TK2102 – ANALYTICAL & MEASUREMENT METHODS

2021/2022

MODULE 43 - TEMPERATURE MEASUREMENT:

THERMOCOUPLE (APPLICATION OF JOULE CALORIMETER) &
GRAVIMETRY ANALYSIS

PRACTICUM REPORT

Arranged By:
A2.2122.60

Ulayya Ardhyanesha Adiprana 13020101

Arvin Raditya Athallah 13020121

Practicum Date: Thursday, 14 April 2022

CHEMICAL ENGINEERING PROGRAM

FACULTY OF INDUSTRIAL TECHNOLOGY
INSTITUT TEKNOLOGI BANDUNG
2022
 ABSTRACT

In this Module 43: Temperature Measurement, the practican were asked to firstly calibrate a
thermocouple using the relationship of the acquired voltage reading from the thermocouple and the acquired
temperature reading from a standard mercury thermometer. This part of experiment used 6 variations of
water temperature, which are iced water at approximately 0℃, boiled water at approximately 83℃, and
mixed water with 4 different temperatures namely 26℃, 30℃, 39℃, and 51℃. After the thermocouple had
been calibrated, its time constant was then calculated to determine its responsivity towards the temperature
change in the measured object. The responsivity was measured for a step change from room temperature
water to iced water (decrement variation) and boiled water (increment variation). The thermocouple was
then utilized to measure a calorimeter heat capacity. This measurement used variations of voltage and
electric current to create heat that transferred into the water inside the calorimeter. The three variations were
using voltages of 7 Volt, 9 Volt, and 11 Volt. Lastly, using different devices, we applied gravimetric
analysis to determine the water quantity inside a solid sample. This analysis was based on the evaporation
of water in an oven and multiple weighing using a digital analytical balance. The total amount of weighing
that was done was 5 times.
The thermocouple calibration resulted in a linear calibration curve. This graph of voltage in mV
over temperature in celsius showed a parallel relationship between the two, meaning that as the voltage
increases, the temperature also increases. The thermocouple time constant is the required time for the sensor
to respond to 63.2% of its total output signal when subjected to a step change in temperature. The resulting
value in this experiment was an average of 18.29 seconds. In the measurement of calorimeter heat capacity,
the process was repeated in three runs with each differing voltage and current income. This resulted in three
different results, which were calculated to be 133.103 J/K in average. Lastly, the gravimetric analysis was
repeated 5-6 times until the weight number shown in the digital analytical balance was no longer declining.
At the end, the calculation result showed the water percentage in the solid sample to be 40.45%

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 CONTENTS

ABSTRACT ................................................................................................................................. ii
CONTENTS ................................................................................................................................ iii
LIST OF FIGURES ....................................................................................................................... v
LIST OF TABLES ....................................................................................................................... vi
CHAPTER 1 ................................................................................................................................ 1
INTRODUCTION ........................................................................................................................ 1
1.1 Background ........................................................................................................................ 1
1.2 Research Question ............................................................................................................... 2
1.3 Experimental Objective ........................................................................................................ 2
CHAPTER II ............................................................................................................................... 3
EXPERIMENTAL BASIC THEORY ............................................................................................. 3
2.1 Thermocouple ..................................................................................................................... 3
2.2 Joule Calorimeter ................................................................................................................ 4
2.3 Gravimetric Analysis ........................................................................................................... 5
CHAPTER III .............................................................................................................................. 7
EXPERIMENTAL METHODOLOGY ........................................................................................... 7
3.1 Tools and Materials ............................................................................................................. 7
3.1.1 Tools ........................................................................................................................... 7
3.1.2 Materials ...................................................................................................................... 7
3.2 Experimental Equipment Series ............................................................................................. 8
3.3 Experimental Diagram ......................................................................................................... 9
3.3.1 Thermocouple Calibration .............................................................................................. 9
3.3.2 Measurement of thermocouple time constant ...................................................................10
3.3.3 Heat Capacity Measurement Using Calorimeter ...............................................................11
3.3.4 Water Content Measurement using Gravimetry Analysis ...................................................12
3.4 Experimental Procedure ......................................................................................................13
3.4.1 Thermocouple Calibration .............................................................................................13
3.4.2 Measurement of Thermocouple Time Constant ................................................................13
3.4.3 Heat Capacity Measurement Using a Calorimeter .............................................................13

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 3.4.4 Water Content Analysis using Gravimetry Analysis ..........................................................14
4.1 Thermocouple Calibration ...................................................................................................15
4.2 Measurement of Thermocouple Time Constant ......................................................................16
4.3 Measurement of Calorimeter Heat Capacity ...........................................................................16
4.4 Gravimetric Analysis: Water Content Measurement ................................................................17
4.5 Discussion .........................................................................................................................18
APPENDIX ................................................................................................................................22
Calculations ................................................................................................................................22
Thermocouple Calibration.........................................................................................................22
Temperature increase calculation: ...........................................................................................22
Temperature decrease calculation: ..........................................................................................23
Calorimeter Heat Capacity ........................................................................................................23
Gravimetric Analysis: Water Content Measurement .....................................................................24

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 LIST OF FIGURES

Figure 2.1.1 Simple Thermocouple Diagram…………………………………………………………….…3

Figure 2.2.1 Thermocouple calibration curve for different types…………………………………………..4
Figure 2.2.2 Simple Joule Calorimeter Diagram…………………………………………………………...5
Figure 3.2.1 Thermocouple Series……………………………………………………………………….…8
Figure 3.2.2 Gravimetry Analysis Equipment……………………………………………………………...8
Figure 3.3.1 Thermocouple Calibration Experimental Diagram…………………………………………...9
Figure 3.3.2 Thermocouple Time Constant Experimental Diagram………………………………………10
Figure 3.3.3 Heat Capacity Measurement Experimental Diagram………………………………………..11
Figure 3.3.4 Water Content Measurement Experimental Diagram……………………………………….12
Figure 4.1.1 Thermocouple Calibration Curve……………………………………………………………15

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 LIST OF TABLES

Table 4.1.1 Temperature and Voltage Measurement……………………………………………………...15

Table 4.2.1 Experimental Data of Thermocouple Time Constant Measurement…………………………16
Table 4.3.1 Calorimeter Time and Temperature Measurement………………………………………...…17
Table 4.4.1 Measurement Data of Gravimetric Analysis………………………………………………….18

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 CHAPTER 1

INTRODUCTION

1.1 Background

In the chemical industry, the temperature is very essential in every process. Each plant has
set its reactor to a specific temperature and pressure for optimal conversion. The temperature must
be taken into account in all processes by process engineers. On the other hand, industrial
procedures are frequently carried out at high temperatures. Instruments like mercury thermometers
and alcohol thermometers are less effective when measuring at extreme temperatures (very high
or low). Other temperature measurement instruments with a larger temperature range and the
ability to achieve high temperatures are required. Thermocouples are a versatile measurement tool
that can be used in a variety of applications.

Utilization of a thermocouple can be used to monitor the temperature with a higher degree
of accuracy than a thermometer. A thermometer can be used to determine the temperature of an
object or an environment. When the thermometer's measurements are limited, the thermometer can
only measure temperatures up to 100°C. Temperature measurement in industry, whether for tin
smelting or similar, necessitates an instrument to measure the temperature, and a thermometer
cannot be used because it only has a range of 0°C to 100°C. One of the most significant
characteristics to assess in order to evaluate the loss or balance of heat energy is temperature.

Thomas Johann Seebeck discovered in 1821 that a conductor made of metal produces an
electric voltage when subjected to a gradient heat differential named the thermoelectric effect
phenomenon. This new conductor will then experience a temperature gradient, with a voltage
change inversely proportional to the temperature difference of the object. Using different
conductors to complete the circuit will result in different voltages, leaving a minor voltage
differential that allows us to collect measurements that rise with temperature. For the range
provided by current metal combinations, this difference typically runs from 1 to 70 microvolts per
degree Celsius. However, it's vital to keep in mind that thermocouples measure the difference in
temperature between two places, not the absolute temperature. In terms of cost, availability,
convenience, melting point, chemical characteristics, stability, and yield, certain combinations
have been established by industry standards.

Gravimetry is an analytical chemistry method for determining the content of a component

that makes up a compound by using a separation procedure. Volatile gravimetry is a sort of
gravimetry that is frequently used to determine a substance's water content. Because it is important
in the industry to obtain a product that is as close to pure as possible, gravimetric analysis can be
used to determine what components and how many components are present in a sample.

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 Gravimetric analysis techniques are divided into four categories. The separation of an
analyte using thermal analytical procedures, such as heating or chemically degrading a sample by
the vaporization of volatile chemicals, resulting in significant mass reduction, is known as
volatilization gravimetry. Precipitation gravimetry is another sort of technique that can be used to
detect the number of ions in a substance by dissolving the component in a solvent. The next type
is thermogravimetry, in which thermogravimetric measurements (TGA) are carried out as a
function of temperature under constant heating circumstances or as a function of time under
constant mass loss and temperature.TGA allows us to investigate the behavior of changing
physical and chemical events, allowing us to quickly estimate the mass loss or gain. Finally,
electrogravimetry is a technique for determining the ion content of metals using electroplating.
Electroplating is done with electrodes, and the mass of the metal is determined by the difference
between the final and initial electrodes after electroplating.

1.2 Research Question

1. How to perform thermocouple calibrations based on the relationship of the voltage and
temperature acquired from the thermocouple?
2. How to calculate the thermocouple time constant?
3. How to calculate heat capacity by measuring the current and voltage of each variation to
increase the temperature of the calorimeter?
4. How to determine the water quantity of a solid sample using analytical gravimetric
measurement?

1.3 Experimental Objective

1. To determine the calibration curve and linear regression of the thermocouple

2. To determine the thermocouple time constant
3. To determine the heat capacity of the calorimeter
4. To determine the water quantity of a solid sample

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 CHAPTER II
EXPERIMENTAL BASIC THEORY

2.1 Thermocouple

The thermocouple is a temperature measurement device made composed of two-conductor

metals joined by a knot or junction. The thermoelectric effect is the name given to this
phenomenon. The Seebeck effect is the difference in voltage at both ends of a conductor at various
temperatures. The change in temperature is proportional to the change in voltage. The
thermocouple time constant is a measurement of the thermocouple's sensitivity to temperature
changes. The temperature measurement tool can be calibrated by comparing the quantity of the
measurement tool to the physical/chemical phenomena occurring in the media. The temperature
(Celcius) of the measured material is used to calibrate a thermocouple by comparing the quantity
of potential difference (mV) measurement obtained with the temperature (mV).

Figure 1. Simple Thermocouple Diagram

(Source: https://www.watelectrical.com/what-is-a-thermocouple-definition-working-principle-diagram-applications/)

After connecting the thermocouple to the substance to be tested, a potential difference will
appear at the ends of the thermocouple that is directly proportional to the observed temperature
gradient. This can be seen in the following equation:

𝑑𝑉 = 𝐾(𝑇)𝑑𝑇
Where:
● dV= measure voltage potential difference
● K(T)= Seebeck coefficient by a function of temperature
● dT= measured temperature gradient

Because the temperature measured by the thermocouple is not an absolute temperature, a

thermocouple calibration curve must be used to calibrate the thermocouple. An example of a
thermocouple calibration curve is as follows:

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 Figure 2. Thermocouple calibration curve for different types
(source: https://www.digikey.com/en/articles/designing-thermocouple-applications-with-a-sensor-afe)

There will be an increase or drop in temperature and voltage when a thermocouple is

immersed in the liquid to be monitored. As a result of this, a temporal constant emerges. The time
it takes to attain 63.2 percent of the final output voltage is the time constant. The thermocouple's
accuracy and reaction time are represented by the time constant. The time constant expresses the
time difference between a temperature change and a voltage change. Thermocouples offer an edge
over mercury thermometers when it comes to temperature measurement as a thermocouple's
measuring range is substantially larger than that of a mercury thermometer, reaching 1500 degrees
Celsius. findings are also given digitally whereas traditional thermometers use manual
determination which may be less accurate and more succumbed to human error. Temperature
measurement using a thermocouple delivers more accurate results and is easier to read.
Thermocouples also have a faster response time when the temperature of an object changes

2.2 Joule Calorimeter

A calorimeter is a device that measures the amount of heat required for calorimetry.
Calorimetry is a branch of science concerned with determining the condition of an object in terms
of its thermal properties in order to investigate its physical and chemical changes. This calorimeter
is constructed up of a metal vessel made of electrically conductive elements like copper and
aluminum. To minimize heat loss to the environment, this metal jar with a stirrer is housed in an
insulating jacket. A thermometer can only be placed through one hole to measure changes in its
thermal characteristics.

Electrical energy is utilized to raise the temperature of the water and the calorimeter
because Joule calorimeters are usually connected to a power source, and electrical energy is energy
that will subsequently be used as a source of heat energy flowing through the calorimeter. The heat

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absorbed by the water and calorimeter, as well as the heat given by the power source, can be
expressed as follows:

𝑄= 𝑚 𝑤𝑎𝑡𝑒𝑟 ∗ 𝑐𝑝 𝑤𝑎𝑡𝑒𝑟 ∗ 𝛥𝑇 + 𝑐 𝑐𝑎𝑙𝑜𝑟𝑖𝑚𝑒𝑡𝑒𝑟 ∗ 𝛥𝑇

Where the energy absorbed by the calorimeter can be calculated by the equation:

𝑄 = 𝑉∗𝑖∗𝑡

Where:
● m = Substance’s Mass (kg)
● Cp = Heat Capacity of substance that’s inside the Calorimeter (J/kg.deg C)
● Ccalorimeter = Calorimeter’s Heat Capacity (J/deg C)
● ∆𝑻 = Change of Temperature
● Q = electrical energy (joule)
● V = potential difference (volt)
● t = time (seconds)

Figure 3. Simple Joule Calorimeter Diagram

(source: https://university.listenlights.com/2018/02/07/joules-law-heating/)

The quantity of heat required to raise the temperature of the calorimeter per unit
temperature, in this example per degree Celsius, is referred to as heat capacity. It is assumed that
the electrical energy flowing through the calorimeter will be transformed into heat energy.

2.3 Gravimetric Analysis

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 Gravimetry is a chemical analytic method to determine the quantity of a certain substance
or component that is known by measuring the weight of a component when it is pure after a
separation process. There are 4 type of gravimetry analysis method, which include Precipitation
gravimetry which is an analytical technique that uses a precipitation reaction to separate ions from
a solution and uses the formation and mass of a precipitate to determine the mass of an analyte,
where the precipitate must have a low solubility, high purity, and known composition if its mass
is to accurately reflect the analyte's mass and be easy to separate from the reaction mixture. Then,
By heating or chemically degrading the sample, we can separate components of our mixture using
volatilization gravimetry. Any volatile molecules are separated out by heating or chemical
decomposition, resulting in a change in mass that we can measure. Then there is Electrogravimetry
which is a technique for electroplating a metal onto a platinum electrode in a quantitative manner.
Finally, the miscellaneous physical method which involving changes in the phase of the analyte to
separate it from the rest of a mixture, resulting in a change in mass. Gravimetry analysis is tied
with the change of an element whose contents are made into a pure compound that is stable and
can be changed into a shape that can be measured.

The following formula is used to determine the liquid analyte content within a solid sample by
heating and drying it repeatedly using the volatilization gravimetry method:

𝑤𝑖𝑛 −𝑤𝑜𝑢𝑡
𝑊𝑎𝑡𝑒𝑟 𝐶𝑜𝑛𝑡𝑒𝑛𝑡 (%𝑤𝑡) = ∗ 100%
𝑤0 − 𝑤𝑒𝑚𝑝𝑡𝑦

Where:
● Win = Initial mass of evaporating dish with sample before heating (gr)
● Wout = Final mass of evaporating dish with sample final heating. (gr)
● Wo = mass of evaporating dish with sample (gr)
● Wempty = mass of evaporating dish without sample (gr)

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 CHAPTER III

EXPERIMENTAL METHODOLOGY

3.1 Tools and Materials

3.1.1 Tools
● Thermocouple
● Glass Beaker 400 mL
● Voltmeter
● Amperemeter
● Stopwatch
● Joule Calorimeter
● Mercury Thermometer
● Oven
● Evaporating Dish
● Water Bath
● Crucible Tongs
● Desiccator
● Analytical Scale
● Spatula
● Measuring cylinder 100 mL

3.1.2 Materials
● Tap Water
● Aqua DM
● Ice Water
● Boiling Water
● Gravimetry Analysis Sample (zeolite)

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3.2 Experimental Equipment Series

Figure 4. Thermocouple Series

(Source: https://www.watelectrical.com/what-is-a-thermocouple-definition-working-principle-diagram-applications/)

The measurement junction, which is the end of the meeting between two different types of
metal where the temperature is detected, is explained in the thermocouple circuit diagram above.
The temperature at which a thermocouple is used as a reference temperature. A heat source is just
that: a heat source. Finally, the Voltmeter is used to determine the voltage differential between two
network points. Within the measuring temperature range, the aforementioned set of gadgets must
be calibrated. The voltage at the end of the temperature range and numerous locations between
that range is measured with a thermocouple, and the voltage calibration curve is then plotted
against the temperature measured by the thermometer. Connecting the multimeter and ammeter to
the measuring instrument, which was assembled in parallel and series correspondingly, was the
first step in assembling the circuit based on the experiment technique. The output voltage was then
measured using connecting cables from the measurement equipment to the calorimeter to
determine the temperature via electrical heating.

For the gravimetry Analysis, several types of equipment were used to complete the
experiment which are the evaporating dish, oven, crucible tongs, desiccator, and analytical scale.

Figure 5. Gravimetry Analysis Equipment

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3.3 Experimental Diagram

3.3.1 Thermocouple Calibration

Figure 5. Thermocouple Callibration Experimental Diagram

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3.3.2 Measurement of thermocouple time constant

Figure 5. Thermocouple Time Constant Experimental Diagram

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3.3.3 Heat Capacity Measurement Using Calorimeter

Figure 6. Heat Capacity Measurement Experimental Diagram

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3.3.4 Water Content Measurement using Gravimetry Analysis

Figure 7. Water Content Measurement Experimental Diagram

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3.4 Experimental Procedure

3.4.1 Thermocouple Calibration

1. Measure laboratory conditions (T, P).

2. Measure the temperature of iced water and boiling water with a mercury
thermometer.
3. Record the freezing and boiling temperatures of water measured by the
thermometer at laboratory pressure and the voltage recorded from the thermocouple
measurements.
4. Prepare 4 additional calibration points in the range of 20 – 70 °C by mixing hot
water and cold water (ice).
5. Plot the temperature curve measured by the thermometer against the measured
voltage on measurements using a thermocouple to obtain a linear equation of
thermometer calibration

3.4.2 Measurement of Thermocouple Time Constant

1. Prepare hot water at a temperature of 40 °C in a beaker.

2. Dip the thermocouple in the heated water.
3. Record the measured voltage every second when the thermocouple is immersed.
4. Perform similar steps to measure the thermocouple response to decreasing
temperature. Use ice water in this variation.

3.4.3 Heat Capacity Measurement Using a Calorimeter

1. Pour 150 mL of aqua dm into the calorimeter,

2. Assemble the system according to the schematic.
3. Record the initial temperature of the system (measure with a thermometer) and the
measured voltage on the thermocouple.
4. Set and record the incoming voltage and current.
5. Activate the stopwatch.
6. When the temperature reaches the desired T stop the stopwatch; note the time
needed to reach the T.
7. Turn down the supply voltage, and unplug the thermocouple wire.
8. Replace the aqua dm contained in the calorimeter.
9. Repeat the experiment with variations in the incoming voltage and current (do it
with 5 voltage variations in this measurement from the 5-15 volt range).
10. Other data that must be recorded PLab, Tlab, water mass, and calorimeter mass.
Water heat capacity and water density are prepared by the practitioner.

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3.4.4 Water Content Analysis using Gravimetry Analysis

1. Weigh the mass of an empty evaporating dish that has been cleaned and dried, and
weigh 2 to 3 times to get more accurate data.
2. Weigh the mass of the evaporating dish that has been filled with the sample, and
weigh 2 to 3 times to get more accurate data.
3. Put the evaporating dish containing the sample into the oven using crucible pliers
(not to be touched by hands) at a temperature of ±100°C – 105° for 10 minutes.
4. Remove the dish using pliers and put it in a desiccator for 5 minutes.
5. Transfer the dish to the analytical balance using crucible pliers (must not be touched
by hands) and re-weigh the mass of the cup and record the mass of the cup,
weighing 2 to 3 times to get more accurate data.
6. Repeat heating (steps 3 to 5) until it has been done 4 times.

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 CHAPTER IV

EXPERIMENTAL RESULTS AND DISCUSSION

4.1 Thermocouple Calibration

At first, we measured laboratory conditions at 12.56 pm which showed 26℃ for temperature and
694 mmHg for pressure. Then, we proceed for water temperature measurement in six different
calibration points. These points are ice water, boiling water, and four random temperatures in the range
of 20-70℃. The measurement itself was done using mercury thermometer and thermocouple, with
obtained data as presented below:

Table 4.1.1 Temperature and Voltage Measurement

From the data, we can form a relation curve between measured temperature and voltage which will
become the thermocouple calibration curve. The x-axis represents temperature while the y-axis is for
voltage. The mentioned calibration curve can be seen in the graph below:

Figure 4.1.1 Thermocouple Calibration Curve

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 Based on the graph above, the resulting calibration equation is

y = 0.8614x + 278.84

If the variables are changed into the experiments’, the equation becomes

V(mV) = 0.8614T(℃) + 278.84

4.2 Measurement of Thermocouple Time Constant

In this part of the experiment, we measure the thermocouple's response time towards temperature
changes. The temperature changes are a decrement using iced water and an increment using boiled
water. The iced water was marked as 0℃ while the boiled water was 83℃. This response time
would show the measurement’s time constant, which is the required time for the sensor to respond to
63.2% of its total output signal when subjected to a step change in temperature. The quality of a
thermocouple is better with a smaller time constant value because it would need less time to reach a
constant value when measuring temperature.
The initial voltage of boiled water in increment variation was 308.8 mV while the initial voltage
of iced water in decrement variation was 297 mV. And then, the data recording was done until the
number shown in thermocouple reading was constant. The resulting voltage is marked as Vf which
has a value of 349.7 mV for increment variation and 279.9 mV for decrement variation.
From calculation using the formula
Vt = Vo + 63.2%(Vf-Vo)
we obtained the Vt values for increment was equal to 334.58 mV and for decrement was equal to
286.26 mV. These values were then interpolated using the experimental time and voltage data. From
here we got the increment time constant as 16.52 s and the decrement time constant as 20.06 s. With
the two values being averaged, the thermocouple time constant is 18.29 s.

Table 4.2.1 Experimental Data of Thermocouple Time Constant Measurement

4.3 Measurement of Calorimeter Heat Capacity

This measurement used 150 ml of water to fill the calorimeter. With the lab condition that is
assumed to be standard, we take the value of 997.08 kg/m³ for water density and 4184 J/g.K for
water heat capacity. The experiment itself was done in three runs in which the water was changed for
each run. The used voltages for all runs were in the range of 6-12 Volt. Each run went on for 10
minutes where a temperature increment was measured.

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 Table 4.3.1 Calorimeter Time and Temperature Measurement

From this data, we can calculate calorimeter heat capacity using the formula
𝑄𝑖𝑛 = 𝑄𝑜𝑢𝑡

𝑉 × 𝐼 × 𝑡 = 𝑚𝑤𝑎𝑡𝑒𝑟 × 𝐶𝑝𝑤𝑎𝑡𝑒𝑟 × 𝚫𝑇 + 𝐶𝑝𝑐𝑎𝑙𝑜𝑟𝑖𝑚𝑒𝑡𝑒𝑟 × 𝚫𝑇

𝑉 × 𝐼 × 𝑡 − × 𝐶𝑝𝑤𝑎𝑡𝑒𝑟 × 𝚫𝑇
𝑚𝑤𝑎𝑡𝑒𝑟
𝐶𝑝𝑐𝑎𝑙𝑜𝑟𝑖𝑚𝑒𝑡𝑒𝑟 =
𝚫𝑇
And we obtained different results between run 1 to 3, which are 53.43 J/K, 71.99 J/K, and 273.89 J/K
respectively. Finally, the average calorimeter heat capacity is 133.103 J/K.

4.4 Gravimetric Analysis: Water Content Measurement

Water content measurement is based on the mass difference between before and after heating
occurs. The heating itself was done in an oven with a temperature of 150℃ for around 10 minutes.
After that, the sample was cooled down in a desiccator for around 5 minutes for its use is to protect
hygroscopic materials or materials that react with water from humidity. Moreover, every displacement
of the sample in an evaporating dish was done using a crucible tong to prevent additional humidity
from human skin from transferring to the surface of the dish. Each process of weighing itself was done
three times to make sure the measurement is accurate. At last, the whole process from heating to
weighing was repeated 5-6 times until the final weight was no longer declining. The obtained
measurement data is presented in the table below:

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 Table 4.4.1 Measurement Data of Gravimetric Analysis

From the data above, the mass of sample can be calculated by subtracting mass of evaporating
dish+sample by mass of empty evaporating dish, which resulted in the value of 4.2207 gram. After 75
minutes, the final sample mass can be done by subtracting the average final mass in the last interval
by the mass of empty evaporating dish, which gives the value of 2.5136 gram. Lastly, to calculate the
water content in the sample, we can use the formula:
𝑖𝑛𝑖𝑡𝑖𝑎𝑙 𝑠𝑎𝑚𝑝𝑙𝑒 𝑚𝑎𝑠𝑠 − 𝑓𝑖𝑛𝑎𝑙 𝑠𝑎𝑚𝑝𝑙𝑒 𝑚𝑎𝑠𝑠
𝑊𝑎𝑡𝑒𝑟 𝑝𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 (%𝑤𝑡) = × 100%
𝑖𝑛𝑖𝑡𝑖𝑎𝑙 𝑠𝑎𝑚𝑝𝑙𝑒 𝑚𝑎𝑠𝑠
and we obtain the water percentage value of 40.45%

4.5 Discussion
Thermocouple calibration is done to compare the temperature measurement result from a standard
mercury thermometer and a thermocouple. The used mercury thermometer has a reference temperature
of 0℃ (water melting point) and 100℃ (water boiling point) so that it can be considered as a
standardized measurement device. However , the measurement itself was not exactly done at the exact
points due to the rapid change of temperature in the laboratory.

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The resulting calibration curve shows that the measured temperature is parallel to the measured
voltage. This is aligned with the Seeback effect,

The line itself is very close to a linear and has no outliers, which can be considered as a quite good
experiment result. Nevertheless, there were noises that we could not ignore which disturbed the
sensitivity of the thermocouple itself.
Secondly, we measured the thermocouple time constant by recording the thermocouple response
time. This response time would show the measurement’s time constant, which is the required time for
the sensor to respond to 63.2% of its total output signal when subjected to a step change in temperature.
The quality of a thermocouple is better with a smaller time constant value because it would need less
time to reach a constant value when measuring temperature. From the experiment and calculation, we
obtain the average time constant value of 18.29 seconds. Again, the result might not be so accurate
due to the present noises in the laboratory.
Thirdly, a calorimeter heat capacity measurement was done. That heat capacity is the amount of
heat which a calorimeter would absorb. In this part of the experiment, we use the principle of energy
balance, where we subtract the heat produced by electricity by the heat absorbed by water. Water mass,
water heat capacity, and temperature variation would affect the number of absorbed heat by water.
Meanwhile, voltage, current, and interval would affect the number of produced heat by electricity.
With 3 variations of voltage, we obtained 3 different results. This might happen due to the imperfect
isolation in the calorimeter which causes a heat transfer from the calorimeter to the environment. In
addition, the incoming current was not constant (there were slight deviations along the time interval).
This resulted in a non homogeneous distribution of heat in the water inside of the calorimeter. At last,
we obtained the average calorimeter heat capacity value of 133.103 J/K.
Last, we did a gravimetric analysis to measure water content in a sample. The analysis is based on
water evaporation through a heating process using an oven with a temperature around 150℃. The
heating itself was done for 10 minutes before the sample was then placed inside a desiccator for 5
minutes. The sample placement in the desiccator was absolutely necessary, not only to cool down the
sample, but also because the sample’s hygroscopic characteristic enhanced after it was heated. All of
the displacement of the dish was done using a crucible tong. This is useful to protect the practican
from getting a skin burn and also to preserve the original sample mass (not even added by the littlest
humidity in practican’s hand). In the end, we can see that weight trend was decreasing with the addition
of heating repetition. When the weight had finally showed a relatively flat trend, we concluded that
the experiment was done and we calculated the water percentage in the sample which was 40.45%.

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 CHAPTER V

CONCLUSION AND SUGGESTION

5.1 Conclusion
Based on this experiment, there are few conclusions that we acquaire, which are:
5.1.1 In thermocouple calibration, we obtained the linear regression equation equals to
y = 0.8614x + 278.84 with R² equals 0.998. If it is translated into the variables of thermocouple,
the equation becomes V(mV) = 0.8614T(℃) + 278.84
5.1.2 The obtained thermocouple time constant for the increment variation was 16.52 seconds, while
for the decrement variation was 20.06 seconds. The average time constant value is 18.29 seconds
5.1.3 The obtained calorimeter heat capacity value for voltage variation of 7 V, 9 V, and 11 V was
53.43 J/K, 71.99 J/K, and 273.89 J/K respectively. The average calorimeter heat capacity value
is 133.103 J/K.
5.1.4 The calculated water percentage in the solid sample is 40.45%

5.2 Suggestion
Based on the experimental result and discussion, we came up with a few suggestions that might be
taken into consideration:
5.2.1 The devices in the laboratory, especially the thermocouple set, must be maintenanced well to
reduce the equipment error
5.2.2 Practican need to be more precise regarding the timing and measuring to reduce human error

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 REFERENCES

Geankoplis, C.J. 2003. Transport Processes and Separation Process Principles. New Jersey: Pearson
Education, Inc.

Van Ness, H.C., J.M. Smith, M. M. Abbot. 2005. Introduction to Chemical Engineering Thermodynamics
(7th Edition). Boston: McGraw-Hill.

Pollock, Daniel D. 1971. The Theory and Properties of Thermocouple Elements. Philadelphia: American
Society for Testing and Materials.

Skoog, Douglas., Douglas M. West., F James Holler. 1996. Fundamentals of Analytical Chemistry (7th
Edition). Fort Worth: Saunders College Publishing Harcourt Brace.

Reklains, G.V. 1942. Introduction to Material and Energy Balances. New York: John Wiley and Sons.

21
 APPENDIX

Calculations

Thermocouple Calibration

To calibrate the thermocouple star by measuring the voltage by:

𝑉𝑡 = 𝑉𝑜 + 63.2%(𝑉𝑓 − 𝑉𝑜)
Where:
Vt = Voltage
Vo = Initial voltage
Vf = final voltage

Once the voltage has been calculated, we interpolate the data to find the time constant by:

𝑡𝑐 − 𝑡𝑎 𝑉𝑡 − 𝑉𝑎
=
𝑡𝑏 − 𝑡𝑎 𝑉𝑏 − 𝑉𝑎
Where:
tc = time constant
tb and ta = time within tc
Va and Vb = voltage within Vt

Once the time constant for both the increase and decrease of temperature has been calculated,
average both to acquire time constant.

Temperature increase calculation:

22
Temperature decrease calculation:

Averaging both time constants will give an average of 18.29 seconds.

Calorimeter Heat Capacity

We first calculate the mass of water using the given density and volume of water used in the
experiment by:

We then use the energy balance to formulate an equation to calculate the capacity of the calorimeter
by:

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Calculations are done for each variation of voltage at 7, 9, and 11 volts respectively:

Where the average heat capacity is 133.1 J/K

Gravimetric Analysis: Water Content Measurement

First, a calculation is performed to determine the empty cup's average mass. The three mass
weighings of empty plates in the experiment yielded exactly the same results, i.e. 20.0391 grams.
As a result, the average weight is 20.0391 grams. The sample mass is then calculated.

Then we can calculate the water content in the sample by:

𝑖𝑛𝑖𝑡𝑖𝑎𝑙 𝑠𝑎𝑚𝑝𝑙𝑒 𝑚𝑎𝑠𝑠 − 𝑓𝑖𝑛𝑎𝑙 𝑠𝑎𝑚𝑝𝑙𝑒 𝑚𝑎𝑠𝑠

𝑊𝑎𝑡𝑒𝑟 𝑝𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 (%𝑤𝑡) = × 100%
𝑖𝑛𝑖𝑡𝑖𝑎𝑙 𝑠𝑎𝑚𝑝𝑙𝑒 𝑚𝑎𝑠𝑠

24