CS254886B1 - Method of pyrocatechol determination in vinyl pyridine - Google Patents
Method of pyrocatechol determination in vinyl pyridine Download PDFInfo
- Publication number
- CS254886B1 CS254886B1 CS856187A CS618785A CS254886B1 CS 254886 B1 CS254886 B1 CS 254886B1 CS 856187 A CS856187 A CS 856187A CS 618785 A CS618785 A CS 618785A CS 254886 B1 CS254886 B1 CS 254886B1
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- determination
- pyrocatechol
- pyrocatechin
- vinyl pyridine
- vinylpyridine
- Prior art date
Links
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 title claims abstract description 9
- KGIGUEBEKRSTEW-UHFFFAOYSA-N 2-vinylpyridine Chemical compound C=CC1=CC=CC=N1 KGIGUEBEKRSTEW-UHFFFAOYSA-N 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 title claims description 11
- 230000003647 oxidation Effects 0.000 claims abstract description 5
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 5
- 230000007935 neutral effect Effects 0.000 claims abstract 2
- 150000003839 salts Chemical class 0.000 claims abstract 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- 238000011088 calibration curve Methods 0.000 claims description 2
- 238000011156 evaluation Methods 0.000 claims description 2
- 229910021397 glassy carbon Inorganic materials 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Substances OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229940075397 calomel Drugs 0.000 description 3
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000003969 polarography Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- OZFIGURLAJSLIR-UHFFFAOYSA-N 1-ethenyl-2h-pyridine Chemical compound C=CN1CC=CC=C1 OZFIGURLAJSLIR-UHFFFAOYSA-N 0.000 description 1
- 102100032843 Beta-2-syntrophin Human genes 0.000 description 1
- 108050004003 Beta-2-syntrophin Proteins 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000000699 topical effect Effects 0.000 description 1
- 238000004832 voltammetry Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Pyridine Compounds (AREA)
Abstract
Řešeni se týká přímého voltametriokého stanovení pyrokatechinu ve 2-vinylpyridinu, provádí se anodickou oxidací na rotační diskové elektrodě ze skelného uhlíku v prostředí neutrálních solí.The solution concerns a direct voltametric determination of pyrocatechin in 2-vinylpyridine, it is performed by anodic oxidation to rotary glass carbon disk electrode in the environment neutral salts.
Description
Vynález se týká stanovení pyrokateohinu ve vinylpyridinů přímou voltametrií anodickou oxidací na rotační diskové elektrodě ze skelného uhlíku.The present invention relates to the determination of pyrocateohine in vinylpyridines by direct voltammetry by anodic oxidation on a glass-fiber rotary disk electrode.
Problematika stanovení pyrokateohinu ve vinylpyridinů je nyní aktuální z důvodu stabilizace vinylpyridinů jako důležitého meziproduktu, který bez přídavku pyrokateohinu během několika hodin polymeruje a tím je pro další zpracování znehodnocen. Pyrokatechin je v malém množství používán jako inhibitor polymerace, který se však také pomalu rozkládá. Stanovením pyrokateohinu lze polymeraci předejít.The problem of determination of pyrocateohine in vinylpyridines is now topical because of the stabilization of vinylpyridines as an important intermediate, which polymerizes without addition of pyrocateohine in a few hours and is thus degraded for further processing. Pyrocatechin is used in small amounts as a polymerization inhibitor, but it also slowly decomposes. The determination of pyrocateohin can prevent polymerization.
Dosud užívaná titrace bromem v prostředí kyselin je pro stanovení ve směsích z hlediska neselektivnosti a pro užívaný systém nepoužitelná. K využíváni selektivity polarografie brání v tomto případě polarografická neúčinnost pyrokateohinu, která se obchází nepřímým stanovením po nitraci nebo nitrizaci. Ve směsi, kde i jiné složky podléhají těmto reakcím, je stanovení ztíženo, ne-li znemožněno.The bromine titration used so far in the acid medium is unusable for the determination in mixtures in terms of non-selectivity and for the system used. To exploit the selectivity of polarography, the polarographic ineffectiveness of pyrocateohin, which is circumvented by indirect determination after nitration or nitrization, is prevented in this case. In a mixture where other components are also subject to these reactions, determination is made difficult, if not impossible.
Dále je možno stanovit pyrokatechin v nevodném prostředí titrací tetrabutylamoniem hydroxidu ve směsi burzen-metanol se skleněnou elektrodou a modifikovanou standardní kalomelovou elektrodou v metanolu. Výsledky mohou zkreslovat přítomné látky kyselé povahy. Tato metoda je popsána v Quantitative org. Analysis Functional Group - S. Siggin. Pyrokatechin ve vodě lze stanovit jedometricky - retitraci přebytku I2 pomocí Na2S20j. Pro neselektivnost nelze tuto metodu použít při stanovení pyrokateohinu ve směsích. (Analytická příručka - Zýka a kol. - SNTL 1974). Stanovení pyrokateohinu je možné také kombinací jodometrie a bromometrie s moderními instrumentálními metodami. Tato metoda ale není selektivní. (Analyst 1984, 109 (6)).Further, pyrocatechin can be determined in a non-aqueous medium by titration with tetrabutylammonium hydroxide in a burzen-methanol mixture with a glass electrode and a modified standard calomel electrode in methanol. The results may distort the acidic substances present. This method is described in Quantitative org. Functional Group Analysis - S. Siggin. Pyrocatechin in water can be determined po- tometrically - retitration of excess I 2 with Na 2 S 2 0j. For non-selectivity, this method cannot be used in the determination of pyrocateohin in mixtures. (Analytical Handbook - Zyk et al. - SNTL 1974). The determination of pyrokateohin is also possible by combining iodometry and bromometry with modern instrumental methods. However, this method is not selective. (Analyst 1984, 109 (6)).
Tyto nedostatky odstraňuje způsob přímého voltametrického stanovení pyrokateohinu ve 2-vinylpyridinu anodickou oxidací na rotační diskové elektrodě ze skelného uhlíku v roztoku solí, například v roztoku dusičnanu sodného. Za těchto podmínek vykazuje vlna pyrokateohinu Ejy2=+0,45 V proti standardní kalomelové elektrodě. Uvedená metoda je metodou přímou a selektivní pro stanovení pyrokateohinu. Zanedbatelná není ani rychlost stanovení, která je srovnatelná s běžnou polarografickou analýzou. Protože se jedná o anodickou oxidaci, není nutno zbavovat vzorek kyslíku probubláváním inertním plynem.These drawbacks are overcome by the direct voltammetric determination of pyrocateohine in 2-vinylpyridine by anodic oxidation on a glassy carbon rotary disk electrode in a salt solution, such as sodium nitrate solution. Under these conditions, the pyrocateohine wave Ejy 2 = + 0.45 V shows a standard calomel electrode. Said method is a direct and selective method for the determination of pyrocateohin. The rate of determination, which is comparable to conventional polarographic analysis, is not negligible. Since this is anodic oxidation, it is not necessary to de-oxygenate by bubbling with inert gas.
Příklad 1Example 1
Vzorek 1-vinylpyridinu s pyrokateohinem v množství 2 ml se odpipetuje do odměrné baňky a doplní roztokem 0,2 N NaNO^ jako základním elektrolytem, polarografuje od -0,2 V do +1,2 V a odečte se velikost vlny. K vyhodnocení výšky vln se použije metoda kalibrační křivky, kde se do grafu vynesou výšky vln se známým množstvím pyrokatechinu. Graf udává závislost difusního, proudu na koncentraci pyrokatechinu.A 2 ml sample of 1-vinylpyridine with pyrocateohin is pipetted into a volumetric flask and made up with 0.2 N NaNO4 as the basic electrolyte, polarographed from -0.2 V to +1.2 V and the wave size is read. For the wave height evaluation, a calibration curve method is used where the wave heights with a known amount of pyrocatechin are plotted. The graph shows the dependence of diffuse current on pyrocatechin concentration.
Příklad 2Example 2
Do tři baněk 100 ml odpipetujeme po 1 ml standardního roztoku tercbutylpyrokatechinu v 50% etanolu. Poté do těchto baněk odpipetujeme 1,2 a 3 ml vzorku tercbutylpyrokatechinu v 2-vinylpyridinu a podrobíme voltamperometrickému měření od -0,2 V do +1,2 V proti standardní kalomelové elektrodě. Vzorek vyhodnotíme z poměru výšek vln podle metodiky standardního přídavku.Pipette 1 ml of a standard solution of tert-butylpyrocatechin in 50% ethanol into three 100 ml flasks. Then pipette 1.2 and 3 ml of a sample of tert-butylpyrocatechin in 2-vinylpyridine into these flasks and voltamperometrically measure from -0.2 V to +1.2 V against a standard calomel electrode. The sample is evaluated from the ratio of wave heights according to the standard addition methodology.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS856187A CS254886B1 (en) | 1985-08-29 | 1985-08-29 | Method of pyrocatechol determination in vinyl pyridine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS856187A CS254886B1 (en) | 1985-08-29 | 1985-08-29 | Method of pyrocatechol determination in vinyl pyridine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CS618785A1 CS618785A1 (en) | 1987-06-11 |
| CS254886B1 true CS254886B1 (en) | 1988-02-15 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS856187A CS254886B1 (en) | 1985-08-29 | 1985-08-29 | Method of pyrocatechol determination in vinyl pyridine |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS254886B1 (en) |
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1985
- 1985-08-29 CS CS856187A patent/CS254886B1/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| CS618785A1 (en) | 1987-06-11 |
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