SI21110A - Method and optical sensor for continous measurement of dissolved hydrogen peroxide - Google Patents
Method and optical sensor for continous measurement of dissolved hydrogen peroxide Download PDFInfo
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- SI21110A SI21110A SI200100317A SI200100317A SI21110A SI 21110 A SI21110 A SI 21110A SI 200100317 A SI200100317 A SI 200100317A SI 200100317 A SI200100317 A SI 200100317A SI 21110 A SI21110 A SI 21110A
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Abstract
Description
Področje tehnikeThe field of technology
Izum sodi v področje preizkušanja in analize materialov s pomočjo optičnih sredstev oziroma bolj natančno, metode in optični senzorji kot miniaturne naprave, ki omogočajo kontinuirano merjenje analita preko optičnih lastnosti indikatorja.The invention falls within the field of testing and analysis of materials by optical means, or more precisely, methods and optical sensors as miniature devices that allow continuous measurement of the analyte through the optical properties of the indicator.
Tehnični problemA technical problem
Tehnični problem je enostaven postopek in izdelava miniaturnega kemijskega optičnega senzorja, v katerem interakcija indikatorja z analitom omogoča spektrofotometrično merjenje vodikovega peroksida v širokem koncentracijskem območju. Interakcija se odraža v optičnih lastnostih indikatorja, ki se kažejo v spremembi intenzitete absorbance, pri čemer omogočajo zaznavo hitrih sprememb koncentracije. Naloga izuma je postopek izdelave, ki bo omogočal pripravo takšnega senzorja s senzorsko membrano, v kateri se indikator ne bo izpiral ob stiku z analitom in bo imela visoko občutljivost za vzorec ter dobro ponovljivost priprave senzorske membrane. Senzorska membrana mora imeti široko koncentracijsko območje, hitre odzivne čase, stabilnost, reverzibilnost, enostavno imobilizacijo indikatorja v sol-gel material in enostavno pripravo senzorja.The technical problem is a simple process and the manufacture of a miniature chemical optical sensor in which the interaction of the indicator with the analyte enables spectrophotometric measurement of hydrogen peroxide over a wide concentration range. The interaction is reflected in the optical properties of the indicator, which are reflected in changes in the absorbance intensity, allowing the detection of rapid changes in concentration. It is an object of the invention to provide a manufacturing method for the preparation of such a sensor with a sensor membrane, in which the indicator will not be flushed upon contact with the analyte and will have high sample sensitivity and good repeatability of preparation of the sensor membrane. The sensor membrane must have a wide concentration range, fast response times, stability, reversibility, easy immobilization of the indicator into sol-gel material and easy preparation of the sensor.
Znano stanje tehnikeThe prior art
Do sedaj objavljeni in patentirani izdelki zajemajo predvsem določanje vodikovega peroksida v raztopini. US patent št. 4,647,532 opisuje visoko občutljivo metodo za določanje H2O2 s kemiluminiscenco brez interferenc komponent iz živega organizma. Določanje temelji na reakciji H2O2 z oksidirano nefluorescentno substanco ob prisotnosti oksidiranega katalizatorja, ki spremeni nefluorescentno substanco v fluorescentno obliko, ki reagira z diestrom oksalne kisline in H2O2 ob prisotnosti inhibitorja, kateri inaktivira oksidirani katalizator in se meri količina pri tem nastale emitirane svetlobe.The published and patented products so far mainly cover the determination of hydrogen peroxide in solution. U.S. Pat. No. 4,647,532 describes a highly sensitive method for the determination of H2O2 by chemiluminescence without interference from living organism components. The determination is based on the reaction of H2O2 with an oxidized non-fluorescent substance in the presence of an oxidized catalyst that converts the non-fluorescent substance into a fluorescent form that reacts with an oxalic acid diester and H2O2 in the presence of an inhibitor that inactivates the oxidized catalyst and measures the amount of light emitted.
US 5,094,943 opisuje kolorimetrično določanje H2O2, ki nastane pri reakciji iz oksidaze proizvedenega H2O2 z dodatkom kromogena. Reakcija kromogena in H2O2 ob prisotnosti peroksidaze, ki jo navaja US 4,916,058, in merjenje absorbance v vidnem področju prav tako zajema kolorimetrično določanje.US 5,094,943 describes the colorimetric determination of H2O2 resulting from the oxidase reaction of H2O2 produced by the addition of chromogen. The reaction of chromogen and H2O2 in the presence of peroxidase, cited in US 4,916,058, and measurement of absorbance in the visual field also involves colorimetric determination.
Patent US 4,794,079 določuje H2O2 z fluorogenim diquinolonom in dihidrokumarinom, kateri dajejo visoko fluorescenčne produkte pri oksidaciji z H2O2 ob prisotnosti peroksidazno aktivnih substanc.U.S. Patent 4,794,079 provides H2O2 with fluorogenic diquinolone and dihydrocoumarin, which yield highly fluorescent products upon oxidation with H2O2 in the presence of peroxidase-active substances.
Naslednji patent EU 0 585 212 A2 opisuje pripravo senzorske membrane iz različnih polimerov: celuloze, etilacetata in polistirola ter indikatorja Rutenijev kompleks.The following EU patent 0 585 212 A2 describes the preparation of a sensor membrane of different polymers: cellulose, ethyl acetate and polystyrene and the indicator Ruthenium complex.
Ostale najbolj pogoste metode za določanje H2O2 poleg kemiluminiscence [1] in spektrofotometrije [2] vključujejo še spektrofluorometrijo [3], pretočne kontinuirane analize [4] in pretočno injeciranje [5].Other common methods for determining H2O2 in addition to chemiluminescence [1] and spectrophotometry [2] include spectrofluorometry [3], continuous continuous flow analyzes [4] and flow injection [5].
[1] P. Van Zoonen, D.A.Kamminga, C. Gooijer, N.H. Velthorst and R.W. Frei, A solid-state chemiluminescence detector for hydrogen peroxide based on immobilized luminophore, Analytica Chim. Acta, 174, pp. 151,1985.[1] P. Van Zoonen, D.A.Kamming, C. Gooijer, N.H. Velthorst and R.W. Frei, A solid-state chemiluminescence detector for hydrogen peroxide based on immobilized luminophore, Analytica Chim. Acta, 174, pp. 151,1985.
[2] P.A. Clapp and D.F. Evans, Spectrophotometric determination of hydrogen peroxide with leuco Patent Blue Violet, Analytica Chim. Acta 243, pp.217,1991.[2] P.A. Clapp and D.F. Evans, Spectrophotometric determination of hydrogen peroxide with leuco Patent Blue Violet, Analytica Chim. Acta 243, pp.217,1991.
[3] M. Zhou, Z. Diwu, N.P. Voloshina and R.P. Haugland, A stable nonfluorescent derivative of resorufin for the fluorometric determination of trače hydrogen peroxide, Anal.Biochem., 253, pp. 162,1997.[3] M. Zhou, Z. Diwu, N.P. Voloshina and R.P. Haugland, A stable nonfluorescent derivative of resorufin for the fluorometric determination of gossip hydrogen peroxide, Anal.Biochem., 253, pp. 162,1997.
[4] D. Priče, P.J. VVorsfold, R. Fauzi, Determination of hydrogen peroxide in sea water by flowinjection analysis with chemiluminescence detection, Analytica Chim.Acta, 298, pp.121,1994.[4] D. Stories, P.J. Vorsfold, R. Fauzi, Determination of hydrogen peroxide in sea water by flowinjection analysis with chemiluminescence detection, Analytica Chim.Acta, 298, pp.121,1994.
[5] D. Janasek, U. Spohn, D. Becmann, Novel chemiluminometric H2O2 sensor for the selective flow injection analysis, Sensors and Act. B 51, pp. 107,1998.[5] D. Janasek, U. Spohn, D. Becmann, Novel chemiluminometric H2O2 sensor for selective flow injection analysis, Sensors and Act. B 51, pp. 107,1998.
Opis rešitve tehničnega problemaDescription of solution to a technical problem
Bistvo metode in optičnega senzorja za kontinuirano merjenje raztopljenega vodikovega peroksida je v tem, da je za polimerno osnovo bil izbran sol-gel material zaradi optične prepustnosti, mehanske stabilnosti, kemijske inertnosti, fleksibilnosti pri oblikovanju senzorske konfiguracije in kot indikator Meldola Blue, ki je imobiliziran v polimerno osnovo z doping tehniko, pri čemer je izpiranje barvila manjše kot pri drugih tehnikah imobilizacije. Meldola Blue je uporabljen kot najprimernejši indikator, ker izniči večino interferenc ter ima visoko absorptivnost in topnost.The essence of the method and the optical sensor for continuous measurement of dissolved hydrogen peroxide is that the sol-gel material was selected for the polymeric base due to its optical permeability, mechanical stability, chemical inertness, flexibility in forming the sensor configuration and as an Meldola Blue indicator, which is immobilized to a polymer base with a doping technique, with the dye leaching being less than that of other immobilization techniques. Meldola Blue is used as the most appropriate indicator because it eliminates most interferences and has a high absorption and solubility.
Metoda in optični senzor za kontinuirano merjenje raztopljenega vodikovega peroksida po izumu bo v nadaljevanju opisan s pomočjo slik, ki kažejo:The method and optical sensor for continuous measurement of dissolved hydrogen peroxide according to the invention will be described below with the help of figures showing:
Slika 1 - shemo postopka za pripravo senzorske membrane.Figure 1 - Schematic of the process for preparing the sensor membrane.
Slika 2 - odzivnost senzorske membrane na raztopljen H2O2 pri pH 7 in njeno reverzibilnost pri izpostavitvi Na2S20s.Figure 2 - Response of the sensor membrane to dissolved H2O2 at pH 7 and its reversibility on Na2S20s exposure.
Kot prikazuje slika 1, se priprava izdelave optičnega senzorja s sol-gel senzorsko membrano začne z mešanjem indikatorja in etanola na magnetnem mešalniku. Temu koraku sledi dodajanje tetrametoksi Silana čemur sledi mešanje na ultrazvočnem mešalu v trajanju 5. minut pred dodatkom katalizatorja vodne raztopine HCI in končno 5 minutno mešanje na ultrazvočnem mešalu. Raztopina se gelira pri sobni temperaturi v zaprtih posodicah, preden so narejene senzorske membrane s potapljanjem okroglih stekelc v raztopino (sol). Filmi so se sprva sušili 5 dni pri sobni temperaturi, nato pa še 24 h pri 50 °C.As shown in Figure 1, the preparation of the optical sensor fabrication with the sol-gel sensor membrane begins by mixing the indicator and ethanol on a magnetic stirrer. This step is followed by the addition of tetramethoxy Silane followed by stirring on an ultrasonic mixer for 5 minutes before adding an HCI aqueous solution catalyst and finally mixing for 5 minutes on an ultrasonic mixer. The solution is gelled at room temperature in sealed containers before sensor membranes are made by immersing the round slides in the solution (salt). The films were first dried at room temperature for 5 days and then at 50 ° C for 24 h.
Reakcija indikatorja z H2O2 se odraža v optičnih spremembah, ki se kažejo v spremembi absorbance, katera je sorazmerna koncentraciji H2O2. Absorbanca je bila merjena s spektrofotometrom (Ocean Optics SD2000). Halogenska žarnica je služila kot izvor svetlobe. Svetloba potuje preko optičnega vlakna do pretočne celice, v katero je montirana senzorska membrana, in naprej preko drugega optičnega vlakna do detektorja v spektrofotometru. Dotok H2O2 omogoča peristaltična črpalka, katere hitrost je bila konstantna 1 ml/min.The reaction of the indicator with H2O2 is reflected in the optical changes that result in a change in absorbance that is proportional to the H2O2 concentration. Absorbance was measured with a spectrophotometer (Ocean Optics SD2000). The halogen bulb served as the light source. The light travels through the optical fiber to the flow cell into which the sensor membrane is mounted, and then through the second optical fiber to the detector in the spectrophotometer. The supply of H2O2 was made possible by a peristaltic pump whose rate was constant at 1 ml / min.
Graf na sliki 2 prikazuje odzivnost senzorske membrane po izumu na raztopljen H2O2 pri pH 7 in njeno reverzibilnost pri izpostavitvi Na2S20s. Relativna sprememba signala (ΔΙ) med koncentracijama 10'8 in 10-1 M je 20% celotne spremembe signala, odzivni čas tgs (čas za dosego 95% celotne spremembe signala je 1.5 min). Senzorska membrana kaže -95% reverzibilnosti signala dobljenega z 10'1 in -90% z 10-s M vodikovim peroksidom.The graph in Figure 2 shows the responsiveness of the sensor membrane of the invention to dissolved H2O2 at pH 7 and its reversibility upon exposure to Na2S20s. The relative change in the signal (ΔΙ) to a concentration of 10 "8 and 10 of 1 M, 20% of the total signal change, the response time of TGS (time to reach 95% of the total signal change is 1.5 min). The sensor membrane exhibits -95% of the signal reversibility obtained with 10 ' 1 and -90% with 10-M hydrogen peroxide.
V spodnjem proizvedenem postopku je navedena receptura za pripravo senzorske membrane po sliki 1.The procedure below for the preparation of the sensor membrane according to Figure 1 is provided.
Primer 1:Example 1:
mg barvila raztopimo v 2.5 ml etanola, dodamo 2 ml tetrametoksisilana in 1 ml HCI (pH=3). Po geliranju v zaprtih posodicah naredimo membrane s potapljanjem na površino okroglih stekelc (φ 20 mm). Sušimo 5 dni na zraku pri sobni temperaturi in 24 h pri 50 °C.mg of the dye is dissolved in 2.5 ml of ethanol, 2 ml of tetramethoxysilane and 1 ml of HCl (pH = 3) are added. After gelation in sealed containers, membranes are made by dipping them onto the surface of the round slides (φ 20 mm). It is air-dried at room temperature for 5 days and at 50 ° C for 24 hours.
SKLEPICONCLUSIONS
1. Metoda za določanje H2O2 zajema:1. The method for the determination of H2O2 shall include:
a) enostavno pripravo senzorske membrane z imobilizacijo indikatorja v polimerno osnovoa) simple preparation of the sensor membrane by immobilization of the indicator into the polymer base
b) senzorska membrana iz točke a) je bila pripravljena iz sol-gel materialab) The sensor membrane referred to in point a) was prepared from sol-gel material
c) Meldola Blue je najprimernejši indikator za imobilizacijo v sol-gel materialc) Meldola Blue is the most appropriate indicator for immobilization into sol-gel material
2. Odzivnost senzorske membrane po sklepu 1 na H2O2 je bila določena z merjenjem absorbance.2. The response of the sensor membrane according to Decision 1 to H2O2 was determined by measuring the absorbance.
3. Reverezibilnost senzorske membrane je bila dosežena z izpostavitvijo le-te raztopini Na2S2Os.3. The reversibility of the sensor membrane was achieved by exposure to the Na2S2Os solution.
4. Senzorska membrana izvedena po sklepu 1 je primerna za določanje raztopljenega H2O2 v širokem koncentracijskem območju od 10-® do 0.7 M.4. The sensor membrane made according to decision 1 is suitable for the determination of dissolved H2O2 over a wide concentration range of 10-® to 0.7 M.
Senzorska membrana optičnega senzorja za merjenje vodikovega peroksida je bila razvita z imobilizacijo indikatorskega redoks barvila v sol-gel material. Barvilo v neposrednem stiku z analitom, vodikovim peroksidom, spremeni optične lastnosti, ki jih merimo. Indikatorje imobiliziran v sol-gel material. Senzorske membrane so pokazale velike spremembe signala ter hitre odzivne čase v širokem koncentracijskem območju 10-® - 0.7 M kot prikazuje slika 2.The optical membrane sensor membrane for hydrogen peroxide measurement was developed by immobilizing the indicator redox dye into sol-gel material. The dye in direct contact with the analyte, hydrogen peroxide, alters the optical properties being measured. Indicators immobilized in sol-gel material. The sensor membranes showed large signal changes and fast response times over a wide concentration range of 10-® - 0.7 M as shown in Figure 2.
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WO2012071019A1 (en) | 2010-11-26 | 2012-05-31 | IOS, Inštitut za okoljevarstvo in senzorje, d.o.o. | Sol-gel based optical chemical sensor for detection of organophosphates and method for preparation thereof |
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Cited By (1)
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WO2012071019A1 (en) | 2010-11-26 | 2012-05-31 | IOS, Inštitut za okoljevarstvo in senzorje, d.o.o. | Sol-gel based optical chemical sensor for detection of organophosphates and method for preparation thereof |
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