CN102539511A - Method for detecting content of bromine in fire retardant through automatic potentiometric titration - Google Patents

Method for detecting content of bromine in fire retardant through automatic potentiometric titration Download PDF

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CN102539511A
CN102539511A CN2012100218233A CN201210021823A CN102539511A CN 102539511 A CN102539511 A CN 102539511A CN 2012100218233 A CN2012100218233 A CN 2012100218233A CN 201210021823 A CN201210021823 A CN 201210021823A CN 102539511 A CN102539511 A CN 102539511A
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sample
crucible
fire retardant
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CN102539511B (en
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朱伯明
王鹏
欧阳晓岳
刘奇祥
袁绍彦
叶南飚
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Kingfa Science and Technology Co Ltd
Shanghai Kingfa Science and Technology Co Ltd
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Shanghai Kingfa Science and Technology Co Ltd
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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

Automatic potentiometric titration is measured the method for fire retardant bromine content
Technical field
The present invention relates to bromo element pre-treatment and a kind of method of assay of the fire retardant of high bromine content.
Background technology
The bromide fire retardant good flame retardation effect has the stable and anlistatig characteristic of light, is widely used in the tartans such as various plastics such as polyolefin, polyamide, polystyrene, fiber and silicon rubber.Wherein, bromo element shared content in fire retardant systems is the important parameter of estimating the bromide fire retardant fire resistance, and its size directly has influence on the quality and the flame retardant effect of product.
(1) pretreatment technology: the classic method of measuring for bromo element in the organic bromide has sodium to melt method, oxygen flask combustion method, potassium dichromate oxidation, reducing process, biphenyl sodium method etc.Adopt oxygen flask combustion method, this method sample weighting amount is too little, general 3～7mg, and high to the analytical instrument accuracy requirement, weighing need be joined precision 100,000/above balance; Accuracy and precision are all undesirable, and since bromine content high, fire retardation is arranged, cause incomplete combustion easily, cause the result on the low side, it is bigger to measure result's fluctuation; And potassium dichromate oxidation, biphenyl sodium method etc. are high to the requirement of reagent, instrument, and are dangerous big in operating process; The reducing process narrow in application range is not suitable for analyzing some aromatic halides that contains the inertia halogen and polyhalides, need use sodium metal, and operation easier is big.
The traditional high temperature alkali fuse method of main at present employing, said high temperature alkali fuse method is: with NaOH and sample mix, carry out carburizing reagent under the heating condition, high-temperature fusion (650～800 ℃) adds water after the material that the obtains cooling and absorbs subsequently.Its decomposition principle is that at high temperature NaOH resolves into bromide ion with the bromine in the testing sample.Reaction equation is following:
Figure BDA0000133363130000011
But it is relevant with the size of high-temperature fusion temperature, NaOH powder to measure the result: temperature is low excessively, decomposes not exclusively; Temperature is too high, splashes easily or overflows, and makes to measure the less than normal greatly and too high easy nickel crucible life-span that influences of temperature of result.Because solid NaOH is that solid covers on the sample, its hole is big, and sample is heated and is prone to go out from the slit; Cause absorption efficiency to descend, therefore need it is clayed into power, the slit will reduce; Sample is covered fully, but troublesome poeration is made moist in solid NaOH easy suction in process of lapping.
(2) determination techniques: the mensuration of bromine content adopts mercurimetry, argentometry and potentiometric titration more.Instrument analytical methods such as also available liquid chromatography, chromatography of ions and spectrophotometric are measured, but because organic bromide has certain acidity more, there is stronger corrosion on the surface of instrument, so use chemical analysis method more economical and practical.
Said chemical analysis method comprises mercurimetry: use rare HNO 3Regulating the pH value of sample solution, make it between 3.2～3.4, is indicator with the diphenylcarbazone, adds Hg (NO 3) 2Standard solution titration makes Hg and Br form the HgBr of difficult disassociation 2, and excessive Hg and diphenylcarbazone indicator form the arrival that the reddish violet complex compound comes directing terminal.The mercurimetry finding speed is very fast, receives the judgement of pH size, color terminal point that bigger influence is arranged but measure the result, and can only measure bromide ion separately, is not suitable for the mensuration of bromine content in many halogenated flame, and the operation of mercuric nitrate also has certain danger.
Moire technique: be with K 2CrO 4Be indicator, use AgNO 3Standard solution carries out titration, because the solubleness of AgBr is less than Ag 2CrO 4, titration is to stoichiometric point, and little excessive silver ion and chromate form brick-red siliver chromate deposition.Moire technique is applicable to AgNO 3Standard solution is made titrant direct titration Cl-or Br-, and what when both coexist, record is both total amounts.
Because the preparation of bromide fire retardant can be a raw material with the chlorine-containing compound usually; Thereby in product the inevitable chlorine atom of introducing; The fire retardant that other has part to have the cooperative flame retardant effect contains two halogens such as biphosphonate flame-retardant plasticizer simultaneously; What adopt mensuration such as traditional precipitation titration, argentometry is both total amounts, is difficult to reach the purpose of real assessment flame retardant performance.
Summary of the invention
The technical matters that the present invention solves is to overcome the weak point that above-mentioned prior art exists, and providing a kind of needs to use conventional instrument, easy and simple to handle, the fire retardant bromo element decomposition method of good reproducibility.
Automatic potentiometric titration is measured the method for fire retardant bromine content, and its step comprises:
(1) directly take by weighing sample with nickel crucible after, add emulsifying agent, dropwise add potassium hydroxide or sodium hydroxide solution again, up to soaking into evenly;
(2) after sample surfaces adds the sodium carbonate covering that grinds on a small quantity earlier, add the NaOH that grinds again and cover the surface, cover the crucible lid, but do not cover completely;
(3) slowly heating on the pressure regulation electric furnace makes sample fusion and absorption in aqueous slkali, no white powdery solid in crucible;
(4) shut electric furnace, make the sample cooling, add the high water of 1/3～1/2 crucible, heating makes fused mass all soluble in water, and solution is transferred in the beaker, cleans nickel crucible and lid, and cleansing solution changes beaker in the lump over to;
(5) with solution constant volume, survey fully;
(6) adopt automatical potentiometric titrimeter, select electrode to make indicator electrode, use AgNO with silver electrode/bromide ion 3The standard solution titration sample solution.
Said emulsifying agent is ethers emulsifying agent or ester class nonionic emulsifier, comprises one or more combination of polyoxyethylene Zhong Xin phenolic ether-10 (OP-10), AEO (MOA-7), polyglycol, NPE (NP-10).
The method of potentiometric determination sample solution is following: at first prepare NaCl reference solution and silver nitrate standard solution;
Next pipettes testing sample solution in beaker, and transfers to acidity, uses AgNO 3Standard solution carries out potentiometric titration, and potentiometer is write down E, V reading automatically automatically, and makes the E-V curve, the E when reading the hop terminal point automatically, V reading; With identical condition, do a blank test once more, measure the volume of the silver nitrate standard titration solution of blank test solution consumption.
Compared with prior art, the present invention has following beneficial effect:
1. simple, the safety of institute's with medicament and instrument, emulsification-alkali fusion sampling amount is big, uses ten thousand/balance can satisfy the analysis precision requirement, requires low to analytical instrument;
2. adopt emulsifying agent and aqueous slkali preimpregnation profit, help sample and fully contact with aqueous slkali, it is relatively low to accelerate absorption and heating-up temperature;
3. adopt common pressure regulation electric furnace to replace the high temperature muffle furnace, sample fusion situation is visible, controlled, has avoided under 650-800 ℃ the high temperature that traditional alkali fusion method adopted, and sample is prone to splash or overflow;
4. adopt in advance after sample surfaces covers the sodium carbonate that grinds on a small quantity, to add NaOH again, avoided again in the heating and melting process sample from the slit, to go out;
5. emulsification-alkali fusion mode because temperature is relatively low, has avoided nickel crucible more than 700 ℃, the shortcoming that the alkali fusion following life-span of mode is low;
6. adopt the automatical potentiometric titrimeter sample solution, judge terminal point and record terminal point volume automatically, need not indicator and naked eyes and judge that the result is accurate;
7. the multiple halogen of automatical potentiometric titrimeter titration titration simultaneously produces a plurality of tangible hop terminal points, can calculate the content of Br, Cl etc. respectively;
8. automatical potentiometric titrimeter connects computer, directly exports the result, need not each calculating.
Embodiment
Provide embodiment below more specifying the present invention, but the present invention is not limited to these embodiment, some nonessential change and adjustment that one of skill in the art makes according to the invention described above still belong to protection scope of the present invention.
Embodiment 1
(1) pre-treatment of sample
(1) with clean, the dry direct weighing sample of nickel crucible 0.3g (accurately to 0.0002g), add 1 OP-10 emulsifying agent then, 10 potassium hydroxide solutions all soak into sample and shake up;
(2) add the sodium carbonate that about 1g grinds and cover sample surfaces; And then the solid sodium hydroxide 3.5g that evenly goes into to grind on the surface; Cover lid (not covering completely) in that slowly heating (not going out degree of being with sample) on the pressure regulation electric furnace of refractory brick is arranged, makes potassium hydroxide, dissolution of sodium hydroxide;
(3) continue to heat up, make sample fusion and absorption in aqueous slkali, no white powdery solid in crucible;
(4) shut electric furnace, make the sample cooling.Add the high water of 1/2 crucible, heating makes fused mass all soluble in water, and it is changed in the 100ml beaker, cleans nickel crucible and lid, and cleansing solution changes beaker in the lump over to;
(5) solution is settled in the 250ml volumetric flask, shakes up, to be measured.
(2) measure
(1) NaCl reference solution (0.1mol/L): take by weighing 1.4gNacl (accurately being weighed to 0.0001g), levigate and 600 ℃ of calcinations to constant weight, after 100ml beaker dissolving, move in the 250ml volumetric flask, thin up shakes up to scale;
(2) silver nitrate standard solution (0.1mol/L): take by weighing 8.5gAgNO 3(AR), be made into 500ml solution, be dissolved in the brown bottle.(demarcating) with the Nacl standard solution;
(3) pipette testing sample solution 50.00ml in the 150ml beaker, add stirrer, be placed on the magnetic stirring apparatus, transfer to acidity, use 0.1mol/l AgNO with (1+2) nitric acid 3Standard solution carries out potentiometric titration, and potentiometer is write down E, V reading automatically automatically, and makes the E-V curve, and the E when reading the hop terminal point automatically, V reading if two hop terminal points are arranged, then possibly contain the Cl element of trace;
(4) with identical condition, do a blank test, measure the volume of the silver nitrate standard titration solution of blank test solution consumption, Vo (ml).
(3) account form of the percentage composition X of bromine is following:
Figure 000005
In the formula: V0---the volume of the silver nitrate standard titration solution that the blank test solution of titration consumes, mL
The volume of the silver nitrate standard titration solution that V1---titration sample solution consumes, mL
C---the actual concentrations of silver nitrate standard solution, mol/L
The quality of M---sample, g
If under the situation that two hop terminal points are arranged, the volume V1 when the titration volume should deduct first hop point again.Bromine content calculates and should be:
X ( % ) = ( V g - V 1 - V 0 ) × c × 79.90 m × 250 50 × 100 .
Embodiment 2
(1) pre-treatment of sample
(1) with clean, the dry direct weighing sample of nickel crucible 0.4g (accurately to 0.0002g), add 2 emulsifying agents then, 15 sodium hydroxide solutions all soak into sample and shake up;
(2) add the sodium carbonate that 2g grinds and cover sample surfaces; And then the solid sodium hydroxide 3.5g that even adding grinds on the surface; Cover lid (not covering completely) in that slowly heating (not going out degree of being with sample) on the pressure regulation electric furnace of refractory brick is arranged, makes potassium hydroxide, dissolution of sodium hydroxide;
(3) continue to heat up, make sample fusion and absorption in aqueous slkali, no white powdery solid in crucible;
(4) shut electric furnace, make the sample cooling.Add the high water of 1/3 crucible, heating makes fused mass all soluble in water, and it is changed in the 200ml beaker, cleans nickel crucible and lid, and cleansing solution changes beaker in the lump over to;
(5) solution is settled in the 250ml volumetric flask, shakes up, to be measured.
(2) calculating of assay method and bromine content is with embodiment 1.

Claims (3)

1. automatic potentiometric titration is measured the method for fire retardant bromine content, and its step comprises:
(1) directly take by weighing sample with nickel crucible after, add emulsifying agent, dropwise add potassium hydroxide or sodium hydroxide solution again, up to soaking into evenly;
(2) after sample surfaces adds the sodium carbonate covering that grinds on a small quantity earlier, add the NaOH that grinds again and cover the surface, cover the crucible lid, but do not cover completely;
(3) slowly heating on the pressure regulation electric furnace makes sample fusion and absorption in aqueous slkali, no white powdery solid in crucible;
(4) shut electric furnace, make the sample cooling, add the high water of 1/3～1/2 crucible, heating makes fused mass all soluble in water, and solution is transferred in the beaker, cleans nickel crucible and lid, and cleansing solution changes beaker in the lump over to;
(5) with solution constant volume, survey fully;
(6) adopt automatical potentiometric titrimeter, select electrode to make indicator electrode, use AgNO with silver electrode/bromide ion 3The standard solution titration sample solution.
2. measure the method for fire retardant bromine content according to claims 1 said automatic potentiometric titration; It is characterized in that; Said emulsifying agent is ethers emulsifying agent or ester class nonionic emulsifier, comprises one or more combination of polyoxyethylene Zhong Xin phenolic ether-10, AEO, polyglycol, NPE.
3. measure the method for fire retardant bromine content according to claims 1 said automatic potentiometric titration, it is characterized in that the method for working sample solution is following in the step (6): at first prepare NaCl reference solution and silver nitrate standard solution; Next pipettes testing sample solution in beaker, and transfers to acidity, uses AgNO 3Standard solution carries out potentiometric titration, and potentiometer is write down E, V reading automatically automatically, and makes the E-V curve, the E when reading the hop terminal point automatically, V reading; With identical condition, do a blank test once more, measure the volume of the silver nitrate standard titration solution of blank test solution consumption.
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CN103412028A (en) * 2013-08-01 2013-11-27 中国航空工业集团公司北京航空材料研究院 Method for testing content of sodium oxide in silica sol
CN103412027A (en) * 2013-08-01 2013-11-27 中国航空工业集团公司北京航空材料研究院 Analysis method for testing cobalt in high-chrome and high-temperature alloy
CN103645274A (en) * 2013-12-03 2014-03-19 河北钢铁股份有限公司邯郸分公司 Method for determining content of chlorine ion in cold-rolled emulsified liquid
CN104502434A (en) * 2014-12-25 2015-04-08 北京彤程创展科技有限公司 Method for determining content of halogen in rubber and rubber product
CN105866219A (en) * 2016-04-26 2016-08-17 重庆鹏凯精细化工有限公司 Quick determination method for sodium chloride content in ethoxyl/hydroxypropyl methyl cellulose
CN105954343A (en) * 2016-04-26 2016-09-21 重庆鹏凯精细化工有限公司 Device for rapid determination of content of sodium chloride in hydroxyethyl/hydroxypropyl methyl cellulose
CN108020629A (en) * 2016-11-02 2018-05-11 定州市荣鼎水环境生化技术有限公司 The method for continuously measuring of active ingredient in efficient sterilization disinfectant
CN110412208A (en) * 2019-06-28 2019-11-05 山东省地质矿产勘查开发局第八地质大队(山东省第八地质矿产勘查院) Method for measuring bromine content in soot product
CN112557449A (en) * 2020-12-11 2021-03-26 湖北三江航天江河化工科技有限公司 Method for measuring boron content in bonding agent
CN112924518A (en) * 2019-12-05 2021-06-08 中核四0四有限公司 Method for analyzing neptunium content in neptunium dioxide sample
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CN103412028B (en) * 2013-08-01 2015-04-15 中国航空工业集团公司北京航空材料研究院 Method for testing content of sodium oxide in silica sol
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