellow
7.0 Green
8.0 Blue
9.0 Dark blue
10.0 Violet

Data analysis (after the experiment):

1. Fill in the given table.


2. For each given salt identify the acid and the base from which this salt was formed; write the
neutralization reaction (acid + base = salt + water) and balance it.
3. Write the hydrolysis reactions (salt + water) – molecular and ionic form of the reaction
(molecular and ionic equation).
4. What type of salts hydrolyze?

Experiment 3 – The effect of temperature on hydrolysis reaction

Materials and reagents:

Glass test tube set, measuring cylinder, test tube holder, solution of sodium acetate (0.1
M CH3COONa), phenolphthalein.

Experimental procedure:

Pour 4 cm3 of sodium acetate (0.1 M CH3COONa) solution into the test tube and add
2 – 3 drops of phenolphthalein. Heat the solution in the laboratory water bath and then cool it
down. Record the obtained colors of the solution.

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Data analysis (after the experiment):

1. Write the hydrolysis reaction (CH3COONa + water) – molecular and ionic equation.
2. Explain the effect of temperature on the reaction of interest.

Experiment 4 – pH of a buffer solution

Materials and reagents:

Glass beakers, measuring cylinder, solutions of sodium acetate (0.1 M CH3COONa),


acetic acid (0.1M CH3COOH), ammonium chloride (0.1M NH4Cl), ammonium hydroxide
(0.1M NH4OH), pH indicators: litmus strips, pH color strips, universal pH indicator.

Experimental procedure:

Pour 4 cm3 of ammonium chloride (0.1M NH4Cl) and 8 cm3 of ammonium hydroxide
(0.1M NH4OH) into the first beaker. Pour 4 cm3 of sodium acetate (0.1 M CH3COONa) and 8
cm3 of acetic acid (0.1M CH3COOH) into the second beaker. Determine the pH of the buffer
solutions using pH color strips (different pH ranges: pH:1 – 7; pH: 7 – 14), pH meter and also
determine the color of the buffer solutions after adding a few drops of universal indicator and
also after immersing the litmus strip in the buffer solution for 2 seconds.
How to use pH color strips? Immerse the strip in the test solution for a few seconds then
compare the developed color to the sequence chart on the package and read the pH.

Data analysis (after the experiment):

Fill in the table below

Testing methods for Beaker I Beaker Beaker II Beaker


measuring pH values (alkaline buffer solution) I (acidic buffer solution) II
colour of a buffer pH colour of a buffer solution pH
solution
Litmus strip (litmus paper) – –
pH color strips
(pH ranges: 1 – 7 and 7 – 14) – –
Universal pH indicator
pH meter – –
Calculation of the pH value
(obtained buffer solution) – –

3. GUIDELINES FOR WRITING THE FINAL LABORATORY REPORT


1. First page of the report – The Laboratory Report Cover Sheet found on our website:
https://www.am.szczecin.pl/en/facilities/institute-of-mathematics-physics-and-
chemistry/department-of-chemistry/chemistry-lab-manuals/
2. Second page of the report – „The Theoretical Part” – on a maximum of one page including
brief description of keywords (should be written by hand).

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3. Third page of the report – „The Experimental Part” – including all performed experiments
with titles, raw data, reactions, calculations, tables, graphs, etc. It should be written in
accordance with „Data analysis (after the experiment)” (should be written by hand).
4. Additional task/tasks given by the academic teacher.
5. References.

4. IN ORDER TO PASS THE LABORATORY EXERCISE STUDENTS MUST PASS „THE


ENTRY TEST” AND SUBMIT THE FINAL LABORATORY REPORT AT THE NEXT
LABORATORY MEETING. THE LAB REPORT MUST BE ACCEPTED BY THE
ACADEMIC TEACHER.

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