Method for synchronously detecting plurality of organophosphorus fire retardants in bottom mud
A simultaneous detection and organophosphorus technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of poor detection effect of organophosphorus flame retardants, and achieve the effect of high degree of automation, good reproducibility, and sensitive quantitative detection.
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[0035] Example 1
[0036] This example focuses on the optimization of the GC-MS determination method of the organophosphorus flame retardant in the standard solution.
[0037] Step 1. Preparation of standard samples: prepare mixed standard solution with a gradient of 5-500ng / L. Specifically, use a pipette to take a certain amount of organophosphorus flame retardant mixed standard stock solution and internal standard recovery rate mixed stock solution into a sample vial, then add 240ng internal standard PCB156-d3, and dilute with ethyl acetate to 1mL, get the standard solution of corresponding concentration.
[0038] Step 2: Perform GC-MS detection with the above-mentioned mixed standard solution of each concentration. Set the chromatographic conditions as follows: flow rate 1mL / min; injection port temperature 250℃, injection volume 1μL, pulse splitless injection; initial column temperature 50 After keeping the temperature for 1 minute, program the temperature to 280°C at 25°C / min a...
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[0045] Example 2 OPFRs spiked recovery experiment in sediment samples
[0046] Step 1: Take 6 parts of 5g lyophilized and sieved sediment samples, 5 parts of which are added with 100ng OPFRs mixed standard stock solution, and 100ng of four recovery indicator internal standard mixed stock solutions are added. In the other one, only the recovery indicating internal standard mixed stock solution was added as a control blank.
[0047] Step 2: Load 6 samples into the ASE extraction cell, use ethyl acetate as the extraction solvent, heat for 5 min, static extraction for 5 min under the conditions of 1500 psi pressure and 90°C extraction temperature, cycle twice, use 60% of the volume of the extraction cell % Solvent was used to flush the extraction cell, and finally it was purged with nitrogen for 110s. After the extraction, the extract (about 60 mL) was collected, rotary evaporated to 1 mL, and then ethyl acetate: cyclohexane (1:1, v / v) mixed solvent was added, and the volume was adjus...
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[0052] Example 3 Sampling analysis and detection of organophosphorus flame retardants in the bottom mud of Taihu Lake
[0053] Step 1: Sample collection and processing. When sampling, a grab-type mud picker is used to collect the surface bottom mud and freeze it immediately. After being transported back to the laboratory, it was frozen in a refrigerator at -20°C, freeze-dried with a freeze dryer, ground with a mortar, passed through a 100-mesh metal sieve, and stored at -20°C for analysis.
[0054] Step 2: Take 5 g of the sediment sample at each point, and pre-treat the sample according to the sample pre-treatment method of step 2 to step 4 in Example 2.
[0055] Step 3: Perform GC-MS qualitative and quantitative detection on the processed sample solution according to Step 5 in Example 2. The OPFRs concentrations at the five points measured are shown in Table 3.
[0056] Table 35 Concentrations of OPFRs in the sediments of Taihu Lake sampled at 35 points
[0057]
[0058] Note: nd: no...
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