Determination of Alkyl Mercury in Solid Waste Leachate Purge and Trap/Gas Chromatography-Cold Atomic Fluorescence Method (2)

Six, analysis and testing

(1) Instrument conditions (for examination only, can be adjusted appropriately according to the actual instrument)

All determinations are done on the alkyl mercury analyzer

GC column oven temperature: 36℃; running time: 10min; heating time: 9.

(2) Calibration curve

Prepare standard series of more than 5 points (such as 2.

(Three) determination

Add 30uL sodium acetate buffer solution and 50% sodium tetrapropylboride reagent to the 42mL prepared series standard solution sample bottle , and then fill the bottle with pure water for testing

7.

(1) Qualitative target compound

Qualitatively based on the retention time of each component of the standard material

(2) Quantitative calculation

The target compound was quantified by an external standard method, and the mass concentration of the target compound ρ (ng/L) in the leachate was calculated according to formula (1)

ρ=ρ _x /V _i

Where ρ _x — the mass concentration of the target compound calculated from the calibration curve, pg/L;

V _i -sample volume, mL

8.

(1) Calibration curve

Use the linear fitting curve to calibrate, the correlation coefficient should be greater than or equal to 0.

(Two) blank

Each batch of samples (up to 10 samples) should be a laboratory blank, and the mass concentration of the target compound in the blank result should be less than the detection limit of the method

(3) Parallel sample determination

Each batch of samples (up to 10 samples) should be subjected to at least one parallel determination, and the relative deviation of the parallel sample determination results should be within 30%

(4) Standard addition of actual samples

Each batch of samples (up to 10 samples) should be spiked with actual samples at least once, and the spike recovery rate should be between 60% and 120%

Nine, matters needing attention

(1) The solvents and reagents used in the experiment have certain toxicity.

(2) For the detected samples, the accuracy of the results should be judged based on the recovery rate of the standard addition

(3) Sodium tetrapropyl boride solution is easy to decompose and should be stored at -18°C.
After configuration, it can be divided into 4mL vials, and one bottle is taken each time it is used
.