CN101825561B - Quantitative analysis method for residual phosphorus oxychloride in flame retardant bisphenol A bis (diphenyl phosphate) intermediate - Google Patents
Quantitative analysis method for residual phosphorus oxychloride in flame retardant bisphenol A bis (diphenyl phosphate) intermediate Download PDFInfo
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- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000004445 quantitative analysis Methods 0.000 title claims abstract description 8
- 239000003063 flame retardant Substances 0.000 title abstract description 7
- 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 title abstract description 4
- BQPNUOYXSVUVMY-UHFFFAOYSA-N [4-[2-(4-diphenoxyphosphoryloxyphenyl)propan-2-yl]phenyl] diphenyl phosphate Chemical compound C=1C=C(OP(=O)(OC=2C=CC=CC=2)OC=2C=CC=CC=2)C=CC=1C(C)(C)C(C=C1)=CC=C1OP(=O)(OC=1C=CC=CC=1)OC1=CC=CC=C1 BQPNUOYXSVUVMY-UHFFFAOYSA-N 0.000 title description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 25
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011574 phosphorus Substances 0.000 claims abstract description 25
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 25
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 13
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 12
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 12
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 12
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 12
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 12
- 235000011007 phosphoric acid Nutrition 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 150000007524 organic acids Chemical class 0.000 claims abstract description 10
- 230000031700 light absorption Effects 0.000 claims abstract description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 8
- 239000000706 filtrate Substances 0.000 claims abstract description 5
- 238000007710 freezing Methods 0.000 claims abstract description 4
- 230000008014 freezing Effects 0.000 claims abstract description 4
- 238000000967 suction filtration Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 23
- 239000000543 intermediate Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 230000007062 hydrolysis Effects 0.000 claims description 14
- 238000006460 hydrolysis reaction Methods 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 13
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- ASMQGLCHMVWBQR-UHFFFAOYSA-M diphenyl phosphate Chemical compound C=1C=CC=CC=1OP(=O)([O-])OC1=CC=CC=C1 ASMQGLCHMVWBQR-UHFFFAOYSA-M 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000012086 standard solution Substances 0.000 claims description 6
- 238000002485 combustion reaction Methods 0.000 claims description 5
- 239000003112 inhibitor Substances 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 239000012267 brine Substances 0.000 claims description 4
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 230000002452 interceptive effect Effects 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 230000003287 optical effect Effects 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 8
- 238000002835 absorbance Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 229940106691 bisphenol a Drugs 0.000 description 5
- 235000002639 sodium chloride Nutrition 0.000 description 5
- 229960002668 sodium chloride Drugs 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 238000002798 spectrophotometry method Methods 0.000 description 4
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- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 3
- 235000019796 monopotassium phosphate Nutrition 0.000 description 3
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- -1 tetrachlorobisphenol A phosphate ester Chemical class 0.000 description 2
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 2
- 229910003208 (NH4)6Mo7O24·4H2O Inorganic materials 0.000 description 1
- 229930185605 Bisphenol Natural products 0.000 description 1
- 0 C*(C)(Cc(cc1)ccc1OP(O)(O)=O)c(cc1)ccc1OP(O)(O)=O Chemical compound C*(C)(Cc(cc1)ccc1OP(O)(O)=O)c(cc1)ccc1OP(O)(O)=O 0.000 description 1
- KFZIIBXDCUYALU-UHFFFAOYSA-N CP(C1CC1)(Oc1ccccc1)=O Chemical compound CP(C1CC1)(Oc1ccccc1)=O KFZIIBXDCUYALU-UHFFFAOYSA-N 0.000 description 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Cc1ccccc1 Chemical compound Cc1ccccc1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 1
- ASMQGLCHMVWBQR-UHFFFAOYSA-N Diphenyl phosphate Chemical class C=1C=CC=CC=1OP(=O)(O)OC1=CC=CC=C1 ASMQGLCHMVWBQR-UHFFFAOYSA-N 0.000 description 1
- 241000237502 Ostreidae Species 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 241001249696 Senna alexandrina Species 0.000 description 1
- 150000001263 acyl chlorides Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
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- 230000032050 esterification Effects 0.000 description 1
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- 239000004744 fabric Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
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- 238000012417 linear regression Methods 0.000 description 1
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- 235000020636 oyster Nutrition 0.000 description 1
- RLOWWWKZYUNIDI-UHFFFAOYSA-N phosphinic chloride Chemical compound ClP=O RLOWWWKZYUNIDI-UHFFFAOYSA-N 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
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- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 1
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Abstract
The invention relates to a quantitative analysis method of residual phosphorus oxychloride, which comprises the steps of quickly weighing a sample in frozen saline, and fully hydrolyzing to convert the phosphorus oxychloride into orthophosphoric acid; freezing the hydrolyzed sample at-20-10 ℃, and performing suction filtration by using slow filter paper to separate phosphoric acid from organic acid components; taking the filtrate, and carrying out color development and color comparison under the following conditions: the color development time is 3-5 min; color development temperature: room temperature; a color developing medium: adding 8mLHNO3And 25mL of 0.04mol/L ammonium molybdate solution and 12.5mL of 0.02mol/L ammonium metavanadate solution are respectively added into a 250mL volumetric flask; at 420nm, taking a color development liquid without a sample as a reference liquid, and measuring the light absorption value by using a cuvette with the optical path of 1 cm; calculating the phosphorus concentration according to the standard working curve of phosphorus, and converting into the content of phosphorus oxychloride; the method is simple to operate, rapid and accurate, and is suitable for analyzing the synthesis of the flame retardant by taking phosphorus oxychloride as a raw material.
Description
Technical field
The present invention relates to the quantitative analysis method of residual phosphorus oxychloride in two (diphenyl phosphate) intermediates of a kind of combustion inhibitor bisphenol A bis, it is a kind of spectrophotometric method.
Background technology
In plastics industry, the fire safety of plastic products is had higher requirement, particularly aspect electronics, electric wire, cable and indoor building material, not only demanding anti-flammability also requires Halogen or nuisanceless.Bisphenol-A two (diphenyl phosphates) is called for short BDP, is colourless viscous liquid, is the important additives of a kind of good halogen-free flame retardants as plastics, has a wide range of applications.
But in synthetic BDP process,, be unfavorable for the postprocessing working procedures such as purification of product, have a strong impact on product quality because residual phosphorus oxychloride energy and phenol reacts in the intermediate.William B Harold was once arranged; W moral gram Crow cloth card is based on the fire retardant [P] of bis-phenol (diphenyl phosphate). and Chinese patent CN1355808 only adopts magnetic nuclear resonance method in patent, phosphorus oxychloride content in the intermediate is measured, but there is not clear and definite labor step, and exist common laboratory not possess the problems such as restriction of large-scale instrument, do not find other analytical approach report in addition.Therefore, set up quick, easy, the practical analytical approach of a kind of phosphorus oxychloride and have important directive significance guaranteeing product quality.
Summary of the invention
The object of the invention is the quantitative analysis method that provides a kind of phosphorus oxychloride quick, easy, practical to help the raising of flame retardant products quality.Analytical approach of the present invention is by combustion inhibitor bisphenol A bis (diphenyl phosphate) intermediate being handled, made phosphorus oxychloride be hydrolyzed into phosphoric acid, separate with other interfering component, again through a kind of spectrophotometric method of colorimetric, calculation procedure.Specifically comprise the steps:
1), sample preparation: the sample that takes by weighing 0.2-5g fast is in chilled brine, and fully hydrolysis 1～3min is transformed into orthophosphoric acid with phosphorus oxychloride;
2), separate: the sample of hydrolysis through freezing 3～10min, under-20～10 ℃, with filter paper suction filtration at a slow speed, is separated phosphoric acid and organic acid composition;
3), colorimetric: get filtrate, develop the color then and colorimetric, its condition: developing time 3～5min; Colour temp: room temperature; Colour developing medium: with the 8mL nitric acid (HNO of (water and 63% red fuming nitric acid (RFNA) mixed in by volume 1: 1)
3) and the 0.04mol/L ammonium molybdate solution of 25mL and the 0.02mol/L ammonium metavanadate solution of 12.5mL add respectively in the 250mL volumetric flask; At the 420nm place, as reference liquid, be that the 1cm cuvette is measured light absorption value with light path with the colour developing liquid that do not add sample;
4), calculate: contrast the standard working curve of phosphorus, calculate phosphorus concentration, be converted to the content of phosphorus oxychloride.
Chilled brine is a saturated nacl aqueous solution.
The quantitative analysis method of phosphorus oxychloride content in the spectrophotometry flame retardant intermediate of the present invention, simple to operate, quick and precisely, do not need special large-sized analytic instrument, be applicable to the phosphorus oxychloride to be the scientific research of the synthetic fire retardant of raw material and the control analysis method in the production.
Description of drawings
Fig. 1 is the standard working curve of phosphorus.
Embodiment
Experimental principle
Phosphorus oxychloride very easily generates orthophosphoric acid and hydrochloric acid with the water reaction:
POCl
3+3H
2O＝H
3PO
4+3HCl
Adopt the phosphorus acid content (in phosphorus) in the ammonium molybdate spectrophotometry intermediate hydrolysate, be converted to the content of phosphorus oxychloride.
Orthophosphoric acid, ammonium molybdate, ammonium metavanadate can form yellow complex in acid solution:
7H
3PO
4+7NH
4VO
3+16(NH
4)
6Mo
7O
24·4H
2O+75HNO
3→
7[(NH
4)
3PO
4·NH
4VO
3·16MoO
3]+48H
2O+75NH
4NO
3
Measure the light absorption value of yellow complex, the standard working curve of contrast phosphorus calculates phosphorus concentration.
But phosphorus oxychloride is in the process of hydrolysis, and hydrolysis also takes place intermediate acyl chlorides (tetrachlorobisphenol A phosphate ester monomer), becomes corresponding organic acid:
This organic acid produce to disturb measurement result, so we utilize the hydrolysate-phosphoric acid and the organic acid of intermediate, and the different solubility under different temperature in the water makes it to separate.
This method is applicable to phosphorus oxychloride and bisphenol-a reaction, at first prepares tetrachlorobisphenol A phosphate ester monomer (intermediate), and intermediate carries out the intermediate controlled analysis of two (diphenyl phosphate) products (BDP) of synthesis of bisphenol A again by the mode of linear condensation with phenol.Its reaction equation is as follows
(1) intermediate preparation
(2) esterification
Key instrument and reagent
Lambda 25UV/VIS Spectrometer (U.S. PerkinElmer company);
It is pure, commercially available that ammonium molybdate, ammonium metavanadate, red fuming nitric acid (RFNA), potassium dihydrogen phosphate, sodium chloride etc., above reagent are analysis.
Vacuum extractor, 1 cover;
Solvent filter, 1 cover.
Refrigerator, 1
Experimental technique
1, the preparation of phosphorus standard solution
Under 110 ℃, after potassium dihydrogen phosphate dried about 3 hours, getting the 43.93g potassium dihydrogen phosphate is dissolved in the proper amount of deionized water, again this solution is injected the 1L volumetric flask, and be diluted to scale with deionized water, and get above-mentioned solution 10mL, place the 1L volumetric flask, and being diluted to scale with deionized water, this solution is the phosphorus standard solution of 0.1g/L.
2, the preparation of ammonium molybdate solution
In the 1L beaker, add about 500mL deionized water, and then 150mL sulfuric acid is slowly injected beaker, after this solution is cooled to room temperature, add the 49.44g ammonium molybdate again, stirring and dissolving, change at last in the 1L volumetric flask, be diluted to scale with deionized water, this solution concentration is 0.04mol/L.
3, the preparation of ammonium metavanadate solution
In the 1L beaker, add about 200mL deionized water, inject the 11mL red fuming nitric acid (RFNA), add the 2.34g ammonium metavanadate again, stirring and dissolving changes this solution in the 1L volumetric flask over to then, is diluted to scale with deionized water, and ammonium metavanadate solution concentration is 0.02mol/L.
4, the determination step of sample
Sample is through weighing, adopts the sodium-chloride water solution of cooling, through hydrolysis, freezing, with separation means such as filter paper filterings at a slow speed, collect filtrate, filtrate is transferred in the 250mL volumetric flask, add 8mL1+1HNO
3, adding 25mL ammonium molybdate and 12.5mL ammonium metavanadate, water is settled to scale, at room temperature, colour developing 3min surveys its light absorption value with spectrophotometer 420nm place in the 1cm cuvette then, the standard working curve of contrast phosphorus calculates phosphorus concentration, is converted to phosphorus oxychloride content.
The selection of condition determination
1, measures the selection of wavelength
With the phosphorus standard solution from 380nm to 540nm, scan absorption curve, absorption maximum appears at the 420nm place on the curve, therefore it is comparatively suitable to select for use wavelength to be that 420nm carries out the quantitative test of phosphorus.
2, the selection of hydrolysis time and cool time
Same sample is carried out different hydrolysis time experiments, found that the measured phosphorus content of sample of hydrolysis 1min, 3min, 5min, 15min is respectively 0.09%, 0.16%, 0.15%, 0.17%; Therefore, hydrolysis time is elected 3min as.
Simultaneously same sample is carried out difference experiment cool time, this moment, hydrolysis time was all identical.Found that the phosphorus content that the sample of the cold 3min of going records is 1.80%; The sample phosphorus content of cold 5min of going and 10min is 0.16%, and the sample of cooling 3min through suction filtration, add nitric acid after, solution presents the white casse phenomenon, adds developer again, forms the oyster precipitation, colour developing is unstable.This is because cool time is short, and organic acid is not separated out fully, due to the interference.So this experimental selection cool time is 5min.
3, chilling temperature is to the influence of measurement result
This experiment makes the phosphorus oxychloride hydrolysis complete at first with the abundant hydrolysis of intermediate, adopts the method for cooling that the formed organic acid of intermediate is separated out from water again, and temperature is low more, and the solubleness of intermediate in water is more little, can reach the purpose of separating fully with phosphoric acid more.If organic acid can not be separated out fully, sample produces precipitation after adding developer, measurement result is had interference, therefore, should organic acid be separated out fully.A large amount of different temperatures experimental results show that under-20 ℃～10 ℃ temperature, preferably preference temperature is-10 ℃～0 ℃, can reach and separate purpose fully.
4, the selection of filter paper kind
Adopt respectively 0.45um moisture film, fast quantification filter paper, quantitative filter paper carries out filtration experiment at a slow speed, drawing quick filter paper result by experiment disturbs bigger, the moisture film result of filter paper and 0.45um is suitable and collimation good at a slow speed, but taking cost into account, determined that with filter paper at a slow speed be that filtering material is more suitable.
5, developing time is to the influence of absorbance
Chromophoric solution is placed 3,5,10,20, and 30min measures its absorbance, finds that 5～30min internal absorbance is basicly stable constant, 3～5min, and absorbance has only changed 2%.Required in view of the intermediate controlled analysis, developing time can be chosen 3min.
The drafting of standard working curve
Accurately draw the phosphoric acid standard solution 0,2,4,6,8,10 of 0.1g/L, 12mL is with 3mL 1+1 HNO
3Add respectively in the 100mL volumetric flask with 10mL 0.04mol/L ammonium molybdate solution and 5mL0.02mol/L ammonium metavanadate solution, be diluted to scale with deionized water, the 3min that at room temperature develops the color is at the 420nm place, as reference liquid, measure light absorption value with the colour developing liquid that do not add sample.With phosphorus concentration (C) is horizontal ordinate, and corresponding light absorption value A is an ordinate, the drawing standard working curve.As Fig. 1, its equation of linear regression is A=-0.00511+0.05472C, linearly dependent coefficient R=0.9997.As can be seen from Figure 1, in the 0-12mg/L scope, curve is favorable linearity.
The accuracy of method
The phosphorus oxychloride content that this law is recorded is converted into the content of triphenyl phosphate, with liquid chromatography (patent: the method for introducing among the CN1355808) content of the triphenyl phosphate that records compares, its as a result relative error see table 1 for details less than 3.4%.
Table 1 accuracy experimental result
The precision of method
Under selected experiment condition, same sample is carried out 5 times measure, the result, its relative standard deviation is 2.16%, sees table 2 for details.
Table 2 precision experimental result
Interference experiment
According to " drafting of standard working curve " step, get the phosphorus standard solution of 4.00mL, place the 100mL volumetric flask, add the 30g solid sodium chloride, add 3mL 1+1 HNO again
3With 110mL 0.04mol/L ammonium molybdate solution and 5mL0.02mol/L ammonium metavanadate solution, its absorbance is surveyed in the constant volume colour developing; With the colour developing liquid phase that does not add sodium chloride relatively, its absorbance no change illustrates that 30g does not disturb the mensuration of phosphorus with the sodium chloride of interior consumption.
Claims (2)
1. the quantitative analysis method of residual phosphorus oxychloride in two (diphenyl phosphate) intermediates of a combustion inhibitor bisphenol A bis is characterized in that: may further comprise the steps:
A, sample preparation: the sample that takes by weighing 0.2-5g fast is in chilled brine, and fully hydrolysis 1～3min is transformed into orthophosphoric acid with phosphorus oxychloride;
B, separation: the sample of hydrolysis through freezing 3～10min, under-20～10 ℃, with filter paper suction filtration at a slow speed, is separated phosphoric acid and organic acid interfering component;
C, colorimetric: in filtrate dislocation 250mL volumetric flask, develop the color and colorimetric its condition: developing time 3～5min; Colour temp: room temperature; Colour developing medium: by volume 1: 1 mixed nitric acid of 8mL water and 63% red fuming nitric acid (RFNA) and the 0.04mol/L ammonium molybdate solution of 25mL and the 0.02mol/L ammonium metavanadate solution of 12.5mL are added respectively in the 250mL volumetric flask; At the 420nm place, as reference liquid, be that the 1cm cuvette is measured light absorption value with light path with the colour developing liquid that do not add sample.
D, calculating: the standard working curve of contrast phosphorus, calculate phosphorus concentration, be converted to the content of phosphorus oxychloride;
The standard working curve of described phosphorus is to draw in the following manner: the phosphoric acid standard solution 0,2,4 of promptly accurately drawing 0.1g/L, 6,8,10,12mL, by volume 1: 1 mixed nitric acid of 3mL water and nitric acid and 10mL 0.04mol/L ammonium molybdate solution and 5mL0.02mol/L ammonium metavanadate solution are added respectively in the 100mL volumetric flask, be diluted to scale with deionized water, the 3min that at room temperature develops the color is at the 420nm place, as reference liquid, measure light absorption value with the colour developing liquid that do not add sample; With the phosphorus concentration is horizontal ordinate, and corresponding light absorption value is an ordinate.
2. according to the quantitative analysis method of residual phosphorus oxychloride in two (diphenyl phosphate) intermediates of right 1 described combustion inhibitor bisphenol A bis, it is characterized in that: employed chilled brine is a saturated nacl aqueous solution in a, the b step.
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| CN103439278A (en) * | 2013-09-04 | 2013-12-11 | 江苏元景锂粉工业有限公司 | Measurement method of spectrophotometer |
| CN104502618B (en) * | 2014-12-26 | 2016-08-24 | 深圳市朗诚科技股份有限公司 | A kind of many cuvettes automatic analysis system and colorimetric methods and application |
| CN105987982A (en) * | 2015-02-16 | 2016-10-05 | 艺康美国股份有限公司 | Composition for measuring concentration of orthophosphoric radicals in water system, measuring method and application of composition |
| CN110455731A (en) * | 2019-08-28 | 2019-11-15 | 新疆农垦科学院 | Composite phosphate detection method in a kind of meat products |
| CN111948202A (en) * | 2020-08-15 | 2020-11-17 | 内蒙古自治区农牧业科学院 | Method for determining protein in food by using flow injection method |
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| CN1349094A (en) * | 2000-10-13 | 2002-05-15 | 杜廷发 | Fast test method and test device for residual organophosphate and carbamate pesticide |
| CN1699981A (en) * | 2005-05-13 | 2005-11-23 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | Process for preparation of nano print polymer microballoon for detecting long-lasting phosphorus |
| CN101210908A (en) * | 2006-12-29 | 2008-07-02 | 中国科学院沈阳应用生态研究所 | GC-MS for determining soil amino acid chiral isomer isotope enriching rate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1349094A (en) * | 2000-10-13 | 2002-05-15 | 杜廷发 | Fast test method and test device for residual organophosphate and carbamate pesticide |
| CN1699981A (en) * | 2005-05-13 | 2005-11-23 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | Process for preparation of nano print polymer microballoon for detecting long-lasting phosphorus |
| CN101210908A (en) * | 2006-12-29 | 2008-07-02 | 中国科学院沈阳应用生态研究所 | GC-MS for determining soil amino acid chiral isomer isotope enriching rate |
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