CS248490B1 - A method for determining phenol and substituted phenol content - Google Patents
A method for determining phenol and substituted phenol content Download PDFInfo
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- CS248490B1 CS248490B1 CS948484A CS948484A CS248490B1 CS 248490 B1 CS248490 B1 CS 248490B1 CS 948484 A CS948484 A CS 948484A CS 948484 A CS948484 A CS 948484A CS 248490 B1 CS248490 B1 CS 248490B1
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Abstract
Riešenie sa týká sposobu stanovenia ob- ' sáhu fenolu a substituovaných fenolov v medziproduktoch, technických produktoch a finálnych prípravkoch přísad do polymérov na báze esterov kyseliny fosforečné] priamo metodou plynové] chromatografie. Riešenie je možné využiť v chemickom priemysle — v analytickej chémii.The solution concerns a method for determining the content of phenol and substituted phenols in intermediates, technical products and final preparations of additives to polymers based on phosphoric acid esters directly by the method of gas chromatography. The solution can be used in the chemical industry — in analytical chemistry.
Description
Riešenie sa týká sposobu stanovenia ob- ' sáhu fenolu a substituovaných fenolov v medziproduktoch, technických produktoch a finálnych prípravkoch přísad do polymérov na báze esterov kyseliny fosforečnej priamo metodou plynovej chromatografie.The present invention relates to a process for the determination of the content of phenol and substituted phenols in intermediates, technical products and final polymer additive compositions based on phosphoric acid esters directly by gas chromatography.
Riešenie je možné využil v chemickom priemysle — v analytickej chémii. 248490 248490The solution can be used in the chemical industry - in analytical chemistry. 248490 248490
Vynález sa týká sposobu stanovenía obsahu fenolu a substituovaných fenolov v medziproduktoch, technických produktoch a finálnych prípravkoch přísad do polymérov na báze esterov kyseliny fosforečnej metodou plynovej chromatografie.BACKGROUND OF THE INVENTION The present invention relates to a method for the determination of phenol and substituted phenols content in intermediates, technical products and final polymer additive compositions based on phosphoric acid esters by gas chromatography.
Doterajši postup stanovenía obsahu fenolu a substituovaných fenolov v medziproduktoch, technických produktoch a finálnych prípravkov přísad do plymérov na báze esterov kyseliny fosforečnej je založený na extrakcii do vodného roztoku hydroxidu draselného a následnej spektrofotometrickej kvantifikácii na základe absorpcie UV žiarenia viď Zolotaevova G. P., Strutskaja V. G.: Chim. Prom-st., Ser. Metody Anal. Kontroly a Kač. Prod. Chim. Prom-sti 10, 14—17, 1980. Tiež sa využívajú reakcie fenolických látok so selektívnymi činidlami a absorpcia žiarenia vzniknutými produktami viď Jerzy Urbanski, Chemia Analit. 15, 3, 615—627, 1970.The current method for determining the content of phenol and substituted phenols in intermediates, technical products, and final formulations of phosphoric acid esters is based on extraction into an aqueous solution of potassium hydroxide followed by spectrophotometric quantification based on UV absorption, see Zolotaevova GP, Strutskaja VG: Chim . Prom-st., Ser. Methods Anal. Checks and Duck. Art.-No. Chim. The reactions of phenolic compounds with selective agents are also used, and the absorption of radiation produced by the products is shown in Jerzy Urbanski, Chemia Analit. 15, 3, 615-627, 1970.
Nevýhodou doteraz známých sposobov stanovenia je skutočnosť, že neumožňujú stanovenie přesného zloženia fenolu a substituovaných fenolov ani přesné stanovenie obsahu vzhtadom na rozdielne molové absorpčně koeficienty fenolu a substituovaných fenolov a navýše sú značné neselektívne.A disadvantage of the methods of the hitherto known methods is that they do not allow the determination of the exact composition of phenol and substituted phenols, nor the exact determination of the content relative to the different molar absorption coefficients of phenol and substituted phenols, and in addition, are highly non-selective.
Teraz sa zistilo, že obsah fenolu a substituovaných fenolov v medziproduktov a finálnych prípravkoch přísad do polymérov na báze esterov kyseliny fosforečnej možno stanovit priamo, sposobom podfa vynálezu.It has now been found that the content of phenol and substituted phenols in intermediates and final additives of phosphoric acid ester-based polymers can be determined directly according to the invention.
Podstata vynálezu spočívá v tom, že sa presne navážené množstvo vzorky prevedie do rozpustnej formy se konštantným objemom přidáním organického rozpúšťadla zo skupiny zahrňujúcej alkoholy, ketony, étery a acetonitril. Takto připravená vzroka sa následné priamo analyzuje na chromatografickej kolóne pri teplote v rozsahu 140 až 170 °C, pričom obsah jednotlivých stanovovaných suhstitovaných fenolov a fenolu vyhodnocuje porovnáním chromatografického záznamu so záznamom zmesi štandardov substitnovaných fenolov a fenolu upravených a chromatografických rovnakým sposobm ako vzorka.SUMMARY OF THE INVENTION The subject of the present invention is that the accurately weighed sample is transferred to a soluble, constant volume form by addition of an organic solvent from the group consisting of alcohols, ketones, ethers and acetonitrile. The sample thus prepared is then directly analyzed on a chromatographic column at a temperature in the range of 140-170 ° C, whereby the content of the individual fixed phenols and phenol to be determined is evaluated by comparing the chromatographic recording with a mixture of substituted phenols and phenol-treated and chromatographic standards in the same manner as the sample.
Pe elúcii stanovovaných látok sa estery kyseliny fosforečnej vypudia z kolony zvýšením teploty minimálně na 250 °C.By eluting the substances to be determined, the phosphoric acid esters are removed from the column by raising the temperature to at least 250 ° C.
Stanovenie podfa vynálezu je výhodné uskutočniť na chromatografickej kolóne so zakotvenou tážou typu silikónového polyméru.The assay of the invention is preferably carried out on a chromatography column with an anchored silicone polymer type.
Okrem umožnenia priameho stanovenia obsahu fenolu a substituovaných fenolov, ďalšie výhody vynálezu oproti známým postupom spočívajú v tom, že umožňuje rýchle a dostatočne spofahlivé stanovenie obsahu jednotlivých substituovaných fenolov a fenolu v medziproduktoch, technických produktoch a finálnych prípravkoch přísad do polymérov na báze esterov kyseliny fosforečnej vo vzorkách fubovofných fyzikálnochemických vlastností.In addition to allowing a direct determination of phenol and substituted phenol content, other advantages of the invention over the prior art are that it allows rapid and sufficiently reliable determination of the individual substituted phenols and phenol content of the intermediates, technical products and final additives of the phosphoric acid ester-based polymers samples of any physicochemical properties.
Predmet vynálezu ilustruje, ale neobmedzuje nasledujúci příklad. Příklad prevedeniaThe invention is illustrated but not limited by the following example. Example of execution
Stanovenie obsahu fenolu, o-izopropylfenolu, p-izopropylfenolu, 2,4-diizopropylfenolu, 2,6-diizopropylfenolu, 2,4,5-triizopropylfenolu a 2,4,6-triizopropylfenolu v retardére horenia na báze izopropylfenyl, fenylester kyseliny fosforečnej.Determination of the content of phenol, o-isopropylphenol, p-isopropylphenol, 2,4-diisopropylphenol, 2,6-diisopropylphenol, 2,4,5-triisopropylphenol and 2,4,6-triisopropylphenol in isopropylphenyl, phenyl phosphate flame retardant.
Do 25 cm3 odmernej banky sa naváži 2,5 g vzorky a rozpustí sa v acetone. Roztok sa dávkuje na chromatografickú kolonu. Obsah jednotlivých zložiek sa stanoví porovnáním ploch příslušných píkov s plochami píkov chromatografovaného kalibračného roztoku obsahujúceho v 25 cm3 po 10 mg standardu fenolu, standardu o-izopropylfenolu, standardu p-izopropylfenolu, standardu 2,4-diizopropylfenolu, standardu 2,6-diizopropylfenolu, standardu 2,4,5-triizopropylfenolu a štandardu 2,4,6-triizopropylfenolu.Weigh 2,5 g of the sample into a 25 cm3 volumetric flask and dissolve in acetone. The solution is loaded onto a chromatography column. The content of the individual components is determined by comparing the areas of the respective peaks with the peak areas of the chromatographed calibration solution containing 10 mg of phenol standard, o-isopropylphenol standard, p-isopropylphenol standard, 2,4-diisopropylphenol standard, 2,6-diisopropylphenol standard, standard. 2,4,5-triisopropylphenol and 2,4,6-triisopropylphenol standard.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS948484A CS248490B1 (en) | 1984-12-07 | 1984-12-07 | A method for determining phenol and substituted phenol content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS948484A CS248490B1 (en) | 1984-12-07 | 1984-12-07 | A method for determining phenol and substituted phenol content |
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| CS248490B1 true CS248490B1 (en) | 1987-02-12 |
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| CS948484A CS248490B1 (en) | 1984-12-07 | 1984-12-07 | A method for determining phenol and substituted phenol content |
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1984
- 1984-12-07 CS CS948484A patent/CS248490B1/en unknown
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