Appendix 02. Lab Report Example 1

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Appendix 2.

Lab Report Example 1


Construction of water-phenol phase diagram
Full Name: Do Thi Huong
Student ID: 20171234
Group: 12
Partners: Le Yen Linh, Bui Thi Thu Thao
Instructor: Dr. Nguyen Van Anh

Abstract
The miscibility of two liquids depends on the interactions between their molecules. Complete miscibility
forms a homogeneous solution. This experiment tested a hypothesis that phenol and water are partially
miscible and aimed to determine their critical solution temperature. Different composition mixtures of
the two compounds were prepared. The temperatures at which the mixtures turned from turbid to clear
and vice versa were recorded and plotted against composition. The maximum point on the fitting curve
was taken as the critical solution temperature. The obtained result, 69.4 degrees Celsius, is slightly
higher than that recorded in the literature. Certain errors might be minimized by generating more
statistical points.

I. Introduction
The miscibility of two liquids depends on their intermolecular attraction forces. For two liquids to be
completely miscible, the attraction force between two molecules of the same kind must approximately
equal to those between two molecules of different kinds. If two liquids are not completely miscible, the
degree of difference in their intermolecular forces determines whether they are partially or completely
immiscible.
Two partially miscible liquids may become completely miscible at higher temperatures. As the
temperature increases, the intermolecular forces of the two liquids decrease and can be reduced to
roughly equal values. The temperature above which two partially miscible liquids become fully miscible
is called the critical solution temperature (CST). Each pair of partially miscible liquids has its own
characteristic CST at atmospheric pressure [1, 2].
This experiment investigated the mutual miscibility of phenol and water. The former is an important
precursor to numerous materials and pharmaceutical products. The latter is the most widely used solvent
in daily life and industry. The purpose of the experiment was to construct a water-phenol phase diagram
and to determine the critical solution temperature of the system. The hypothesis to be tested was that the
mutual miscibility of phenol and water would vary with temperature, and above a certain temperature,
phenol and water would be fully miscible at any concentrations.

II. Methodology
Phenol-water mixtures were prepared from distilled water and a phenol 90% aqueous solution (stock
solution). Nine clean and dried glass test tubes were labeled 1, 2, 3, 4, 5, 6, 7, 8, and 9. Two pipettes
were used to draw and transfer the liquids to the test tubes. The amounts of liquids that were added to
the test tubes are presented in Table 1. Phenol drawing and transferring were done in the fume hood to
avoid inhaling the phenol vapor. All the obtained test tubes were sealed carefully with parafilm and
aluminum foils. The appearance of the mixture in each test tube, whether homogeneous or
heterogeneous, was recorded.
Table 1. Composition of phenol-water mixture
Test tube number 1 2 3 4 5 6 7 8 9
Volume of water (mL) 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0
Volume of phenol 90% aqueous solution 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0
(mL)
The mutual miscibility of phenol and water was recorded by heating the prepared mixtures and
observing their appearance change. A water bath was prepared by adding about 400 mL of distilled
water into a 500-mL glass beaker. A thermometer was placed in the beaker to measure the water bath
temperature. The test tubes were dipped and gently shaken in the water bath such that the liquid levels
in the test tubes were lower than the water level in the beaker. The beaker was heated up gradually using
a hot plate (Figure 1). The temperature at which the mixture in each test tube turned from turbid to clear
was recorded as Tclear . After that, the beaker was removed from the hot plate. During natural cooling,
the temperature at which the mixture in each test tube turned from clear to turbid was recorded as Tturbid .
Room temperature and atmospheric pressure were also recorded.
The water-phenol phase diagram was constructed by plotting phase-transition points versus phenol
weight percentages. The phase transition temperature (Ttrans ) of the mixture in each test tube was
calculated by Eq. 1 as follows:
Tclear +Tturbid
T!"#$%. = 2
(Eq.1)

The weight percent of phenol was calculated by Eq. 2 as follows:


Vstock ×dstock ×Cstock
%phenol=100× V (Eq. 2)
stock ×dstock +Vwater ×dwater

Where Vstock , dstock , and Cstock are the volume, density, and concentration of the stock solution,
respectively. Vwater and dwater are the volume and density of distilled water. At 22ºC, the density of the
stock solution and water are 1.07 g/cm3 and 1.00 g/cm3, respectively.
A trendline was fitted to the processed data points using Microsoft Excel. The maximum point of the
obtained curve was taken as the CST of phenol-water system [3].

(1)

Figure 1. Apparatus setup


(1) Hot plate, (2) Beaker, (3) Test tube, (4) Aluminum foil, (5) Thermometer.

III. Results
As presented in Figure 2, the water-phenol phase diagram is an inverted U-shaped curve and fits a
quadratic trendline y = - 0.03x2 + 2.4x + 25.77 with an R2 of 0.99. Solving this equation gives a
maximum value at (40; 69.4). This data indicates that the CST of phenol-water system is 69.4oC. Extra
observations are presented in Table 2. The detailed experimental data is presented in Table A1,
Appendix 1.
80
y = -0.03x2 + 2.40x + 25.77
70 R² = 0.99
60

Temperature (oC) 50
40
30
20
10
0
0 10 20 30 40 50 60 70 80
Concentration of phenol (wt.%)

Figure 2. Limited miscibility diagram of phenol-water system

Table 2. Extra observations


Parameters Observation
Room temperature (oC) 22
Atmospheric pressure (mmHg) 760
Mixtures in test tubes numbered 1 – 8: colorless and
transparent but layered
Appearance of phenol-water Mixture in the test tube numbered 9: colorless,
mixtures at room temperature transparent, and homogeneous
Phenol 90% aqueous solution: colorless, transparent, and
homogeneous

IV. Discussion
Phenol and water are soluble in each other only at specific concentrations at room temperature. Liquid
mixtures in test tubes numbered 1 to 8 were initially colorless and transparent but separated into two
layers. However, the stock solution and the liquid mixture in the test tube numbered 9 are colorless,
transparent, and homogeneous. The phenol concentrations of these two solutions are 90% and 76%,
respectively, which are higher than those of the other eight solutions. These observations indicate that
phenol and water are partially miscible.
The range of phenol-water insoluble compositions contracts gradually with increasing temperature and
ends at about 66.8 to 67.3oC (Appendix A1). The contraction of this range is rather symmetrical and
smooth. It builds a quadratic curve with a maximal point of 69.4oC. Above this point, phenol and water
are soluble in each other at any concentration. The decrease of intermolecular attraction forces at
increasing temperature can be applied to explain these observations. Above 69.4oC, water-water,
phenol-phenol, and water-phenol intermolecular attraction forces are approximately equal.
The obtained CST is slightly higher than that recorded in the literature, 66.6oC [1], implying that
experimental errors might occur. By tracking back the experimental procedure, at least three factors
could be the causes of errors. Firstly, on cooling, the mixtures become opalescent before turning turbid,
making transition identification inaccurate. Secondly, there might be mismatches between transition
noticing moments and thermometer reading moments. Thirdly, the phenol used to prepare the stock
solution might not be highly purified. The presence of impurities might profoundly affect the CST.
Possible solutions to minimize the first two errors are to prepare more mixture compositions and repeat
the experiment for better statistical data.

V. Conclusion
Phenol and water are partially miscible at room temperature. They form an inverted U-shaped phase
diagram. Their mutual miscibility varies with temperature by a quadratic equation. The critical solution
temperature obtained from the fitting curve is 69.4oC. It is slightly higher than the value reported in the
literature. Possible errors include inaccurate identification of the transition points, mismatches between
transition noticing moments and thermometer reading moments, and the presence of impurities in the
stock solutions. Preparing more mixture compositions and repeating the experiment might help to
minimize the first two mentioned errors.
References
[1] P. W. Atkins and J. de Paula, Atkins' Physical Chemistry. OUP Oxford, 2014.
[2] Dao Van Luong, Nhiet dong hoa hoc [Chemical thermodynamics], (in Vietnamese), 2 ed. Nha
xuat ban khoa hoc ky thuat, 2004.
[3] Cao Hong Ha et. al., Thi nghiem hoa ly [Physical chemistry laboratory manual], (in Vietnamese).
Nha xuat ban Bach Khoa Ha Noi, 2020.

Appendix 1. Raw and Processed Experimental Data


Table A1. Raw and processed experimental data
Volume of Weight
Test Volume
phenol 90% percent of
tube of water Tclear (oC) Tturbid (oC) Ttrans (oC)
aqueous phenol in
number (mL)
solution (mL) mixture (%)
1 5.0 1.0 16 54.5 54.0 54.3
2 4.5 1.5 24 66.0 65.5 65.8
3 4.0 2.0 31 67.0 66.5 66.8
4 3.5 2.5 39 67.5 67.0 67.3
5 3.0 3.0 47 66.0 65.5 65.8
6 2.5 3.5 54 55.0 54.5 54.8
7 2.0 4.0 61 46.5 46.0 46.3
8 1.5 4.5 69 31.5 31.0 31.3
9 1.0 5.0 76 Colorless, transparent, and
homogeneous at room temperature
90
(22oC) on the day of the experiment
Nouns
appearance /əˈpɪə.rən t  s/ bề ngoài miscibility /mɪsɪˈbɪlɪti/ sự tan lẫn
beaker /ˈbiː.kə r / bình tam giác mismatch /ˌmɪsˈmætʃ/ sự không phù
hợp
composition /ˌkɒm.pəˈzɪʃ. ə n/ thành phần mixture /ˈmɪks.tʃə r / hỗn hợp
compound /ˈkɒm.paʊnd/ họp chất molecule /ˈmɒl.ɪ.kjuːl/ phân tử
concentration /ˌkɒn t .s ə nˈtreɪ.ʃ ə n/ nồng độ observation /ˌɒb.zəˈveɪ.ʃ ə n/ sự quan sát
curve /kɝːv/ đường cong pipette /pɪˈpet/ pi pét
density /ˈden t  .sɪ.ti/ mật độ plate /pleɪt/ đĩa
error /ˈer.ə r / sai số precursor /ˌpriːˈkɜː.sə r / tiền thân
factor /ˈfæk.tə r / yếu tố pressure /ˈpreʃ.ə r / áp suất
former /ˈfɔː.mə r / cái trước product /ˈprɒd.ʌkt/ sản phẩm
hypothesis /haɪˈpɒθ.ə.sɪs/ giả thuyết purpose /ˈpɜː.pəs/ mục đích
identification /aɪˌden.tɪ.fɪˈkeɪ.ʃ ə n/ sự xác định solution /səˈluː.ʃ ə n/ dung dịch
impurity /ɪmˈpjʊə.rɪ.ti/ tạp chất solvent /ˈsɒl.vənt/ dung môi
industry /ˈɪn.də.stri/ công nghiệp system /ˈsɪs.təm/ hệ thống
interaction /ˌɪn.təˈræk.ʃ ə n/ sự tương tác trendline /ˈtrendlaɪn/ đường xu
hướng
latter /ˈlæt.ə r / cái sau tube /tjuːb/ ống
liquid /ˈlɪk.wɪd/ chất lỏng vapor /ˈveɪ.pə r / hơi
literature /ˈlɪt. ə r.ɪ.tʃə r / tài liệu volume /ˈvɒl.juːm/ thể tích
material /məˈtɪə.ri.əl/ vật liệu

Adjectives
atmospheric /ˌæt.məsˈfer.ɪk/ khí quyển mutual /ˈmjuː.tʃu.əl/ lẫn nhau
characteristic /ˌkær.ɪk.təˈrɪs.tɪk/ đặc trưng numerous /ˈnjuː.mə.rəs/ nhiều
complete /kəmˈpliːt/ hoàn toàn pharmaceutical /ˌfɑː.məˈsuː.tɪ.k ə l/ dược phẩm
critical /ˈkrɪt.ɪ.k ə l/ tới hạn quadratic /kwɒdˌræt.ɪk. / bậc hai
heterogeneous /ˌhet. ə r.əˈdʒiː.ni.əs/ không đồng smooth /smuːð/ trơn, nhẵn
nhất
homogeneous /ˌhɒm.əˈdʒiː.ni.əs/ đồng nhất statistical /stəˈtɪs.tɪ.k ə l/ thống kê
immiscible /ɪˈmɪs.ə.b ə l/ không tan lẫn symmetrical /sɪˈmet.rɪ.k ə l/ đối xứng
intermolecular giữa các transparent /trænˈspær. ə nt/ trong suốt
phân tử
miscible tan lẫn turbid /ˈtɜː.bɪd/ đục

Verbs
add /æd/ thêm investigate /ɪnˈves.tɪ.geɪt/ nghiên cứu
aim /eɪm/ nhằm mục label /ˈleɪ.b ə l/ dán nhãn
đích
avoid /əˈvɔɪd/ tránh measure /ˈmeʒ.ə r / đo đạc
become /bɪˈkʌm/ trờ nên mention /ˈmen. t  ʃ ə n/ nhắc tới
calculate /ˈkæl.kjʊ.leɪt/ tính toán minimize /ˈmɪn.ɪ.maɪz/ giảm thiểu
contract /ˈkɒn.trækt/ co lại observe /əbˈzɜːv/ quan sát
depend /dɪˈpend/ phụ thuộc obtain /əbˈteɪn/ thu được
determine /dɪˈtɜː.mɪn/ xác định plot /plɒt/ vẽ sơ đồ
dip /dɪp/ nhúng prepare /prɪˈpeə r / chuẩn bị
distill /dɪˈstɪl/ chưng cất present /prɪˈzent/ trình bày
draw /drɔː/ hút, rút record /rɪˈkɔːd/ ghi lại
fit /fɪt/ phù hợp separate /ˈsep. ə r.ət/ phân tách
form /fɔːm/ tạo thành shake /ʃeɪk/ lắc
generate /ˈdʒen. ə r.eɪt/ tạo ra transfer /trænsˈfɜː r / chuyển sang
increase /ɪnˈkriːs/ tăng vary /ˈveə.ri/ thay đổi
indicate /ˈɪn.dɪ.keɪt/ biểu thị weaken /ˈwiː.k ə n/ làm yếu

Adverbs
completely /kəmˈpliːt.li/ hoàn toàn partially /ˈpɑː.ʃ ə l.i/ một phần
gradually /ˈgræd.jʊ.li/ từ từ

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