Method for detecting content of bromine in fire retardant through automatic potentiometric titration
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A potentiometric titration and potentiometric titration technology, applied in the direction of electrochemical variables of materials, can solve the problems of inevitable introduction of chlorine atoms, difficulty in achieving flame retardant performance, etc., and achieve the effects of low requirements, simple drugs and instruments, and accurate results.
Active Publication Date: 2012-07-04
KINGFA SCI & TECH CO LTD +1
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[0010] Since the preparation of brominated flame retardants usually uses chlorine-containing compounds as raw materials, chlorine atoms are inevitably introduced into the product, and some flame retardants with synergistic flame retardant effects also contain double hal...
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Embodiment 1
[0033] (1) Sample pretreatment
[0034] (1) Use a clean and dry nickel crucible to directly weigh 0.3g of the sample (accurate to 0.0002g), then add 1 drop of OP-10 emulsifier and 10 drops of potassium hydroxide solution, soak the sample completely and shake it evenly;
[0035] (2) Add about 1g of ground sodium carbonate to cover the surface of the sample, then evenly add 3.5g of ground solid sodium hydroxide on the surface, cover the lid (not tightly closed), and put it on the pressure-regulated electric furnace with refractory bricks Slowly heat (with the sample coming out as the degree) to dissolve potassium hydroxide and sodium hydroxide;
[0036] (3) Continue to heat up to melt and absorb the sample in the alkali solution until there is no white powdery solid in the crucible;
[0037] (4) Turn off the electric furnace to cool the sample. Add 1 / 2 of the crucible high water, heat to dissolve all the molten material in water, transfer it to a 100ml beaker, clean the nickel...
Embodiment 2
[0053] (1) Sample pretreatment
[0054] (1) Use a clean and dry nickel crucible to directly weigh 0.4g of the sample (accurate to 0.0002g), then add 2 drops of emulsifier and 15 drops of sodium hydroxide solution, soak the sample completely and shake it evenly;
[0055] (2) Add 2g of ground sodium carbonate to cover the surface of the sample, then add 3.5g of ground solid sodium hydroxide evenly on the surface, cover the lid (not tightly closed), and slowly Slowly heat (with the sample not coming out as the degree) to dissolve potassium hydroxide and sodium hydroxide;
[0056] (3) Continue to heat up to melt and absorb the sample in the alkali solution until there is no white powdery solid in the crucible;
[0057] (4) Turn off the electric furnace to cool the sample. Add 1 / 3 of the crucible high water, heat to dissolve all the molten material in water, transfer it to a 200ml beaker, clean the nickel crucible and lid, and transfer the washing liquid into the beaker;
[0058...
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Abstract
The invention discloses a method for detecting content of bromine in fire retardant through automatic potentiometric titration, which comprises the steps of 1 utilizing nickel crucible to directly weigh a sample, adding emulsifier and potassium hydroxide solution or sodium hydroxide solution into the sample, and evenly infiltrating the mixture in advance; 2 after adding small amount of ground sodium carbonate on the surface of the sample to cover the sample, adding solid sodium hydroxide to cover the surface, covering a crucible cover on the crucible with gaps reserved; 3 slowly heating the sample on a pressure regulating electric stove and enabling the sample to fuse in alkali solution and absorb the alkali solution till no white powder solid exits in the crucible; 4 turning off the electric stove, enabling the test sample to cool down, adding water into the crucible till 1/2-1/3 of the height of the crucible, heating the water, enabling fusant to be completely melt in the water, transferring the mixture into a beaker, cleaning the nickel crucible and the cover and transferring cleaning solution into the beaker together; 5 metering the volume of the solution for standby measurement; and 6 utilizing the automatic potentiometric titrimetor, utilizing a silver/bromine iron selection electrode to serve as an indication electrode and utilizing silver nitrate (AgNO3) standard solution to titrate sample solution. The method for detecting the content of the bromine in the fire retardant through the automatic potentiometric titration has the advantages of being high in weighing accuracy, safe and reliable.
Description
technical field [0001] The invention relates to a method for bromine element pretreatment and content determination of flame retardants with high bromine content. Background technique [0002] Brominated flame retardants have good flame retardant effects, light stability and antistatic properties, and are widely used in various plastics such as polyolefins, polyamides and polystyrene, fibers and synthetic rubber materials such as silicone rubber. Among them, the content of bromine element in the flame retardant system is an important parameter to evaluate the flame retardant performance of brominated flame retardants, and its size directly affects the quality of the product and the flame retardant effect. [0003] (1) Pretreatment technology: The traditional methods for the determination of bromine in organic bromides include sodium melting method, oxygen bottle combustion method, potassium dichromate oxidation method, reduction method, sodium biphenyl method, etc. Oxygen c...
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