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Tittle
Analysis of Chloropyrifos in Water by Solid Phase Extraction (SPE) and Gas
Chromatography-Electron Capture Detector (GC-ECD).
Abstract
A pesticide multiresidue method for determining dichlorvos, naled. lindane, diazinon.
chlorpyri-fos-methyl, dichlofluanid, chlorpyrifos, folpet, and -endosulfan, endosulfansulphate, fen-propathrin and acrinathrin in water samples at the levels required by the EEC
Drinking Waters Directive has been developed. The pesticides were selected among the most
used during die last 20 years in Almeria (Spain), where there is a high agricultural activity.
Solid Phase Extraction (SPE) was selected as extraction method after being compared with
Liquid-Liquid Extraction (LLE).
Solid Phase Extraction (SPE) is becoming popular to extract pesticides from may
sample matrices. This method is more economical and few operational steps are required for
the extraction process when compared to liquid-liquid extraction. In the study, C-18 bonded
silica was utilized as a solid phase to extract pesticides form water. Water samples (500 ml)
were passed through the C-18 cartridges (500 mg) at a constant flow rate (12 ml/min) using
vacuum manifold. Adsorbed analytes were eluted with ethyl acetate and analysed by
GC/ECD, NPD. Acceptable recoveries (range: 80% -120%) were obtained for alachlor,
captan, chlorpyrifos, diazinon, profenophos and oxyfluorfen.
Several liquid-liquid extraction methods have been developed to determine
organohelide and organophosphate pesticides and these are time consuming methods.
Dichloromethane is the most commonly used solvent for the extraction processes. Discharge
of dichloromethane to the environment is a serious air pollution issue.
The aim of this work was to apply the SPME technique for determining two important
pesticides (chlorpyrifos and chlorpyrifos-methyl) in waste water and to show the effective
application of SPME methods for determining these residues.
applying vacuum.
The filtered water sample (50 mL) was passed through the preconditioned
column using a vacuum manifold at ~ 6 mL per min (48 drops per min).
iv.
v.
The column was not allowed to dry during this sample enrichment step.
The column was dried by vacuum for 15 minutes.
After that, the interference was removed by eluting the column with 10 mL
vi.
of deionized water. Then, again the catridge was dried for 10 minutes.
Lastly, the pesticide was eluted using 5 mL of hexanee. By blowing down
using gentle nitrogen, the sample was concentrated to 1 mL. The sample
was ready for GC analysis.
: 280 C.
: 300 C.
: 20.0 mL min-1 (nitrogen).
iv.
Column temperature
iii.
Results
a. Comparison in retention time of standard and samples
Retention time of standard
Sample.
(ppm).
Retention time of
Average retention
sample (min).
time of sample
(min).
1
2
3
6.722
Trial 1
6.723
6.724
6.724
Trial 2
6.724
6.723
6.724
6.724
6.724
6.724
Area (Hz*s)
Amount of
chlorpyrifos (ppm)
1
2
3
Trial 1
485893
507099
624548
Trial 2
519338
506456
667543
502615
506777
646045
44.87
45.24
57.67
1
2
3
(ppm)
44.87
45.24
57.67
149.57
150.80
192.23
So, we had do some further learning to find out what is the error for our experiment.
Data may be wrong because the chromatographer uses his equipment only 8 hours per day,
switches off energy and gases and restarts his equipment without the early morning test.
The latter can be just a well selected quantitative test mixture to be injected together with a
non sorbed but detectable inert gas, may be methan. The quantitative test values must
correlate with with late evening value which means it is a good idea to check the whole
working period per day by inclusion into two test run values. Each column has a limited
working range for the nature of substances : their molecular weight, their polarity, their
temperature stability. As the majority of all quantitative GC analyses is done by temperature
programming we have working range limits for the low starting temperature, the upper end of
the temperature program and the heating rate. For isocratic GC the selection of the column
temperature is limited by working ranges. The higher quantity of chlorphyrifos that our group
got because of the waste water that had been collected at the area which is freshly spray with
insectices. We assumed that, the insecticide was absorbed by the soil and water was flow in
them.
Conclusion
As the conclusion, the average amount of chlorpyrifos in sample is 49.26 ppm and the
percentage recovery is 164.2 %.
References
1.
2.
3.
4.
http://npic.orst.edu/factsheets/chlorpgen.pdf
https://www.epa.gov/ingredients-used-pesticide-products/chlorpyrifos
http://www.interchromforum.com/html/qnt_err_gc.html
Analytical Separation Methods laboratory Guide, 2nd Edition, n.d, Norashikin Saim,
Ruziyati Tajudin and Mardiana Saaid.
Appendix
1. Calculation of responce factor (RF) of standard compund.
Rf =
= 11 202 ppm/Hz*s
2. Calculation of amount of chlorpyrifos in sample.
Sample amount (1) =
Peak area
R f standard
502615
11202
= 44.87 ppm
Sample amount (2) =
506777
11202
= 45.24 ppm
Sample amount (3) =
646045
11202
= 57.67 ppm
3. Average amount of chlorpyrifos.
=
44.87+ 45.24+57.67
3
= 49.26 ppm
4. Percentage recovery of samples.
Sample (1) =
amount of samples
100
amount of standard
44.87 ppm
100
30 ppm
= 149.57%
Sample (2) =
45.24 ppm
100
30 ppm
= 150.80%
Sample (3) =
57.67 ppm
100
30 ppm
= 192.23%
5. Average percentage recovery of samples.
= 164.20%