CN113109502A - Method for analyzing peroxide residue in polymer - Google Patents
Method for analyzing peroxide residue in polymer Download PDFInfo
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- CN113109502A CN113109502A CN202110427467.4A CN202110427467A CN113109502A CN 113109502 A CN113109502 A CN 113109502A CN 202110427467 A CN202110427467 A CN 202110427467A CN 113109502 A CN113109502 A CN 113109502A
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- 238000000034 method Methods 0.000 title claims abstract description 29
- 229920000642 polymer Polymers 0.000 title claims abstract description 17
- 125000002081 peroxide group Chemical group 0.000 title 1
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims abstract description 45
- 239000007864 aqueous solution Substances 0.000 claims abstract description 37
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 28
- 150000002978 peroxides Chemical group 0.000 claims abstract description 26
- CBXWGGFGZDVPNV-UHFFFAOYSA-N so4-so4 Chemical compound OS(O)(=O)=O.OS(O)(=O)=O CBXWGGFGZDVPNV-UHFFFAOYSA-N 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000010355 oscillation Effects 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002474 experimental method Methods 0.000 claims abstract description 9
- 238000004448 titration Methods 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 18
- 239000011790 ferrous sulphate Substances 0.000 claims description 18
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 18
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 6
- 238000001514 detection method Methods 0.000 abstract description 8
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 abstract description 5
- 229940079593 drug Drugs 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 3
- 238000004364 calculation method Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 26
- 229930182470 glycoside Natural products 0.000 description 18
- -1 peroxy acid salts Chemical class 0.000 description 18
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical class OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 16
- 230000008569 process Effects 0.000 description 10
- 229920001451 polypropylene glycol Polymers 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 239000002202 Polyethylene glycol Substances 0.000 description 7
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 7
- 229920001223 polyethylene glycol Polymers 0.000 description 7
- 229920000604 Polyethylene Glycol 200 Polymers 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 6
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 5
- 239000011630 iodine Substances 0.000 description 5
- 229910052740 iodine Inorganic materials 0.000 description 5
- 150000001451 organic peroxides Chemical class 0.000 description 5
- 239000012086 standard solution Substances 0.000 description 5
- 150000002338 glycosides Chemical class 0.000 description 4
- QZMAEZWZCGBZFK-UHFFFAOYSA-N 28-(beta-D-Glucopyranosyloxy)-28-oxoolean-12-en-3beta-yl 3-O-(beta-D-glucopyranosyl)-beta-D-glucopyranosiduronic acid Natural products C12CC(C)(C)CCC2(C(=O)OC2C(C(O)C(O)C(CO)O2)O)CCC(C2(CCC3C4(C)C)C)(C)C1=CCC2C3(C)CCC4OC(C1O)OC(C(O)=O)C(O)C1OC1OC(CO)C(O)C(O)C1O QZMAEZWZCGBZFK-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000004737 colorimetric analysis Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- KPJWZUAARPJYSB-UHFFFAOYSA-N glycoside C Natural products CC1(C)OC(=O)C23CCC1C2(O)CCC(C1(CCC24)C)(C)C3CCC1C2(C)CCCC4(C)COC(C(C(O)C1O)OC2C(C(O)C(CO)O2)O)OC1COC1OC(CO)C(O)C(O)C1O KPJWZUAARPJYSB-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 125000000864 peroxy group Chemical group O(O*)* 0.000 description 3
- 239000002861 polymer material Substances 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 238000004061 bleaching Methods 0.000 description 2
- 239000007844 bleaching agent Substances 0.000 description 2
- 238000003421 catalytic decomposition reaction Methods 0.000 description 2
- 229960001701 chloroform Drugs 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000004811 liquid chromatography Methods 0.000 description 2
- 150000004972 metal peroxides Chemical class 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 239000003712 decolorant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 150000002432 hydroperoxides Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000007870 radical polymerization initiator Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
Abstract
A method for analyzing peroxide residue in a polymer relates to the technical field of peroxide analysis, a sample to be tested is weighed and placed in an iodometric flask, then solvent water or ethanol is added, 25ml of ferrous sulfate-sulfuric acid solution is added, the mixture is uniformly mixed and then stands for 10 minutes, then indicator o-phenanthrene or o-phenanthrene ferrous is added dropwise, and under continuous oscillation, standard aqueous solution of cerium sulfate is used for titration until blue appears; performing a blank experiment without the sample to be tested under the condition that other conditions are the same as the experiment conditions of the sample to be tested; and then the residual value of the peroxide in the polymer is obtained by calculation through a formula. The invention solves the limitations that the existing detection method has high cost, narrow detection value range, easy-to-prepare drugs as consumed reagents, more concentrated analyzed product types and the like. The detection value range of the method is wide and ranges from several mg/kg to thousands of mg/kg.
Description
Technical Field
The invention relates to the technical field of peroxide analysis, in particular to a residual analysis technology of peroxide in a polymer.
Background
The polymer generally refers to a high molecular compound, also called a high polymer, which is an organic compound with a relative molecular mass from thousands to hundreds of thousands or even millions, and is a compound with high strength, high elasticity, high toughness and other properties. Peroxide refers to a compound containing peroxy groups "-O-" and can be considered as a derivative of hydrogen peroxide, and the presence of peroxy groups in the molecule is characteristic and can be classified into metal peroxides, hydrogen peroxide, peroxy acid salts, and organic peroxides. Elements of groups IA, IIA, IIIB, IVB of the periodic Table and certain transition elements (e.g., copper, silver, mercury) can form metal peroxides. One or both of the hydrogens are replaced with an organic group and the resulting compound is referred to as an organic peroxide.
Since the polymer contains an organic peroxide and has an ability to release radicals, it can be used as a radical polymerization initiator, a crosslinking agent for a polymer material, a modifier, etc., and is widely used in the field of polymer material industry. The oxidant can be used for disinfection of medical instruments and foods, and bleaching agents, decolorants, bactericides, cleaning agents and the like in daily chemical industries such as textiles, paper and the like. However, the peroxy group "— O", which contains a peroxy bond, has a weak performance due to a bond length, and has a high reduction electrode potential, a high internal energy, and a poor stability, and can undergo redox reactions with many unsaturated olefins, oxygen-containing compounds, sulfur-containing compounds, aromatic compounds, and the like, and thus is liable to cause oxidation or aging of a polymer material. Due to the thermal decomposition property of peroxide, the peroxide can be decomposed and generate trace gas under the condition of heating, and the expansion phenomenon of packages can be caused, so that the products or the environment are polluted.
The alkyl glycoside is used as a novel nonionic surfactant with comprehensive functions, has the characteristics of common anionic and nonionic surfactants, has high surface activity and good ecological safety and compatibility, and is an internationally recognized preferred green functional surfactant. The production process of alkyl glycoside needs bleaching process, the current popular at home and abroad is peroxide oxidation bleaching method, the most ideal bleaching agent is industrial hydrogen peroxide, partial peroxide can be remained in the product, and if the content of the peroxide is too high, the color of the alkyl glycoside product can be darkened in the long-time storage process, which affects the sale color. Allyl polyethers are exposed to oxygen during the production process and, because of the presence of traces of aldehydes in the starting materials ethylene oxide and propylene oxide, to oxygen during the production process, so that more or less peroxide is produced and in severe cases reacts with the double bonds in the polymer, resulting in a polymer with a lower double bond content during downstream addition and thus a lower reactivity.
At present, common peroxide analysis methods mainly comprise an iodometry method, a colorimetric method and a wave spectrum analysis method. In the iodometry test process, a toxic product trichloromethane is usually needed, and simultaneously, iodine reacts with a product with more complex components, so that side reactions occur, and the titration cannot correctly determine the end point. The colorimetric method is usually suitable for measuring a small amount of organic peroxides such as saturated hydrocarbons, alcohols, ethers, ketones and other organic solvents, hydroperoxides and the like, and is influenced by the color quality of the product, so the application range of the colorimetric method is narrow. Conventional methods for wave-spectrum analysis include gas chromatography and liquid chromatography. Most organic peroxides have thermal instability and are not easy to volatilize, so that the method has certain limitation in the gas chromatography test process, and in addition, as a plurality of solvents are used as mobile phases in the liquid chromatography operation, the operation process is complex, the analysis cost reaches dozens or even millions, and certain requirements are also met on the qualification of experimenters, so that the method is not suitable for most enterprises, and therefore, a common laboratory cannot be invested and applied necessarily.
Therefore, there is a need to develop a method for analyzing peroxide residue in polymer, which is simple in operation, short in time consumption, low in toxicity and wide in applicability.
Disclosure of Invention
The invention aims to provide a method for analyzing peroxide residue in a polymer, which is simple to operate, short in time consumption, low in toxicity and wide in applicability.
The invention comprises the following steps:
1) preparing a cerium sulfate standard aqueous solution; preparing a ferrous sulfate-sulfuric acid solution;
adding a dilute sulfuric acid solution in the process of preparing a ferrous sulfate-sulfuric acid solution to prevent ferrous sulfate from hydrolyzing and keeping the acidic condition of the solution;
2) experiment with sample to be tested: accurately weighing a sample to be detected, placing the sample into an iodometry bottle, adding solvent water or ethanol, adding 25ml of ferrous sulfate-sulfuric acid solution, uniformly mixing, standing for 10 minutes, dropwise adding indicator o-phenanthrene or o-phenanthrene ferrous, and titrating with a cerium sulfate standard aqueous solution under continuous oscillation until blue appears;
performing a blank experiment without the sample to be tested under the condition that other conditions are the same as the experiment conditions of the sample to be tested;
3) calculating and analyzing: calculated as follows:
Wis H2O2Content, unit: mg/kg;
Cconcentration of the standard aqueous solution of cerium sulfate, unit: mol/L;
V 1the volume of the cerium sulfate standard aqueous solution consumed for titrating the sample to be tested is as follows: ml;
V 0volume of cerium sulfate standard aqueous solution consumed for titration of blank, unit: ml;
mthe unit is the mass of the sample to be measured: g;
34.01 is H2O2Molar amount of (c), unit: g/mol.
The mechanism of the invention is as follows:
(1) reducing hydrogen peroxide by excessive ferrous sulfate under an acidic condition (reacting for a period of time, and then titrating downwards);
2H++2Fe2++H2O2→2Fe3++3H2O ；
(2) the cerium sulfate standard solution titrates the remaining ferrous sulfate.
Ce4++Fe2+→Ce3++Fe3+ ；
The invention takes water or ethanol as solvent, has higher compatibility with the sample to be detected, does not generate side reaction, and has low cost and no pollution.
The indicator adopted by the invention is o-phenanthroline or ferrous o-phenanthroline. The pH value of the phenanthroline is 2-9 (generally controlled between 5-6), and Fe2+Form stable orange red complex with reagent [ (C)12H8N2)3Fe]2+lgK itStable=21.3, the selectivity of the method is high, which is equivalent to Sn with 40 times of iron content2+、Al3+、Ca2+、Mg2+、Zn2+、SiO3-20 times of Cr3+、Mn2+And 5 times of Co2+、Ni2+、Cu2+Does not interfere with the assay. The two specific products are adopted as indicators, the color development is obvious in the reaction process, the end point is easy to judge, and the accuracy of the difficult test result can be effectively guaranteed.
The invention solves the limitations that the existing detection method has high cost, narrow detection value range, easy-to-prepare drugs as consumed reagents, more concentrated analyzed product types and the like. The detection value range of the method is wide and ranges from several mg/kg to thousands of mg/kg.
Extra staff does not need to be added in the experiment, higher equipment cost does not need to be invested, an easily manufactured drug reagent trichloromethane is not used, harm to the body of an experimenter is small, the variety of a detection target is wide, and the detection value range is wide. The method has higher precision and accuracy, and is easy to be mastered by operators, so the method has good application and popularization values.
Furthermore, the concentration of the cerium sulfate standard aqueous solution is 0.1-1 mol/L.
The concentration of the ferrous sulfate in the ferrous sulfate-sulfuric acid solution is 0.1-1 mol/L.
Reducing peroxide by excessive ferrous sulfate under an acidic condition, and titrating the rest of ferrous sulfate by adopting a cerium sulfate standard solution: ce4++Fe2+→Ce3++Fe3+。
When the concentration of ferrous sulfate in the ferrous sulfate-sulfuric acid solution is 0.1-1 mol/L, if the concentration of cerium sulfate is too high, the consumption volume of the cerium sulfate standard aqueous solution is too small, the concentration is too low, and generally a burette cannot be filled, so that the relative error of the result is large. Too large or too small, the difference between the standard solution blank and the sample consumption is too small or too large, and the result accuracy is affected.
The concentration of ferrous sulfate in the ferrous sulfate-sulfuric acid solution is 0.1-1 mol/L, and excessive ferrous sulfate is added at one time to reduce residual peroxide in the polymer, so that catalytic decomposition of heavy metal ions on the peroxide in the slow titration process of the cerium sulfate standard solution is avoided. If the concentration of ferrous sulfate is too low, more ferrous sulfate is consumed, and accurate removal is difficult in the test.
When the residual peroxide in the sample is fixed, excessive ferrous sulfate needs to be added at one time to reduce the residual peroxide, so that the catalytic decomposition of heavy metal ions on the residual peroxide in the slow titration process of cerium sulfate is avoided. The concentration of ferrous sulfate in the existing ferrous sulfate-sulfuric acid solution is 0.1mol/L, and if the concentration is less than 0.1mol/L, the problems are that the dosage of the ferrous sulfate is too high, the transferring is not accurate, and the accuracy of the result is directly influenced.
Detailed description of the invention
Preparing a ferrous sulfate-sulfuric acid solution:
preparing 1000mL of sulfuric acid aqueous solution from sulfuric acid and water in a volume ratio of 1: 5, cooling, and adding 28g of ferrous sulfate (FeSO)4·7H2O), a ferrous sulfate-sulfuric acid solution with ferrous sulfate concentration of 0.1mol/L is obtained.
Example 1 and blank 1:
20.0089 alkyl glycoside C was weighed in a 500ml iodometric vial8-10Adding 100ml of boiled and cooled distilled water, and adding 25mL, uniformly mixing the ferrous sulfate-sulfuric acid solution, standing for 10 minutes, then dropwise adding 3-5 drops of indicator o-diazaphenanthrene ferrous, under the condition of continuous oscillation, titrating by using a cerium sulfate aqueous solution with the concentration of 0.1mol/L until blue appears, and recording alkyl glycoside C8-10The consumption V of the titrated aqueous solution of cerium sulfate in the test (2)1。
In another 500ml iodometric flask, the process was followed to obtain the alkyl-free glycoside C8-10And recording the absence of alkyl glycoside C8-10The consumption V of the titrated cerium sulfate solution in the test (2)0。
Example 2 and blank 2:
20.2345 alkyl glycoside C was weighed in a 500ml iodometric vial8-10Adding 100ml of boiled and cooled distilled water, adding 25ml of ferrous sulfate-sulfuric acid solution, uniformly mixing, standing for 10 minutes, then dropwise adding 3-5 drops of indicator o-diazaphenanthrene ferrous, titrating with 0.2mol/L cerium sulfate aqueous solution under continuous oscillation until blue appears, and recording alkyl glycoside C8-10The consumption V of the titrated aqueous solution of cerium sulfate in the test (2)1。
In another 500ml iodometric flask, the process was followed to obtain the alkyl-free glycoside C8-10And recording the absence of alkyl glycoside C8-10The consumption V of the titrated cerium sulfate solution in the test (2)0。
The values obtained in examples 1 and 2 above and the corresponding respective blank tests 1 and 2 were substituted into the formula:
wherein the content of the first and second substances,Wis H2O2Content, unit: mg/kg;
Cconcentration of cerium sulfate standard solution, unit: mol/L;
V 1for titration of alkyl glycoside C8-10Volume of the consumed standard aqueous solution of cerium sulfate, unit: ml;
V 0volume of cerium sulfate standard aqueous solution consumed for titration of blank, unit: ml;
mis the alkyl glycoside C of the sample to be tested8-10Mass, unit: g;
34.01 is H2O2Molar amount of (c), unit: g/mol.
Calculated to obtain the results of the above examples 1 and 2WThe values, results are shown in Table 1.
TABLE 1
Example 3 and blank 3:
20.1142g of alkylglycoside C were weighed in a 500ml iodometric vial12-14Adding 100ml of boiled and cooled distilled water, adding 25ml of ferrous sulfate-sulfuric acid solution, uniformly mixing, standing for 10 minutes, then dropwise adding 3-5 drops of indicator phenanthroline, titrating with 0.1mol/L cerium sulfate standard aqueous solution under continuous oscillation until blue appears, and recording alkyl glycoside C12-14The consumption V of the titrated aqueous solution of cerium sulfate in the test (2)1。
In another 500ml iodometric flask for the preparation of alkyl-free glycoside C12-14And recording the absence of alkyl glycoside C12-14The consumption V of the titrated cerium sulfate solution in the test (2)0。
Example 4 and blank 4:
20.2531g of alkylglycoside C were weighed in a 500ml iodometric vial12-14Adding 100ml of boiled and cooled distilled water, adding 25ml of ferrous sulfate-sulfuric acid solution, uniformly mixing, standing for 10 minutes, then dropwise adding 3-5 drops of indicator phenanthroline, titrating with 0.2mol/L cerium sulfate standard aqueous solution under continuous oscillation until blue appears, and recording alkyl glycoside C12-14The consumption V of the titrated aqueous solution of cerium sulfate in the test (2)1。
In another 500ml iodometric flask for the preparation of alkyl-free glycoside C12-14And recording the absence of alkyl glycoside C12-14The consumption V of the titrated aqueous solution of cerium sulfate in the test (2)0。
The values obtained in examples 3 and 4 and corresponding blank tests 3 and 4 were substituted into the formula for calculation:
calculated to obtain the results of examples 3 and 4 respectivelyWThe values and results are shown in Table 2.
TABLE 2
The recovery of the four alkyl glycosides from the above calibration is shown in Table 3.
TABLE 3
As can be seen from table 3: adding a certain amount of hydrogen peroxide to the alkyl glycoside, mixing well, and measuring the value (H)2O2Content) and the measured value (H) of the original sample to be measured2O2Content) is calculated, and is basically consistent with the quantitative hydrogen peroxide added, so that the prepared reagent can be judged to meet the standard, and the measured result is basically accurate.
Example 5 and blank 5:
weighing 20.0136g of polyethylene glycol PEG-200 in a 500ml iodine measuring flask, adding 100ml of distilled water, adding 25ml of ferrous sulfate-sulfuric acid solution, uniformly mixing, standing for 10 minutes, then dropwise adding 3-5 drops of indicator o-diazophenanthrene ferrous, titrating by using a cerium sulfate standard aqueous solution with the concentration of 0.1mol/L under continuous oscillation until blue appears as an end point, and recording the consumption V of the cerium sulfate aqueous solution titrated in the test with the polyethylene glycol PEG-2001。
A blank test without PEG-200 was performed in another 500ml iodometric vial, and the sulfuric acid titrated in the test without PEG-200 was recordedConsumption of aqueous cerium solution V0。
Example 6 and blank 6:
weighing 19.9356g of polyethylene glycol PEG-200 in a 500ml iodine measuring flask, adding 100ml of distilled water, adding 25ml of ferrous sulfate-sulfuric acid solution, uniformly mixing, standing for 10 minutes, then dropwise adding 3-5 drops of indicator o-diazophenanthrene ferrous, titrating by using 0.2mol/L cerium sulfate standard aqueous solution under continuous oscillation until blue appears as an end point, and recording consumption V of the titrated cerium sulfate aqueous solution in the test with the polyethylene glycol PEG-2001。
A blank test without polyethylene glycol PEG-200 was conducted in another 500ml iodometric flask, and the consumption V of the aqueous solution of cerium sulfate titrated in the test without polyethylene glycol PEG-200 was recorded0。
The values obtained in examples 5, 6 and corresponding blanks 5, 6 above are substituted into the formula:
calculated to obtain the products of examples 5 and 6 respectivelyWThe values and results are shown in Table 4.
TABLE 4
Example 7 and blank 7:
weighing 20.1356g of polypropylene glycol PPG-2000 in a 500ml iodine measuring flask, adding 100ml of absolute ethyl alcohol, adding 25ml of ferrous sulfate-sulfuric acid solution, uniformly mixing, standing for 10 minutes, adding 3-5 drops of indicator phenanthroline, titrating with 0.1mol/L cerium sulfate standard aqueous solution under continuous oscillation until blue appears as an end point, and recording consumption V of the titrated cerium sulfate aqueous solution in the test with the polypropylene glycol PPG-20001。
A blank test without polypropylene glycol PPG-2000 was conducted in another 500ml iodometer, and the consumption V of the aqueous solution of cerium sulfate titrated in the test without polypropylene glycol PPG-2000 was recorded0。
Example 8 and blank 8:
weighing 19.9753g of polypropylene glycol PPG-2000 in a 500ml iodine measuring flask, adding 100ml of absolute ethyl alcohol, adding 25ml of ferrous sulfate-sulfuric acid solution, uniformly mixing, standing for 10 minutes, adding 3-5 drops of indicator phenanthroline, titrating with 0.2mol/L cerium sulfate standard aqueous solution under continuous oscillation until blue appears as an end point, and recording consumption V of the titrated cerium sulfate aqueous solution in the test with the polypropylene glycol PPG-20001。
A blank test without polypropylene glycol PPG-2000 was conducted in another 500ml iodometer, and the consumption V of the aqueous solution of cerium sulfate titrated in the test without polypropylene glycol PPG-2000 was recorded0。
The values obtained for examples 7, 8 and corresponding blanks 7, 8 were substituted into the formula:
calculated to obtain the products of examples 7 and 8WThe values, results are shown in Table 5.
TABLE 5
The recovery rates of the four polyether addition standards are shown in Table 6.
As can be seen from table 6: adding quantitative hydrogen peroxide into polyethylene glycol and polypropylene glycol, mixing, and measuring value (H)2O2Content) and the measured value (H) of the original sample to be measured2O2Content) is calculated, and is basically consistent with the quantitative hydrogen peroxide added, so that the prepared reagent can be judged to meet the standard, and the measured result is basically accurate.
Claims (4)
1. A method for analyzing peroxide residue in a polymer, characterized by comprising the steps of:
1) preparing a cerium sulfate standard aqueous solution; preparing a ferrous sulfate-sulfuric acid solution;
2) experiment with sample to be tested: accurately weighing a sample to be detected, placing the sample into an iodometry bottle, adding solvent water or ethanol, adding 25ml of ferrous sulfate-sulfuric acid solution, uniformly mixing, standing for 10 minutes, dropwise adding indicator o-phenanthrene or o-phenanthrene ferrous, and titrating with a cerium sulfate standard aqueous solution under continuous oscillation until blue appears;
performing a blank experiment without the sample to be tested under the condition that other conditions are the same as the experiment conditions of the sample to be tested;
3) calculating and analyzing: calculated as follows:
Wis H2O2Content, unit: mg/kg;
Cconcentration of the standard aqueous solution of cerium sulfate, unit: mol/L;
V 1the volume of the cerium sulfate standard aqueous solution consumed for titrating the sample to be tested is as follows: ml;
V 0volume of cerium sulfate standard aqueous solution consumed for titration of blank, unit: ml;
mthe unit is the mass of the sample to be measured: g;
34.01 is H2O2Molar amount of (c), unit: g/mol.
2. The method for analyzing peroxide residues in a polymer according to claim 1, wherein the concentration of the standard aqueous solution of cerium sulfate is 0.1 to 1 mol/L.
3. The method for analyzing the residual peroxide in the polymer according to claim 1, wherein the concentration of ferrous sulfate in the ferrous sulfate-sulfuric acid solution is 0.1-1 mol/L.
4. The method for analyzing peroxide residues in a polymer according to claim 3, wherein the concentration of ferrous sulfate in the ferrous sulfate-sulfuric acid solution is 0.1 mol/L.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102426169A (en) * | 2011-11-09 | 2012-04-25 | 天津市天骄辐射固化材料有限公司 | Method for detecting content of peroxide in polyether polyol |
| CN103712930A (en) * | 2013-12-30 | 2014-04-09 | 华南理工大学 | Method for determining content of hydrogen peroxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102426169A (en) * | 2011-11-09 | 2012-04-25 | 天津市天骄辐射固化材料有限公司 | Method for detecting content of peroxide in polyether polyol |
| CN103712930A (en) * | 2013-12-30 | 2014-04-09 | 华南理工大学 | Method for determining content of hydrogen peroxide |
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