CHM510:
Experiment	5	
Analysis	of	Chlorpyrifos	in	water	by	Solid	Phase	Extrac9on	(SPE)	and	
Gas	Chromatography-Electron	Capture	Detector	(GC-ECD)	
	
The	objec9ves	of	this	experiment	is	to	analyse	traces	of	chlorpyrifos	
in	 wastewater	 using	 solid	 phase	 extrac9on	 (SPE)	 and	 Gas	
Chromatography-Electron	Capture	Detector	(GC-ECD)	and	as	well	as	
to	to	calculate	the	percentage	recovery	
	
The	 following	 links	 containing	 procedure	 of	 SPE.	 Please	 watch	 the	
video.	
hGps://drive.google.com/file/d/1daRyVHbRgM0-
KOn8yQ7dhOG0g3pmPZke/view?usp=sharing	
Introduc7on	
•  Solid	phase	extrac9on	(SPE)	is	an	extrac9on	method	that	uses	solid	
   and	 liquid	 phase	 to	 isolate	 analyte	 from	 solu9on.	 It	 is	 a	 rapid	 and	
   selec9ve	sample	prepara9on.	The	purpose	of	using	the	SPE	is	purity,	
   trace	enrichment,	solvent	exchange	and	deriva9za9on.		
•  The	 advantages	 of	 the	 SPE	 over	 liquid-liquid	 extrac9on	 are	 high	
   recovery	analyte,	concentra9on	of	analyte,	ease	of	automa9on	and	
   reduc9on	of	organic	consump9on.		
•  Step	 of	 SPE	 are	 from	 column	 solva9on	 and	 equilibra9on	
   (condi9oning),	 sample	 loading,	 interference	 elu9on	 (washing)	 and	
   lastly	the	analyte	elu9on.	
Solid	Phase	Extrac7on	(SPE)	Procedure		
10	mL	Methanol	                   50	mL	water	sample	            10	mL	deionized	   10	mL	hexane	
6	mL	deionized	water	                                            water	
                   C18	sorbent	                  48	drops/min	
Quan7ta7ve	analysis	of	chlorpyrifos:	
1)  Inject	 1	 μL	 of	 sample	 onto	 the	 column	 and	 repeat	 to	 get	
    reproducible	peak	areas.	
2)  Inject	 1	 μL	 of	 standard	 onto	 the	 column	 and	 repeat	 to	 get	
    reproducible	peak	areas.	
3)  Use	 the	 data	 from	 the	 standard	 solu9on	 to	 calculate	 the	
    concentra9on	of	chlorpyrifos	in	sample.	
Results	and	Discussion:	
•  From	standard	chromatogram,	calculate	the	response	factor	(RF)	by	
   using	the	following	formula:			
•  Then	 calculate	 the	 amount	 of	 chlorpyrifos	 in	 sample	 by	 using	 RF	
   value.	
•  Tabulate	all	the	data	in	appropriate	tables	and	discuss	your	answer.		
Conclusion	
Should	answer	the	objec9ve	of	experiment		
References	
List	of	all	references	used	in	preparing	the	report	
Standard	Chlorpyrifos	(30	ppm)	–	1st	injec7on	
Standard	Chlorpyrifos	(30	ppm)	–	2nd		injec7on	
Standard	Chlorpyrifos	(30	ppm)	–	3rd		injec7on	
Chlorpyrifos	in	Sample	(1st	Injec7on)	
Chlorpyrifos	in	Sample	(2nd		Injec7on)	
Chlorpyrifos	in	Sample	(3rd		Injec7on)