Method for detecting content of total organic bromine through catalytic reduction debromination
An organic bromine and organic technology, applied in the field of catalytic reduction debromination determination of total organic bromine content in samples, can solve the problems of inability to distinguish between organic and inorganic bromine special combustion devices, inability to measure, low organic bromine content, etc., and achieves a low detection limit. , low cost, accurate results
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Embodiment 1
[0038] Embodiment 1: A kind of method based on the total organic bromine content in the determination sample of catalytic reduction debromination
[0039] Step 1: Weigh 10mg Cu / TiO 2 Catalysts were placed in 18 beakers, and 50 mL of methanol solutions of TBBPA, HBCD and BDE209 with mass concentrations of 1, 10, 25, 50, 75 and 100 mg / L were added to them, and dispersed uniformly by ultrasonic. In this way, the reaction solutions at various concentrations were obtained, collected and filtered quickly to obtain the filtrate. Step 2: Under stirring, quickly add hydrazine hydrate to the above 18 parts of the dispersion, and after reacting for 5 minutes, add the same amount of hydrazine hydrate to the dispersion as when adding it for the first time, continue to react for 5 minutes, and then add the same amount as when adding it for the first time The same amount of hydrazine hydrate was added 5 times in total, and the final concentration of hydrazine hydrate added was 1mol L -1 Af...
Embodiment 2
[0040] Embodiment 2: A kind of method based on the total organic bromine content in the determination sample of catalytic reduction debromination
[0041] Step 1: Weigh 10mg TiO respectively 2 Supported nano-Cu catalyst (Cu / TiO 2 , wherein the mass fraction of Cu is 5%) and 45mL of methanol in 5 beakers, and 5mL of 3-bromodiphenyl ether (hereinafter referred to as BDE3), tetrabromobisphenol A (hereinafter referred to as TBBPA), 2,2 ',4,4'-Tetrabromodiphenyl ether (hereinafter referred to as BDE47), hexabromocyclododecane (hereinafter referred to as HBCD) and decabromodiphenyl ether (hereinafter referred to as BDE209) stock solution (1000mg L -1 , for the respective methanol solutions) and ultrasonically disperse evenly, so that the concentration of the catalyst in the dispersion is 0.2g L -1 , the initial concentrations of BDE3, TBBPA, BDE47, HBCD and BDE209 were all 100mg·L -1 .
[0042] Step 2: Under stirring, quickly add hydrazine hydrate to the above 5 parts of the dis...
Embodiment 3
[0043] Embodiment 3: a kind of method based on catalytic reduction debromination determination total organic bromine content in the sample
[0044] Different from Example 2: (1) TiO in step 1 2 Supported nano-Cu catalyst (Cu / TiO 2 , wherein the mass fraction of Cu is 5%) into commercial copper powder; (2) the catalyst mass is increased from 10mg to 100mg, so that the concentration of the catalyst in the dispersion is 2g L -1 (3) get certain reaction solution after adding hydrazine hydrate 5min at every turn in step 2, obtain the reaction solution of 5 stages thus, get filtrate after rapid filtration, then adopt the test method of embodiment 2 to measure its bromide ion concentration respectively, Thereby calculating the debromination rate, the obtained results are as follows image 3 As shown, the histogram represents BDE3, TBBPA, BDE47, HBCD and BDE209 respectively from left to right. image 3 It was shown that BDE3, TBBPA, BDE47, HBCD and BDE209 can be almost completely d...
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