Solid Waste-Determination of Dioxins-Isotope Dilution High Resolution-Gas Chromatography-High Resolution Mass Spectrometry (2)

Six, analysis and testing (for reference only, can be adjusted appropriately according to the actual instrument)

(1) Gas chromatographic conditions

Injection port: temperature is 280℃, column flow (constant flow mode) is 1.

(2) Mass spectrometry conditions

Resolution: greater than 10000 (the resolution needs to be tuned to higher than 10000 before each sample analysis), solvent delay time 20min; electron bombardment source: EI, EI source temperature: 280℃; SIM scanning mode; transmission pipeline temperature: 280℃

(3) Qualitative quantitative ion and toxicity equivalent

Use EI source to analyze the retention time of each compound.

Table 3-14 Retention time, quantitative qualitative ion and toxicity equivalent of each compound

(4) Calibration curve

Take five standard solutions of EPA-1613CS1, EPA-1613CS2, EPA-1613CS3, EPA-1613CS4, and EPA-1613CS5, directly inject the sample for analysis, and quantify with the internal standard relative response factor method.

Where Q _es — the absolute amount of the internal standard substance extracted in the standard solution, pg;

Q _s —the absolute amount of the compound to be tested in the standard solution, Pg;

A _s —the sum of the peak areas of the monitored ions of the compounds to be tested in the standard solution;

A _es —the sum of the peak areas of the monitored ions of the internal standard substances extracted from the standard solution leaves

Similarly, formulas (3) and (4) are used to calculate the relative response factors RRFrs and RRFss of the injected internal standard relative to the extracted internal standard and the extracted internal standard relative to the sampled internal standard

In the formula, Q _rs — the absolute amount of the internal standard substance injected in the standard solution, pg;

Q _es — the absolute amount of the internal standard substance extracted in the standard solution, pg;

A _es -the sum of the peak areas of the monitored ions extracted from the internal standard substance in the standard solution;

A _rs —the sum of the peak areas of the monitored ions of the injected internal standard substances in the standard solution

Where Q _es -the absolute amount of the internal standard substance extracted in the standard solution, pg;

Q _ss —the absolute amount of the internal standard substance sampled in the standard solution, Pg;

A _ss — the sum of the peak areas of the monitored ions of the internal standard substances sampled in the standard solution;

A _es —The sum of the peak areas of the monitored ions extracted from the internal standard substance in the standard solution

(5) Sample determination

The sample after pretreatment is measured under the same conditions as the calibration curve, and quantification is performed based on the peak area