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Experiment 3 CHM510

This experiment aimed to analyze chlorpyrifos in water samples using solid phase extraction (SPE) and gas chromatography-electron capture detector (GC-ECD). SPE was used to isolate chlorpyrifos from water samples based on its physical and chemical properties. GC-ECD was then used to separate and detect chlorpyrifos due to its halogen functional group. The average concentration of chlorpyrifos found across three samples was 24.73 ppm. The percent recovery of chlorpyrifos using this method was calculated to be 82.42%.

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396 views6 pages

Experiment 3 CHM510

This experiment aimed to analyze chlorpyrifos in water samples using solid phase extraction (SPE) and gas chromatography-electron capture detector (GC-ECD). SPE was used to isolate chlorpyrifos from water samples based on its physical and chemical properties. GC-ECD was then used to separate and detect chlorpyrifos due to its halogen functional group. The average concentration of chlorpyrifos found across three samples was 24.73 ppm. The percent recovery of chlorpyrifos using this method was calculated to be 82.42%.

Uploaded by

Dang Humairah
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EXPERIMENT 3

Analysis of Chlorpyrifos in Water using


Solid Phase Extraction (SPE) and Gas
Chromatography Electron Capture
Detector (GC-ECD)

NAME: DANG HUMAIRAH BT ANUAR

MATRIC NO: 2020989185

CLASS: RAS2453B

DATE OF SUBMISSION: 22/1/2021

LECTURER’S NAME: DR SHARIZAL HASAN


OBJECTIVE

1) To determine the analysis of chlorpyrifos in water by using Solid-phase Extraction


(SPE) and Gas Chromatography-Electron Capture Detector (GC-ECD) methods.
2) To calculate amount of chlorpyrifos in each sample and their percentage of recovery
in average.

INTRODUCTION

Chlorpyrifos is a solid-like white crystal that is also an insecticide. In water, it is not


soluble. This compound is commonly used in houses and fields. This insecticide is used in
households to combat cockroaches, fleas, and termites while on the field, to control ticks on
cattle and to control crop pests as a spray. Solid phase extraction (SPE) is one of the
extraction techniques used to separate solid and liquid phase analytes from the solution. The
compound's separation is based on their physical and chemical properties. The purpose of this
extraction method is to simplify complex sample matrices into less complex compounds,
purify and decrease ion suppression in applications of mass spectrometry. The benefits of
using SPE are lower use of solvents and reagents, separation procedures only require less
steps, and it is safe for protection because it is less exposed to harmful and hazardous agents.
Steps in the performance of SPE are the preparation of the sample, including dilution and pH
modification, cartridge state, loading the sample, then sample elution.

Chlorpyrifos is moderately toxic to humans and exposure induces neurological


consequences due to exposure during pregnancy, such as chronic developmental disabilities,
autoimmune disorders and behavioral growth retardation in infants. Solid-phase extraction
(SPE) is a method of extraction that isolates the analyte from the solution using solid and
liquid phases. It is a sample preparation that is fast and selective. Purification, trace
enrichment, solvent exchange and derivatization are the purposes of using the SPE. High
analyte recovery, analyte concentration, ease of automation and reduction of organic solvent
use are the benefits of SPE. SPE's general procedure is the loading of the solution through the
SPE process, washing away undesired components and eventually washing the desired
analytes into the collection tube with other solvents. The SPE steps are column solving and
balancing, sample loading, interference elution and, finally, analyte elution. The goal of this
experiment is to measure the quantity of Chlorpyrifos and each sample of waste water and
also the percentage of recovery.
PROCEDURE

a)      Filter Water Sample Through A Glass Fibre Filter Paper


It was prepared well by Supervisor.

b)      Solid-phase Extraction Procedure


C18 SPE cartridge was conditioned by passing 10 mL of methanol. The cartridge was
rinsed by passing 6 mL of deionized water without applying vacuum. Then, the filtered
water sample was passed through the preconditioned column using a vacuum manifold at
~6 mL per min (about 48 drops min -1). The column should not be allowed to dry during
this sample enrichment step. The column was dried by vacuum for 15 minutes. The
interference was removed by eluting the column with 10 mL of deionized water and the
cartridge was dried by vacuum for 30 minutes. The cartridge was placed into tube rack.
After that, the pesticide was eluted using 5 mL of hexane. The sample was concentrated to
1 mL by blowing down using gentle nitrogen and the sample were sealed by using
parafilm for GC analysis.

c)      Instrument Set-up
Injector Temperature: 280 oC
Detector Temperature: 300 oC
Carrier Gas Flow Rate: 20.0 mL min -1 (Nitrogen)
Column Temperature: Initial Temperature 165 oC for 3 minutes, increase to 260 oC at 3oC
min-1 with final time of 2 minutes

d)      Quantitative Analysis Of Chlorpyrifos


1 µL of sample was injected onto the column. The injection was repeated to get
reproducible peak areas. Then, 1 µL of standard chlorpyrifos were injected and repeated to
get reproducible peak area. The concentrations of chlorpyrifos in the sample were
calculated using the data from standard solution
RESULTS

Injection Concentration Peak Area (Hz*s) Response Factor


(ppm) [ppm/(Hz*s)]

1 30 2.05954e^6 1.4566e^(-5)

2 30 2.05954e^6 1.4566e^(-5)

Average 1.4566e^(-5)

Table 1 shows the Response Factor of Standard Chlorpyrifos


Injection Response factor Peak area Concentration
[ppm/(Hz*s) (Hz*s) (ppm)
Sample 1 1 1.4566e^(-5) 1.19924e 6 17.47
6
2 1.4566e^(-5) 1.18178e 17.21
Average 17.34
6
Sample 2 1 1.4566e^(-5) 1.38315e 20.15
6
2 1.4566e^(-5) 1.36710e 19.91
Average 20.03
6
Sample 3 1 1.4566e^(-5) 2.51821e 36.68
6
2 1.4566e^(-5) 2.53506e 36.93
Average 36.81
Table 2 shows the concentration of Chlorpyrifos for each sample
Chlorpyrifos Average concentration of TOTAL average
each sample (ppm) concentration (ppm)
Sample 1 17.34
Sample 2 20.03 24.73
Sample 3 36.81

Table 3 shows the average concentration of Chlorpyrifos

CALCULATION
Percent recovery of Chlorpyrifos
= (concentration in sample/ concentration of standard) x 100%
= (24.73 ppm / 30 ppm) x 100%
= 82.42%

DISCUSSION
Chlorpyrifos is a product that does not mix well with water but can be combined with
liquids that are oily. The low chlorpyrifos concentration makes it difficult to determine the
sample in the compound, so solid phase extraction (SPE) is used to separate compounds
dissolved from other compounds in liquid mixtures depending on their physical and chemical
properties. Compared to other methods and purification prior to chromatographic
examination, SPE has rapid separation. In SPE, in contrast to the sample matrix, the solid
phase must have greater affinity. By eluting solvent with a greater affinity for the analytes,
the compounds retained on a solid phase may be extracted. Gas chromatography in the
Electron Capture Detector (GC-ECD) is also used in this experiment because halogenated
compounds are analyzed by this method and halogenated compounds are the compounds used
in this experiment. Only analytes containing electronegative functional groups that can
capture electrons like halogens, peroxides, quinones and nitro groups can be identified by
ECD. The weaknesses of ECD use include radioactive components, so that the peak of
analysis can be easily affected. The response factor is used to calculate the number of
chlorpyrifos based on the standard compound in the sample. The mean number of
chlorpyrifos obtained from the outcome is 1.4566e^(-5) ppm/(Hz*s). The calculated
percentage recovery data is 82.42% on average. The SPE must be carefully performed to
extract more chlorpyrifos effectively in order to obtain higher quantities of chlorpyrifos or
percentage recovery.

GC with Electron Capture Detector (ECD) is used in this analysis because the halogenated
compound is the analyte to be analyzed. Only analytes containing electronegative functional
groups that can capture electrons, such as halogens, peroxides, quinones, and nitro groups,
can be identified by ECD. The drawbacks of ECD are that radioactive components are
involved. The sum of chlorpyrifos in samples is determined by using reaction factor formula
that based on the standard compound. In the sample, the median amount of chlorpyrifos is
1.4566e^(-5) ppm/(Hz*s). The calculated rate of recovery is an average of 82.42 percent. The
SPE must be deliberately done to remove more chlorpyrifos successfully in order to achieve
larger concentrations of chlorpyrifos or percentage recovery.
CONCLUSION
Solid phase extraction (SPE) and Gas chromatography in Electron Capture Detector
(GC-ECD) is used in this experiment to analyse chlorpyrifos in water. From the result and
calculation, average amount of chlorpyrifos in sample is 1.4566e−5 ppm/(Hz∗s) and the
percent recovery calculated based on result is 82.42% in average.

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