CN102539511B - 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 PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000003063 flame retardant Substances 0.000 title claims abstract description 20
- 229910052794 bromium Inorganic materials 0.000 title claims abstract description 19
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 title claims abstract description 17
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000003918 potentiometric titration Methods 0.000 title claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 51
- 239000000523 sample Substances 0.000 claims abstract description 41
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000243 solution Substances 0.000 claims abstract description 25
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 12
- 239000012488 sample solution Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 11
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 9
- 238000012360 testing method Methods 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 229910052709 silver Inorganic materials 0.000 claims abstract description 3
- 239000004332 silver Substances 0.000 claims abstract description 3
- 238000004448 titration Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 11
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 7
- 230000033228 biological regulation Effects 0.000 claims description 5
- -1 polyoxyethylene Polymers 0.000 claims description 5
- 229940006460 bromide ion Drugs 0.000 claims description 4
- 239000012085 test solution Substances 0.000 claims description 4
- 239000012088 reference solution Substances 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 101710134784 Agnoprotein Proteins 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 150000002170 ethers Chemical group 0.000 claims description 2
- 230000008595 infiltration Effects 0.000 claims description 2
- 238000001764 infiltration Methods 0.000 claims description 2
- 239000012875 nonionic emulsifier Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 239000003513 alkali Substances 0.000 abstract description 8
- 238000005259 measurement Methods 0.000 abstract description 5
- 239000012086 standard solution Substances 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 2
- 229910052742 iron Inorganic materials 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 230000004927 fusion Effects 0.000 description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 4
- 125000001246 bromo group Chemical group Br* 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 4
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- AEBYJSOWHQYRPK-UHFFFAOYSA-N 1,1'-biphenyl;sodium Chemical compound [Na].C1=CC=CC=C1C1=CC=CC=C1 AEBYJSOWHQYRPK-UHFFFAOYSA-N 0.000 description 2
- ZFWAHZCOKGWUIT-UHFFFAOYSA-N 1-anilino-3-phenyliminourea Chemical compound C=1C=CC=CC=1N=NC(=O)NNC1=CC=CC=C1 ZFWAHZCOKGWUIT-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
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- 239000003153 chemical reaction reagent Substances 0.000 description 2
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- ORMNPSYMZOGSSV-UHFFFAOYSA-N dinitrooxymercury Chemical compound [Hg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ORMNPSYMZOGSSV-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000009840 oxygen flask method Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- XGDRLCRGKUCBQL-UHFFFAOYSA-N 1h-imidazole-4,5-dicarbonitrile Chemical compound N#CC=1N=CNC=1C#N XGDRLCRGKUCBQL-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical group [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000005255 carburizing Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
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
The present invention relates to the bromo element pre-treatment of the fire retardant of high bromine content and a kind of method of assay.
Background technology
Bromide fire retardant good flame retardation effect, with light stabilization and anlistatig characteristic, is widely used in the tartans such as the various plastics such as polyolefin, polyamide, polystyrene, fiber and silicon rubber.Wherein, bromo element shared content in fire retardant systems is to evaluate the important parameter of bromide fire retardant fire resistance, and its size directly influences the quality and flame retardant effect of product.
(1) pretreatment technology：There is sodium to melt method, oxygen flask combustion method, potassium dichromate oxidation, reducing process, biphenyl sodium method etc. for the conventional method that bromo element in organic bromide is determined.Using oxygen flask combustion method, this method sample weighting amount is too small, general 3~7mg, high to analytical instrument required precision, and weighing need to match somebody with somebody a ten thousandth above balance of precision ten；The degree of accuracy and precision are undesirable, and because bromine content is high, have fire retardation, are easily caused incomplete combustion, cause Lower result, measurement result fluctuation is larger；It is dangerous big in operation and the requirement to reagent, instrument such as potassium dichromate oxidation, biphenyl sodium method is high；Reducing process application is narrow, is not suitable for analyzing the aromatic halides and polyhalide of some halogens containing inertia, it is necessary to use metallic sodium, operation difficulty is big.
Traditional high temperature alkali fuse method is mainly used at present, and the high temperature alkali fuse method is：NaOH is mixed with sample, carburizing reagent is carried out under heating condition, subsequent high-temperature fusion (650~800 DEG C), add water absorption after obtained material cooling.Its decomposition principle is that the bromine in testing sample is resolved into bromide ion by sodium hydroxide at high temperature.Reaction equation is as follows：
But measurement result is relevant with the size of high-temperature fusion temperature, NaOH powder：Temperature is too low, decomposes incomplete；Temperature is too high, easily splashes or overflows so that measurement result is significantly less than normal and the temperature too high easy influence nickel crucible life-span.Because solid NaOH is that solid is covered on sample, its hole is big, and sample is heated easily to be gone out from gap, cause absorption efficiency to decline, therefore need to be clayed into power, gap will reduce, make sample covering complete, but solid NaOH in process of lapping easily make moist by water suction, troublesome poeration.
(2) determination techniques：Mercurimetry, argentometry and potentiometric titration are used the measure of bromine content more.Also it can be determined with instrument analytical methods such as liquid chromatogram, chromatography of ions and spectrophotometrics, but due to having certain acidity organic bromide, have stronger corrosion to the surface of instrument, so more economical and practical using chemical analysis method more.
The chemical analysis method includes mercurimetry：Use dilute HNO3The pH value of sample solution is adjusted, is allowed between 3.2~3.4, using diphenylcarbazone as indicator, Hg (NO are added3)2Standard liquid is titrated, and Hg and Br is formed the HgBr of difficult dissociation2, and excessive Hg carrys out the arrival of directing terminal with diphenylcarbazone indicator formation reddish violet complex compound.Mercurimetry finding speed is very fast, but measurement result is determined with large effect by pH sizes, color terminal, and can only individually determine bromide ion, is not suitable for the measure of bromine content in polyhalo fire retardant, the operation of mercuric nitrate also has certain danger.
Moire technique：It is with K2CrO4For indicator, AgNO is used3Standard liquid is titrated, because AgBr solubility is less than Ag2CrO4, it is titrated to after stoichiometric point, micro- excessive silver ion forms brick-red siliver chromate with chromate and precipitated.Moire technique is applied to AgNO3Standard liquid makees titrant direct titration Cl- or Br-, and what is measured when both coexist is both total amounts.
Because the preparation of bromide fire retardant would generally be using chlorine-containing compound as raw material; it is thus inevitable in the product to introduce chlorine atom; the another fire retardant for having part to have cooperative flame retardant effect is simultaneously containing double halogen such as biphosphonate flame-retardant plasticizers; what it is using measure such as traditional precipitation titration, argentometry is both total amounts, it is difficult to reach the purpose of real assessment flame retardant performance.
The content of the invention
Present invention solves the technical problem that being the weak point for overcoming above-mentioned prior art to exist, conventional instrument need to be used by providing a kind of, fire retardant bromo element decomposition method easy to operate, reproducible.
The method of detecting content of bromine in fire retardant through automatic potentiometric titration, its step includes：
(1) directly weighed with nickel crucible after sample, add emulsifying agent, then potassium hydroxide or sodium hydroxide solution is added dropwise, until infiltration is uniform；
(2) after sample surfaces first add the sodium carbonate ground on a small quantity to cover, add the sodium hydroxide ground and be covered in surface, cover crucible lid, but do not cover tightly；
(3) it is slowly heated on pressure regulation electric furnace, sample is melted and is absorbed in aqueous slkali, until without white powdery solid in crucible；
(4) electric furnace is shut, sample is cooled down, the high water of 1/3~1/2 crucible is added, heating makes fused mass all soluble in water, solution is transferred in beaker, cleans nickel crucible and lid, cleaning solution is transferred to beaker in the lump；
(5) by solution constant volume, standby survey；
(6) automatical potentiometric titrimeter is used, makees indicator electrode with silver electrode/Bromide ion selective electrode, uses AgNO3Standard liquid titrates sample solution.
The emulsifying agent is ethers emulsifying agent or esters nonionic emulsifier, including polyoxyethylene Zhong Xin phenolic ethers -10 (OP-10), AEO (MOA-7), polyethylene glycol, one or more kinds of combinations of NPE (NP-10).
The method of potentiometric determination sample solution is as follows：NaCl reference solutions and silver nitrate standard solution are prepared first；
Next pipettes testing sample solution in beaker, and is adjusted to acidity, uses AgNO3Standard liquid carries out constant-current titration, and automatic potentiometer writes down E, V reading automatically, and makees E-V curves, E, V reading during automatic reading end point of the sudden change；Again with identical condition, a blank test is done, the volume of the silver nitrate standard titration solution of blank test solution consumption is determined.
Compared with prior art, the invention has the advantages that：
1. used in medicament and instrument be simple, safety, emulsification-alkali fusion sampling amount is big, can meet analysis precision requirement using a ten thousandth balance, require low to analytical instrument；
2. using emulsifying agent and aqueous slkali pre-invasion, be conducive to sample fully to be contacted with aqueous slkali, can accelerate to absorb and heating-up temperature is relatively low；
3. replacing high temperature Muffle furnace using common pressure regulation electric furnace, it is visible, controllable that sample melts situation, it is to avoid at a high temperature of 650-800 DEG C that traditional alkali fusion method is used, sample easily splashes or overflowed；
4. using adding sodium hydroxide after sample surfaces cover the sodium carbonate that grinds on a small quantity in advance, it is to avoid sample is gone out from gap in reheating melting process；
5. emulsification-alkali fusion mode, because temperature is relatively low, it is to avoid nickel crucible is more than 700 DEG C, alkali fusion mode lower life-span low shortcoming；
6. using automatical potentiometric titrimeter sample solution, automatic decision terminal and record terminal volume judge, as a result accurately without indicator and naked eyes；
7. automatical potentiometric titrimeter titration can titrate a variety of halogens simultaneously, multiple obvious end point of the sudden change are produced, Br, Cl etc. content can be calculated respectively；
8. automatical potentiometric titrimeter connects computer, direct output result, without calculating every time.
Embodiment
Embodiment is given below so that the present invention is described in more detail, but the present invention is not limited to these embodiments, and some nonessential changes and adjustment that one of skill in the art is made according to the invention described above still belong to protection scope of the present invention.
Embodiment 1
(1) pre-treatment of sample
(1) sample 0.3g (accurately to 0.0002g) is directly weighed with nickel crucible that is clean, drying, then adds 1 and drip OP-10 emulsifying agents, sample is all infiltrated and shaken up by 10 drop potassium hydroxide solutions；
(2) sodium carbonate for adding about 1g to grind is covered in sample surfaces, then the solid sodium hydroxide 3.5g ground is uniformly entered on surface again, close the lid and (do not cover tightly), slowly heat and (do not gone out with sample for degree) on the pressure regulation electric furnace for have refractory brick, make potassium hydroxide, sodium hydroxide dissolving；
(3) continue to heat up, sample is melted and is absorbed in aqueous slkali, until without white powdery solid in crucible；
(4) electric furnace is shut, sample is cooled down.The high water of 1/2 crucible is added, is heated, is made fused mass all soluble in water, it is transferred in 100ml beakers, nickel crucible and lid is cleaned, cleaning solution is transferred to beaker in the lump；
(5) solution is settled in 250ml volumetric flasks, shaken up, to be measured.
(2) determine
(1) NaCl reference solutions (0.1mol/L)：Weigh 1.4gNacl (precise to 0.0001g), it is levigate and after 600 DEG C of calcination to constant weights, after the dissolving of 100ml beakers, move into 250ml volumetric flasks, be diluted with water scale, shake up；
(2) silver nitrate standard solution (0.1mol/L)：Weigh 8.5gAgNO3(AR) 500ml solution, is made into, is dissolved in brown bottle.(being demarcated with Nacl standard liquids)；
(3) testing sample solution 50.00ml is pipetted in 150ml beakers, is added stirrer, is placed on magnetic stirring apparatus, is adjusted to acidity with (1+2) nitric acid, uses 0.1mol/l AgNO3Standard liquid carries out constant-current titration, and automatic potentiometer writes down E, V reading automatically, and makees E-V curves, and E, V reading during automatic reading end point of the sudden change, if there is two end point of the sudden change, may contain micro Cl elements；
(4) with identical condition, a blank test is done, the volume of the silver nitrate standard titration solution of blank test solution consumption, Vo (ml) is determined.
(3) the percentage composition X of bromine calculation is as follows：
In formula：V0 --- the volume of the silver nitrate standard titration solution of titration blank test solution consumption, mL
V1 --- the volume of the silver nitrate standard titration solution of titration sample solution consumption, mL
The actual concentrations of C --- silver nitrate standard solution, mol/L
The quality of M --- sample, g
If in the case where there is two end point of the sudden change, titration volumes should subtract volume V1 during first hop point again.Bromine content is calculated and should be：
Embodiment 2
(1) pre-treatment of sample
(1) sample 0.4g (accurately to 0.0002g) is directly weighed with nickel crucible that is clean, drying, then adds 2 and drip emulsifying agent, sample is all infiltrated and shaken up by 15 drop sodium hydroxide solutions；
(2) sodium carbonate for adding 2g to grind is covered in sample surfaces, then the solid sodium hydroxide 3.5g ground is uniformly added on surface again, close the lid and (do not cover tightly), slowly heat and (do not gone out with sample for degree) on the pressure regulation electric furnace for have refractory brick, make potassium hydroxide, sodium hydroxide dissolving；
(3) continue to heat up, sample is melted and is absorbed in aqueous slkali, until without white powdery solid in crucible；
(4) electric furnace is shut, sample is cooled down.The high water of 1/3 crucible is added, is heated, is made fused mass all soluble in water, it is transferred in 200ml beakers, nickel crucible and lid is cleaned, cleaning solution is transferred to beaker in the lump；
(5) solution is settled in 250ml volumetric flasks, shaken up, to be measured.
(2) the calculating be the same as Example 1 of assay method and bromine content.
Claims (1)
1. the method for detecting content of bromine in fire retardant through automatic potentiometric titration, its step includes：
（1）Directly weighed with nickel crucible after sample, add emulsifying agent, then potassium hydroxide or sodium hydroxide solution is added dropwise, until infiltration is uniform；
（2）After sample surfaces first add the sodium carbonate ground on a small quantity to cover, add the sodium hydroxide ground and be covered in surface, cover crucible lid, but do not cover tightly；
（3）It is slowly heated on pressure regulation electric furnace, sample is melted and is absorbed in aqueous slkali, until without white powdery solid in crucible；
（4）Electric furnace is shut, sample is cooled down, the high water of 1/3 ~ 1/2 crucible is added, heating makes fused mass all soluble in water, solution is transferred in beaker, cleans nickel crucible and lid, cleaning solution is transferred to beaker in the lump；
（5）By solution constant volume, standby survey；
（6）Using automatical potentiometric titrimeter, make indicator electrode with silver electrode/Bromide ion selective electrode, use AgNO3Standard liquid titrates sample solution.
2. the method for detecting content of bromine in fire retardant through automatic potentiometric titration according to claim 1, it is characterized in that, the emulsifying agent is ethers emulsifying agent or esters nonionic emulsifier, includes one or more kinds of combinations of polyoxyethylene Zhong Xin phenolic ethers -10, AEO, polyethylene glycol, NPE.
3. the method for detecting content of bromine in fire retardant through automatic potentiometric titration according to claim 1, it is characterised in that step（6）The method of middle determination sample solution is as follows：NaCl reference solutions and AgNO are prepared first3Standard liquid；Next pipettes testing sample solution in beaker, and is adjusted to acidity, uses AgNO3Standard liquid carries out constant-current titration, and automatic potentiometer writes down E, V reading automatically, and makees E-V curves, E, V reading during automatic reading end point of the sudden change；Again with identical condition, a blank test is done, the volume of the silver nitrate standard titration solution of blank test solution consumption is determined.
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| 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 |
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