Experiment 7: ANALYSIS OF CHLORPYRIFOS IN WATER BY SOLID-PHASE
EXTRACTION
(SPE) AND
GAS
CHROMATOGRAPHY-ELECTRON
DETECTOR (GC-ECD)
Date of Experiment: 20/4/2016
Group: AS245 3D1
Lecturer:
DR MARDIANA SAAID
PROF ZURAIDAH ABDULLAH MUNIR
Name: AMAR SAFWAN BIN MOHD ALI HANAPIAH
Student ID: 2015272222
Group members:
SALMA IZATI BINTI SINAR MASHURI (2015839778)
NURUL SHAZREENA BINTI ZULKAFLY (2015258246)
CAPTURE
Experiment 7: Analysis of Chlorapyrifos in Water by Solid-Phase Extraction (SPE) and Gas
Chromatography-Electron Capture Detector (GC-ECD)
Introduction
Chlorapyrifos
Chlorpyrifos is a crystalline organophosphate insecticide that acts on the nervous
system of insects by inhibiting acetylcholinesterase. Chlorpyrifos is moderately toxic
to humans and the exposure will cause neurological effects such as persistent
developmental disorders autoimmune disorders and children mental development
retard due to the exposure during pregnancy. In agriculture, chlorpyrifos remains as
one of the most widely used as the pesticide. Solid-phase extraction (SPE) is an
extraction method that uses solid and liquid phase to isolate analyte from solution. It
is a rapid and selective sample preparation. The purpose of using the SPE is to
purify, trace enrichment, solvent exchange and derivatization. The advantages of the
SPE are high recovery of analyte, concentration of analyte, ease of automation and
reduction of organic solvent consumption. The general procedure of SPE is the
loading of solution through SPE phase, wash away undesired components, and
lastly wash off the desired analytes with other solvent into the collection tube. Steps
of SPE are from column solvation and equilibration, sample loading, interference
elution and lastly, the analyte elution.
Procedure
1. The water sample is filter through a glass fibre filter paper.
2. For solid-phase extraction procedure, the C18 SPE catridge in conditioned by
passing 10 mL of methanol.
3. The 50 mL filtered water sample is passed through the preconditioned column using
a vacuum manifold at 6 mL per min (48 drops/min). the column is make sure to not
dry during sample enrichment step.
4. Then, the column is dried by vacuum for 15 minutes.
5. The inteference is removed by eluting the column with 10 mL of deionized water and
again the vacuum is dried for 10 minutes.
6. The pesticide is eluted using 5 mL of hexane. Then, the sample is concentrated to 1
mL by blowing down using gentle nitrogen.
7. The instrument is set up for injector temperature is 280 oC. The detector temperature
is set 300 oC. While, the carrier gas flow rate is fixed 20.0 mL min -1 using nitrogen
gas. And the column temperature initially 165 oC for 3 min, then it is increased to 260
o
C at 3 oC min-1 with a final time of 2 min.
8. The quantitative analysis of chlorpyrifos. Firstly, 1 L of sample is injected onto the
column. The injection is repeated to get reproducible peak areas.
9. 1 L of standard chlorpyrifos is injected. The injection is repeated to get reproducible
peak area.
10. Using the data from the standard solution, the concentration of chlorpyrifos in the
sample is calculated.
Result
A. Comparison in retention time of standard and samples:
Retention time
of
Sample
Retention
standard
time
of
sample
(min)
Average
retention
(ppm)
of
time
sample
(min)
6.797
6.797
6.797
Trial 1
6.970
6.968
6.966
1
2
3
Trial 2
6.977
6.969
6.962
6.974
6.969
6.964
B. Calculation of response factor for standard compound:
amount
peak area
Response Factor (RF) =
=
30
748063
4.01 10
ppm/Hz*s
C. Amount of chlorpyrifos in sample:
Amount of chlorpyrifos in sample = RF standard peak area sample
Sample
1
2
3
Area (Hz*s)
Trial 1
138175
110995
733365
Trial 2
124598
108609
732819
Average amount of chlorphyrifos in sample =
Average
Amount
area
chlorpyrifos
(Hz*s)
(ppm)
131386.5
109802
733092
5.269
4.403
29.397
of
5.269+ 4.403+29.397
3
= 13.023 ppm
Percentage recovery of samples:
Percentage recovery =
amount of chlorpyrifossample
100
amount of chlorpyrifosstandard
Amount of chlorpyrifos in standard = 30 ppm
sample
1
2
3
Amount of chlorpyrifos
5.269
4.403
29.397
Percentage recovery
17.56
14.68
97.99
Average percentage recovery of sample =
17.56+ 14.68+ 97.99
3
= 43.41%
Discussion
In this analysis, GC with Electron Capture detector is used because the analyte which is
chlorpyrifos is to be analysed is halogenated compound, which is only ECD can detect
analytes. The ECD contain electronegative functional groups that can capture electrons such
as halogens, peroxides, quinones and nitro groups which can detect the analyte
(chlorpyrifos). The Electron Capture detector (ECD) is it involve with radioactive component.
The amount of chlorpyrifos in samples is calculated by using response factor calculation that
base on the standard compound. The average amount of chlorpyrifos in the sample is
13.023 ppm, that is about half from the amount of chlorpyrifos in the standard. The
percentage recovery calculated is 43.41% in average. In order to get higher amount of
chlorpyrifos or the percentage recovery, the SPE must be carried out carefully so it will
extract more chlorpyrifos efficiently.
Conclusion
The average amount of chlorpyrifos in the sample is 13.023 ppm, while the percentage
recovery is 43.41% in average.
Reference
1. Solid-Phase Extraction (SPE). University of Ioannina. Retrieved at
http://www.uoi.gr/research/labs/envitech/SPE.htm
2. Clorpyrifos, 9/06/2016, http://en.wikipedia.org/wiki/Chlorpyrifos.
