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1.
This method is suitable for the determination of γ-chlordane and α-chlordane content in solid waste leachate
Second, the principle of the method
Chlordane in the extract was extracted with dichloromethane , and the extract was dehydrated, dried, concentrated, purified, changed solvent, and fixed to volume with anhydrous sodium sulfate, and then separated and separated by a gas chromatograph with an electron capture detector (ECD).
3.
(1) Ultra-pure water: No experimental interference, can be purchased or prepared in the laboratory
(2) Dichloromethane : pesticide residue level
(3) N-hexane : pesticide residue level
(4) Anhydrous sodium sulfate : pure superior grade
(5) Sodium chloride: pure superior grade
(6) Concentrated sulfuric acid : pure superior grade
(7) Concentrated nitric acid : pure superior grade
(8) Extractant: Add a mixture of concentrated sulfuric acid and concentrated nitric acid with a mass ratio of 2:1 to ultrapure water (approximately 2 drops of 1L water) to make the pH 3.
(9) Standard solution γ-Chlordane: ρ=100ug/mL; α-Chlordane: ρ=200ug/mL
Four, instruments and equipment
(1) Gas chromatograph: with electron capture detector (ECD)
(2) Chromatographic column:
Front column: HP-17 (30m×0.
Back column: HP-5 (30m×0.
(3) Concentration device: equipment with equivalent performance such as nitrogen blowing concentrator and rotary evaporator
.
(4) Extraction bottle: 2L PTFE jar with screw cap and inner cap
.
(5) Separation funnel: 250mL
.
(6) Flip-type oscillating device
.
Five, pre-treatment
(1) Preparation of solid waste leachate
"Semi-Volatile Organic Compound Analysis Technology-Preparation of Sulfuric Acid and Nitric Acid from Leachate"
(2) Extraction
Take 100 mL of the solid waste extract in a separatory funnel, add an appropriate amount of sodium chloride and 15 mL of dichloromethane to fully shake, shake, and stand still, remove water through a funnel with an appropriate amount of anhydrous sodium sulfate , and collect the organic phase
.
The extraction was repeated twice as described above, the sodium sulfate was washed thoroughly with dichloromethane , and the organic phases were combined and collected in a pear-shaped flask for concentration
.
(3) Concentration and purification
(1) Concentration: When using a rotary evaporator to concentrate, the temperature of the water bath is 30°C
.
Concentrate to 4mL, add 4mL of n-hexane, continue to concentrate to 1.
0mL for GC-ECD determination
.
(2) Purification: If the color of the extract is dark, it needs to be purified by sulfuric acid before it can be analyzed on the computer
.
Related Links: Solid Waste Leachate—Determination of Organochlorine Pesticides—Gas Chromatography (2)