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EXPERIMENT 4:

DETERMINATION OF VOCS IN AMBIENT AIR BY


UNIVERSITI TEKNOLOGI MARA | FACULTY CHEMICAL ENGINEERING | EH2257C

USING GAS CHROMATOGRAPHY


Degreaser
GROUP 9:
Nurnabila Maisarah Binti Idros 2018693608
Aimy Lyana Binti Ahmad 2018264826
Muhammad Afiq Bin Fadzil 2018287834
T H E T R UT H AB O U T VO C

BACKGROUND OF STUDY
In ambient air, volatile organic compounds (VOCs) derive from different sources that are
biogenic and anthropogenic (human activity) [1]. Volatile organic compounds can be found
especially in degreasers and lubricants that was released in ambient air. As these cleaners include
hazardous chemical entities, many existing grease and oil removers have become increasingly
subject to regulatory restrictions and customer avoidance. Why? These are harmful, carcinogenic
and/or ozone depleting compounds [2]. Degreasing basically requires the removal of grease from
a surface or substrate that is usually performed by using detergents, alkaline solutions and/or
poisonous chemical agents such chromates, phenols and cresols. Due to their toxicity, the use of
such degreasing agents is highly undesirable and usually involves special handling, storage and
disposal [3].
T H E T R UT H AB O U T VO C

BACKGROUND OF STUDY
There are two types of degreasers commonly available in Malaysia which are WD-40 and W-4 and
can be found at a store called “Mr. DIY”. Both of these products will be used as samples for this
experiment.
Conventional degreasers like WD-40 and W-4 may contain VOC such as Methyl Chloroform,
Trichloroethylene, Perchloroethylene [5][6][7], Xylene and Carbon Dioxide [4][8][9][10].
Exposure to degreasers will cause health problems whether through inhalation, ingestion, skin
contact or eye contact. Swallowing a large amount of the aerosol can cause gastrointestinal irritation
and nausea.
For this experiment, we are going to use Gas Chromatography for VOC analysis. Analytical gas
chromatogram (GC) is a mixture part separation technique used for the sample usage of degreasers
named WD-40 and W-4. The aim of Gas Chromatography is to obtain information on its VOC
identities and concentration.
Adverse effects to human and
COMPONENT BOILING POINT
environment
VOC COMPONENTS PRESENT IN WD-40 AND W-4
- Affect when inhaled and may pass
through skin High volatility has low boiling point. A liquid with a low boiling point will boil
Methyl Chloroform 74 °C [11] - Exposure can cause headache, faster than liquids with higher boiling points. Much less energy is required to
dizziness, lightheadedness and break the intermolecular bonds of a volatile liquid then those of liquids having
passing out.
higher boiling points.
-Acute inhalation exposure to a very
high concentration produces narcotic
Trichloroethylene 87 °C [12] effects. The lowest boiling points among the components is Carbon Dioxide, meaning
- Increase slightly for levels of total that it has the highest volatility and the molecule will tend to reach the
cholestrol and high density cholestrol detector and form the first peak at response vs retention time graph.
- Irritation of the upper respiratory Meanwhile, the highest boiling point that has the lowest volatility will form as
121 °C [13] tract and eyes, kidnet dysfunction the last peak at the graph.
Perchloroethylene and neurological effects.
- Groundwater pollution Most of the components in WD-40 and W-4 have the adverse effects mostly
- Difficulty in breathing, impaired to human in terms of health. The components affect when inhaled and
function of the lungs, possible produces narcotic effects that also affect the difficulty in breathing, impaired
Xylene 145 °C [14] changes in the liver and kidneys. function of lungs, liver and kidney.
- Can leak into soil, surface water or
groundwater.
Most of the components have high vapor pressure and low rate of adsorption
- Impact human health by which they will easily leaching the soil then reach the groundwater.
displacing oxygen in the
Carbon Dioxide -78.5 °C [15] atmosphere
- Greenhouse
SAMPLE PRODUCTS

Name: WD-40 Name: W-4


Type: Lubricant Spray Type: Anti-Rust Spray
T H E TR U T H A BO U T FA C E M A S K S

Problem Statement
In general, most industrial goods are coated by an indelible grease that can not be
removed from ordinary detergents. As a result, the goods are degraded easily. So, in
order to solve this problem, industrial cleaners and degreaser are on the market like WD-
40 and W-4.

However, these degreasers may contain VOCs that is harmful to humans. The smell
released from these aerosols can give bad effects to the respiratory system of humans.

Thus, the identification of VOCs content in two samples of degreasers (WD-40, W-4)
is carried out in this experiment by using Gas Chromatography to determine the type of
VOCs that is within each of the cleaner samples and the concentration content in both of
the samples.
Objectives
1. To determine the VOC components present in WD-40 and W-4 sample
solution based on retention time of gas chromatography for a qualitative analysis.

2. To obtain the concentration and compare each of the VOCs in both samples
based on gas chromatography for a quantitative analysis.
GAS CHROMATOGRAPHY
EQUIPMENT
Experimental Procedure
1. Open gas Helium valve 3. Allow the GC to reach the starting 5. When temperature reach
and knob from right to condition which are 50°C for oven 250 °C, take the 0.2ɥL of 7. Record and tabulate the data
the left. Push up the temperature and 250 °C for sample sample A by using syringe and that has been displayed from
switch bar upward. inlet temperature. inject into the GC. GC at the computer

2. Switch on the button 4. Spray the first sample, 6. Let the sample run for 20- 8. Repeat step 4 to
of Gas Chromatography WD-40 into a plastic bag and 25 minutes to separate the 6 for sample W-4
(GC) seal it immediately to avoid hydrocarbons completely
vaporization.
Expected Result
Response

Chloroform

Trichloroethylene
Carbon Dioxide

Methyl
Volatility

Perchloroethylene
1. Carbon Dioxide
2. Methyl Chloroform

Xylene
3. Trichloroethylene
4. Perchloroethylene
5. Xylene

Retention Time
Quantitative Analysis
External Standard Method
1. Take the response vs 5. Estimate the concentration
retention time data of 3. Identify and record the height of
of target compound based on
mixture from previous GC VOC component for each
its peak area to get the exact
experiment (WD-40) for concentration and calculate its peak
concentration on the linear
reference area.
graph

2. Next, run standards 4. Prepare a calibration curve 6. Repeat step 1 to 5 to get


of known concentration of Peak area vs. the precise concentration for
of target compound for Concentration for the 3 other VOC compounds in
3 different different data WD-40 and W-4 sample.
concentration value
EXTERNAL STANDARD METHOD

Concentration is directly proportional to area under the peak

1. Run standards of known compound concentration from the 2. Measure the height of the specific VOC. In this case, we are
mixture going to measure the height of compound Z and calculate the
peak area based on each concentration
X X, Y, Z is the X
Z VOC present in Z
the mixture
Y Y

3. Run 3 different concentration of pure compound Z in GC and


plot a graph of Peak Area vs. Concentration.

4. Lastly, the estimated sample concentration of Z can be


determined by substituting the peak area value into the linear
equation that is generated in Excel ( y = mx + c )
CALCULATI
ON
1.
 
Area of peak of component = Height of component
x
Width at half height

2. Percentage of composition:
= × 100%

Where, = area of a peak component


= total area
RAW DATA TABLE (Qualitative Analysis)
Degreaser Sample Retention time Type of VOCs Area Percent of
(min) present (pA.s) composition (%)

WD-40

W-4

RAW DATA TABLE (Quantitative Analysis)


Name of Compound
Unknown Sample
(WD-40/W-4)
Methyl Chloroform Trichloroethylene Perchloroethylene Xylene Carbon Dioxide

Height (mm)

Peak Area (mm2)

Concentration
(g/L)
RAW DATA TABLE (Quantitative Analysis)

Name of Compound
Standard
Sample
Methyl Chloroform Trichloroethylene Perchloroethylene Xylene Carbon Dioxide

Height (mm)

Peak Area (mm2)

Concentration
(g/L)
Alternative 2:
Internal Standard Method
1. Prepare a standard
sample of known 3. Prepare an unknown sample with 5. Repeat step 1 to 4 to get
concentration containing known concentration of internal the precise concentration for
the targeted compound standard and calculate its peak area other VOC compounds in
and internal standard ratio WD-40 and W-4 sample.

2. Next, run standards 4. Determine the


of known concentration concentration of targeted
of target compound compound in unknown
and internal standard sample by using
and calculate its peak mathematical equation
area ratio

 
Example:
SAFETY CONSIDERATION
Fire extinguishers should be provided in area
The plunger in the syringe is very thin. Be storing combustible gases and these should be
careful when using it with our hand before checked periodically
inject our sample into gas chromatograph
injector port and not to apply too much force .
otherwise it will bend and spoil the syringe.
.

Follow the manufacturer's instructions when


installing columns. Glass or fused capillary Compressed gas cylinders should be kept away
columns are fragile. Handle them with care and from heat sources and in any case not
wear safety glasses to protect eyes from flying subjected to temperatures exceeding 50°C
particles while handling, cutting or installing .
capillary columns [11].
.

Turn off and allow heated areas such as the


oven, inlet and detector, as well as connected
hardware, to cool down before touching them.
.
REFERENCES
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bag/solid-phase microextraction/gas chromatography/mass spectrometry (SPME/GC/MS) in ambient and workplace
air,” Bull. Korean Chem. Soc., vol. 23, no. 3, pp. 488–496, 2002.
[2] Ortega, “( 12 ) Patent Application Publication ( 10 ) Pub . No .: US 2010 / 0035098 A1 Patent Application Publication,”
vol. 1, no. 19, pp. 1–5, 2010.
[3] S. Ganguli, M. Y. Prabhakarrao, and A. Mullick, “Patent Application Publication ( 10 ) Pub . No .: US 2008 / 0283851
A1 Patent Application Publication,” U.S. Pat., vol. 1, no. 19, p. US 2008/0280 138 A1, 2008.
[4] D. Out et al., “Safety Data Sheet 1 –,” pp. 1–8, 2018.
[5] B. R. Vaddula, S. Yalla, and M. A. Gonzalez, “Opportunities for the replacement/minimization of selective hazardous
solvents: Applications, concerns and approaches to identify alternatives,” ACS Symp. Ser., vol. 1186, pp. 69–113, 2014.
[6] N. O. Health and S. Commission, “Solvent Vapour,” no. December, 1989.
[7] N. R. Passant et al., “Biodegradability of the Volatile Organic Compound (VOC) emissions from the food, drink and
metal degreasing industries,” Stud. Environ. Sci., vol. 51, no. C, pp. 315–320, 1992.
[8] P. Code, G. Information, T. Assistance, and C. Service, “Safety data sheet 1.,” vol. 14170, no. 14170, pp. 1–9, 2020.
[9] D. Out and P. S. From, “Safety Data Sheet California CARB Compliant,” pp. 5–9, 2019.
[10] N. Y. S. Department of Health, “Volatile Organic Compounds (VOCs) in Commonly Used Products,” pp. 3–5, 2012.
[11] University, M. (2010, November 2). Gas Chromatography Safety Tips. Retrieved from Lab Health and Safety:
https://www.labmanager.com/lab-health-and-safety/11-gas-chromatography-safety-tips-19204#
[12] U. A. Emirates, “Safety Data Sheet .‫ ة[م[ س[[ال ت[[[انايبةرشن‬Safety Data Sheet,” Mater. Saf. Data Sheet, vol. 4, no. 2, pp. 8–
10, 2012.
[13] CISCO Inc., “Safety Data Sheet : Triethylene Glycol in Case of Transportation Emergency Contact :,” no. 800, pp. 1–8.
[14] ValTech Diagnostics Inc., “Xylenes Safety Data Sheet,” vol. 77, no. 58, 2015.
[15] Safety Data Sheet P-4574, “Carbon dioxide SECTION: 1. Product and company identification,” Praxair, p. 9, 2016.
THANK YOU!

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