EP1389303A2 - Moyen et procede pour determiner la presence d'un acide sulfureux dans des liquides - Google Patents

Moyen et procede pour determiner la presence d'un acide sulfureux dans des liquides

Info

Publication number
EP1389303A2
EP1389303A2 EP02730197A EP02730197A EP1389303A2 EP 1389303 A2 EP1389303 A2 EP 1389303A2 EP 02730197 A EP02730197 A EP 02730197A EP 02730197 A EP02730197 A EP 02730197A EP 1389303 A2 EP1389303 A2 EP 1389303A2
Authority
EP
European Patent Office
Prior art keywords
sample
test strip
sulfite
test
acid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
EP02730197A
Other languages
German (de)
English (en)
Inventor
Karl-Dieter Krenn
Dieter Tanzer
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Merck Patent GmbH
Original Assignee
Merck Patent GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Merck Patent GmbH filed Critical Merck Patent GmbH
Publication of EP1389303A2 publication Critical patent/EP1389303A2/fr
Ceased legal-status Critical Current

Links

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
    • G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
    • G01N31/223—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators for investigating presence of specific gases or aerosols
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00—Chemistry: analytical and immunological testing
    • Y10T436/18—Sulfur containing

Definitions

  • the invention relates to a method for determining the content of sulfurous acid in liquids, in particular in beverages, in which the
  • Determination in the gas space above the sample is carried out using a test stick, and a corresponding test kit.
  • sulfur dioxide or sulfites to foods, referred to in technical jargon as "sulfur", is a frequently used one
  • the sulfurous acid is released in the wine and bound to various ingredients. All forms of state result in the total sulphurous acid.
  • the bound sulphurous acid is the difference between the total sulphurous acid and the free sulphurous acid.
  • potato products may contain up to 100 mg of sulfur dioxide per kilogram.
  • maximum levels of total sulfurous acid are permitted:
  • Grape juice may only contain 10 mg / l.
  • the determination of the sulfurous acid content is therefore of great importance in food analysis, especially in wine analysis.
  • Direct titration methods have the major disadvantage that the determination is disturbed by other reductones in the sample (eg ascorbic acid) and over-results result.
  • the intrinsic coloration of a sample eg red-colored juices
  • the determination is very complex and time-consuming. The determination can only be carried out by specialist personnel and requires appropriate equipment.
  • test sticks In recent times, analysis with solid, absorbent carriers, the so-called test sticks, has become increasingly important.
  • the main advantages of this dry chemical process include, in particular, simple handling and easy disposal due to the small amounts of reagent. All or most of the reagents required for the detection reaction are embedded in appropriate layers of a solid, absorbent or swellable carrier to which the sample is applied. After the reaction zone has come into contact with the sample, the detection reaction takes place.
  • the color formed is a measure of the amount of the analyte to be determined and can be visual, i.e. can be evaluated semi-quantitatively or quantitatively with simple reflectometers.
  • Test strips for the determination of sulfite are commercially available (e.g. Merck MQ or RQ sulfite test, Art. 1.10013 or 1.16987).
  • the test sticks are immersed in the sample for analysis. After suitable sample preparation, a determination of the free and total sulphurous acid is possible (e.g. Merck RQ sulfite test in wine, Art. 1.16122).
  • test strips A major disadvantage of these test strips is that the detection in the range below approx. 30 mg / l SO 2 cannot be carried out with sufficient accuracy. Use with colored samples, such as red wines, is not possible due to the interference caused by the sample's own color.
  • decolorization of the sample with the aim of undisturbed detection using known decolorizing agents is usually carried out with sulfite Loss associated and can not be done before the sulfite analysis.
  • the object of the present invention is to provide a method for the determination of sulfurous acid in aqueous samples which does not have the above disadvantages, which is simple and quick to implement and inexpensive.
  • the method according to the invention should not only be accessible to a semi-quantitative, visual evaluation, but also to a quantitative evaluation with a reflectometer.
  • the present invention therefore relates to a method for the determination of sulfurous acid in aqueous samples, characterized by the following method steps:. Providing a closable sample vessel;
  • the sample is first acidified before the test strip is introduced into the gas space.
  • acidification is only slight.
  • the sample is mixed usually with larger amounts of strong acids or preferably first with caustic to liberate bound S0 2 and then with acid to drive off the SO 2 from the solution.
  • the sample is acidified with sulfuric acid.
  • test strip is wetted with a buffer which has a pH between 8 and 10.
  • test strip is wetted with imidazole buffer.
  • test strip is analyzed reflectometrically.
  • a test strip is used on which sulfite is detected as Nas [Fe (CN) 5 SO 3 ].
  • the present invention also relates to a test kit for carrying out the method according to the invention, which at least consists of a test strip for sulfite analysis and a sealable container.
  • the test kit additionally contains acid for acidifying the sample.
  • test kit additionally contains buffer solution for wetting the test strip.
  • Figure 1 shows possible embodiments of the sample vessel for the test kit according to the invention.
  • the method according to the invention for the determination of sulfurous acid in aqueous solutions is based on a selective detection with an appropriately pretreated test strip in the gas phase above the
  • the SO 2 content in the gas phase above the sample is a measure of the concentration of sulfite in the sample.
  • the detection system is in the form of an impregnated matrix, ie all the reagents required for the selective detection of sulfite (coloring reagent, buffer system, possibly also stabilizers and solubilizers) are embedded in an absorbent carrier. The resulting color reaction is evaluated reflectometrically or visually by comparison with a color card.
  • test sticks for sulfite analysis used according to the invention have a reagent system for sulfite detection. All reagent combinations that lead to a sulfite-selective detection reaction are possible as a detection system. Detection as Na 5 [Fe (CN) 5 SO 3 ] to form a red color is particularly preferred. A possible reagent system for this detection is a mixture of potassium hexacyanoferrate (II), zinc sulfate and nitroprusside sodium. Another possibility for the detection of sulfite is the decolorization of malachite green or fuchsin.
  • absorbent carrier All materials which are usually used for such tests can be used as the absorbent carrier.
  • filter paper is most widespread, but other absorbent cellulose or plastic products can also be used.
  • the absorbent carriers are impregnated in a known manner with impregnation solutions which contain all the reagents necessary for the determination of sulfite.
  • the soaked and dried papers can be suitably cut and glued or sealed onto carrier films in a known manner.
  • test stick reagent system To enable the test stick reagent system, it must be moistened before the reaction. Water has proven to be suitable in principle for moistening. Surprisingly, it was found that moistening with a buffer system in the pH range from 8 to 10 leads to particularly high sensitivity and uniform discoloration on the
  • Suitable buffer systems for adjusting the pH are those that are compatible with the other components of the test and do not interfere with the detection reaction. All systems that set the desired pH range, such as phosphate buffers or Tris buffers, are suitable as buffer systems. Buffer systems based on amines, particularly preferably heterocyclic amines, are also very suitable. Examples of particularly suitable buffer systems are imidazole, 1-methylimidazole, 2-methylimidazole, pyrazole, pyrimidine, pyridazine, piperazine, triazole and triazine buffers, or derivatives or mixtures thereof.
  • the solvents used are preferably water or mixtures of alcohols, typically branched or unbranched C1 to C6 alcohols, or of glycerol with water in question.
  • An alcoholic imidazole buffer is particularly preferred which has an imidazole content of 0.1-2.5% by weight and an alcohol content in the range of 25-75% by volume.
  • buffer systems based on amines especially heterocyclic amines, especially imidazole buffers, have a stabilizing effect on the color effect of the developed test strip. Especially in analyzes in which the development and evaluation of the test strip takes more than 5 to 10 minutes, the test strip dries out and thus a possible
  • Sample vessel e.g. should remain for some time for a visual comparison or for documentation purposes.
  • the method according to the invention is preferably suitable for determining the free sulfurous acid in aqueous samples.
  • Free sulfite in the liquid sample solution can be determined directly with the moistened, sulfite-selective test stick.
  • the sensitivity of the detection system can be increased by slightly acidifying the sample solution. Acidification must be carried out in such a way that bound sulfuric acid is not released and is also recorded.
  • the concentration of the acids in the sample should be between 0.05 and 1 mol / l, preferably between 0.05 and 0.5 mol / l.
  • Sulfuric acid has proven to be particularly suitable.
  • the concentration of sulfuric acid in the sample should typically be in the range of 0.05 - 0.5 mol / l.
  • the bound portion of the sulfurous acid must first be released. This is typically done by treating the sample with larger concentrations of strong acid or by treating the sample with lye and subsequent addition of acid, optionally supported by additional heating.
  • a defined amount of the sample is placed in a closable sample vessel for the determination of the free sulfurous acid.
  • a test strip according to the invention is wetted with water or preferably buffer solution.
  • the sample is then preferably acidified slightly to increase the sensitivity, the test strip is introduced into the sample vessel such that it is located in the gas space above the sample solution, and the vessel is closed.
  • the sample is mixed with strong acid or first with alkali and then with acid and, if necessary, heated before the test strip is introduced in order to digest the sample and release the bound sulfuric acid.
  • an analysis kit according to the invention is particularly suitable for carrying out the method according to the invention.
  • This analysis kit contains at least one test strip for sulfite analysis and a closable sample container in which the test strip can be fixed in the gas space above the sample. It preferably also contains buffer solution for
  • the analysis kit can contain other components such as standard solutions, a description of the procedure or a color chart for visual evaluation.
  • sample vessels for the analysis kit according to the invention are shown schematically in Figure 1. They must be designed in such a way that a sufficiently large amount of aqueous sample (5) can be filled in and a sufficiently large one
  • a closable vessel is also understood to mean a vessel which has a small opening for introducing the test strip.
  • the test strip can be inserted and fixed into the vessel through an opening (3) in the lid. It is also possible to clamp the test strip, as shown in Figure 1 B, when closing the container at the edge of the lid.
  • Figure 1 C shows an embodiment in which the test strip is introduced into the vessel via a lateral opening (3) in such a way that the carrier zone (2) of the test strip points in the direction of the sample.
  • the method and the analysis kit according to the invention offer a sensitive possibility, free or free Determine bound sulfite in aqueous samples without great expenditure on equipment.
  • the analysis can also be carried out outside the laboratory within a few minutes, for example directly at the location of the sampling.
  • the method according to the invention offers the possibility of detecting sulfite contents up to approximately 0.1 mg / l quickly and easily.
  • the following impregnation solution is applied to a filter paper (Binzer, 1450 CV; acid-washed) and then dried with warm air.
  • the paper is melted with hot melt adhesive (e.g. adhesive Dynapol ® S 1401) sealed onto a white carrier film and suitably cut into strips so that a reaction zone of approx. 6 mm x 8 mm results.
  • hot melt adhesive e.g. adhesive Dynapol ® S 1401
  • Standard aqueous solutions are prepared by weighing appropriate amounts of sodium sulfite in distilled water.
  • test strips are evaluated after a suitable reaction time (5 minutes) in a small hand-held reflectometer on a diode basis (reflectometer RQflex ® ).
  • RQflex ® reflectometer
  • the method according to the invention is thus ideally suited for quick and sensitive checking of the SO 2 content.
  • test strips are evaluated after a suitable reaction time (5 minutes) in a small hand-held reflectometer on a diode basis (reflectometer RQflex ® ). The relationship between the measured relative reflectance (%) and the sulfite content is shown in Table 2.

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Biophysics (AREA)
  • Molecular Biology (AREA)
  • Dispersion Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

L'invention concerne un procédé et un kit de test pour déterminer la présence de sulfite, notamment libre, dans des échantillons aqueux. Placé dans un contenant fermé, l'échantillon est légèrement acidifié, de préférence avec de l'acide. Une bande de test permet de déterminer la teneur en sulfite dans la phase gazeuse au-dessus de l'échantillon. L'évaluation peut être visuelle ou réfractométrique. Le kit de test selon l'invention, destiné à la réalisation dudit procédé, comprend un contenant fermé et une bande de test pour l'analyse du sulfite.
EP02730197A 2001-05-23 2002-04-24 Moyen et procede pour determiner la presence d'un acide sulfureux dans des liquides Ceased EP1389303A2 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10125285 2001-05-23
DE10125285A DE10125285A1 (de) 2001-05-23 2001-05-23 Mittel und Verfahren zur Bestimmung von schwefliger Säure in Flüssigkeiten
PCT/EP2002/004491 WO2002095392A2 (fr) 2001-05-23 2002-04-24 Moyen et procede pour determiner la presence d'un acide sulfureux dans des liquides

Publications (1)

Publication Number Publication Date
EP1389303A2 true EP1389303A2 (fr) 2004-02-18

Family

ID=7685965

Family Applications (1)

Application Number Title Priority Date Filing Date
EP02730197A Ceased EP1389303A2 (fr) 2001-05-23 2002-04-24 Moyen et procede pour determiner la presence d'un acide sulfureux dans des liquides

Country Status (5)

Country Link
US (1) US20040147036A1 (fr)
EP (1) EP1389303A2 (fr)
AU (1) AU2002302565A1 (fr)
DE (1) DE10125285A1 (fr)
WO (1) WO2002095392A2 (fr)

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US9557307B2 (en) 2013-05-07 2017-01-31 Sommatic, Llc Beverage diagnostic and preservation devices and methods
US9864823B2 (en) 2015-03-30 2018-01-09 Uop Llc Cleansing system for a feed composition based on environmental factors
TWI593952B (zh) * 2016-08-15 2017-08-01 Ching Wu Wang Portable thermochromic device that detects the quality of air pH
US10545487B2 (en) 2016-09-16 2020-01-28 Uop Llc Interactive diagnostic system and method for managing process model analysis
TWI620923B (zh) * 2016-10-19 2018-04-11 邦睿生技股份有限公司 採集瓶與檢測樣品特性之方法
US10754359B2 (en) 2017-03-27 2020-08-25 Uop Llc Operating slide valves in petrochemical plants or refineries
US10678272B2 (en) 2017-03-27 2020-06-09 Uop Llc Early prediction and detection of slide valve sticking in petrochemical plants or refineries
US10794644B2 (en) 2017-03-28 2020-10-06 Uop Llc Detecting and correcting thermal stresses in heat exchangers in a petrochemical plant or refinery
US10752845B2 (en) 2017-03-28 2020-08-25 Uop Llc Using molecular weight and invariant mapping to determine performance of rotating equipment in a petrochemical plant or refinery
US10962302B2 (en) 2017-03-28 2021-03-30 Uop Llc Heat exchangers in a petrochemical plant or refinery
US11130111B2 (en) 2017-03-28 2021-09-28 Uop Llc Air-cooled heat exchangers
US10670353B2 (en) 2017-03-28 2020-06-02 Uop Llc Detecting and correcting cross-leakage in heat exchangers in a petrochemical plant or refinery
US10663238B2 (en) 2017-03-28 2020-05-26 Uop Llc Detecting and correcting maldistribution in heat exchangers in a petrochemical plant or refinery
US11396002B2 (en) 2017-03-28 2022-07-26 Uop Llc Detecting and correcting problems in liquid lifting in heat exchangers
US10695711B2 (en) 2017-04-28 2020-06-30 Uop Llc Remote monitoring of adsorber process units
US10913905B2 (en) 2017-06-19 2021-02-09 Uop Llc Catalyst cycle length prediction using eigen analysis
US11365886B2 (en) 2017-06-19 2022-06-21 Uop Llc Remote monitoring of fired heaters
US10739798B2 (en) 2017-06-20 2020-08-11 Uop Llc Incipient temperature excursion mitigation and control
US11130692B2 (en) 2017-06-28 2021-09-28 Uop Llc Process and apparatus for dosing nutrients to a bioreactor
US20190003978A1 (en) * 2017-06-28 2019-01-03 Uop Llc Process and apparatus to detect mercaptans in a caustic stream
US11194317B2 (en) 2017-10-02 2021-12-07 Uop Llc Remote monitoring of chloride treaters using a process simulator based chloride distribution estimate
AU2018345841A1 (en) * 2017-10-06 2020-05-21 The Research Foundation For The State University For The State Of New York Selective optical aqueous and non-aqueous detection of free sulfites
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US10901403B2 (en) 2018-02-20 2021-01-26 Uop Llc Developing linear process models using reactor kinetic equations
US10734098B2 (en) 2018-03-30 2020-08-04 Uop Llc Catalytic dehydrogenation catalyst health index
US10953377B2 (en) 2018-12-10 2021-03-23 Uop Llc Delta temperature control of catalytic dehydrogenation process reactors
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Also Published As

Publication number Publication date
WO2002095392A2 (fr) 2002-11-28
AU2002302565A1 (en) 2002-12-03
WO2002095392A3 (fr) 2003-01-30
US20040147036A1 (en) 2004-07-29
DE10125285A1 (de) 2002-11-28

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