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CHM510: Experiment 5: and As Well As To To Calculate The Percentage Recovery

This document outlines an experiment to analyze traces of chlorpyrifos in wastewater using solid phase extraction (SPE) and gas chromatography-electron capture detector (GC-ECD). The objectives are to analyze chlorpyrifos and calculate the percentage recovery. The procedure involves conditioning a C18 sorbent column, loading a 50mL water sample, washing with deionized water, and eluting the analyte chlorpyrifos with hexane. Quantitative analysis involves injecting standard and sample onto the column to calculate the concentration of chlorpyrifos in the sample. Results and discussion will include response factor calculation and tabulating data. The conclusion will answer if the experiment objectives were met.

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441 views16 pages

CHM510: Experiment 5: and As Well As To To Calculate The Percentage Recovery

This document outlines an experiment to analyze traces of chlorpyrifos in wastewater using solid phase extraction (SPE) and gas chromatography-electron capture detector (GC-ECD). The objectives are to analyze chlorpyrifos and calculate the percentage recovery. The procedure involves conditioning a C18 sorbent column, loading a 50mL water sample, washing with deionized water, and eluting the analyte chlorpyrifos with hexane. Quantitative analysis involves injecting standard and sample onto the column to calculate the concentration of chlorpyrifos in the sample. Results and discussion will include response factor calculation and tabulating data. The conclusion will answer if the experiment objectives were met.

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© © All Rights Reserved
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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)

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