Experiment 7

Analysis of Chlorpyrifos in Water by Solid-Phase

Extraction (SPE) and Gas Chromatography - Electron
Captured Detector(ECD)
Name: Hamizan Bin Hashim
Matrix number: 2014960875
Group member:
1.Nur Liyana binti Zainal
2.Siti Shazwani binti Salim *
3.Siti Nur binti Inani Baharuddin
Group: AS2453D1
Lecturer name: Prof Madya Zuraidah Abdullah Munir
Date: 7.4.2015

Introduction:
In this experiment, gas chromatograpgy-electron capture detector(GC-ECD) was use to
determine amount of chlorpyrifos in water sample. Chlorpyrifos is a crystalline
organophospahte insecticide that acts on the nervous system of insects. It is moderately
toxic to humans and the exposure can cause neurological effects such as persistent
developmental disorder. Solid-phase extraction(SPE) method was used to extract
chlorpyrifos in water sample. Sample was loading through SPE, wash away undesired
components and purify with other solvent into collection tube. By using SPE the
concentration of analyte are highly recovery and reduction of organic solvent cosumption.

Figure 1: strusture of chlorpyrifos

Experimental:
A. Solid-phase extraction procedure:
1. 10mL of methanol was let to be passed the C18 SPE cartridge to active the
column.
2. 6mL of deionized water was let be passed through the cartridge.
3. 50mL of filtered water sample was let to be passed through the preconditioned
column using vacuum about 48-55 drops/min. The column should be not allowed
dry during sample enrichment step.

B. Instrument set-up:
Injector temperature: 280C
Detector temperature:300C
Carrier gas flow rate: 20.0mL/min (nitrogen)
Column temperature: initial temperature 165C for 3 minutes, increase to 260C at
3C/min with final time of 2 minutes.

C. Quantitative analysis of chlorpyrifos:

1. 1L of sample was injected onto the column and get the reproducible peak area.
2. 1L of standard chlorpyrifos was injected and repeated to get reproducible peak
area.
3. By using data from standard solution, concentration of chlorpyrifos in sample
were calculated.

Result and discussion:

A. Comparison in retention time of standard and samples.

Concentrati
on of
standard
(ppm)

30

Sample

Retention time of
sample(min)

Area (Hz*s)

Trial 1

Trial 2

Trial 3

Trial 1

Trial 2

Trial 3

average

6.926

6.925

6.924

4.345

4.843

5.178

4.79

6.925

6.924

6.925

6.104

6.349

6.477

6.31

6.925

6.924

6.925

4.629

4.631

4.671

4.64

B. Calculation of response factor for standard compound.

Response factor(RF) =
RF = 30 / 9.5214

amount of sample(std)
peak area

RF= 3.1507

C. Amount of chlorpyrifos in sample:

Amount of chlorpyrifos in sample = RF std x peak area sample.
= 3.1506 x 4.79
=15.09 ppm
Sample

Average area (Hz*s)

Amount of
chlorpyrifos(ppm)

4.79

15.09

6.31

19.88

4.64

14.62

Average amount of chlorpyrifos

in sample =

15.09 19.88 14.62

3
= 16.69 ppm

D. Percent of recovery of samples:

Percent recovery = x
100%

amount of chlorpyrifos in sample

amount of chlorprifos in standard

Amount of chlorpyrifos in standard 15.09 = 30 ppm

Amount of chlorpyrifos in sample 1 30 = 16.69 ppm
Percent recovery = x 100% = 50.30 %

Sample

Amount of chlorpyrifos in
sample (ppm)

Percentage recovery
(%)

15.09

50.30

19.88

66.27

14.62

48.73

Average percent recovery of 50.30 66.27 48.73

sample = = 55.10 %
3
Discussion:
Electron Captured Detector(ECD) was used in this GC experiment because it is suitable
to analyses halogen compound. ECD only can detect analytes that contain electronegetive
functional groups that can captured electron. In this experiment, Chlorpyrifos is
halogenated compound that can captured the electron. There are disadvantage use of
ECD, it involve radioactive component. The amount of chlorpyrifos in sample was
calculated using response factor calculation that base on chlorpyrifos standard. As the
amount calculated, the average amount of chlorpyrifos in sample 16.69 ppm. The percent
recovery calculated was 55.10 %. Low percent of recovery sample might of the
contaminate while SPE carried out. To get high percent of recovery SPE must be carried
out carefully.

Conclusion:
At the end of the experiment, the average amount of chlorpyrifos in sample was
determined there is 16.69 ppm. The percentage recovery is 55.10 %.

Reference:
1. Norashikin S., Ruziyati T., Mardiana S. (2012), Analytical Separation Methods
Laboratory Guide (2nd edition), 3/10/2014.
2. Mardiana Saaid, Electron-Capture Detector (ECD) lecture notes.
3. http://npic.orst.edu/factsheets/chlorpgen.html