PL114675B2 - Indicator for detection and semi-quantitative determination of peroxides,especially hydrogen peroxide - Google Patents

Indicator for detection and semi-quantitative determination of peroxides,especially hydrogen peroxide Download PDF

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Publication number
PL114675B2
PL114675B2 PL20887978A PL20887978A PL114675B2 PL 114675 B2 PL114675 B2 PL 114675B2 PL 20887978 A PL20887978 A PL 20887978A PL 20887978 A PL20887978 A PL 20887978A PL 114675 B2 PL114675 B2 PL 114675B2
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PL
Poland
Prior art keywords
indicator
peroxides
hydrogen peroxide
semi
detection
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Application number
PL20887978A
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Polish (pl)
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PL208879A1 (en
Inventor
Jerzy Ciba
Henryk Stec
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Politechnika Slaska Im Wincent
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Priority to PL20887978A priority Critical patent/PL114675B2/en
Publication of PL208879A1 publication Critical patent/PL208879A1/en
Publication of PL114675B2 publication Critical patent/PL114675B2/en

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Description

Przedmiotem wynalazkujest wskaznik do wykrywania i póilosciowego oznaczania nadtlenków, a zwlaszcza nadtlenku wodoru.Znana jest kompozycja do oznaczania nadtlenku wodoru skladajaca sie z ortotolidyny lub 2,7-dwuamino- fluorenu, jodku potasowego, molibdenianu sodu i bulom o pH 5*2. Inna znana kompozycja zawiera zam¬ iast jodku potasowego i molibdenianu sodu peroksydaze czyli enzym katalizujacy reakcje nadtlenku wodoru z barwnikiem. Kompozycje te sa czule na obecnosc innych utleniaczy zatem wymagaja stosowania srodków masku¬ jacych oraz koniecznejestpozbywanie sieinnych utlenia¬ czy aby sie nimi poslugiwac.Wskaznik wedlug wynalazku do wykrywania i póilos¬ ciowego oznaczania nadtlenków, a zwfaszcza nadtlenku wodoru, zawiera kompozycje o skfadzie w procentach wagowych 3-26% zwiazków kobaltu, 10-62% werse- nianu sodowego, 3-55% buforu o pH^ 10,5-15% poli¬ meru ochronnego w postaci folii oraz korzystnie 0,01-0,5% detergenta niejonowego, 1-3% mocznika i 1-5% tiosiarczanu sodu. Kompozycja naniesionajest na materiale hydrofilowym lub wymieniaczu jonowym anionoczynnym takim jak: potikondensat tioureidowy, Dowex N/CH3A, Wofatyt SBW (sulfoguanidynowo- mocznikowy) Jako material hydrofilowy stosuje sie: bibule, wlókna celulozowe, lniane, bawelniane, welniane, lignine, gabke naturalna i poliuretanowa, zel krzemionkowy.Polimer ochronny jest to trudnoprzepuszczalny dla skladników atmosfery polimer, który w zetknieciu zwod¬ nymi roztworami ulega rozpuszczeniu i podczas magazy¬ nowania wskazników chroni je przed dzialaniem czynników atmosferycznych. Przyktadem takiego poli¬ meru jest: winylo-pirolidyna, rozpuszczalne w wodzie pochodne celulozy (metyloceluloza, etyloceluloza, hyd- roksyceluloza). rozpuszczalne w wodzie poliakryloa- mid, alkohol poliwinylowy, zelatyna, agar-agar. guma arabska, polioctan celulozy, polioctan winylu.W obecnosci kationów tworzacych z anionem werse- nianowym barwne kompleksy o trwalosci wiekszej od kompleksu Co—wersenian, wkskaznikiem wedlug wynalazku moznasie poslugiwacpod warunkiem usunie¬ cia tych kationów z roztworu na zasadzie reakcji wytra¬ cania lub za pomoca wymieniacza jonowego. Do tych kationów naleza Fe*\ CrH, Ni2*.Kompozycja charakteryzuje sie dobra rozdzielczoscia barwy, szczególnie przy wyzszych stezeniach nadtlenków oraz duza odpornoscia na inne utleniacze, na przykfed: nadmanganian, chromian, bromian, chloran, nadsiar¬ czan. Wskaznikiem mozna oznaczac0,3 do 100mg H2O* w dm\ poslugujac sie nim identycznie, jak papierkiem lakmusowym.Opisanym wskaznikiem mozna oznaczyc nadtlenki w obecnosci utleniaczy pod warunkiem usuniecia nadtlen¬ ków z roztworu np. przez destylacje, mikrodyfuzje Wtedy natlenia oznacza sie trzymajac wskaznik w prze- strzeni nad roztworem.Przyklad I. Bibule nasycono roztworem zawieraja¬ cym 3% siarczanu kobaltu 10% werenianu sodowego. 35r buforu weglanowego o pH=12,9, 0,01% detergentu ¦*,l 114 473 4 dodecyiofenvlopoliokyetylouancgo. 3% tiosiarczanu sodu. Bibule po wysuszeniu pokryto blona uzyskana przez zanurzenie bibuly do 5% roztworu wodnego alko¬ holu poliwinylowego.Za pomoca tego wskaznika oznaczono 0,5 mg HjO, w dm3 próbki.Przyklad II. Bibule nasycono roztworem zawieraja¬ cym 6% siarczanu kobaltu. 62% werscnianu sodowego, 35% buforu boraksowego o pH= 10, 0,01% dodecylofe- nolu polioksyetylowanego o liczbie etoksylowania rów¬ nej 14 jako detergentu niejonowego, 15% winylopiroli- dyny, 1% mocznika.Za pomoca tego wskaznika oznaczono 10 mg nadtlenku kumenu w ldm* próbki.Przyklad Ill. Wymieniacz jonowy (sulfoguanidy- nowomocznikowy) osadzony w bibule nasycono roztwo¬ rem zawierajacym 26% azotanu kobaltu, 36% wersenia- nu sodowego, 15% buforu fosforanowego o pH= 12,9. 3% mocznika. 0,5% dodecylofenolu polioksyetylowa¬ nego o liczbie etyIowania równej 14jako detergentu nie¬ jonowego. Po wysuszeniu kompozycje na bibule zabezpieczono warstwa ochronna przez impregnowanie 5°! roztworem polioctanu winylowego w acetonie.Za pomoca tego wskaznika oznaczono 20 mg H£2 w ldm3 próbki.Przyklad IV. Wskaznik jak w przykladzie I z ta róznica, ze nie zawiera ani detergentu niejonowego, ani tiosiarczanu sodów ego.Oznaczono 50 mg BaO: próbki.Przyklad V. Wskaznik jak w przykladzie III z ta róznica, ze nie zawiera mocznika. Oznaczono 80mg nad¬ tlenku mocznika w ldml próbki.Prz klad VI. Postepowano identycznie jak * przy- kkdziel. z ta róznica ze zamiast bibuly uzyto plócien¬ nego paska. Pasek nasycony roztworem, wysuszono i pokryto blona wodnego 1% roztworu winylopirolidyny.Prz klad VII. Postepowano identycznie jak wprzy¬ kladzie II, z ta róznica ze zamiast bibuly uzyto paska z gabki poliuretanowej, który nasycono roztworem zawie¬ rajacym zamiast 15% winylopirolidyny-5% zelatyny.Przyklad VIII. Postepowano identycznie jak w przykfadzie III, z ta róznica, ze zamiast wymieniacza jonowego sulfoguanidynowo-mocznikowego uzyto zelu krzemionkowego osadzonego na bibule. Po wysuszeniu kompozycje zabezpieczono warstwe ochronna 5% roz¬ tworu agar-agaru.Zastrzezenia patentowe 1. Wskaznik do wykrywania i pólilosciowego ozna¬ czania nadltenków a zwlaszcza nadtlenku wodoru, Tiumirwy tym, ze zawiera kompozycje o skladzie w pro¬ centach wagowych 3-26% zwiazków kobaltu. 10-62% wersenianu sodowego, 3-55% buforu o pH^ 10.5-i5% polimeru trudnoprzepuszczalnego dla skladników atmo¬ sfery i rozpuszczalnego w wodnych roztworach, w postaci folii, przy czym kompozycja naniesiona jest na materiale hydrofilowym. lub wymieniaczu jonowym anionoczynnym. 2. Wskaznik wedlug zastrz. I. znamienny tym. ze zawiera 0,01-0.5% detergenta niejonowego. 3. Wskaznik wedlug zastrz. 1. albo 2. znamieany tym. ze zawiera 1-5% tiosiarczanu sodu. 4. Wskaznik wedlug zastrz. 1 albo 2. zaamieaay tym. ze zawiera 1-3% mocznika. h-lisr I P-PRI. Vikfci.l I20l-»/. len.; jiisi <\ PLThe subject of the present invention is an indicator for the detection and semi-quantitative determination of peroxides, especially hydrogen peroxide. There is a known composition for the determination of hydrogen peroxide consisting of orthotolidine or 2,7-diamine-fluorene, potassium iodide, sodium molybdate and bulbs with a pH of 5 * 2. Another known composition comprises, instead of potassium iodide and sodium molybdate, peroxidase, an enzyme catalyzing the reactions of hydrogen peroxide with the dye. These compositions are sensitive to the presence of other oxidants and therefore require the use of masking agents, and it is necessary to remove other oxidants in order to handle them. The indicator according to the invention for the detection and semi-quantitative determination of peroxides, and especially hydrogen peroxide, contains compositions with a percentage by weight 3-26% cobalt compounds, 10-62% sodium versetate, 3-55% buffer with a pH of? 10.5-15% protective polymer in the form of a film and preferably 0.01-0.5% non-ionic detergent, 1-3% urea and 1-5% sodium thiosulfate. The composition is applied on a hydrophilic material or an anionic ion exchanger, such as: thioureide poticondensate, Dowex N / CH3A, SBW (sulfoguanidine-urea) vofatite. , silica gel. A protective polymer is a polymer that is hardly permeable to atmospheric components, which dissolves in contact with aqueous solutions and protects them against the effects of weathering during the storage of the indicators. An example of such a polymer is: vinyl-pyrrolidine, water-soluble cellulose derivatives (methylcellulose, ethylcellulose, hydroxycellulose). water-soluble polyacrylamide, polyvinyl alcohol, gelatin, agar-agar. gum arabic, cellulose polyacetate, polyvinyl acetate. In the presence of cations forming colored complexes with the versate anion, with a stability greater than that of the Co-edetate complex, the indicator according to the invention may be used under the condition of removing these cations from the solution by means of a reduction or deposition reaction. using an ion exchanger. These cations include Fe *, CrH, Ni2 *. The composition is characterized by good color resolution, especially at higher peroxide concentrations, and high resistance to other oxidants, for example: permanganate, chromate, bromate, chlorate, persulfate. The indicator can be used to measure 0.3 to 100 mg of H2O * in dm \ using it in the same way as a litmus paper. The indicator can be used to determine peroxides in the presence of oxidants, provided that peroxides are removed from the solution, e.g. by distillation, microdiffusion, then oxygenation means follow the indicator in above the solution. Example 1 The blotters were saturated with a solution containing 3% cobalt sulfate and 10% sodium vernate. 35r of carbonate buffer with pH = 12.9, 0.01% detergent ¦ *, 1 114 473 4 dodecylphenol polyoxyethylated. 3% sodium thiosulfate. After drying, the blotters were covered with a membrane obtained by dipping the blotting paper into a 5% aqueous solution of polyvinyl alcohol. 0.5 mg of HjO was determined in dm3 of the sample with this indicator. Example II. The blotters were saturated with a solution containing 6% cobalt sulfate. 62% sodium versate, 35% borax buffer at pH = 10, 0.01% polyoxyethylated dodecylphenol with an ethoxylation number of 14 as a non-ionic detergent, 15% vinylpyrrolidine, 1% urea. 10 mg was determined using this index. cumene peroxide in ldm * sample. Example Ill. The ion exchanger (sulfoguanide urea) embedded in the filter paper was saturated with a solution containing 26% cobalt nitrate, 36% sodium edetate, 15% phosphate buffer, pH = 12.9. 3% urea. 0.5% of a polyoxyethylated dodecylphenol with an ethylation number of 14 as a non-ionic detergent. After drying, the blotting compositions were protected with a 5 ° protective layer! solution of polyvinylacetate in acetone. This indicator was used to determine 20 mg H 2 in 1 dm3 of the sample. Example IV. Indicator as in example I with the difference that it contains neither non-ionic detergent nor sodium thiosulphate. 50 mg BaO determined: samples. Example V. Indicator as in example III except that it does not contain urea. 80 mg of urea peroxide in 1 ml of sample was determined. For clade VI. The same procedure was followed as * assign. with the difference that instead of blotting paper, a linen strip was used. The strip is saturated with the solution, dried and covered with a film of an aqueous 1% solution of vinylpyrrolidine. For clade VII. The procedure was identical to that of Example II, except that a strip of polyurethane sponge was used instead of blotting paper, which was impregnated with a solution containing 15% vinylpyrrolidine-5% gelatin instead. Example VIII. The procedure was identical to that in example III, with the difference that instead of the sulfoguanide urea ion exchanger, silica gel deposited on a filter was used. After drying, the compositions were protected with a protective layer of a 5% agar-agar solution. Patent Claims 1. Indicator for the detection and semi-quantitative determination of peroxides, especially hydrogen peroxide, Tyumen in that it contains compositions with a composition of 3-26% by weight. cobalt compounds. 10-62% sodium edetate, 3-55% buffer with a pH? 10.5-15% of a polymer that is difficult to penetrate to atmospheric components and soluble in aqueous solutions, in the form of a film, the composition being applied to a hydrophilic material. or an anionic ion exchanger. 2. The indicator according to claims I. characterized by this. that it contains 0.01-0.5% of non-ionic detergent. 3. Indicator according to claims 1st or 2nd signs of this. that it contains 1-5% sodium thiosulfate. 4. The indicator according to claims 1 or 2 was a blast. that it contains 1-3% urea. h-lisr and P-PRI. Vikfci.l I20l - »/. flax.; jiisi <\ PL

Claims (2)

Zastrzezenia patentowe 1. Wskaznik do wykrywania i pólilosciowego ozna¬ czania nadltenków a zwlaszcza nadtlenku wodoru, Tiumirwy tym, ze zawiera kompozycje o skladzie w pro¬ centach wagowych 3-26% zwiazków kobaltu. 10-62% wersenianu sodowego, 3-55% buforu o pH^ 10.5-i5% polimeru trudnoprzepuszczalnego dla skladników atmo¬ sfery i rozpuszczalnego w wodnych roztworach, w postaci folii, przy czym kompozycja naniesiona jest na materiale hydrofilowym. lub wymieniaczu jonowym anionoczynnym. 2. Wskaznik wedlug zastrz. I. znamienny tym. ze zawiera 0,01-0.5% detergenta niejonowego. 3. Wskaznik wedlug zastrz. 1. albo 2. znamieany tym. ze zawiera 1-5% tiosiarczanu sodu. 4. Wskaznik wedlug zastrz. 1 alboClaims 1. Indicator for the detection and semi-quantitative determination of peroxides, especially Tyumen's hydrogen peroxide, in that it contains compositions with a composition of 3-26% by weight of cobalt compounds. 10-62% sodium edetate, 3-55% buffer with a pH of? 10.5-15% of a polymer that is difficult to penetrate to atmospheric components and soluble in aqueous solutions, in the form of a film, the composition being applied to a hydrophilic material. or an anionic ion exchanger. 2. The indicator according to claims I. characterized by this. that it contains 0.01-0.5% of non-ionic detergent. 3. Indicator according to claims 1st or 2nd signs of this. that it contains 1-5% sodium thiosulfate. 4. The indicator according to claims 1 or 2. zaamieaay tym. ze zawiera 1-3% mocznika. h-lisr I P-PRI. Vikfci.l I20l-»/. len.; jiisi <\ PL2. I struck it off. that it contains 1-3% urea. h-lisr and P-PRI. Vikfci.l I20l - »/. flax.; jiisi <\ PL
PL20887978A 1978-08-03 1978-08-03 Indicator for detection and semi-quantitative determination of peroxides,especially hydrogen peroxide PL114675B2 (en)

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PL20887978A PL114675B2 (en) 1978-08-03 1978-08-03 Indicator for detection and semi-quantitative determination of peroxides,especially hydrogen peroxide

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PL114675B2 true PL114675B2 (en) 1981-02-28

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