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CODE: DRK1411

LAB. NAME: BASIC SCIENCE AND ENGINEERING LABORATORY

2023/2024 Semester 2

Title of Experiment : GRAVIMETRIC ANALYSIS SOLUTION

Lecturer’s Name : TS JOHARIZAL BIN JOHARI

Group of Member :3

Name ID
1.NORRYSH DAYANA BINTI NORRIHAN RK23288
2.NUR AIREEN BATRISYA BT MOHD ASRI RK23326
3.MUHAMMAD FARIS HELMI BIN ABDUL HAMID RK23237

Group No. :4
Section : RK03

FACULTY OF CHEMICAL AND PROCESS ENGINEERING TECHNOLOGY

UNIVERSITI MALAYSIA PAHANG AL-SULTAN ABDULLAH

Subject Code :
Title of Experiment: Date Submitted:
SUBJECT: BASIC SCIENCE AND ENGINEERING LABORATORY MARKS:
EXPERIMENT:1 CODE: DRK1411

REPORT RUBRIC (PO1 &P04)

Name Matric ID
1. NORRYSH DAYANA BINTI NORRIHAN RK23288

2. NUR AIREEN BATRISYA BT MOHD ASRI RK23326

3. MUHAMMAD FARIS HELMI BIN ABDUL HAMID RK23237

Broadly-
defined
Engineering SCORE
LEVEL OF ACHIEVEMENT WEIGHTAGE
Problems (DP) GAINED
Item DESCRIPTORS
& Activities
(NA) with
Knowledge
Profiles (DK) 0 (Poor) 1 (Weak) 2 (Satisfactory) 3 (Good) 4 (Excellent)

PO 2 (Problem Analysis)

Abstract missing Abstract missing


Abstract missing Abstract contains
three of the one of the
two of the complete
information infromation
information information
(Objective, (Objective,
No abstract (Objective, (Objective,
Summary of the Summary of the 3
provided Summary of the Summary of the
methodology, methodology,
Assess the methodology, methodology,
Summary of the Summary of the
comprehension Summary of the Summary of the
results, results,
of the basic results, Conclusion) results, Conclusion)
Conclusion) Conclusion)
concepts,
theories and
Introduction :
principles Introduction :
Introduction is
related to the Very little
complete
topic. background
and well written;
Introduction information or Introduction : Some
provides
DP 1 (Depth of contains topic information is introductory Introduction :
all necessary
knowledge and purpose. incorrect OR, information, but Introduction is
No background
required) Body of content does still nearly
introduction principles and 4
provides not give any missing some major complete, missing
provided theory for the
adequate, information points. OR, gives some minor
experiment.
relevant and about little points
Present a
significant what to expect information
concise lead-in to
information. in
the
Closing the laboratory
laboratory
summarizes the report
experiment.
topic with
impactful.
Conclusion : Closing Conclusion : Conclusion : Closing
Conclusion : Conclusion :
contains some key Closing highlights highlights all key
There is no Closing
ideas and most key ideas, ideas and concludes
closing, and highlights a few 4
concludes with an and concludes with a strong and
no summary ideas and no
acceptable final with a good final impacfful final
made. final statement.
statement. statement. statement.

Assess the ability Results given but Elucidation and


Elucidation of
to explain the significant Results given but a supported
DP 2 (Range of result
experiment amount not tally few not tally with by
conflicting No results but 4
parameters from with the the requirements of proper references
requirements) contains some
multiple requirement/ experiment or logical
flaws
variables scopes explanations.

DP 3 (Depth of Evaluate the No discussion Only mention Attempt to discuss Elucidation of Elucidation and 4
analysis depth of analysis provided the results but failed miserably result but supported by
required) and critical without contains some proper references
thinking applied meaningful flaws. or logical
to the results discussion Use same explanations.
obtained referencing All references from
system reliable resources
Most of citations in
Copy & paste All citations in text
text are not A few citations in
references OR are available in list
Evaluate the available in list of text are not
Ununiformed of reference and
ability to use No citation reference although available in list of
referencing use the same
information and use same reference AND 3
system OR referencing system
from other references referencing system Use same
80% references AND
sources OR referencing
from internet OR All references from
Internet sources > system
Use of Wikipedia reliable resources
60%

Has some
Generally follows a Exhibit an
structure but
logical structure exemplary
may lack
Lack a clear with an Well-structured, structure, with a
Evaluate the coherence or
structure and introduction, body, with a clear compelling
structure of the suffer from
fails to and conclusion, but introduction, introduction, well-
Organization report, focusing inconsistent
provide a improvements well-developed organized and 3
structure on the organization. The
logical could be made in body sections, cohesive body
organization and sections may not
progression terms of section and a coherent sections, and a
layout. be clearly
of ideas. divisions and conclusion. succinct yet
labeled or
overall comprehensive
effectively
organization. conclusion.
linked.

The writing
Evaluate the style is The writing style
overall writing incoherent, is somewhat The writing style
The writing style is
style, grammar, confusing, inconsistent or is clear, engaging,
exceptional,
spelling, and lacks lacks clarity in The writing style is and effectively
exhibiting a high
punctuation and clarity. The certain sections. generally clear and conveys the
level of clarity,
adherence to report is The report coherent, with few intended
coherence, and
proper riddled with contains instances of message. The
precision. The
formatting and numerous noticeable grammatical errors, report
report is virtually
citation grammatical grammatical spelling mistakes, demonstrates a
Writing style error-free,
guidelines. errors, errors, spelling or punctuation good command 3
and quality demonstrating
Assess the spelling mistakes, or errors. Formatting of grammar,
impeccable
author;s ability mistakes, punctuation and citation spelling, and
grammar, spelling,
to convey and poor errors. guidelines are punctuation.
and punctuation.
information punctuation. Formatting and mostly followed but Formatting and
Formatting and
effectively and Formatting citation may have minor citation
citation guidelines
engage the and citation guidelines may inconsistencies. guidelines are
are adhered to
reader through guidelines not be consistently
meticulously.
clear and concise are consistently followed.
writing consistently followed.
ignored.

PO4 (Investigation) TOTAL

No flowchart Missing several Method flowchart Method flowchart Method flowchart is


of the important is is complete. Logical
method is explanations of nearly complete explained with and easily
presented. materials and/or but sufficient detail; followed.
methodology. still missing some some lack detail Description of
Experiment
Not important or procedure is
Procedure, List
sequential. Most experimental are confusing. complete,
of
steps are missing details. Mostly ensuring that it can
Methodology Equipment,
or easy to follow. be
Flowchart Specify the
are confusing. replicated.
value, Make as
Some
flow
procedural
chart
components
generally
described but
are not
replicable. 5

Data Calculations Calculation was Calculation was Corrected Correct and


calculation, not not provided but with calculation. complete
graph shown or provided some Incomplete or in calculation. Data
Data Processing
presentation, totally Or error. Data was adequate data was
&
table wrong. No Data was not organized in term organization in organized well in
Analysis
presentation table or organized in of term term of
graph are term of table or graph. of table or graph table or graph.
present. table or graph. form. 2.5

TOTAL

TABLE OF CONTENTS
No. Content Pages
1 Abstract 1
2 Introduction 2
3 Methodology Chart 3-4
4 Results 5
5 Discussions 6
6 Conclusion 7
7 References 8

8 Appendices 9

1
ABSTRACT

The objective of this experiment is to understand the concept of gravimetric analysis. Other
than that, we need to determine amount of analyte precipitate and predict the percentage of
analyte precipitate. After the experiment being conducted, we will be able to calculate the
weight and percentage of the analyte precipitate that formed by mixing the substances during
the experiment. We need to heat the sample solution of sodium chloride with constant stirring
and add silver nitrate solution slowly into the sample solution until the coagulation stop. The
stirring helps prevent bumping of the solution during heating and the danger of loss of
precipitate. Then, we need to filter and washing the precipitate by pouring the solution down
a stirring rod the precipitate should be disturbed as little as possible. After that, during drying
and weighing the precipitate we need to place the crucibles containing the precipitate in a
covered beaker in the oven for 1 day at 40 – 50 °C and cool the crucibles in the desiccator,
and weigh. The results obtained by the experiment was 0.6809g of silver chloride which is a
white precipitate. In conclusion, the experiment aims to explore the fundamentals of
gravimetric analysis, a key method in analytical chemistry. The goals of determining the
quantity and percentage of the analyte precipitate were accomplished by means of laborious
methods that included precipitating silver chloride from a solution containing sodium
chloride, drying the precipitate, and then weighing it. The experimental process involved
careful manipulation of the reaction conditions, including controlled heating with stirring to
prevent solution bumping and loss of precipitate. Next filtration and washing of the
precipitate were conducted with utmost care to minimize disturbance. Following these steps,
the precipitate was dried and weighed to obtain a precise measurement.

2
INTRODUCTION

Analytical techniques where weight is involved in the last stage of the analysis fall under the
category of gravimetric analysis. One of the most exact and accurate techniques for macro-
quantitative analysis is gravimetric analysis. During this procedure, the analyte is transformed
into an insoluble state on purpose. The separated precipitate is precisely weighed after being
dried or ignited taking on new forms. The weight of the analyte can be calculated in the
desired manner using the precipitate's weight and information about its chemical
composition. The principle behind the gravimetric analysis is that the mass of an ion in a pure
compound and can be determined. After that, it will be used to find the mass percent of the
same ion in a known quantity of an impure compound. There are 4 fundamental types of
gravimetric analysis which is volatilisation gravimetry, precipitation gravimetry,
electrogravimetry and thermogravimetry. We use precipitation gravimetry to conduct the
experiment by combining a precipitation process into a solid, precipitation gravimetry can
separate one or more components of a solution. The objective of this experiment is to
understand the concept of gravimetric analysis and we need to determine amount of analyte
precipitate then predict the percentage of analyte precipitate. We need to weigh a sample
solid sodium chloride of about 0.3 g into 400 mL beaker and dissolve the sample in distilled
water and dilute to about 150 mL before adding about 0.5 mL of concentrated nitric acid.
Then, calculate gram of silver nitrate powder needed to make 150 ml of 0.1 M silver nitrate
solution and heat the sample solution of sodium chloride with constant stirring. Add an
excess of 10% of silver nitrate solution slowly into the sample solution until the coagulation
process stop. During filtration and washing process, pour the solution down a stirring rod the
precipitate should be disturbed as little as possible. To the precipitate in the beaker add about
25 mL of the wash solution, stir well, let the precipitate settle, and decant the solution
through the filter paper. Then, bring the precipitate onto the filter and put into porcelain
crucibles. Use small portions of the wash solution for transfer. During drying and weighing
process, place the crucibles containing the precipitate in a covered beaker in the oven for 1
day at 40 – 50°C. After 1 day, cool the crucibles in the desiccator and weigh. The result for
this experiment is white precipitation and the weight of the silver chloride.
3
METHODOLOGY CHART
1. precipitation

About 0.2 - 0.3 g of sample solid sodium chloride was weighed into a 400 ml beaker.

The sample is dissolved in distilled water and diluted to about 150ml.

About 0.5ml of concentrated nitric acid is added.

The amount of silver nitrate required to make 150ml of 0.1M silver nitrate solution is
calculated.

The sodium chloride solution is heated to boil with constant stirring.

An excess of 10% of silver nitrate solution is added slowly until the coagulation process
stops.

The precipitation is let to settle. Completion of precipitation is tested by carefully adding


a few drops of silver nitrate to clear the supernatant liquid.
The beaker with its contents was covered with aluminum foil and left standing on the
desk for 1 hour.

4
4
2. Filtration and washing of the precipitate

The solution was decanted and poured down a stirring rod.

About 25ml of the wash solution is added to the precipitate left in the beaker and stirred
well.

The solution is decanted through a filter paper after the precipitate is settled.

The precipitate was brought onto the filter paper onto a porcelain crucible.

3. Drying and weighing of the precipitate

The crucible containing the precipitate is placed in the oven for 4 days at 40-50°C.

The crucible is cooled and weighed.

5
RESULTS

TABLE 1
Sample Mass (g)
Mass of filter paper 0.5638
Mass of AgCL and filter paper 1.2447
Mass of precipitate AgCl 0.6809

Actual AgCl weight = 1.2447g – 0.5638g


= 0.6809.g

6
DISCUSSION

1. Explain the function of wash solution (HNO3) during washing step.

During this experiment, AgCl may form that has the ability to capture impurities.
These contaminants could adsorb onto the surface of precipitate. We avoid the
peptization phenomenon by washing the precipitate with diluted nitric acid.

2. Calculate the percentage of chloride in the sample.


݉ܽ

‫ݏݏ‬ ‫݈ܥ݃ܣ‬
ܰ ‫ܾ݁݉ݑ‬ ‫ݎ‬ ݉‫ݏ ܾ݁݉ݑ‬ ‫݊݅ ݈ܥ‬ ‫=݈ܥ݃ܣ‬ ݉ܽ
݉݉ܽ ‫ݎ‬ ‫݈ܥ݃ܣ ݏݏ‬

= 0.6809 g
143.32 g/mol

= 0.00475 mol

‫ܽܯ‬ ݉ܽ
‫ݏݏ‬ ‫ ݈ܥ‬− = ݊‫ܾ݁݉ݑ‬ ‫ݎ‬ ݉‫ݏ ܾ݁݉ݑ‬ ‫ ݈ܥ‬− × ݉݉ܽ ‫ݎ‬ ‫ݏݏ‬ ‫ ݈ܥ‬−

= 0.00475 mol × 34.45 g


mol

= 0.1636 g
݉ܽ

‫݉ܽݏ‬ ‫݈ܥ ݏݏ‬−
% ‫݊݅ ݈ܥ‬ ‫ܾ݁݉ݑ‬ = ݉ܽ ‫݉ܽݏ‬ × 100%
‫ݏݏ‬ ܰܽ‫ܾ݁݉ݑ ݈ܥ‬

= 0.1636 g × 100 %
0.3 g

= 54.53 %

3. How to obtain large precipitate during the experiment?

To obtain large precipitate, we need to use a slow addition of the precipitating agent
to keep the concentration low during the reaction. The solution needs to be stir while
boiling it during the addition of the precipitating agent to avoid concentration
gradients and ensure uniform precipitation.

7
CONLUSION

From the experiment, we can conclude that in analytical chemistry, gravimetric analysis is a
quantitative technique that measures the mass of a sample to ascertain the concentration of a
given material. Stoichiometry and mass conservation are the foundational ideas of
gravimetry. Of all the macro quantitative analysis techniques, gravimetric is also one of the
most precise and accurate. For recommendation, observer should always wear gloves while
handling chemical to avoid the absorption of chemicals through the skin and pores, which can
lead to chronic skin conditions.
10

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