Manual Amali

Edited By
Khairiah Haji Badri

CHEMICAL
TECHNOLOGY
IN PRACTICE
Second Edition
Edited By
Khairiah Haji Badri
Polymer Research Center
Faculty of Science and Technology
Universiti Kebangsaan Malaysia
Second Edition 2018
Copyright Universiti Kebangsaan Malaysia, 2018
All rights reserved. No part of this publication may be reproduced or

transmitted in any form or by any means, electronic or mechanical
including photocopy, recording or any information storage and
retrieval system, without written permission from
Polymer Research Center (PORCE)
Published in Malaysia By
Polymer Research Center (PORCE)
43600 UKM Bangi, Selangor D.E., MALAYSIA
e‐mail: kaybadri@ukm.edu.my
Printed in Malaysia By
Penerbit UKM
Perpustakaan Negara Malaysia Cataloguing‐in‐Publication Data
Khairiah Haji Badri, 1970 –

Chemical technology in practice / Khairiah Badri.
ISBN 978‐967‐5048‐94-4
1. Chemistry, Technical. I. Title.
660
ii
PREFACE
Chemical Technology in Practice is a combination of theoretical and

applied chemistry with an addition of engineering elements. It meets
the requirement in introducing and training the students to
fundamental techniques and application to physical chemistry,
inorganic chemistry, organic chemistry, analytical chemistry,
polymer chemistry and chemical technology. Students are introduced
to qualitative and quantitative experiments and measurements using
various kinds of chemicals and apparatus.
This book is designed to be both a text for qualitative and
quantitative analyses as well as a stepping-stone to research. This
means that many of the students who will use the book will be
seniors or graduate students, and thus several more sophisticated
techniques are introduced.
Students are encouraged to refer to the references at the end
of each practical before running it. This is to ensure that students are
aware of the experiment to be carried out. Thus, students are required
to outline the experimental procedures in the format of a flow chart.
Of great concern to all chemists and technologists is safety in
the laboratory. In each practical, special attention in handling specific
chemicals are highlighted. The procedures are also briefly mentioned
in Appendix C. In numerous cases throughout the book, some points
have been made on the properties of both toxic compounds and
compounds that are hazardous for other reasons. These include
compounds that are irritating, carcinogenic and explosive.
The primary role of Prof. Ibrahim Abdullah was that of
providing well-tried and improved chemical tests. In addition, his
advice due to his many years of teaching and association with
research intensively was invaluable in determining the approach to
the production of this book.
A special thanks to the committee members and those who
assisted in the production and typing of the manuscript and in the
preparation of the illustrations include Assoc. Prof. Dr. Harun Haji
Hamzah, Dr. Azizan Ahmad, Dr. Rizafizah Othaman, Dr Siti Aminah
Mohd Noor, Dr Jason Wong Chee Sien, Dr Maisara Sahrom Raja
Shahrom, Dr Low Schu Ping, Mdm Nissa Nadia, Mdm Nor Hafiza
Yuhana Baderuliksan, Ms Rahmadini Safri and Ms Zahariah Muslim,
for their patience during the preparation of this manuscript. The
iii
revised version was made to fully updated the current practice and
has been conducted with the help of Ms Fatin Afiffah Ahmad Kuthi.
The development of this book as been facilitated by continual
and extensive review, and any future revisions will be successful only
if we continue to be made aware of the opinions of those people who
use this book.
Editor
Prof Dr Khairiah Haji Badri, AMIC, RTTP, CEL
Bangi
iv
AIMS OF THE COURSE
There are a number of reasons for introducing the student to

fundamental chemistry and chemical technology. Some of these go
much beyond the field of chemistry. The purposes for which this
course is taught are listed below. These warrant careful consideration
both prior to starting the laboratory work and as you proceed through
the carefully selected experiments.
Objective 1 Development of an appreciation of accuracy, precision

and limitations of careful scientific measurements.
Objective 2 Development of skill in performing scientific work

which demand careful attention to detail
Objective 3 Development of self-reliance and confidence in

scientific work.
Objective 4 Development of skills in planning and efficient use of

time.
Objective 5 Development of good methods of scientific record

keeping.
Objective 6 Development of an awareness that inaccuracies may

be present in scientific data, that considerable effort
must go into introduction of reliable data and that a
critical evaluation of the data is necessary before it is
accepted.
v
TABLE OF CONTENTS
Preface ii
Objectives iv
Table of Contents v
Practical 1
Addition Polymerization of Polyurethane with Various
Type of Amine Catalysts 1
Khairiah Haji Badri and Roshalina Salleh
Practical 2 5
Vulcanization of Natural Rubber
Ibrahim Abdullah and Chong Ee Lane
Practical 3 11
Polymerization Reaction in the Preparation of Nylon 6,6
Ibrahim Abdullah and Khairiah Haji Badri
Practical 4 15
Recycling of Polyethylene Terephtalate (PET) Bottles
Ishak Ahmad, Siti Farhana Hisham, Mohd Fairus Md Isa
and Mohd Sukor Su’ait
Practical 5 19
Rubber Elasticity
Khairiah Haji Badri
Practical 6 22
Head Loss Due to Friction in Smooth Bore Pipe
Practical 7 30
Head Loss Due to Pipe Fittings
vi
Practical 8 37
Standard Enthalpy of Combustion-Bomb Calorimeter
Khairiah Haji Badri and Fatin Afifah Ahmad Kuthi
Practical 9 44
Preparation and Characterization of Cis- and Trans-
Diaquadioxalatochromate (III) Potassium Complexes
Lee Yook Heng and Lee Kook Guan
Practical 10 51
Separation of Solid-Solid Sample
Practical 11 57
The Dependence of the Mechanical Properties of
Polyurethanes on the Acid Number, Hydroxyl Value and
Molecular Weight of the Polyols
Khairiah Haji Badri and Nor Rabbi’atul ‘Adawiyah
Norzali
Practical 12 61
Synthesis and Properties of Polypyrrole
Rusli Daik & Siti Syahirah Rusli
Practical 13 64
Rate Constant of a Reaction in a Continuous Stirred-
Tank Reactor
Practical 14 74
Purification and Concentration of Proteins Using
Dialysis Membrane
Lee Yook Heng, Lee Kook Guan and Sharina Abu
Hanifah
Practical 15 81
Emulsion Polymerization of Ethyl Acrylate
Khairiah Haji Badri
Practical 16
Tetraamine Copper (II) Sulphate
Ibrahim Abdullah and Lee Kook Guan
86
vii
Practical 17 94
FTIR Spectroscopy Analysis and Thermal
Characterizations of Polyurethanes with Varying
NCO/OH content
Khairiah Haji Badri
Practical 18 97
Extraction and Identification of Natural Ester from
Nutmeg, Myristica Fragrans
Practical 19
Iron (II) Oxalate and Potassium Triozalatoferrate (III) 104
Trihydrate
Practical 20 109
Preparation and Characterizations of Polymer Blends
Ishak Ahmad, Ibrahim Abdullah and Mohd Fairus Md
Isa
Appendices 114
Appendix A-1 Accuracy and Precision 115

Appendix A-2 Significant Figures 120
Appendix B Analytical Laboratory Techniques 124
Appendix C Laboratory Regulations and Procedures 140
Appendix D Testing Standards 143
Index 144
Chemical Technology in Practice
Polymerization Reaction in the Preparation of Nylon 6, 6
PRACTICAL 3
Polymerization Reaction in the Preparation of Nylon 6,6
Ibrahim Abdullah & Khairiah Haji Badri
Objectives
 To understand how the polymerization reaction happen.
 To understand that polymer consists of repeating units.
 To carry out a physical observation on the prepared polymer.
 To determine functional group that is present in the prepared
polymer through infrared spectroscopy analysis.
Introduction
Polymers are substances that have very high molecular weight
formed from combination of many small units known as repeating
units. These repeating units in the polymeric chain are connected to
each other by chemical bonds.
Monomers are simple chemical substance used as basic
reactants to form polymers. Bonds in polymer are formed between
these monomers’ molecules repeatedly until a big molecule is
formed.
The polymer structure can be depicted as in equation 3.1
(3.1)
where M is the monomer’s molecule (mer) or the repeating unit.
Polymerization reaction can be divided into two types, that is,

addition and condensation polymerizations. Addition polymerization
occurs by addition of monomer to the polymeric chains. The
condensation polymerization on the other hand, occurs when
11
monomers that have at least two functional groups are joined together
while smaller molecules are eliminated from the reaction.
Nylon is a polyamide formed from the reaction of linear
aliphatic monomers. It is produced in principle, by reacting a
diamine with a dicarboxylic acid. The two monomers form amide
linkages to produce the polymer chain. Experimentally, nylon is
prepared using acid chloride rather than carboxylic acid since the
reaction between an acid chloride and an amine is more rapid than
that between carboxylic acid and amine. However, commercial nylon
6,6 (the 6,6 indicates that each monomer contains six carbon atoms)
is produced from adipic acid and hexamethylenediamine. This
reaction is represented by the equation shown in Figure 3.1.
O O H H
Cl C (CH2)4 C Cl + nH N (CH2)6N H
adipoyl chloride hexamethylenediamine
O O H H
(C (CH2)4 C N (CH2)6N)n + nHCl
Figure 3.1 Reaction between adipoyl chloride and
hexametylenediamine to form nylon 6, 6.
Chemicals
 10 ml 5% adipoyl chloride
 10 ml 5% hexamethylenediamine
 Hexane (as solvent to adipoyl chloride)
Apparatus/Equipment
 Beakers
 Petri dish
 Paper clip/ hook
 Scissors
 Cardboard
 Oven
 Infrared spectrophotometer
12
Experimental Procedures
1. Pour 10 ml of a 5% of hexamethylenediamine solution into a
50-mL beaker.
2. Carefully pour 10 ml of a 5% adipoyl chloride solution to the
side of this beaker.
Note an immediate formation of polymer at the interface of

the two immiscible monomers.
wire hook
collapsed film
adipoyl chloride
nylon film
hexamethylenediamine solution
Figure 3.2 The nylon is hooked to the wire to pull it away from
the mixture.
3. Use a wire hook made from a paper clip to hold the polymer
film in the center and gently lift it to form a thread of about 30
cm long (Figure 3.2).
4. Cut the thread near the liquid surface. Record its physical
properties.
5. Rinse it several times with distilled water.
6. Dry it at ambient conditions for half an hour. Record its
physical properties.
7. Dry the nylon in the oven at 60oC for an hour. Record its
physical properties.
8. Prepare a thin film of the sample. Dry it in the oven and run
an IR analysis. Analyze the IR spectrum and record the
important peaks observed.
13
Analysis of Data
 Tabulate the physical properties of the polymer after reaction,
after half an hour and after oven-drying. Note on the color,
odor and texture (rigid/flexible).
 Analyze the IR spectrum. Identify the functional group at
absorption peaks. Tabulate your observations.
 Compare the IR spectrum of the standard nylon with the
prepared nylon. Discuss your findings.
 If the prepared polymer in this experiment is nylon 6,6 as
shown in Figure 3.1, name the nylon shown in Figure 3.3.
Figure 3.3 Nylon
 Use a reactant from dicarboxylic acid group that has six-

atomic carbon chain or less to synthesize a polymer as shown
in Figure 3.4 (nylon-4, 6). Write the chemical reaction.
Figure 3.4 Nylon-4, 6
References
Marc Loudon, G. 1988. Chemistry of Carboxylic Acid Derivatives: Organic
Chemistry, 2nd ed., California: The Benjamin/Cummings Publishing
Company, Inc.
Mat Bin Zakaria. 1988. Prinsip Kimia Polimer, Kuala Lumpur: Dewan Bahasa dan
Pustaka.
Seager, S.L. & Slabaugh, M.R. 1997. Safety-scale Laboratory Experiments For
Organic and Biochemistry, 3rd ed., New York: Brook/Cole Publishing
Company.
Silverstein, R.M., Bassler, G.C. & Morrill, T.C. 1991. Spectrometric Identification
of Organic Compounds, 5th ed., New York: John Wiley & Sons, Inc.
14
PRACTICAL 10

Objective
 To determine and analyze size distribution of fine crush solid
particle by means of sieve-shaking.
 To reduce particle size using ceramic ball, and observing its
effect on the size distribution of fine crush solid particle.
 To determine the effect of using different quantity of ceramic
ball in the ball-mill on the size distribution of fine crush solid
particle.
Introduction
Each test sieve consists of wire gauze with square apertures with
specific sizes. Size of these apertures indicates size of solid particle.
A vibrator, namely a mechanical shaker is required to shake the sieve.
This is important to get a precise data in a very short period.
The size of solid particle is then determined from the sieve
size. The size range will be taken from the sieve used and another
from the sieve that retain the particle. This method is use to measure
the size distribution of solid particle. The result can be presented in
various ways such as in the form of table or figure. The most useful
way of presenting the figure is by mean of semi-logarithm diagram.
Size of materials can be reduced by crushing the sample using
a ball-mill. High impact at the contact points between the ceramic
balls and the particles resulted in crushing of the particles into smaller
size. The effect of this phenomenon can be observed by analyzing the
size distribution of the particle using the method mentioned earlier.
Chemicals
 Oil palm empty fruit bunch fiber
 Rubber wood fiber
 Silica gel
51
Apparatus/Equipment
 Sieve-shaker
 Sieve of various sizes
 Ceramic balls of various sizes
 Ball-mill
Figure 10.1 A set-up of a sieve-shaker

1. Arrange the sieves with the largest aperture on the top and
the smallest at the bottom.
2. The receiver is placed at the bottom of the smallest sieve
before the arrangement is mounted onto the sieve-shaker
(Figure 10.1).
3. Weigh an amount of solid particle (50 g for each silica gel
and oil palm empty fruit bunch fiber or the rubber wood).
Place this sample on the top sieve. Put on the lid and lock
the arrangement to the shaker with the clamping nuts.
4. Switch on the shaker and the controller speed. Select
moderate speed and run the sample for five minutes.
5. Once finish, switch off the speed controller and the shaker.
Unlock the clamping nuts.
6. Carefully, remove the sieves and the receiver from the
shaker.
52
7. Collect the contents of each sieve in separate containers.

8. Weigh them separately and record the readings. Total mass
of the separated sample should be equal to the mass of the
initial sample before sieving.
9. Repeats the experiment using sample that has been crushed
using the ball-mill (Figure 10.2).
Speed Controller
Figure 10.2 Ball-mill

10. This is carried out as follows:
i. Add 10 pieces of the ceramic balls to an amount of the
sample and place them in the ball-mill. Close the lid.
ii. Run the ball-mill with moderate speed initially and
gradually increase it to maximum speed.
iii. Adjust the speed so that the ceramic balls are free-
falling and allows this for 30 minutes.
iv. Once finish, remove the sample from the ball-mill and
analyze the size distribution using the above screening
procedures using sieve-shaker.
v. Compare the result by ball-milling the sample with 30
pieces of ceramic ball. Repeat the ball-milling
procedures.
Analysis of Data
 Record the result in Table 10.1,Table 10.2 and Table 10.3.
 Analyze the size distribution of sample as shown in Figure
10.3.
53
 Compare the result before and after ball-milling with 10 and

30 ceramic ball. Discuss.
 State the sieve arrangement that was in the separation of
solid-solid sample in this experiment (from the largest to the
smallest aperture).
 What is the function of the shaker in the separation of solid-
solid sample?
 What is the function of ceramic balls in this separation
process?
 List two separation methods of solid-solid sample that can be
used other than this separation method.
Table 10.1 Accumulated data of the sample’s size without ball-

milling.
Initial mass of sample : kg

Accumulated final mass of sample : kg
Sieve Mass of Trapped Accumulative Accumulative

aperture size sample in the sample oversize of undersize of
(microns) sieve (kg) (%) sample (%) sample (%)
54
Table 10.2 Accumulated data of the sample’s size after ball-milling

the sample with 10 pieces of the ceramic balls.

Accumulated final mass of sample: kg

Table 10.3 Accumulated data of the sample’s size after ball-milling

the sample with 30 pieces of the ceramic balls.

Accumulated final mass of sample: kg
55
Figure 10.3 Size distribution of sample
References
Karger, B.L., Snyder, L.R. and Horvath, C. 1973. An Introduction to Separation
Science, New York: John Wiley & Sons.
Mc Cabe, W.L. and Smith, J.C. 1995. Operasi Unit Kejuruteraan Kimia. Trans.
Chin, F.W., Teh, J.W and Teng, T.T. Kuala Lumpur: Dewan Bahasa dan
Pustaka.
56
Extraction and Identification of Natural Ester from Nutmeg, Myristica Fragrans
PRACTICAL 18
Extraction and Identification of Natural Ester from Nutmeg,
Myristica Fragrans
Khairiah Haji Badri and Fatin Afifah Ahmad Kuthi
Objectives
 To separate lipid from natural products.
 To carry out hydrolysis of base triglyceride ester
 To understand thin layer chromatography technique in the
identification of compounds.
Introduction
Trimyristin is a triglyceride, which is a lipid ester formed from
glycerol and myristin acid. This glyceride presents in a large amount
in nutmeg, Myristica fragrans and easily separated from other esters.
Therefore, separating trimyristin can be a good example for
extraction of any other natural products. A pure component can be
obtained by extraction followed by recrystallization. The ground
nutmeg or commercial nutmeg powder is extracted by refluxing with
chloroform and the filtrate is recrystallized using acetone.
After hydrolysis, ester acid in trimyristin produces glycerol
and a kind of acid, that is myristic acid (Figure 18.1).
trimyristin glycerol myristic acid
This experiment illustrating the separation of lipid from the

natural product. Saponification or base hydrolysis of trimyristin is
catalysed by sodium hydroxide.
97
Chemicals
 Nutmeg powder
 Chloroform
 Acetone
 6 M sodium hydroxide solution
 Ethanol
 Concentrated hydrochloric acid.
Apparatus/Equipment
 Round bottom flask (100 ml, 250 ml)
 Reflux condenser
 Water bath
 Funnel
 Conical flask (125 ml, 250 ml)
 Beaker (250 ml)
 Buchner funnel
Part I Trimyristin separation
1. Place 4 g of nutmeg powder in a 25 ml round bottom flask
equipped with a reflux condenser.
2. Subsequently, add 20 ml chloroform and slowly reflux the
mixture by heating it in the heat dissipation block on a hot
plate for 20 minutes. Cool the mixture.
3. Filter the solution by gravitational filtration.
Use coarse filter paper.
4. Transfer the solution into a 50 ml round bottom flask.
5. Evaporate the chloroform by connect receiver distilling still
in between condenser and solution.
6. Dissolve the filtrate with 30 ml acetone and continue reflux
for another 5 minutes. Transfer the solution into beaker.
7. Let the mixture cool at room temperature for a while and cool
it in ice bath until it forms crystal.
Crystallization is a slow and sensitive process.
98
8. Collect the crystal by suction glass funnel. Wash the crystal

with cold acetone.
9. Weigh the dried sample. Determine its melting point by
inserting a small amount of sample into a capillary tube and
observe it through the melting point determination bullet.
10. Keep the sample in a small bottle and label it.
Part II Saponification of trimyristin

Trimyristin identification with base hydrolysis
1. Place 0.1 g trimyristin extracted in Part I in a 100 ml round
flask.
2. Add 10 ml sodium hydroxide 6 M solution, followed by 10
ml ethanol.
3. Slowly, reflux the mixture for 20 minutes and cool the
mixture. Transfer it into small beaker.
4. Add 10 ml concentrated hydrochloric acid followed by 30 ml
distilled water until it forms white solid.
5. Filter the myristic acid formed using Buchner/ suction glass
funnel. Wash with 10 ml distilled water and dry.
6. Weigh it and determine the melting point.
7. Determine the melting point of trimyristin and myristic acid
mixture in a 1:1 ratio.
Thin layer chromatography (TLC) analysis

The laboratory assistant will hand over a 5 cm × 5 cm × 0.2
cm glass plate coated with 0.25 mm thickness of silica powder#.
# Prepare the slurry by stirring 30 g silica gel in 60 ml distilled
water until a homogenous mixture is obtained. Spread the
slurry on a 5cm × 20 cm plate using a prepared spreader. Dry
the thin film of silica powder at room temperature for 30
minutes and further drying in the oven at 110-120 °C for
another 15 minutes.
Once the sample has been placed carefully on the plate, the
plate is placed in a chromatography chamber containing
99
mixture of 90 % toluene and 10 % ethanol (9:1) at a level of 1

cm high from the base of the chamber.
Procedure:
1. Dilute a few mg of trimyristin and myristic acid separately in

acetone to obtain a solution with ~5% concentration. Place it
in a small bottle.
2. Drag the prepared solution with capillary tube, holding it

upright above the TLC plate.
3. Place a drop of the solution at a point about 2 cm from the

bottom of the TLC plate and 1.5 cm from the side of the plate.
This step requires proper handling. Be careful not to scratch

or damage the TLC plate.
4. Repeat the same procedure for the other solution, using a new
capillary tube and at a new point about 2 cm apart from the
first spot (Figure 18.1).
Figure 18.1 Sample spots on TLC plate.
5. Air-dry the TLC plate to evaporate the solvent.
6. Slowly place the TLC plate in the chromatography chamber

containing toluene-ethanol (9:1) eluent with slanting position
(Figure 18.2). Put the lid on.
100
Figure 18.2 The TLC plate is slanted in the solvent mixture.
7. Observe the solvent moves upward in a quick manner. Leave

the plate in the chromatography chamber until the solvent
level reach about 3 cm from the edge of the upper part of the
TLC plate. Remove the plate from the chamber and quickly
mark the solvent level before it evaporates.
20mm
Figure 18.3 The TLC plate is removed and the level of the solvent is
marked.
8. Air-dry the plate at room condition. Detect the spot using

iodine vapor chamber inside the fume hood. Mark the spot
with pencil before the brown spots disappear.
101
Analysis of Data
 Based on trimyristin structure, discuss on the selectivity in
choosing suitable solvents for recrystallization. Acetone is
used instead of water or ether petroleum. Explain.
 Explain why sodium salt myristate is considered as soap.
 Explain how the thin-layer chromatography is used to

differentiate trimyristin and myristic acid.
 Draw the finished TLC plate in your report (Figure 18.4) and
calculate the value of Rf using equation 18.1.
moving distance of the compound

Rf  moving distance of the solvent
(18.1)
45 mm
Compound
Compound
40.3 mm
21.5 mm
Figure 18.4 Finished TLC plate.

21.5
Rf A   0.33
65
40.3
Rf B   0.62
65
 Determine whether the difference in the Rf values can be used

to elucidate structure of the extracted products and nature of
the solvent used. Explain.
102
References
Campbell, B. N. and Ali, M.M. 1994. Organic Experiments: Microscale and Semi-
Microscale, Belmont California: Brookes/Cole Publishing Company.
Roberts, F. T., Snell, J. and Yates, C. 1971. Trimyristin from Nutmeg. Journal of
Chemical Education, 48, 155-156.
Landgrebe, J.A. 1982. Theory and Practice in the Organic Laboratory, 3rd Edition,
Washington D.C.: Heath and Co.
103
Amali Kimia III
Ujikaji 10
Penentuan permintaan Oksigen Kimia Dalam suatu Sampel Air Buangan

(COD)
Objektif
• Memahami salah satu parameter penting dalam menentukan kualiti air iaitu nilai
PermintaanOksigen Kimia (Chemical Oxygen Demand).
• Memahirkan UJIKAJI pengiraan dan permasalahan teknik tersebut.
Pengenalan
Satu daripada parameter yang sering digunakan untuk menyatakan mutu air ialah Perrnintaan
Oksigen Kimia (POK). POK merupakan satu kaedah penentuan jirim organik di dalam sampel.
Analisis POK dapat dilakukan melalui beberapa kaedah. Satu kaedah yang baik dan selalu
digunakan ialah kaedah yang berdasarkan kepada pengoksidaan oleh dikromat. Di sini bahan-
bahan organik di dalam air dioksidakan oleh dikromat dalam keadaan asid ke karbon dioksida dan
air (persamaan 1 ). Argentum sulfat digunakan sebagai mangkin. Dikromat yang digunakan pada
mulanya berada dalam keadaan berlebihan. Kelebihan dikromat ini kemudiannya ditentukan
kembali dengan pentitratan menggunakan Fe(II).
Ion klorida mengganggu dalam penentuan ini. Gangguan ini dapat dihapuskan dengan
menambahkan raksa sulfat terlebih dahulu sebelum direfluks untuk mengubahkan semua klorida
kepada kompleks raksa klorida,
Hg2+ + 2Cl- HgCl2 (3)
Argentum (I), di samping berfungsi sebagai mangkin ia juga memudahkan pengoksidaan sebatian
organik berantai lurus.
Kesempurnaan pengoksidaan bergantung kepada lamanya masa refluks. Masa refluks selama dua
jam dianggap sudah mencukupi dan biasa digunakan.
40
Amali Kimia III
Bahan Kimia
Argentum (I) sulfat, Ag2SO4
Besi (II) ammonium sulfat, (NH4)2SO4FeSO4.6H2O
Asid sulfurik, 98%
Raksa (ll) sulfat, HgSO4
1, 10-fenantrolin
Alat Radas
Alat radas untuk titratan seperti buret, pipet dan kelalang kun.
Alat radas untuk *refluks terdiri daripada kelalang, kondenser dan pemanas .
Beberapa kelalang isipadu, corong kaca dan bikar.
*Cari gambar set refluks.
Kaedah UJIKAJI
I. Penyediaan larutan-larutan stok
a. Larutan argentum sulfat.
Larutkan 6.60g Ag2SO4 ke dalam sedikit asid sulfurik 98%. Kemudian cairkan ke 1000mL
dengan asid tersebut.
b. Larutan besi (II) amonium sulfat 23.25g (NH4)2SO4FeSO4.6H2O dicampurkan dengan
5.0mL asid sulfurik 98% dan kemudian dicairkan kepada 250mL dengan air suling.
c. Larutan kalium dikromat, 0.25 N
Larutkan 3.065g kalium dikromat ke dalam air suling dan cairkan ke 250mL isipadu
dengan air suling.
d. Larutan penunjuk feroin - l.485g 1,10-fenantrolin dicampurkan dengan 0.69g besi (II)
sulfat, dilarutkan di dalam air suling dan kemudian dicairkan ke 1000mL isipadu dengan
air suling.
II. Pemiawaian larutan besi (II) ammonium sulfat
Pipet 25.0mL larutan kalium dikromat (0.25 N) dimasukkan ke dalam kelalang kun 500mL,
dicairkan ke 250mL dengan air suling, ditambah 75.0mL asid sulfurik dan kemudian dibiarkan
sejuk. Beberapa titis penunjuk feroin ditambah dan larutan dititrat dengan besi (Il) amonium sulfat
sehingga larutan berubah menjadi merah unggu. Kira kepekatan larutan besi (ll) tersebut.
41
Amali Kimia III
III. Penentuan POK suatu sampel air

a. Anda akan diberikan satu sampel air buangan yang didapati di sekitar karnpus UKM.
b. Pipet 50mL sampel air tersebut dan masukkan ke dalam kelalang bulat 500mL. Kepada
sampel air ini, ditambah 1.0g HgS04 dan 5mL asid sulfurik yang mengandungi argentum
sulfat.
c. Larutan digoncang agar pemelarutan sempuma dan jika perlu, larutan dipanaskan. Pipet
sebanyak 25mL kalium dikromat 0.25N ditambah dan diikuti dengan penambahan 70mL
asid sulfurik yang mengandungi argentum sulfat.
d. Larutan berserta sedikit batu didih direfluks selama 2 jam, disejukkan dan kemudian
dicairkan kepada 350mL isipadu dengan air suling. Beberapa titik feroin ditambah dan
larutan dititrat dengan larutan piawai besi (II) amonium sulfat.
e. Kira nilai POK bagi sampel air yang dianalisis menggunakan kaedah pengiraan di bawah.
42
Amali Kimia III
Soalan
1. Mengapa ion klorida mengganggu penentuan POK ini,
2. Pada pendapat, anda apa akan jadi pada nilai POK jika masa refluks yang lebih lama
digunakan.
3. Apa yang anda tahu mengenai Permintaan Oksigen Biokimia?
4. Tunjukkan bagaimana hubungan seperti dalam persamaan (4) dan (5) diperolehi.
43
Practical Chemistry IV
Experiment 1
Phase Diagram of A Two-Component System
Objectives
At the end of this experiment, student should be able to

 explore the utilization of phase rule in explaining equilibrium stage between two
components at specified temperature.
 know that the degree of freedom at eutectic point is zero where the solution
completely solidified.
Introduction
When a pure compound in liquid form is cooled, the temperature falls until it reaches the
freezing point. However, if there is a crystal nucleus in the solution, the temperature of
the liquid will not change (Figure 5.1). As soon as the entire system has solidified, the
temperature once again falls due to insufficient heat.
Liquid only, F = 1
Cool freezing liquid,

F=0
Temperature (T), oC
Solid only, F = 1
Time (t)
Figure 5.1 Cooling curve for pure liquid
The relationship between the number of component (C) and the number of phase (P) can
be described using the phase rule in equation 5.1
F = C–P+2 (5.1)
1
In this equation, F is the degree of freedom, which is a variable, either temperature or

pressure. If an open system used, one of the variables namely the pressure is fixed. Under
this condition, the number of variable is set as 1. Therefore, the phase rule can be expressed
as in equation 5.2:
F = C–P+1 (5.2)
This form of equation is described in Figure 5.1 and Figure 5.2.
When there is only one component (C = 1), the phase rule becomes F = 1 – P + 1 or 2 –
P. Thus, P = 1 and F = 1 for the case of liquid or solid phases. These values indicate that
there is only one degree of freedom; thus only one variable can be varied without forming
second new point. In fact, degree of freedom in general, depends on either one of the
variables, temperature or pressure. Normally, pressure is always fixed at a value. Therefore,
only temperature should vary. At freezing point, where there is an existence of two phases,
liquid and solid phases, F becomes 0. The temperature remains constant as long as the two
phases coexist (Figure 5.1). This point is called invariance point. If the temperature is
varied at this point, one of the phases either liquid or solid will disappear. Once the liquid
phase turns to solid phase, once again F becomes 1. At this stage, temperature can be
changed without forming any new phase (only solid phase exists).
When there are two components (C = 2) in a mixture, the system is no longer invariance.
The degrees of freedom F = 2 – P + 1 shows that one of the variables, either temperature
or composition is still varied. Thus, the solution can be cooled up to its freezing point.
However, if the solution is cooled below its freezing point (until both solid and liquid phase
coexist) both variables are no longer independent. Once the temperature is reduced and the
solution concentration is increased, solid will continuously crystallise and new equilibrium
point is achieved. On the order hand, if the temperature is increased and the solution
concentration is decreased, the solid melts and new equilibrium point at new temperature
is reached.
When a solution is cooled, the temperature falls at a rate depending on the heat capacity
and temperature difference in the freezing point of the existing components. Since heat is
released during crystallisation, the rate of cooling becomes low. Thus, there will be a
change in the slope or a turning point at crystallisation point (Tb) as shown in Figure 5.2.
If the cooling process continues, the concentration of solution will increase until it becomes
saturated with both components (Figure 5.2 and point ‘E’ in Figure 5.3 b, c, d and e). At
this point, there are three phases, which are liquid (solution), pure A and pure B as solid.
2
Temperature (T) oC B
C
Tb
D
Time (t)
where A liquid only, F = 2

B crystallisation of one component, F = 1
C crystallisation of both components (eutectic), F = 0
D eutectic mixture of both solid phases
Figure 5.2 Cooling curve of a two-component solution
At this point, once again F = 0 and the system becomes invariance where the temperature
becomes constant at Te until the solution is completely solidified. This temperature is
called eutectic temperature; while the saturated solution consists of both components and
other solid crystallises from it is called eutectic mixture. The solid crystallised from this
eutectic mixture (known as eutectic solid) is a mixture of two types of crystals although the
temperature is constant and the cooling curve has the same characteristics as a pure
substance (Figure 5.1 and 5.2).
The graph of temperature against composition of mixture is used to describe clearly the
phase difference as shown in Figure 5.3. Although temperature variable is used in this phase
diagram, other variables such as pressure, electrical properties and others can also be used.
Whenever required, other variables can also be used to replace the percentage of
composition.
As shown in Figure 5.3, phase diagram can be drawn using the turning point, melting point
and eutectic point from the cooling curve (or heating curve). Curves TB (A) - e and TB (B)
- e show the freezing point of each solution from 100% composition of pure A until
100% of pure B. Each composition at the curve shows the solution composition at
equilibrium with pure A (on the left), pure B (on the right) or with both pure A and B (at
point C).
If the is no crystal nucleus in the solution, the crystallisation will not occur. In this case, the
solution usually will undergo super cooling until the nucleus is formed at 1-20C below
3
the freezing point. However, once the crystallisation started, the heat released during the
crystallisation resulted in an increase in temperature until it reaches the freezing point
(Figure 5.4).
TB (B)
P
TB (A)
Temperature (T) 0C
A (c) B
0 20 40 60 80 100
(a) (b) % mol B (d) (e)
Figure 5.3 Developing a phase diagram using the cooling curve from (a) pure A, (b)
20% of B, (c) eutectic point, (d) 80% of B and (e) pure B
Temperature (T)
o
C T
Time (t) time (t)
(a) (b)
Figure 5.4 Overcooling for (a) pure liquid and (b) solution
4
Materials and Methods
Chemicals:
Naphthalene, p- dichlorobenzene
Apparatus:
6 test tubes with lid, beakers, thermometer
Experimental Outcomes:
 To use the cooling method in constructing phase diagrams for pure component and
a two-component mixture.
 To determine the eutectic point of a two-component mixture.
Experimental procedures:
1. Two groups are working together for this experiment. Based on Table 5.1, each
group need to weigh about 5-6 g of the following samples.
Table 5.1 Samples of pure or two component mixture
Samples (by weight total percentage, wt%)

Group 1 Group 2
Pure naphthalene Pure p-dichlorobenzene
Naphthalene and p-dichlorobenzene Naphthalene and p-dichlorobenzene
(20 wt% of naphthalene) (60 wt% of naphthalene)
Naphthalene and p-dichlorobenzene Naphthalene and p-dichlorobenzene
(40 wt% of naphthalene) (80 wt% of naphthalene)
2. Melt each sample in a test tube by immersing the test tube in a beaker filled with
hot water.
3. Fix the thermometer (0-1100C) on the lid and immerse it in the test tube until the
thermometer bulb is about ¼” – ½” from the bottom of the test tube.
4. Remove the test tube from the beaker and let the retort stand hold the test tube
while it is cooled slowly to room temperature.
5. Record the temperature to the nearest 0.10C in a second interval. Stop the
measurement when the temperature of the sample reaches 100C below the eutectic
point (if the eutectic point is shown on a curve). This experiment is carried out in
pair, where a student reads and records the temperature while another student plots
the readings on a graph paper. If a horizontally eutectic point is obtained, stop the
temperature reading at least 150C below the freezing point for samples containing
20% or 40% naphthalene, 250C for 60% naphthalene, and 350C for 80%
naphthalene. Note that there is no eutectic point for pure substance.
6. If a good horizontal eutectic point is not obtained, melt the sample again until the
temperature reached 500C and let the sample to cool down at room temperature. In
order to achieve this, a bigger test tube is needed for larger space. Cooling at lower
rate can also be carried out by immersing the test tube containing sample in warm
5
water. On the other hand, if the sample is cooled at a very slow rate, a beaker filled
with cool water can be used.
7. Once a good cooling curve is obtained, melts the same sample again to get the
second curve.
8. Once it reaches the room temperature, remove the thermometer and clean it using a
small amount of chloroform. Repeat the whole procedure using other samples.
Analysis of Data
1. Draw a cooling curve by plotting temperature (y-axis) against time (x-axis) on a

graph paper. Mark the position of each turning point with arrow as indicator. For each
indicator, write the cooling temperature.
2. Record the freezing temperatures, turning points and eutectic points for each
concentration of the solutions in a table. By using this data, draw a phase diagram for
0%, 20%, 40%, 60%, 80% and 100% composition of naphthalene at specified
temperature. Label the phases and plotted lines.
Question
1. Determine the composition and number of solid phase and liquid phase exist at
700C, 600C, 500C, 400C and 300C by assuming that a mixture of 20%
dichlorobenzene is cooled slowly until it reach the equilibrium at all time, (let the
amount of the mixture to be 100g).
6
Experiment 2
Solid Phase of A Three-Component System
Objectives
At the end of this experiment, student should be able to

 understand that a three-component system can be represented by a triangular phase
diagram if temperature and pressure are constant.
 know the method of plotting, labeling and using a three-component phase diagram.
Introduction
To depict the phase behavior of three-component systems on a two-dimensional diagram,

it is necessary to consider both the pressure and temperature as fixed. The phase of the
system as a function of the composition can then be shown. The relative amounts of the
three components, usually presented as percentages by weight, can be shown on a
triangular plot as shown in Figure 6.1.
The corners of the triangle labeled A, B and C are corresponded to the pure components A,
B and C, respectively. The side of the triangle opposite the corner labeled A for example
implies the absence of A. Thus, the horizontal lines across the triangle show increasing
percentage of A from zero at the base to 100 percent at the apex. In a similar way, the
percentage of B and C are given by distances from the other two sides to the remaining
two apices.
A
0 %C 1 0 0 %A
2 0 %C 8 0 %A
4 0 %C 6 0 %A
6 0 %C 4 0 %A
8 0 %C 2 0 %A
1 0 0 %C 0 %A
0 %B 2 0 %B 4 0 %B 6 0 %B 8 0 %B 1 0 0 %B
C B
Figure 6.1 Diagram for plotting the composition of a three-component system
7
Three-component systems involving solids and liquids can be introduced by considering

systems of two salts and water. The simplest behavior is that shown in figure 6.2 where
the two salts are somewhat soluble and the diagrams give the curves for the saturated-
solution compositions.
W ater
Uns aturated s olution
Saturated s olution
+
E Solid C
D
Saturated s olution Saturated s olution
+ + Solid
Solid B B
F
+
Solid C
s alt B s alt C
Figure 6.2 Phase diagram for two salts and water at fixed temperature and pressure
A tie line is drawn to show saturated solutions along DF and EF lines are in equilibrium
with the solid salts B and C, respectively. Point F corresponds to a system in which the
solution is in equilibrium with both salts. Removal of water from point F moves the total
composition toward the base of the triangle. More solid salts will be formed which
remain in equilibrium with the decreasing amount of water but at constant concentration
of saturated solution.
If both B and C salts can produce a new compound, BC; then the solubility of BC in
water will also appear in the phase diagram as shown in Figure 6.3.
Materials and Methods
Chemicals:
Sodium nitrate, NaNO2, Sodium chloride, NaCl
Apparatus:
Test tube, beaker, watch glass, hot plate
Experimental Outcome:
To construct a phase diagram for a three-component mixture consists of NaCl, NaNO2
and water.
8
Experimental procedures:
1. Prepare the following solutions in a separate closed test tube (the mass of the
chemicals need not have to be exact but close 1% deviation):
i. 1 g of NaNO2 + 8 mL of distilled water

ii. 1 g of NaCl + 9mL of distilled water
iii. 2.5 g of NaCl + 3.5 g of NaNO2 + 4 mL of distilled water
iv. 3 g of NaCl + 5 mL of distilled water
v. 5 g of NaNO2 + 5 mL of distilled water
vi. 2 g of NaNO2 + 7 mL of distilled water
2. Add NaCl salt into solution (i) and (vi) until a saturated solution is formed and a layer
of insoluble crystal settled at the bottom of the test tube. Add NaNO2 to (iv) until it
formed a saturated solution and an insoluble layer of crystal appeared at the bottom.
3. Attach the lid and shake the test tube one by one for a minute alternately for at least 15
minutes. Filter the solution with an ordinary filter paper into a respective weighed conical
flask (50 mL or 100 mL).
4. Place a glass stopper on the top of the conical flask. Heat it slowly on a hot plate to
evaporate the water. Avoid sample from splashing out of the conical flask. If the solution
splashed onto the glass stopper, wash it with sufficient amount of distilled water and pour
it back into the conical flask towards the end of the evaporation process.
5. Do the final drying in an oven. Final drying must be done carefully to avoid any loss
of compound.
6. Allow the dried crystal to cool at room temperature and weigh the yield. Repeat the
drying process until the yield reaches a constant mass.
Analysis of Data:
1. Calculate the composition of the saturated solutions (weight %) in this experiment.

This can be done by calculating the weight loss of water for sample (ii), the percentage of
NaCl and NaNO2 while others are determined from the weight differences.
2. Only the percentage of water could be determine in (ii) due to the formation of
saturated solid. Further analysis need to be done to determine percentage of NaCl and
NaNO2. Isothermal invariant point could be determined by using water percentage and
measured from a plotted curve.
3. Plot the value of the obtained percentage on a triangular plot sketched on a graph
paper with water at the top, NaCl at the left plane and NaNO2 at the right plane. Draw the
curve starting from the pure compound to mixture of salts and water. Determine the
invariance point.
Questions:
1. Pure NaCl and NaNO2 salts are presence in solid phase at room temperature. How can
these be verified experimentally?
2. What do you know about wet residue process? Research and explain this process.
9
Accuracy and Precision
APPENDIX A-1
ACCURACY AND PRECISION
The desired result of a quantitative chemical analysis is a close
approximation of the true value of the quantity or concentration of a
component in the sample. The closeness of the experiment result to
the true value is the accuracy of the determination. The deviation of
the experimental value from the true value is the error. Although it
would be nice to be able to perform analyses which give exactly
correct results (zero error), it is neither necessary nor possible to do
so in most cases. It is generally true that the more accurate a method
of analysis, the more costly and time consuming it is to perform. One
job of the analytical chemist is therefore selection of a method which
will provide the required accuracy while being economical of time
and money.
Most analyses are performed on samples which are truly
unknowns. How, then, does the analyst know that his results are
within the required accuracy? The answer is that he does not.
However, there are certain practical methods of assuring the required
accuracy within a high degree of probability. One of these methods is
to perform the analysis on several subsamples and obtain an average
value. The extent to which these analyses agree with one another is
the reproducibility or precision of the analysis. Good precision of
results is not necessarily a guarantee of accuracy in the analysis, but
good accuracy is very unlikely without good precision.
A second method of assuring good accuracy in analysis of
unknowns is to perform the analysis in the same way on samples of
known composition. If reliable results are obtained for the standards,
there is good reason to expect that the results are also reliable for the
unknowns. But since there are differences in chemical composition of
standards and unknowns, good results on one do not guarantee good
results on the other.
A third method of checking the accuracy of analyses is to
determine the desired component by another independent method. If
two or more independent methods give the same result, chances are
good that the result is accurate.
Another point that should be noted is that “the analysis can be
no better than the sample”. It is usually both impractical and
115
undesirable to use all the available material (e.g. a trainload of ore) to

determine the composition. A sample must be taken for analysis. If
the analysis is to be meaningful, the sample must have the same
average composition as the bulk material. Various methods have been
devised for splitting and blending materials so that a representative
sample can be obtained. In certain situations a stratified sampling
procedure must be used. In any event, a reliable sample of the bulk
material must be used. In any event, a reliable sample of the bulk
material must be used for analysis in order for meaningful results to
be obtained.
As a general rule, the person for whom analyses are
performed would like to have not only the analyst’s best estimate of
the true concentration (composition, quantity, etc.) of the sample but
also his best estimate of the reliability, or precision, of the data. In
most cases the assumption is made that the method is completely
reliable, although it may be imprecise. That is to say that if a very
large number of analysis were performed on the sample, the average
value would be the true value, but the individual measurements may
differ significantly from the mean. If we accept this premise, the data
for replicate analysis of a sample can be treated in a statistical manner
to give a measure of the reliability of the mean and of individual
values.
The statistical quantity generally used to express the precision
of data is called the standard deviation. It is given by the equation:

( x  x ) 2
S (A1.1)
n 1
where S = experimental standard deviation


x = mean value of the measurements
x = value of an individual measurement
n = the number of measurements
Calculation of standard deviation requires two or more
measurements, but is rarely used unless three or more values are
obtained. (For only two data points the standard deviation is always
70.7% of the range; i.e. 0.707 x (max. value – min. value)). In all
experiments in this course you are asked to report the standard
deviation along with the average value of your analyses.
116
In order for equation (A1.1) to be applicable, certain

requirements must be satisfied; specifically, the probability of small
errors is greater than the large errors, and the probability of negative
error is equal to the probability of a positive error of the same
magnitude. More generally, the data must fit a so-called normal
distribution, shown schematically below.

In the diagram x is the mean value and σ is the standard deviation (σ
is used for an infinite number of measurements or values, s for a
finite series). It can be shown mathematical that for a large number of
measurements of x, 68.3% will fall within the range ± σ of the mean,
90.0% within the range ± 1 of the mean, and 95.0% within the range

± 1.960 σ of the mean x . The percentages are called the confidence
level of the data. We might say, for instance that are 95% confident
that an arbitrarily selected single measure will fall within ± 1.96 σ of

the true mean, x .
For a finite series of measurements, the experimental standard
deviation, s, as defined above is used in place of confidence limits
now depend upon the number of measurements. For a set of three
measurements the true mean is 90% probable to be within ± 1.69 and
95% probable to be within ± 2.48 s of the experimental mean. An
explanation of these factors may be found in the statistics text or in a
117
more advance textbook on quantitative analysis (e.g. Fundamentals of

Analytical Chemistry by D.A. Skoog and D.M. West). The 90% and
95% ranges are called the confidence limits and the percent is called
the confidence level. Other confidence levels may be used (e.g. 50%,
99%, etc.) as desired, but the 90% and 95% confidence levels are
most common used in analytical chemistry.
The results of analyses may be reported to any desired
confidence limits providing the data fits a normal distribution and
sufficient data points are taken to determine s. What confidence limits
are used is largely a matter of personal preference or company policy,
but the confidence level must always be stated. It would be of little
value to state that the % Fe in an ore is 38.65 ± 0.12 %. This gives an
uncertainty range, or interval, but does not attach any meaning to that
range.
In experiments performed in this course, a report of the
standard deviation of the analysis is required as part of the report.
This is done here even if only two values are reported. As noted
above, 90% confidence limits are1.69 s for three measurements. The
factor, 4.46 is used if only two values are reported. The uncertainty
limits are thus more than twice as large with two values as with three.
Finally, it should be kept in mind that the value of s is a
measure of precision, not of accuracy. Only if the analytical method
will produce a true value with a large number of measurements is the
uncertainty, as expressed by the standard deviation, a measure of the
actual uncertainty in the result.
Rejection of Outlying Values
It is often found, especially in performing analyses with
which you have no prior experience, that one value is quite a bit
different from the others. This is more likely due to the occurrence of
a non-random error. If you are fairly certain that the outlying value is
“bad” data, it should be rejected. There are two bases on which
values may be discarded and not used in the average.
1. You observed some irregularity with a particular sample (e.g. it
boiled over, or the color change at the end-point of a titration
wasn’t just right). In this case you may choose to discard the
results if it doesn’t agree with the other samples. Your
118
observations of the irregularity recorded in the lab notebook are

sufficient to justify rejection of that sample.
2. The value doesn’t agree with the others, but you have no idea
why. In this case a statistical test is applied to determine whether
the value may be rejected or not. The test we will use is called the
“Q Test” and is based on statistics. The test is as follows:
Calculate the value of Q for your data from the equation:
Q=
where range = maximum value – minimum value and denotes

absolute value. If Q > 0.76 for four analyses used in calculation of
the result, or Q > 0.94 for three analyses, the outlying value may
be rejected. If Q is less than the appropriate one of three numbers,
the outlying value must be included in calculations of the average
and standard deviation.
The Q Test, as used here, allows rejection of an outlying value
only if it is at least 90% certain that it contains non random error.
119
Significant Figures
APPENDIX A-2
SIGNIFICANT FIGURES
It is important when reporting results of measurements to report them
in such a way to give an indication of the reliability of the
measurements. If a volume of 12 mL was measured to the nearest one
milliliter in a graduated cylinder, it would be improper to record this
volume as 12.00 or even 12.0 mL. Likewise, if a volume of 500 mL
is measured in a 500 mL volumetric flask, that volume should not be
reported as 500 mL. The correct expression would be 500.0 mL or
5.000 x 102 mL. It is customary to report measured quantities in such
a manner that the last significant digit is the only one which is
uncertain.
There are certain rules which must be followed in writing
numbers so that there is no ambiguity as to how many significant
digits (significant figures or sig. fig.) they contain. These are listed
below. It is required that this course that all the experimental results
be reported to the correct number of significant digits. Improper use
of sig. figs. may results in a lower grade on your experiment.
Rules for Counting Significant Digits
1. Both measured and calculated numbers are reported so that only
the last digit is uncertain.
2. For a number which contains no decimal point, the number of
significant digits is the number of digits starting with the first
non-zero digit on the left and ending with the last non-zero digit
on the right. The following numbers all contain 3 significant
digits:
0255, 2050, 255000, 255 × 104, 205 × 10-2
3. For numbers which contain a decimal point, all digits, whether
zero or not, are significant starting with the first non-zero digit on
the left. Some examples follow:
Sig. fig. Examples
2 18, 180, 20., 0.020, 4.5 x 10-5, 4.0 × 102
3 2.50, 180., 1.80 × 103, 0.0100
4 2500., 6.020 × 10-1, 485.0, 0.01030
120
Significant Figures
For calculated numbers, the final value must be properly rounded to

the correct number of significant figures. There are specific rules
which apply for (a) addition and subtraction, and (b) multiplication
and division. A description of these follows.
Rule for Significant Figures in the Sum or Difference of Numbers
The sum or difference is written to the smallest place (hundredths,
tenths, units, tens, etc.) common to all numbers added or subtracted.
Example 1
Add the numbers 14.0, 0.625, 835.14 and 0.5 and express the answer
to the correct number of significant figures.
14.0
0.625
835.14
0.5
850.265 round to 850.3
Note that the rounding should be done after addition rather than
before. Rounding first would have led to the incorrect value 850.2.
Note also that the answer has four significant figures despite the fact
that one of the numbers added has only one sig. fig.
Example 2
2550. + 128 = 2678 (4 sig. fig.)
but, 2550 + 128 = 2680 (3 sig. fig.)
Example 3
2.500 × 10-3 - 2.800 x10-3 = -3.00 × 10-4 (only 3 sig. fig.)
Rule for Number of Significant Figures in a Product or Quotient
The product or quotient has a number of significant figures equal to
the fewest number of digits in any term involved in the multiplication
or division. The location of the decimal point has no effect.
Example 1
121
Significant Figures
144.5 × 0.565 = 81.6 (0.565 limits the number of sig. figs., in the
answer to 3)
Example 2
.04522 × 1820 = 1.37 ×10-22 (1820 contains only 3 sig. figs.)
6.023 × 1023
Rule for Calculations Involving Both (Addition-Subtraction) and

(Multiplication-Division)
Write the problem as you would for computer programming. Perform
operations in the following sequence
a) Evaluate quantities in parentheses first
b) Perform multiplications and/or divisions next
c) Perform additions and subtractions next
It is generally desirable to carry one extra (non-significant) digit
through the calculation and round off to the correct number of sig.
figs. at the end.
Example:
Y = (48.5 – 52.1) × 1.954 x 10-3 + 6.00 × 10-5
proceed as below
a) 48.5 – 52.1 = -3.6
b) -3.6 x 1.95 x 10-3 = 7.03 × 10-3 (only 2 sig. fig., but
carry 3rd digit)
c) -7.03 x 10-3 + 0.00060 = -6.97 × 10-3 (only 2 sig. fig.,
but carry 3rd digit)
d) Round to -7.0 × 10-3
Note that the answer contains 2 sig. fig. because of step (a) despite
the fact that all numbers in the original equation contain at least 3 sig.
fig. Also note that if step (b) is rounded to -7.0 × 10-3 before step (c),
the incorrect answer of -6.9 x 10-3 is obtained. Furthermore, if each
term in parentheses is multiplied by 1.954 × 10-3 and the subtraction
is then performed on numbers rounded to 3 sig. fig., the incorrect
result of -7.1 × 10-3 is obtained.
122
Significant Figures
Rule for Rounding Off

1. Where the final digit is less than five, the number is rounded off
by dropping this final digit
8.534 rounded to 2 sig. fig. is 8.53
2. Where the final digit is five or above, round up by adding 1 to the
second to last digit
8.535 rounded to 3 sig. fig. is 8.54
3. Avoid doubly rounding. For example, if your calculator do the
rounding by displaying only two decimal places (it will follow the
above rules) or display four decimal places so that you are certain
not to round up a number like 4.3448 × 10-2.
Note: Some scientists and mathematicians prefer to round terminal
5’s to even numbers; e.g. 3.45 would be rounded to 3.4, but 3.55
would be rounded to 3.6. Since electronic calculators do not use this
method, we will use the more common procedure outlined above.
123
Analytical Laboratory Techniques
APPENDIX B
ANALYTICAL LABORATORY TECHNIQUES
There are several common laboratory operations used in a typical
analytical laboratory which require some preliminary attention to
assure that they do not unnecessarily limit the accuracy of the
analyses. The proper techniques of weighing, drying, filtering and
volume measurements are described below.
Drying Samples
Most, but not all, solid samples are dried prior to weighing portions
for analysis. The purpose of drying is to remove any loosely held
water which may be present I the sample (but it is not intended to
remove chemically bound water such as is present in hydrates). Since
the amount of moisture present in powdered samples may vary
considerably with the particle size, extent of exposure to the
atmosphere, and the humidity, meaningful results are best reported on
a dry-sample basis. Metal samples do not normally dried because
they have a small surface area per unit weight and do not usually
absorb measurable weights of moisture. Furthermore, some metals
will oxidize on heating and sample will therefore increase in weight.
The temperature at which samples are dried is usually slightly
above the normal boiling point of water; i.e. 105˚C to 110˚C. In some
cases a somewhat higher temperature is used to dry the sample more
completely and more rapidly where there is no anger of chemically
altering the sample. In the experiments in this course, the iron ore and
organic acid samples should be dried at 105˚C to 110˚C, whereas the
recommended drying temperature for the soluble sulfate sample is
140˚C.
The weighing bottle containing the sample is placed in a
beaker on top of which is placed a ridget watch glass. The purpose of
this arrangement is to prevent contamination of the sample due to
particular matter falling in from above, while still allowing moisture
to escape. With many students using the same drying oven this is
particularly important. The watch glass must be ridget so that it is
raised slightly above the beaker, allowing moisture to escape. The lid
of the weighing bottle is usually dried in the beaker at the same time,
but obviously should not be placed on the weighing bottle at this
stage.
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The recommended drying time is usually one hour at

prescribed temperature, but longer times will normally do no harm.
After completion of drying, the weighing bottle and lid are removed
from the beaker and are placed in a desiccator to cool to room
temperature. When removing the sample from the desiccator for
weighing, the weighing bottle lid is used to prevent absorption of
atmospheric moisture.
The recommended technique for drying samples in a drying
oven is illustrated below.
A desiccator is a closed container which contains a solid

(desiccant) which readily absorbs moisture from the air. The air in the
desiccators will therefore be very dry and uptake of moisture by the
sample should be negligible. The most commonly used desiccants are
magnesium perchlorate, Mg(ClO4)2; calcium sulfate, CaSO4; calcium
chloride, CaCl2. The latter is used in this course because it is
relatively inexpensive and will take up large quantities of water. An
interesting experiment is to place some CaCl2 on a watch glass in the
open air and measured its weight periodically. A pronounced increase
in weight can be observed due to absorbtion of atmospheric moisture.
In preparing your dessicator, put it only enough calcium chloride to
cover the bottom to a depth of about one half inch. If the particles
start to stick together after a period of time, discard the CaCl2 and put
some fresh in desiccators.
WEIGHING
In the discussion which follows, the terms weight and mass are used
interchangeably to mean mass, as in common usage. Although all
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“weight” measurements in the course are actually mass

determinations, who ever heard of “massing” a sample?
Most of the mass measurements in this course require
accuracy to the nearest 0.1 or 0.2 mg (0.0001 to 0.0002g). Single pan
substitution-type analytical balances are available for these
measurements. These rather expensive instruments are capable of
excellent accuracy and reproducibility if treated with care. The basic
principal of operation is illustrated schematically below.
The balance is first adjusted to read zero deflection of the

beam. The object to be weighed is place on the balance pan. The
balance beam is lowered onto the fulcrum and weights are than
removed from the beam to compensate for the weight of the sample.
Rotating knobs on the front or side (depending on balance make) of
the cabinet operate lifting devices inside which raise and lower
calibrated weights on the beam. When the weight is compensated as
closely as possible with these lifters, the fractional weight remaining
is determined by the extent of beam deflection from the null position.
The illuminated scale on the front of the balance is actually a
projected image of a scale etches on the back end of the beam. Some
people call balances of this type “electric balances”. However, the
only thing electric about them is the small light bulb used to
illuminate the scale on the end of the beam, permitting it to be
projected onto the ground-glass window in the front.
In obtaining accurate weighing certain precautions must be
taken. In most analytical work, weighing is made by difference so
that it is not absolutely necessary to zero the balance. For instance, in
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weighing a sample into a beaker, the beaker may be weighed, the

sample added, and the beaker plus sample weighed. The difference in
the two weighings is the weight of the sample. In the case, any error
in the zero setting on the balance will affect both weighings equally
and net weigh (weight of sample) will be obtained correctly.
However if a crucible is weighed today and weighed again tomorrow,
it is very likely that the zero adjustment will not be the same both
items unless the balance is intentionally zeroed before each weighing.
It is thus generally advisable to get in the habit of zeroing the balance
before each weighing so that unexpected errors are not encountered.
A common source of error in weighing is lack of temperature
equality between the object being weighing and the balance. In such
cases, convection currents may be set up within the balance causing
an error of a few tenths of a milligram or more. In most cases where
the weight appears to “drift” with time, the cause is the gradual
equilibration of temperatures of balance and object being weighed.
Another cause of drift is the uptake or loss of moisture by the
sample. When hygroscopic materials are weighed in an open
container, their weight will gradually increase due to sorption of
water. To eliminate errors of this type, hygroscopic materials should
be weighed in covered weighing bottles. Solid samples used in this
course should not change in weight due to water uptake rapidly
enough to detect, and they can therefore be weighed in containers
open to the air even though they should be stored in desiccators.
When liquids are weighed, they must be kept in covered containers to
avoid weight loss.
Objects to be weighed should not be handled directly with the
hands; even fingerprints are often weighable. Either use clean tongs
or use a piece of paper to handle objects to be placed on the balance.
A brief outline of weighing procedures is given below.
A. Weighing into a beaker
1. Place a clean, dry beaker on the balance pan, close the
balance doors, and measure its weight (tare weight).
2. Calculate the total (gross) weight of beaker plus sample
for the desired sample weight.
3. Using a clean spatula, tap in enough of the solid to
bring the gross weight to approximately the required
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value. Close the balance doors and obtain the accurate

weight.
4. Enter the gross (G) and tare (T) weights in your
notebook as obtained and subtract to obtain the net
weight (N).
B. Weighing from a weighing bottle

1. Weigh the weighing bottle containing the sample
2. Grasp the weighing bottle by using a strip of paper
wrapped around it. Tilt the weighing bottle over the
beaker ad tap the side of it with a spatula so that some
sample falls into the beaker.
3. Return the weighing bottle to an upright position and
again tap the side so that sample falls back into the
bottom. Reweigh.
4. Subtract the final weight of weighing bottle plus
sample (T) from the original weight (G) to get the net
weight (N) of sample transferred to the beaker. Repeat
steps 2 and 3 as required to get sufficient sample into
the beaker.
Comparison of methods A and B
Method A is simpler and generally preferable if a clean, dry
beaker is available and the capacity of the balance is sufficiently large
to accommodate the weight of the beaker. It is susceptible to errors,
however, if there is any moisture on the beaker which may evaporate,
causing a change in its weight. One must also exercise particular care
to make sure that none of the sample skids off the spatula onto the
balance pan rather than into the beaker. Method B is usually safer,
but may require several weighings to obtain the desired amount of
sample transferred. Both methods are susceptible to accidental
transfer of too much sample into the beaker, trying to remove the
excess is usually not very satisfactory.
C. Use of a watch glass or weighing paper
1. Weigh a clean watch glass or a glazed paper or cup
2. Transfer onto the glass or paper the desired amount of
sample from the weighing bottle.
3. Transfer the sample to the beaker, being certain that the
transfer is complete. A jet of water from a wash bottle
may be used to assure complete transfer when a watch
glass s used.
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4. Reweigh the glass, paper, or cup (if water was not used
in transfer) and record as tare weight.
Method C suffers from the fact that two transfers are needed
with a corresponding increase in the possibility of some
sample loss. It also takes particular care to transfer a solid
from a watch glass to a beaker without loss. Filter paper,
notebook paper, etc., should never be used because the
surface is too rough and complete transfer to the beaker is
difficult or impossible.
D. Determining the absolute weight of an object (e.g. a crucible)
1. Zero the balance
2. Place the object on the balance pan and measure its
weight.
E. Use of a triple beam balance
Certain reagents need to be weighed only roughly (to the
nearest 0.1 or 0.01 g) and in such cases of triple beam balance
is much faster than the analytical balance. Weighings on a
triple beam balance usually use the following procedure.
1. Place a beaker, watch glass, or piece of (any) clean
paper on the balance pan and adjust the weights to zero
beam deflection. Record the tare weight.
2. Add the desired weight of reagent to the tare weight
and adjust the balance weights to this value (or slightly
less).
3. Using a spatula, add reagent to the beaker, or other
container until the balance beam deflection returns to
zero.
4. Transfer the reagent to the desired container – it is not
necessary to reweigh the beaker, etc.
Since not all of all the analytical balances used in this course
are of the same manufacture, specific operating instructions are not
given here. Note, however, that these balances all have some means
of adjusting the weights to the approximate value of the object
weighed before the beam is completely released. It is important to use
this feature so that the delicate knife edges are not damaged. Consult
your laboratory instructor for details on the use of your specific
balance.
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Finally, all related weighings should be made on the same

balance. Slight differences can be detected between balances. These
should be inconsequential if weighings are all made on the same
instrument, but may cause slight errors in changing from on balance
to another.
VOLUME MEASUREMENTS
A variety of volume measuring devices are used in analytical
chemistry with accuracies ranging about ± 10% to ± 0.05% or better.
Proper selection of the device to be used requires knowledge of the
accuracy required in the measurement. There is no point in using a
pipet when a graduated cylinder will do, and one most certainly
doesn’t use a graduated cylinder when the accuracy of pipet is
required. The volumetric glassware used in this course includes
volumetric flasks, pipets (two types), burets, graduated flasks and
beakers. These are illustrated as follows.
Volumetric Glassware
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Volumetric Flasks
These containers are the most accurate volume measuring devices in
common usage in chemical laboratories. They are calibrated to
contain a specified volume of solution at a specified temperature,
usually 20˚C. An etched ring in the neck of the flask shows the level
of the bottom of the meniscus of the solution in the flask when it
contains the calibrated volume. A 250 mL “Class A” volumetric flak
is calibrated to within 0.12 mL (0.048%) of that volume. The non
class A flasks used in most student laboratories are still quite
accurate; within ± 0.24 mL for a 250 mL flask. Since the coefficient
of thermal expansion for glass is relatively small, volume
measurements made within a few degrees of 20ºC are sufficiently
accurate for most work. The change in volume of water with
temperature is much greater than that of glass, so solution prepared in
volumetric flasks should be brought to volume at room temperature –
i.e., the temperature at which they will be used. If the contents of a
volumetric flask are emptied into another container, less than the
calibrated volume is transferred because a small amount of liquid is
left on the walls of the flask. In other words, the flask is calibrated to
certain rather than to deliver a particular volume.
Volumetric or Transfer Pipets

This type of pipet is the most accurate device for transferring a
volume of liquid from one container to another. Typical accuracies
are within about 0.1% of the calibrated volume. On the upper stem of
the pipet is etched a circular calibration mark of the meniscus when
the pipet is ready to deliver the calibrated volume. The liquid is
allowed to gravity drain into the receiving vessel until no more will
drain up. The drop at the tip of the pipet is then touched off by
bringing the tip in contact with the wall of the receiving vessel. Note
that the pipet delivers the calibrated volume. This is slightly less than
the volume it contains, since some of the liquid is left on the inner
walls of the pipet when it is properly drained. If you look at the
manufacturer’s marking at the top of the pipet you will probably see a
TD which stands for “to deliver”. (Some pipets, not used in this
course, are calibrated to contain the specified volume and have a TC
etched on the upper stem).
In using any type of pipet, liquid is drawn in by use of
suction. A rubber bulb is invariably used for this purpose; you should
never use your mouth to draw up the liquid. A general procedure for
filling and draining a pipet is given below. Note that it is difficult to
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thoroughly clean and dry a pipet, so it is customary to rinse the pipet

2 or 3 times with small amounts of the solution to be transferred. The
pipet should always be rinsed thoroughly with distilled water after
use.
1. Dip the tip of the pipet well below the surface of the solution
to be transferred so that there is no possibility of drawing in
any air.
2. Squeeze the syringe bulb with the left hand (if you are right
handed), fit it over the upper and of the pipet and release the
hand pressure a little to draw a small amount of liquid into the
pipet. Slip the bulb off and immediately place your right
index finger over the top of the pipet so that the liquid does
not drain out (this required some practice). Lift the pipet and
tip and rotate it so that the liquid rinses the inner walls, then
discard the rinse solution into the sink (out delivery tip, not
the top). Repeat this two or three times.
3. Now fill the pipet with solution to a little above the
calibration mark, being careful not to draw any liquid into the
syringe bulb. Remove the bulb and quickly seal the top of the
pipet with your finger.
4. With the tip of the pipet against the glass above the surface of
the filling liquid, very carefully allow the bottom of the
meniscus to drop to the calibration mark. Then lift the pipet
and tip it slightly so that a little air enters the tip.
5. Wipe the tip with a clean towel or Kimwipe then drain the
pipet into the receiving vessel. The pipet should be nearly
vertical. After it has drained, touch off the droplet at the tip
against the wall of the container. Do not blow out the small
amount of liquid still in the pipet.
6. If no further transfers of the solution are to be made,
thoroughly rinse the pipet inside and out wit demineralized
water from a wash bottle. Drain, but do not try to dry the
inside.
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Proper Pipeting Technique
Mohr Pipets
A Mohr pipet is a graduated pipet calibrated to deliver volumes
typically in the range of 0-5 mL or 0-10 mL. The pipet is rinsed and
filled in the same manner as a volumetric pipet, but it is not allowed
to drain completely. Finger pressure is used to allow the liquid to
drain from the zero mark near the top of the pipet to the desired
graduation mark lower on the pipet. It is thus necessary to stop the
meniscus at both the initial and final marks on the pipet. Mohr pipets
are considerably less accurate than the transfer pipets, having a
typical accuracy of about ±0.05 mL.
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Burets
A buret is a graduated volume-measuring device capable of
delivering, typically, 0-25 mL or 0-50 mL of solution in increments
which may be as small as 0.01mL. Although it is superficially
somewhat similar to a Mohr pipet, it is much more accurately
calibrated and its flow is carefully control by use of a stopcock.
Burets are normally use for titrations in which a reagent (titrant) is
gradually added to a solution of the substance being determined
(analyte) until an indicator gives the evidence that the amount of
titrant added is equivalent to the amount of analyte originally present.
By careful manipulation of the stopcock, the volume of titrant
required to reach the end-point of the titration can be accurately
determined. The concentration of the analyte solution can then be
calculated from the volume and concentration of titrant and the
volume of analyte solution, as explained in greater detail in the
volumetric experiments.
Burets can be cleaned by use of detergents and a buret brush
available in the laboratory. Accurate volume measurements are
obtained only when the buret drain cleanly without leaving droplets
in the inner walls. When the droplets form, they are evidence of
grease or dirt on the glass. A clean buret will leave only an invisible
film of solution on the walls when drained. After cleaning, the buret
should be thoroughly rinsed with demineralized water and then with
the reagent to be used. When ready for use, the buret is filled nearly
full and enough liquid is drained through the stopcock and discarded
to flush out the tip and purge it of air bubbles.
In operating a buret, open the stopcock to allow reagent to
flow out into a waste beaker until the lower level of the meniscus is
even with or below the zero mark. Trying to get the meniscus exactly
even with the zero mark is unnecessarily effort; just be certain to
record the actual initial reading. The droplet on the end of the buret is
touched off against the wall of the waste beaker and the titration can
now be carried out.
Be sure that the Teflon stopcock is fitted snugly in the buret.
Tighten the Teflon nut so that the stopcock turns fairly easily but
without leakage. It is a good idea to check the nut form time to time
to make sure it hasn’t loosened. When titrating in an Erlenmayer
flask and using an indicator for endpoint detection, operate the
stopcock with your left hand (around the buret) while swirling the
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flask with your right hand. Using this technique the titration should
go fairly rapidly. You may want to ask your instructor for a
demonstration.
When the end point is reached, again read the lower edge of
the meniscus. The difference between initial and final volume
readings is the net volume of the titration:
Init reading ________ mL
Final reading ________ mL
Net volume ________ mL
Note that in performing a titration, any droplet on the buret tip
at the end of a titration is part of the volume removed from the
measuring section. The end-point should therefore be approached
slowly. Very close to the end-point hanging drops should be touched
off into the receiving beaker or flask and washed down with a jet of
demineralized water from a wash bottle. A drop of most dilute
aqueous solutions has a volume of approximately 0.05 mL.
Readings of the buret should be estimated to the nearest 0.01

mL. As you will notice, the appearance and position of the bottom of
the meniscus changes significantly with the lighting and background
of the buret. For accurate measurements it is therefore necessary to
place a suitable constant background behind the meniscus to obtain
consistent and reliable readings. This may be a pieced of colored
paper (to help make the bottom of the meniscus more visible) or a
135
piece of plastic or paper which has sharply divided dark and light
sections. Whatever is used to enhance the readability of the meniscus
must be used consistently for all readings. It is also important to have
your eye even with the meniscus when making the reading.
Significantly different readings may be obtained if the eye level is
well above or below the meniscus (Try it!). Graduated cylinders
Graduated cylinders may be calibrated either to deliver (TD)
or to contain (TC) the volumes indicated and are manufactured in
several capacities (5 mL to 2000 mL). They are useful for
approximate measurements of liquid volumes. Expected accuracies of
volumes measured are typically in the range of 1 to 2 % of the
volume of the cylinder. For example, measurement of 25 mL of
solution with a 100 mL graduate should be accurate within 1 or 2 mL.
Graduated Beakers and Flasks

These should be considered to be volumetric glassware, but
the markings are sometimes useful for rough volume measurements.
Errors of the order of ± 10% in marked volumes can be anticipated.
Filtration
One of the most common means of separating a component of
a mixture is to precipitate it from a solution and then separate the
liquid and solid phases by filtration. Although a variety of materials
are used as filter media, low-ash filter paper is probably still the most
widely used. The low ash contain allows the filter paper to be burned
off without leaving a weighable residue. Recovery of the precipitate
on the filter paper followed by washing to remove impurities, and
heating (ignition) to drive off water, provides a means of recovering
the solid virtually free of contamination.
The basic requirements of the filtration process are (1) that all
(within the limits of measurement) of the precipitate be retained by
the filtration medium (paper in this case), and (2) that all measurable
impurities pass through the filter or are destroyed in the ignition
process.
A filter paper has a network of channels and pores through
which the solution is able to pass. If the solid particles are sufficiently
large they will not pass through the paper although some of them may
penetrate part way into the pores. Papers are available which are
136
designated as coarse, medium, or fine porosity (or as fast, medium

and slow). The coarse papers are used where a rapid filtration is
desired and where quantitative recovery is not required. They may
also be used for certain gelatinous precipitates that are adequately
retained by the greater porosity. For most crystalline precipitates, like
tetraamine copper (II) sulfate, a fine porosity paper is needed.
When filtration is performed, solid particles gradually tend to
clog the pores of the filter and to coat it so that the more solid
transferred to the filter, the more slowly the filtration proceeds. For
this reason it is desirable to wash the residue in its original container
as thoroughly as possible before transferring it to the filter. Less
washing of the residue in the filter is required when this is done.
Quantitative recovery of a residue by filtration requires very
careful laboratory technique. All the precipitate must be transferred to
the filter and all the impurities must be removed, but the washing
must be insufficient to dissolve a measurable amount of the residue.
A typical filtration set-up is as shown.
Set-up for gravity filtration
Filter paper with corner removed for used in gravity filtration
137
A filter rack capable of holding four funnels is used so that

four samples may be filtered simultaneously. The filter papers are
provided as circles must be folded in quarters to fit into the funnel.
To obtain a good air-tight seal between the moist paper and the glass
of the funnel, a corner of the folded paper is torn off as shown in
Figure 2. A pocket is then formed with the portion of the paper which
does not have the torn-off corner, and the filter is inserted in the
funnel. A stream of water is used to moisten the paper while it is held
snugly against the glass. The paper should be kept wet from this point
on until filtration is complete. It has been found that the filtration will
proceed significantly more rapidly if a good paper-to-glass seal is
maintained so that air bubbles do not get under the paper.
Proper method of decanting supernatant liquid through filter paper
Washing precipitate into filter with stream of demineralized water

from wash bottle
138
In transferring the precipitate, as much washing should be

performed in the beaker as possible. Allow the residue to settle in the
beaker, then decant (pour off) as much of the supernatant liquid as
possible through the filter without transferring much residue. The
decantation is facilitated by use of stirring rod to direct the liquid into
the funnel (Figure 3). Be sure the stirring rod is kept in contact with
the lip of the beaker until any remaining liquid is tipped back into the
beaker. The drop of the liquid on the stirring rod can be touched off
against the filter and the rod returned to the beaker. Fresh washing
solution is then added to the beaker, the mixture is slurried to rinse
the residue and the process of settling and decantation is repeated.
After two or three washing of the residue in the beaker, the
precipitate is transferred to the filter. This is accomplished by
slurrying the residue with water and rapidly pouring into the funnel.
In this case it is not necessary to use the stirring rod except to catch
any drop on the lip of the beaker when it is tipped back. When most
of the residue has been transferred using small volumes of water, any
remaining residue is washed into the funnel by using a jet of water
from the wash bottle (Figure 4).
Through the filtration process it is important that the liquid
level in the funnel be kept below the top edge of the paper solid
which gets onto the glass may wash down under the paper and be
lost, or may not be recovered easily from the glass surface.
Finally, once the transfer is complete, further washing of the
residue in the funnel is accomplished by use of stream of water from
the wash bottle. Completeness of washing is tested as described in the
sulfate experiment.
When the filtration is completes, the filter paper should be
removed from the funnel while still moist. The top is folded in so that
the precipitate is enclosed, and the paper is placed in a crucible for
ignition.
139
Laboratory Regulation and Procedure
APPENDIX C
LABORATORY REGULATION AND PROCEDURE
A. Laboratory Regulation
1. Except when using instruments which are stationed in special

rooms or at particular places in the laboratory, you are to
work at the unit where you are assigned to.
2. You are to work independently on assigned experiment unless

directed otherwise by the instructor or by the written
instructions for the experiment.
3. For many of these experiments, apparatus and special

equipment is checked out from the dispensing room at the
beginning of the laboratory period. All such apparatus and
equipment must be returned to the stockroom in good
condition at the end of the laboratory period. See the
supplementary sheet for a list of equipment needed.
4. You must wear safety goggles whenever you are in the

laboratory. You must also wear adequately protective
clothing.
5. Smoking, eating, or drinking are not permitted in the

laboratory.
6. No unauthorized experiments may be done in the laboratory.
7. Do not put spatulas, pipets, or anything else into reagent

bottles. Pour from the stock bottle into your own container.
Do not return anything to a stock bottle of reagent unless
specifically directed to do so by an instructor or by the written
instructions for the experiment. Don’t waste reagents. Taken
only the quantity needed.
8. Clean up any spilled materials, and leave your working space

in a clean condition at the end of the laboratory period.
138
9. Dispose of excess or waste materials according to the

direction given in this manual or in the laboratory. If no
explicit directions are given, put water-insoluble solids in the
waste jar at your desk and flush water-soluble solids and
liquids down the drain with a large quantity of cold water.
10. Be familiar with and observe the safety precautions which

apply to the experiment you are holding.
Important Attentions!!
1. Use the fume hoods when working with acids. Solutions
or acids usually give off significant quantities of fumes
which irritating and bad for the lungs. Hot acid solution
should be allowed to cool before being taken from the
hood to your lab bench, and they should be kept covered
at all times when not in the hoods (and most of the time
when they are in the hoods). Ventilation in the labs is
sufficient to prevent much buildup of acid fumes in the air
if you make appropriate use of the hoods. Even cold
hydrochloric and nitric acids (HC1 and HNO3) give off
irritating fumes and should be kept covered and used in
the hoods as much as possible.
2. Know the location of the safety eye wash and shower. In
the event of a spill or splash, wash the affected area with
copious quantities of water as quickly as possible. Don’t
hesitate to use the eye wash if chemical get into your eyes.
The safety shower may save your clothing and skin from
serious damage.
3. Report all accidents to your instructor immediately. In the
case of a serious injury he may send you to the infirmary
for medical attention.
4. Use a rubber bulb for pipetting. Always use a bulb for
drawing liquid into the pipet, even if you are only
pipetting water.
5. Label everything. You may avoid both injury and errors in
your analyses by having your beakers, flasks, weighing
bottles, etc.,
139
6. Use suitable tongs when handling hot objects.

7. Clean up all spills and broken glass. Don’t leave these
around and risk a letter injury to yourself or someone else.
Clean your lab bench before leaving the lab when you are
through. If you receive a glass cut be sure to have it
attended to.
8. Use proper methods of waste disposal. Toxic substances
should not be poured down the drain. Since we do not
expect you to be completely knowledgeable on what is
toxic/hazardous and what is not, the policy in this course
is to not permit students to dispose of nay chemicals in the
sink. Waste disposal containers labeled for specific
materials are located in the laboratory and these must be
used for disposable of all chemicals. Be sure to use the
correct disposal container for each of your waste solution
and solids. If you are uncertain of the correct container,
ask the instructor. Subsequent proper disposal of
laboratory waste by instructors and stockroom personnel
depends upon your cooperation in using only the correct
containers for each experiment. Your cooperation is
needed and appreciated.
B. Procedure for Handling Data
All data are to be recorded directly in the notebook and not on
scraps of paper or other sheets. Mistakes in recording should
be crossed out--they should not be erased. If a measurement is
thought to be bad, make a note of the reason in the notebook.
Before leaving the laboratory at the completion of an
experiment, have your data checked and initialed by an
instructor. Place the carbon copy in the box provided for it
before you leave the laboratory. The original copy is to be
attached to the laboratory report as the back page. The data
from your lab notebook are to be properly organized into
tables and graphs which are to be part of the body of your
report.
140
Testing Standards
APPENDIX D
TESTING STANDARDS
ASTM D5712-99
Standard Test Method for the Analysis of Aqueous Extractable
Protein in Natural Rubber and its Products" (the modified Lowry
Method).
ASTM D 412-87
Standard Test Methods for Rubber Properties in Tension.
ASTM D 638-91
Standard Test Method for Tensile Properties of Plastics
ASTM D412 98a

Standard Test Methods for Vulcanized Rubber and Thermoplastic
Rubbers and Thermoplastic Elastomers.
ASTM D256 90b

Standard Test Methods for Impact Resistance of Plastics and
Electrical Insulating Materials.
ASTM D4274-88
Determination of hydroxyl value for polyurethane polyol.
ASTM D974 -08

Standard Test Method for Acid and Base Number by Color-
Indicator Titration
143
Index
2,4-diphenylmethane diisocyanate, 2 Iodometry titration, 88

Acid number, 55, 56 Loss coefficients, 31
Acrylonitrile, 37, 38 Microcentrifuge, 74
Adipic acid, 12 Moody diagram, 22, 23, 27
Adipoyl chloride, 12, 13 Natural rubber, 5, 6, 107
Antioxidant, 6 Nutmeg, 95
Ball-mill, 49 Nylon, 12
Bovine serum albumin, 73 Oil palm empty fruit bunch fiber, 49
Catalyst, 1 Optical microscope, 3
Amine, 1, 12, 37 Organometallic, 42
Tertiary amine, 1 Oxalic acid, 44, 45, 102
Ceramic balls, 50 Pentametyhl diethylenetriamine, 2
Chain length, 1 Pipe, 22, 30
Conjugated polymer, 59 Fittings, 30
Continuous stirred tank reactor, 62 Smooth Bore, 22, 29
Crystallization, 96 Polyacrylonitrile, 38
Cross-linking, 6, 19 Polyamide, 12
Darcy-Weisbach equation, 22 Polyisoprene, 6
Dialysis membrane, 72 Polyester, 1, 55
Diamine, 12 Polyether, 1, 55, 92
Diaquadioxalatochromate (III), 42 Polyethylene, 15, 107
Cis-, 40, 45, 46 Terephtalate, 15
Trans-, 40, 44- 46 Polyhydroxyl, 1
Dicarboxylic acid, 12 Polymerization, 1, 11, 37
Dimethylcyclohexaneamine, 56, 92 Addition, 1, 11
Ester, 95 Chain-growth, 59
Ethyl acrylate, 79 Condensation, 11
Ethyl alcohol, 62 Emulsion, 79-82
Filtration, 96-98 Radical, 79
First order, 62 Redox, 37
Friction, 22, 23, 26, 29 Polyol, 2, 55
Free-radicals, 37 Polypyrrole, 59
Gel permeation chromatography, 56 Polyurethane, 1, 55, 92
Glycerol, 95 Potassium dichromate, 44, 77
Head Loss, 22, 29, 30, 35 Potassium trioxalatoferrate (III)
Hexamethylenediamine, 12-13 trihydrate, 102, 104
Hydrolysis, 95 Protein, 5, 6, 8
Hydroxyl value, 55, 56 Redox Titration, 44, 46, 47
Impact strength, 110 Reynold’s, 22, 26
Infrared spectroscopy, 11, 60, 92 Rubber, 19
Intrinsic viscosity, 40 Rubber wood, 49
Iron (II) oxalate, 102-104 Saponification, 95
Isocyanate, 1, 55, 92 Sieve shaker, 49
Diisocyanate, 1- 2, 55, 92 Silica gel, 49
Isomers, 43, 46 Surfactant, 79
Isoprene, 5 Silicone, 2, 55, 92
144
Index
Sodium acetate, 62
Sodium phosphate, 76, 77
Tetraamine copper (II) sulphate, 84
Tetramethylhexanediamine, 2
Thermoplastic, 15, 107
Thin layer chromatography, 97-98
Triglyceride, 95
Time, 2
Mixing, 1
Cream, 2, 3
Gel, 2, 3
Rise, 2, 3
Tack-free-time, 2, 3
Trimyristin, 95
Vulcanization, 5
Young’s modulus, 110
145
POLYMER RESEARCH CENTER (PORCE)
Website: www.ukm.my/porce

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Khairiah Haji Badri

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Perpustakaan Negara Malaysia Cataloguing‐in‐Publication Data

Khairiah Haji Badri, 1970 –

Chemical Technology in Practice is a combination of theoretical and

AIMS OF THE COURSE

There are a number of reasons for introducing the student to

Objective 1 Development of an appreciation of accuracy, precision

Objective 2 Development of skill in performing scientific work

Objective 3 Development of self-reliance and confidence in

Objective 4 Development of skills in planning and efficient use of

Objective 5 Development of good methods of scientific record

Objective 6 Development of an awareness that inaccuracies may

Appendix A-1 Accuracy and Precision 115

The polymer structure can be depicted as in equation 3.1

where M is the monomer’s molecule (mer) or the repeating unit.

Polymerization reaction can be divided into two types, that is,

Note an immediate formation of polymer at the interface of

Figure 3.3 Nylon

 Use a reactant from dicarboxylic acid group that has six-

Figure 3.4 Nylon-4, 6

Separation of Solid-Solid Sample

Figure 10.1 A set-up of a sieve-shaker

7. Collect the contents of each sieve in separate containers.

Figure 10.2 Ball-mill

 Compare the result before and after ball-milling with 10 and

Table 10.1 Accumulated data of the sample’s size without ball-

Initial mass of sample : kg

Sieve Mass of Trapped Accumulative Accumulative

Table 10.2 Accumulated data of the sample’s size after ball-milling

Initial mass of sample : kg

Sieve Mass of Trapped Accumulative Accumulative

Table 10.3 Accumulated data of the sample’s size after ball-milling

Initial mass of sample : kg

Figure 10.3 Size distribution of sample

trimyristin glycerol myristic acid

This experiment illustrating the separation of lipid from the

8. Collect the crystal by suction glass funnel. Wash the crystal

Part II Saponification of trimyristin

Thin layer chromatography (TLC) analysis

mixture of 90 % toluene and 10 % ethanol (9:1) at a level of 1

1. Dilute a few mg of trimyristin and myristic acid separately in

2. Drag the prepared solution with capillary tube, holding it

3. Place a drop of the solution at a point about 2 cm from the

This step requires proper handling. Be careful not to scratch

Figure 18.1 Sample spots on TLC plate.

5. Air-dry the TLC plate to evaporate the solvent.

6. Slowly place the TLC plate in the chromatography chamber

Figure 18.2 The TLC plate is slanted in the solvent mixture.

7. Observe the solvent moves upward in a quick manner. Leave

8. Air-dry the plate at room condition. Detect the spot using

 Explain why sodium salt myristate is considered as soap.

 Explain how the thin-layer chromatography is used to

moving distance of the compound

Figure 18.4 Finished TLC plate.

 Determine whether the difference in the Rf values can be used

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