UNIVERSITI KUALA LUMPUR

MALAYSIAN INSTITUTE OF CHEMICAL & BIOENGINEERING TECHNOLOGY

:
CEB30103
COURSE CODE

: POLLUTION PREVENTION & INDUSTRIAL

COURSE
WASTE MINIMIZATION

SEMESTER / YEAR : JAN 2019

PROBLEM-BASED LEARNING REPORT

Solutions on Minimizing the n-Hexane Loss during Conducting Oil-Solid

Extraction using Soxhlet Extractor

Name ID
1. Amir Shahidul Nillah Bin Abdullah 55214116110
2. Farah Huda Binti Md Reduan 55214117132
3. Hanis Nazirah Binti Mat Rahim 55213117204
4. Mohammad Asri Bin Christopher 55214116181
5. Muhammad Danial Bin Kamarluddin 55214117242
6. Nor Amirah Fakhira Binti Abdul Aziz 55214116102
7. Nur Azzanie Binti Mohammad Zahid 55214117201
8. Nur Fatihah Binti Sukor 55214117171
 TABLE OF CONTENTS

CHAPTER PAGE NO.

TABLE OF CONTENTS i
LIST OF FIGURES ii

SESSION 1
INTRODUCTION 1
UNDERSTANDING PHRASES 1
FACTS 3
CUE RECOGNITION AND PROBLEM STATEMENT 3
BRAINSTROM 4
LEARNING NEEDS 5
DATA COLLECTION AND ANALYSIS 5-6

SESSION 2
DISCUSSION 7-9
THREE SOLUTIONS 10-11
SUGGESTION FOR IMPROVEMENT 11
COMPARISON OF SOLUTION 12-13
CONCLUSION 13

REFERENCE 14

i
 LIST OF FIGURES

FIGURE NO. TITLE PAGE NO.

Figure 1 Soxhlet Extractor Model B-811 2

Figure 2 Molecular Structure of n-Hexane 2

Figure 3 Elaeis Guineensis Palm Oil Tree 2

Figure 4 Moringa Oleifera Tree 2

Figure 5 Accelerated Solvent Extractor 4

Figure 6 Soxhlet Extractor with Label 7

Figure 7 Rotary Evaporator with Label 8

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1.1 Introduction

In this case study, a group of 8 students gathered together to solve the high cost of n-
hexane solvent due to its loss during conducting oil-solid extraction using Soxhlet extractor.
This problem was noticed by the HoS of the Process Engineering Technology Section during
conducting an audit at UniKL MICET process pilot plant. The extractor, modelled as Buchi
Extraction System B-811, consumes a lot of n-hexane solvent, categorized as HPLC grade
from Merck, which cost a high price of RM 235 per 2.5 Liter. The Soxhlet device has 4
extraction units that are operated 6 hours per run, 5 days a week, 52 weeks a year with an
electricity consumption of 3 kWh per hour. Its main use is to determine the oil content inside
oil fruits from plants such as Elaeis guineensis and Moringa oleifera. Meanwhile, the
condenser of the extractor is using tap water as coolant with a water flowrate of 60 L per hour.
Besides that, 10 g of solid sample are used per extraction unit and run requiring 150 mL of n-
hexane as solvent. Based on observation, the loss of n-hexane solvent into the laboratory
environment is 50-60 vol% per run which poses a health and safety hazard. Due to that, the
Soxhlet extractor is operated in a fume cupboard which consumes 0.3 kWh per hour.
Therefore, the HoS of the Process Engineering Technology Section requires the group of 8
students to act as the technical team and come up with solutions to reduce the departmental
spending on n-hexane. It involves suggesting three solutions to minimize the loss of n-hexane
and recommend the most cost effective one in terms of payback time.

1.2 Understanding Phrases

First of all, Soxhlet extractor is a laboratory apparatus used to extract oil content from
a solid sample which was invented back in 1879 by Franz von Soxhlet (Jensen, 2007). Next
is n-hexane solvent. This solvent is categorized as saturated alkane compounds with six
carbon atoms and having only single bonds to each other. The letter “n” at the front of the
hexane is referring to its isomer structure, which means the carbon atoms inside the
compound are connected with each other in a straight line and does not have any branch
(PubChem, n.d.). Meanwhile, HPLC grade refers to the high purity or quality of the prepared
solvent, usually around 95-99.7% purity. Other than that, Elaeis guineensis is a palm oil tree,
while Moringa oleifera is a multipurpose tree that is native to the foothills of the Himalayas in
north-western India (Sefa-Dedeh, 2003) (Arora et al., 2013).

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Figure 1: Soxhlet Extractor Model B-811

Figure 2: Molecular Structure of n-Hexane

Figure 3: Elaeis Guineensis Palm Oil Tree

Figure 4: Moringa Oleifera Tree

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1.3 Facts

Amongst of the fact that were provided are:

1. Cost, n-Hexane : RM 235/ 2.5 L

2. Electrical consumption, Soxhlet : 3.0 kWh/ hr

3. Electrical consumption, Fume cupboard : 0.3 kWh/ hr

4. Time, operation : 6 hr/ day, 5 day/ week, 52 weeks/ year

5. Volume Flowrate, water coolant : 60 L/ hr

6. Mass, solid sample : 10 g/ extractor unit

7. Volume, n-Hexane : 150 mL/ extractor unit

8. Percentage Loss, n-Hexane : 50 – 60 vol%

1.4 Cue Recognition and Problem Statement

For this case study, the Soxhlet extractor used in the pilot plant consumes a lot of n-
hexane, which is a solvent that are very expensive. Plus, for every run, half of the n-hexane
volume are loss, at minimum, during conducting extraction. This big amount of loss has posed
a health and safety hazard to the person conducting the extraction. Therefore, the aim of this
case study are to propose minimum three solutions to minimize the loss of n-hexane, and to
recommend the most cost-effective solution in terms of payback time.

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1.5 Brainstorm

There were three solutions suggested during the brainstorming session. First of all, the
group had suggested to substitute the n-hexane solvent with other solvents that are known to
be used for Soxhlet extractor. According to the given title, there were no specific sample aimed
to be used for the extraction. It was only stated that Elaeis guineensis and Moringa oleifera
are amongst of the plant that are mainly used for the Soxhlet extractor. Plus, it was stated in
the title that “10 gram of sample are used”, backing up the statement that there are no specific
sample used for the extraction. Therefore, the whole group agreed on the assumption made
where the efficiency of the substitute solvents are negligible. There are three solvents
proposed to substitute the n-hexane, namely acetone, ethyl acetate and ethanol.

For the next solution, the group had proposed to change the technology used for
extracting the oil content from the solid sample. Like the previous solution, the group agreed
on the assumption made where the efficiency of the substituted technology is negligible. Thus,
it was suggested to use accelerated solvent extractor.

After that, the group had argued and debated on each other, on where does the loss
of the n-hexane actually occurs. At the end of the argument, the group agreed that most of the
loss of n-hexane happened during the separation of n-hexane solvent from the oil mixture
obtained. The group also agreed that apparatus used for the separation is rotary evaporator.
Therefore, for the third solution, the group had suggested to do audit and changes on the
rotary evaporator, and also on the Soxhlet extractor.

Figure 5: Accelerated Solvent Extractor

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1.6 Learning Needs

At the end of the first discussion, the group had agreed to do data collection and
analysis, to prepare for the next discussion. Amongst them includes the principle of Soxhlet
extractor and rotary evaporator, the capital and operating cost of accelerated solvent extractor,
and the details on the alternative solvents, namely their prices, boiling point, their polarity, and
their Safety Data Sheets.

1.7 Data Collection and Analysis

Price of acetone: RM80.00/L (Lelong.com) Purity: 99.5%

Boiling Point: 56°C Polarity: Non-polar (Hydrophobic)

Safety and hazards:

1. H225: Highly Flammable liquid and vapor [Danger Flammable liquids]

2. H319: Causes serious eye irritation [Warning Serious eye damage/eye irritation]
3. H336: May cause drowsiness or dizziness [Warning Specific target organ toxicity,
single exposure; Narcotic effects]

Price of ethyl acetate: RM6.00/L (Alibaba.com) Purity: 99%

Boiling Point: 74°C Polarity: Non-polar (Hydrophobic)

Safety and hazards:

1. H225: Highly Flammable liquid and vapor [Danger Flammable liquids]

2. H319: Causes serious eye irritation [Warning Serious eye damage/eye irritation]
3. H336: May cause drowsiness or dizziness [Warning Specific target organ toxicity,
single exposure; Narcotic effects]

Price of ethanol: RM 4.20/L (Alibaba.com) Purity: 99%

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Boiling Point: 78°C Polarity: Polar (Hydrophilic)

Safety and hazards:

1. H226: Highly Flammable liquid and vapor [Danger Flammable liquids]

2. H319: Causes serious eye irritation [Warning Serious eye damage/eye irritation]
3. H350: May cause cancer [Warning Carcinogenic effect through ingestion]

Price of n-hexane from other supplier: RM 2.50/L (Alibaba.com)

Purity: 98% Boiling Point: 71°C

Safety and hazards:

1. H226: Highly Flammable liquid and vapor [Danger Flammable liquids]

2. H319: Causes serious eye irritation [Warning Serious eye damage/eye irritation]
3. H350: May cause cancer [Warning Carcinogenic effect through ingestion]

Capital Cost of accelerated solvent extractor: USD 20 000 (Labx.com)

Solvent consumption: 50 mL/ 20 g solid sample

Price of grease: RM 10/kg

Density of grease: 700 kg/m3

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2.1 Discussion

For the second discussion, the group started with explaining the principle of Soxhlet
extractor. This apparatus is consist of three parts, which are the boiling flask, the Soxhlet and
the condenser.

Condenser

Soxhlet

Boiling flask

Figure 6: Soxhlet Extractor with Label

Conducting oil-solid extraction using this apparatus, it starts off with providing the solid
sample into the Soxhlet labelled with the number 5. The solvent, which is n-hexane is also
provided, but inside the boiling flask. The n-hexane is the heated until it boils into gas. The
gas will travel into the condenser through the space labelled with the number 3. As it reached
and stayed in the condenser, the n-hexane gas will be condensed back into liquid. It will fall
into the Soxhlet where the solid sample is located. As the solvent made contact with the solid
sample, the oil content will be dissolved inside the n-hexane. This process keeps on going
until the Soxhlet is full with the mixture of n-hexane and dissolved oil, where eventually they
will overflow at the top of the Soxhlet. The overflow of the mixture will then go back into the

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boiling flask. This process is repeated until the oil content of the solid sample are fully
extracted. After the extraction process ends, the oil content needs to be separated from the
solvent. This will be done by using the rotary evaporator.

Condenser

Boiling flask

Collecting
flask

Figure 7: Rotary Evaporator with Label

Conducting distillation of two types of liquid with different boiling point using rotary
evaporator, it starts of by providing the mixture inside the boiling flask. They are heated until
one of the liquids that has lower boiling point, which is the n-hexane, to boiled into gas. In
order to improve the heating efficiency, the boiling flask is rotated. The n-hexane gas will travel
into the condenser while the oil content stays inside the boiling flask. The solvent will then be
condensed into liquid, and it is captured inside the collecting flask.

After discussing the principle of the equipment, the group started to discuss on the
where the loss of solvent n-hexane is actually occurs. During the discussion, it was agreed by
the group that solvent had loss due to two reasons. For the first reason, a part of the n-hexane
that was in the form of gas, and condensed into liquid at the condenser, has managed to stick
on the surface of both Soxhlet extractor and rotary evaporator, and stayed there as residue.
Second, a part of the n-hexane has managed to escape from the apparatus, both intentionally
and unintentionally, during conducting the extraction and separation via distillation. For the

8
fugitive emission, the group had suggested that it may occurred at the joint of the apparatus.
Meanwhile, for the intentional release of n-hexane, it occurs mostly at the vent located at the
top of the condenser, made to release the pressure inside the system.

Before the group continues to discuss on the solution, the operational cost of the
Soxhlet extractor was calculated first, also the range of the loss during conducting the
extraction. The calculation is as shown below.

Operating cost of Soxhlet extractor

150 mL 4 extraction units RM 235 RM 56.40

Price, n-Hexane = × × =
1 extraction unit 1 time run 2500 mL 1 time run

(3.0 + 0.3) kWh RM 0.218 RM 0.7194 × 6 RM 4.32

Price, Electrical Cost = × = =
1 hr 1kWh 1 hr × 6 1 time run

150 mL 4 extract units 50 vol% RM 235 RM 28.20

Price, Minimum Loss = × × × =
1 extract unit 1 time run 100 vol% 2500 mL 1 time run

150 mL 4 extract units 60 vol% RM 235 RM 33.84

Price, Maximum Loss = × × × =
1 extract unit 1 time run 100 vol% 2500 mL 1 time run

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2.2 Three Solutions

For the substitution of n-hexane, there were three alternative solvents, which are
acetone, ethyl acetate and ethanol. During the second discussion, the group had calculated
the operating price for substituting the solvent. During the calculation, the group had agreed
on the assumption where the volume of the alternative solvent required are equal to the
volume of n-hexane used. The calculation is as shown below.

Price after substituting n-hexane

150 mL required 4 extraction units RM80.00 RM 48.00

Price, Acetone = × × =
1 extraction unit 1 time run 1000 mL 1 time run

150 mL required 4 extraction units RM6.00 RM 3.60

Price, Ethyl Acetate = × × =
1 extraction unit 1 time run 1000 mL 1 time run

150 mL required 4 extraction units RM4.20 RM 2.52

Price, Ethanol = × × =
1 extraction unit 1 time run 1000 mL 1 time run

Meanwhile, for the substitution of Soxhlet extractor with the accelerated solvent
extractor, the group had calculated the capital price of the machine, and also the operating
cost of the solvent used. However, the electrical and other operating cost, such as the
subcomponent cost, are unable to be calculated due to insufficient data regarding the electrical
consumption and others. The calculation is as shown below.

Price after substituting Soxhlet extractor

RM 4.13
Capital Price .= USD 20000 × = RM 82600
USD 1

50 mL required 10 g solid sample RM235 RM 2.35

Price, n-Hexane = × × =
20 g solid sample 1 time run 2500 mL 1 time run

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 Next is the changes made on the rotary evaporator and Soxhlet extractor. This part of
the solutions are mainly aimed to minimize any fugitive emission of n-hexane during the
extraction and distillation processes while they are conducted. The group had suggested to
repair any loose seal, apply grease on the joints of the apparatus and reduce the temperature
of the boiling process. However, during data collection and analysis, the group failed to look
for and specify on the cost involved for repairing any loose seal and reducing the temperature
of the boiling process. Therefore, the only calculation made for this part of the solution is the
cost of grease used for operation. The group had also agreed on few assumptions, which are
the amount of grease used for one-time operation and the type of grease used. The calculation
is as shown below.

Price after changes on the apparatus are made

50 mL required 1 m3 700 kg RM 10 RM 0.35

Price, Grease = × 6 × × =
1 time run 10 mL 1m 3 1 kg 1 time run

2.3 Suggestions for Improvement

During the second discussion, there was also suggestion given to improve the
proposed solutions. The suggestion agreed by the group was to buy n-hexane from other
supplier. The n-hexane has lower purity, manufactured from overseas and cost cheaper. The
calculation is as shown below.

Price after substituting n-hexane

150 mL required 4 extraction units RM2.50

Price, Lower Quality n-Hexane = × ×
1 extraction unit 1 time run 1000 mL
RM 1.50
=
1 time run

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2.4 Comparison of Solutions

After providing minimum of three solutions to minimize the loss of n-hexane, the group
had to chose one solution that has the most cost effective in terms of payback time. In order
to do so, all the solutions had to be compared to each other, not just in terms of their cost, but
from other perspective as well. For example, according to the calculation, the cost of using
lower quality n-hexane seems to be the cheapest. But since it poses greater hazard towards
human health compared to ethanol, therefore, the group had suggested that ethanol is the
best substituent for the n-hexane. However, there are some disadvantage of using it, which
are, ethanol is a polar molecule, which makes it hydrophilic. Therefore, this may effect on the
efficiency of dissolving oil content, which is hydrophobic. Plus, ethanol has the highest boiling
point amongst the others, and this will affect the separation efficiency between the solvent and
the oil content during the distillation process at the rotary evaporator. In addition to that, using
greater temperature at the heating process will also increases the amount of the fugitive
emission. But, since it is cheap and less hazardous compared to the others, the group agreed
to use ethanol as the substituent for n-hexane.

Meanwhile, for the substitution of Soxhlet extractor, in order to find out whether it is
worth it to change the technology to the accelerated solvent extraction, its payback time needs
to be determined. However, it is impossible to calculate the payback time without knowing the
amount of budget given by the HoS of the Process Engineering Technology Section.
Therefore, the group had agreed on the best way to do this, is by using the reduced cost for
the solvent consumption as their amount of budget to get the payback time, as the solvent
consumed for the newer technology is significantly lower than Soxhlet extractor. The
calculation is as shown below.

Payback time for accelerated solvent extractor

RM 56.40 1 time run 5 days 52 weeks RM 14664

Price, n-Hexane, Soxhlet ...= × × × =
1 time run 1 day 1 week 1 year 1 year

RM 2.35 1 time run 5 days 52 weeks RM 611

Price, n-Hexane, Accelerated = × × × =
1 time run 1 day 1 week 1 year 1 year

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 Capital Price RM 826000
Payback Time = =
The Cost that Managed to be Reduced is RM 14664 RM 611
−
Considered as the Budget to Payback the 1 year 1 year
Equipment
= 59 years

After doing some arguments, the group had agreed that substituting the Soxhlet
extractor into newer technology is not worth it, as it requires 59 years for the machine to be
fully payed back by using the money gained after the reduction of solvent used by the newer
technology.

In the other hand, minimizing the fugitive emissions of n-hexane by doing changes on
the Soxhlet extractor and rotary evaporator, has insufficient calculations for them to be
considered as a promising solution. Plus, the efficiency of these changes were failed to be
estimated accurately, which the group had finally agreed on the assumption, that this solution
will only help to reduce 10% of the solvent loss. Even thought, the operating price of grease
used to reduce the fugitive emission on the joints, are really cheap, which is RM0.35 per one-
time run, however, it only contributes small amount of reduction to the loss of solvent, and not
to mention that it poses a chance for contamination on the process during conducting the
extraction and separation via distillation.

2.5 Conclusion

For conclusion, the group had suggested three solutions to minimize the loss of n-
hexane. The first solution was substituting the n-hexane itself with, acetone, ethyl acetate and
ethanol. Other than that, Soxhlet extractor was suggested to be substituted with accelerated
solvent extractor. And finally, the group had proposed to make audits and some changes on
the Soxhlet extractor and the rotary evaporator. After the discussion was done, the group had
agreed that substituting the solvent n-hexane with ethanol is the most cost effective as it is the
cheapest and the least hazardous solvent amongst them all.

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3.0 Reference

Arora, R., Malhotra, P., Sharma, A., Haniadka, R., Yashawanth, H.S., & Baliga, M.S. (2013).
Medical Efficacy of Indian Herbal Remedies for the Treatment of Arthritis. Bioactive
Food as Dietary Interventions for Arthritis and Related Inflammatory Diseases, 45, 601-
617.

Factory Supply Best Price Cas No 141-78-6 Ethyl Acetate 99% Liquid - Buy Ethyl Acetate,141-
78-6,Cas 141-78-6 Product on Alibaba.com. (2019). Retrieved April 22, 2019,

Jensen, W.B. (2007). The Origin of the Soxhlet Extractor. Journal of Chemical Education, 84,
1913-1914.

National Center for Biotechnology Information. PubChem Database. Acetone, CID=180,

https://pubchem.ncbi.nlm.nih.gov/compound/180 (accessed on Apr. 30, 2019).

National Center for Biotechnology Information. PubChem Database. Ethyl acetate, CID=8857,
https://pubchem.ncbi.nlm.nih.gov/compound/8857 (accessed on Apr. 30, 2019).

National Center for Biotechnology Information. PubChem Database. Hexane, CID=8058,

https://pubchem.ncbi.nlm.nih.gov/compound/8058 (accessed on May 3, 2019)

Sefa-Dedeh, S. (2003). Traditional Food Technology. In B. Caballero (2nd Edition)

Encyclopedia of Food Science and Nutrition (pp. 5828-5834). Massachusetts:
Academic Press.

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