WO2002095392A2 - Mittel und verfahren zur bestimmung von schwefliger säure in flüssigkeiten - Google Patents
Mittel und verfahren zur bestimmung von schwefliger säure in flüssigkeiten Download PDFInfo
- Publication number
- WO2002095392A2 WO2002095392A2 PCT/EP2002/004491 EP0204491W WO02095392A2 WO 2002095392 A2 WO2002095392 A2 WO 2002095392A2 EP 0204491 W EP0204491 W EP 0204491W WO 02095392 A2 WO02095392 A2 WO 02095392A2
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- sample
- test strip
- sulfite
- test
- acid
- Prior art date
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.
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
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- Biophysics (AREA)
- Molecular Biology (AREA)
- Dispersion Chemistry (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
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Abstract
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP02730197A EP1389303A2 (de) | 2001-05-23 | 2002-04-24 | Mittel und verfahren zur bestimmung von schwefliger säure in flüssigkeiten |
AU2002302565A AU2002302565A1 (en) | 2001-05-23 | 2002-04-24 | Means and method for determining the content of sulfurous acid in liquids |
US10/477,591 US20040147036A1 (en) | 2001-05-23 | 2002-04-24 | Means and method for determining the content of sulfurous acid in liquids |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10125285A DE10125285A1 (de) | 2001-05-23 | 2001-05-23 | Mittel und Verfahren zur Bestimmung von schwefliger Säure in Flüssigkeiten |
DE10125285.4 | 2001-05-23 |
Publications (2)
Publication Number | Publication Date |
---|---|
WO2002095392A2 true WO2002095392A2 (de) | 2002-11-28 |
WO2002095392A3 WO2002095392A3 (de) | 2003-01-30 |
Family
ID=7685965
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2002/004491 WO2002095392A2 (de) | 2001-05-23 | 2002-04-24 | Mittel und verfahren zur bestimmung von schwefliger säure in flüssigkeiten |
Country Status (5)
Country | Link |
---|---|
US (1) | US20040147036A1 (de) |
EP (1) | EP1389303A2 (de) |
AU (1) | AU2002302565A1 (de) |
DE (1) | DE10125285A1 (de) |
WO (1) | WO2002095392A2 (de) |
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JP2008516221A (ja) * | 2004-10-08 | 2008-05-15 | ハネウェル アナリティクス アーゲー | ガス検知システム |
US20080085563A1 (en) * | 2006-10-10 | 2008-04-10 | Idexx Laboratories, Inc. | Detection of Gadolinium Chelates |
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 |
US10222787B2 (en) | 2016-09-16 | 2019-03-05 | Uop Llc | Interactive petrochemical plant diagnostic system and method for chemical process model analysis |
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US10678272B2 (en) | 2017-03-27 | 2020-06-09 | Uop Llc | Early prediction and detection of slide valve sticking in petrochemical plants or refineries |
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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 |
US11953479B2 (en) * | 2017-10-06 | 2024-04-09 | The Research Foundation For The State University Of New York | Selective optical aqueous and non-aqueous detection of free sulfites |
US11105787B2 (en) | 2017-10-20 | 2021-08-31 | Honeywell International Inc. | System and method to optimize crude oil distillation or other processing by inline analysis of crude oil properties |
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 |
CN110146487B (zh) * | 2019-06-11 | 2022-01-04 | 中国热带农业科学院分析测试中心 | 一种原位测定食品中总so2的方法 |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5578251A (en) * | 1978-12-11 | 1980-06-12 | Mitsubishi Chem Ind Ltd | Estimation method for sulfite ion and quantitative analysis unit |
US4543336A (en) * | 1982-02-12 | 1985-09-24 | Dragerwerk Aktiengesellschaft | Indicator for determining sulfur dioxide |
US4623613A (en) * | 1984-12-25 | 1986-11-18 | Konishiroku Photo Industry Co., Ltd. | Method of processing light-sensitive silver halide photographic material |
US4946705A (en) * | 1987-04-29 | 1990-08-07 | Assay Technologies, Inc. | Integrated exposure monitoring device |
EP0603657A2 (de) * | 1992-12-23 | 1994-06-29 | Willi Möller AG | Sensor zur Bestimmung von Sulfiten in flüssigen oder gasförmigen Medien und Verfahren zu dessen Herstellung |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH09315806A (ja) * | 1996-05-28 | 1997-12-09 | Mitsubishi Gas Chem Co Inc | 硫酸および過酸化水素を含む廃液からの硫酸の回収方法 |
-
2001
- 2001-05-23 DE DE10125285A patent/DE10125285A1/de not_active Withdrawn
-
2002
- 2002-04-24 US US10/477,591 patent/US20040147036A1/en active Pending
- 2002-04-24 AU AU2002302565A patent/AU2002302565A1/en not_active Abandoned
- 2002-04-24 EP EP02730197A patent/EP1389303A2/de not_active Ceased
- 2002-04-24 WO PCT/EP2002/004491 patent/WO2002095392A2/de not_active Application Discontinuation
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5578251A (en) * | 1978-12-11 | 1980-06-12 | Mitsubishi Chem Ind Ltd | Estimation method for sulfite ion and quantitative analysis unit |
US4543336A (en) * | 1982-02-12 | 1985-09-24 | Dragerwerk Aktiengesellschaft | Indicator for determining sulfur dioxide |
US4623613A (en) * | 1984-12-25 | 1986-11-18 | Konishiroku Photo Industry Co., Ltd. | Method of processing light-sensitive silver halide photographic material |
US4946705A (en) * | 1987-04-29 | 1990-08-07 | Assay Technologies, Inc. | Integrated exposure monitoring device |
EP0603657A2 (de) * | 1992-12-23 | 1994-06-29 | Willi Möller AG | Sensor zur Bestimmung von Sulfiten in flüssigen oder gasförmigen Medien und Verfahren zu dessen Herstellung |
Non-Patent Citations (2)
Title |
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DATABASE WPI Section Ch, Week 199808 Derwent Publications Ltd., London, GB; Class D15,Page 3, AN 1998-082429 XP002219240 & JP 09 315806 A (MITSUBISHI GAS CHEM CO INC), 9. Dezember 1997 (1997-12-09) * |
PATENT ABSTRACTS OF JAPAN vol. 004, no. 122 (P-025), 29. August 1980 (1980-08-29) & JP 55 078251 A (MITSUBISHI CHEM IND LTD), 12. Juni 1980 (1980-06-12) * |
Also Published As
Publication number | Publication date |
---|---|
AU2002302565A1 (en) | 2002-12-03 |
US20040147036A1 (en) | 2004-07-29 |
DE10125285A1 (de) | 2002-11-28 |
EP1389303A2 (de) | 2004-02-18 |
WO2002095392A3 (de) | 2003-01-30 |
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