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Experiment 7: ANALYSIS OF CHLORPYRIFOS IN WATER BY SOLID-PHASE

EXTRACTION (SPE AND !AS CHRO"ATO!RAPHY-ELECTRON CAPT#RE

DETECTOR (!C-ECD

D$te %& Experiment: ')*)'+,

!r%p: AS'*. /D+

Le0trer:

DR "ARDIANA SAAID

PROF 1#RAIDAH ABD#LLAH "#NIR

N$me: A"AR SAFWAN BIN "OHD ALI HANAPIAH

St2ent ID: '+.'7''''

!r%p mem3er4:

SAL"A I1ATI BINTI SINAR "ASH#RI ('+.5/6775

N#R#L SHA1REENA BINTI 1#LAFLY ('+.'.5'*,

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Experiment 7: Analysis of Chlorapyrifos in Water by Solid-Phase Extraction (SPE) and Gas

Chromatography-Electron Captre !etector (GC-EC!)

Introduction

Chlorapyrifos

Chlorpyrifos is a crystalline organophosphateinsecticide that acts on the ner"os

system of insects by inhibiting acetylcholinesterase# Chlorpyrifos is moderately toxic

to hmans and the exposre $ill case nerological effects sch as persistent

de"elopmental disorders atoimmne disordersand children mental de"elopment

retard de to the exposre dring pregnancy# %n agricltre& chlorpyrifos remains as

one of the most $idely sed as the pesticide# Solid-phase extraction (SPE) is an

extraction method that ses solid and li'id phase to isolate analyte from soltion# %t

is a rapid and selecti"e sample preparation# he prpose of sing the SPE is to

prify& trace enrichment& sol"ent exchange and deri"atiation# he ad"antages of the

SPE are high reco"ery of analyte& concentration of analyte& ease of atomation and

redction of organic sol"ent consmption# he general procedre of SPE is the

loading of soltion throgh SPE phase& $ash a$ay ndesired components& and

lastly $ash off the desired analytes $ith other sol"ent into the collection tbe# Steps

of SPE are from colmn sol"ation and e'ilibration& sample loading& interference

eltion and lastly& the analyte eltion#

http://en.wikipedia.org/wiki/Organophosphatehttp://en.wikipedia.org/wiki/Insecticidehttp://en.wikipedia.org/wiki/Acetylcholinesterase_inhibitorhttp://en.wikipedia.org/wiki/Insecticidehttp://en.wikipedia.org/wiki/Acetylcholinesterase_inhibitorhttp://en.wikipedia.org/wiki/Organophosphate

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Procedure

*# he $ater sample is filter throgh a glass fibre filter paper#

+# ,or solid-phase extraction procedre& the C* SPE catridge in conditioned by

passing *. m/ of methanol#

0# he 1. m/ filtered $ater sample is passed throgh the preconditioned colmn sing

a "acm manifold at 2 m/ per min (3 drops4min)# the colmn is ma5e sre to not

dry dring sample enrichment step#

3# hen& the colmn is dried by "acm for *1 mintes#

1# he inteference is remo"ed by elting the colmn $ith *. m/ of deionied $ater and

again the "acm is dried for *. mintes#

2# he pesticide is elted sing 1 m/ of hexane# hen& the sample is concentrated to *

m/ by blo$ing do$n sing gentle nitrogen#

6# he instrment is set p for in7ector temperatre is +. oC# he detector temperatre

is set 0.. oC# While& the carrier gas flo$ rate is fixed +.#. m/ min -*sing nitrogen

gas# And the colmn temperatre initially *21 oC for 0 min& then it is increased to +2.

oC at 0 oC min-*$ith a final time of + min#

# he 'antitati"e analysis of chlorpyrifos# ,irstly& * 8/ of sample is in7ected onto the

colmn# he in7ection is repeated to get reprodcible pea5 areas#

9# * 8/ of standard chlorpyrifos is in7ected# he in7ection is repeated to get reprodcible

pea5 area#

*.# sing the data from the standard soltion& the concentration of chlorpyrifos in the

sample is calclated#

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Result

A# Comparison in retention time of standard and samples:

;etention timeof standard

(ppm)

Sample ;etention time of sample(min)

A"erageretention time

of sample

(min)

rial * rial +

2#696 * 2#96. 2#966 2#963

2#696 + 2#92 2#929 2#929

2#696 0 2#922 2#92+ 2#923

?s

C# Amont of chlorpyrifos in sample:Amont of chlorpyrifos in sample = ;, standard @ pea5 area sample

Sample Area (>?s) A"erage

area

(>?s)

Amont of

chlorpyrifos

(ppm)

rial * rial +

* *0*61 *+319 *0*02#1 1#+29

+ **.991 *.2.9 *.9.+ 3#3.0

0 600021 60+*9 600.9+ +9#096

A"erage amont of chlorphyrifos in sample =5.269+4.403+29.397

3

= *0#.+0 ppmPercentage reco"ery of samples:

Percentage reco"ery =amount of chlorpyrifossample

amount of chlorpyrifosstandard 100

Amont of chlorpyrifos in standard = 0. ppm

sample Amont of chlorpyrifos Percentage reco"ery

* 1#+29 *6#12

+ 3#3.0 *3#2

0 +9#096 96#99

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A"erage percentage reco"ery of sample =17.56+14.68+97.99

3

= 30#3*

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Discussion

%n this analysis&GC $ith Electron Captre detector is sed becase the analyte $hich is

chlorpyrifos is to be analysed is halogenated compond& $hich is only EC! can detect

analytes# he EC! contain electronegati"e fnctional grops that can captre electrons sch

as halogens& peroxides& 'inones and nitro grops $hich can detect the analyte

(chlorpyrifos)# he Electron Captre detector (EC!) is it in"ol"e $ith radioacti"e component#

he amont of chlorpyrifos in samples is calclated by sing response factor calclation that

base on the standard compond# he a"erage amont of chlorpyrifos in the sample is

*0#.+0 ppm& that is abot half from the amont of chlorpyrifos in the standard# he

percentage reco"ery calclated is 30#3* in a"erage# %n order to get higher amont of

chlorpyrifos or the percentage reco"ery& the SPE mst be carried ot careflly so it $ill

extract more chlorpyrifos efficiently#

Conclusion

he a"erage amont of chlorpyrifos in the sample is *0#.+0 ppm& $hile the percentage

reco"ery is 30#3* in a"erage#

Reference

*# Solid-Phase Extraction (SPE)# ni"ersity of %oannina# ;etrie"ed at

http:44$$$#oi#gr4research4labs4en"itech4SPE#htm

2. Clorpyrifos& 94.24+.*2& http:44en#$i5ipedia#org4$i5i4Chlorpyrifos#

http://www.uoi.gr/research/labs/envitech/SPE.htmhttp://www.uoi.gr/research/labs/envitech/SPE.htm