CN103604803A - Method for rapidly detecting content of iron ion in red wine - Google Patents
Method for rapidly detecting content of iron ion in red wine Download PDFInfo
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- CN103604803A CN103604803A CN201310557025.7A CN201310557025A CN103604803A CN 103604803 A CN103604803 A CN 103604803A CN 201310557025 A CN201310557025 A CN 201310557025A CN 103604803 A CN103604803 A CN 103604803A
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Abstract
The invention provides a method for rapidly detecting content of iron ion in red wine. The method comprises the following steps: adding a stabilizer into a sample to be detected, mixing, adding a developing agent, and observing an iron ion developing strip through chromatography; calculating the content of iron ion according to the length of the iron ion developing strip. The stabilizer is added into a sample to be detected, so that the problem that the iron ion content is inaccurate in detection result and even cannot be detected because the developing agent and the red wine act to generate a precipitate in the prior art is solved. According to optimization and surface treatment, the resin selectively adsorb the iron and red color developed by the developing agent, and the color of the red wine is not adsorbed, so that the red wine is not needed to be discolored before detection. Moreover, the reagent and equipment adopted in the method are simple, and the detection cost is low; the detection period is short, the detection result can be rapidly obtained, and the method can be widely applied to rapid field detection.
Description
Technical field
The present invention relates to a kind of method of fast detecting iron ion content, specifically a kind of method of iron ion content in fast detecting red wine.
Background technology
In recent years, from the report of each quality testing department, can see, have in a large number underproof grape wine on market, wherein to exceed standard be one of subject matter to iron ion content.The content overproof of iron not only can affect mouthfeel, makes product occur precipitation, also accelerates oxidation vinous and the process that decays, and causes the qualities such as color vinous that large change occurs, and directly has influence on quality vinous.In addition human body excess intake or wrongly take excessive iron element and also may cause iron poisoning, produces infringement to the heart, liver and pancreas, affects healthy.In order to guarantee that quality vinous must be carried out deironing and iron content detects, the mandatory national standards GB15037 < < of People's Republic of China (PRC) grape wine > > stipulates iron content :≤8.0mg/L.
OIV's (International office of vine and wine is called for short OIV) has issued iron content examination criteria method in grape wine, adopts atomic absorption spectrography (AAS).This standard or World Trade Organization (WTO) be accepted standard aspect grape wine.China standard GB/T/T15038-2006 < < grape wine fruit wine universaling analysis method > > adopts respectively atomic absorption spectrophotometry, o-phenanthroline colourimetry and sulfosalicylic acid colourimetry.On the one hand, adopt instrument to detect, need to buy expensive instrument and equipment, conventional instrument and equipment has Atomic Absorption Spectrometer (AAS), icp ms (ICP-MS) etc. now, needs technical professional to operate simultaneously; On the other hand, while adopting colorimetric determination, conventional colorimetric determination utilizes exactly divalence or ferric ion and developer complexing to generate red complex and detects, and claret itself is exactly red, cannot demonstrate the color of iron complex at all, cannot directly carry out colorimetric detection, therefore two kinds of colourimetrys all need grape wine sample to carry out pre-treatment, Wet or dry method digestion, two kinds of equal complex steps of method, reagent dosage is large, consuming time longer; Moreover, no matter adopting which kind of method, normal sense cycle all needs more than 3 days, cannot meet the needs of fast detecting.
Document " conventional iron ion content exploration of analysis method " (Cheng Fangting etc., Treatment of Industrial Water, 2007,27,61-63) sum up the method for several fast detecting ferric ions, mainly contained sulfosalicylia acid spectrophotometry, Phen photometry and EDTA complexometry etc.Wherein, EDTA complexometry selectivity is not strong, may cause testing result seriously higher.Other method be all by chromogenic reagent and the reacted change color of ferric ion and standard color comparison card to recently judging the iron content in solution, for on-the site analysis, operate cumbersomely, and colorimetric resultant error is larger.In addition, because shown color mostly is red or orange after above-mentioned developer reacts with ferric ion, be difficult to distinguish with the color of orange, red liquid itself, so need to first decolour, then develop the color again, decolorization unavoidably can cause the loss of part ferric ion, and testing result error is large.The more important thing is, for red wine, owing to wherein containing a large amount of tannin class, phenols, alcohols and letones, complicated chemical reaction can occur after developer adds in red wine and produce deposit, cause colorimetric failure, can not accurately detect.
Summary of the invention
Technical matters to be solved by this invention is to provide the method for iron ion content in a kind of fast detecting red wine, to solve above-mentioned deficiency of the prior art, improves accuracy of detection, shortens sense cycle, reduces testing cost.
The scheme that the present invention solves the problems of the technologies described above is to provide the method for iron ion content in a kind of fast detecting red wine, comprise the following steps: (1) is got sample to be checked and added stabilizing agent to obtain mixed liquor I, described stabilizing agent comprises EDTA, pH adjusting agent, aluminium salt, nitrogen-containing compound, jelling agent; Described nitrogen-containing compound is selected from hydrazine class compound, contains amino-compound, amino-contained compound or nitrogen-containing heterocycle compound; (2) in described mixed liquor I, add developer to obtain mixed liquor I I; (3) will after the I of mixed liquor I described in step 2 colour developing, carry out chromatography, observe ferric ion colour developing band, according to ferric ion colour developing strip length, calculate iron ion content.
As a further improvement on the present invention, described chromatography is polymeric adsorbent column chromatography, and described polymeric adsorbent column chromatography resin used is the selective adsorption resin of grain diameter 1-100 micron.
The method of iron ion content in fast detecting red wine provided by the present invention, by add stabilizing agent in sample to be checked, solving in prior art developer and red wine does the used time and can generate and precipitate with the substance reaction such as tannin class, phenols, alcohols and ketone in red wine, cause the inaccurate problem that even cannot detect of iron ion content testing result, effectively improved testing result accuracy; After ferric ion colour developing, be adsorbed onto the fixing color in mutually of chromatography and red wine and carry color and can obviously distinguish by naked eyes, not needing decolorant is observable; Reagent that this method adopts and equipment are simple, do not need the high experimental facilitiess such as Atomic Absorption Spectrometer, and testing cost is cheap; This method sense cycle is short, can obtain fast testing result, can be widely used in field quick detection.
Accompanying drawing explanation
Fig. 1 is iron ion content working curve diagram.
Embodiment
In order to make technical matters to be solved by this invention, technical scheme and beneficial effect clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The method of iron ion content in fast detecting red wine of the present invention, comprises the following steps: (1) is got sample to be checked and added stabilizing agent to obtain mixed liquor I, and described stabilizing agent comprises EDTA, pH adjusting agent, aluminium salt, nitrogen-containing compound, jelling agent; Described nitrogen-containing compound is selected from hydrazine class compound, contains amino-compound, amino-contained compound or nitrogen-containing heterocycle compound; (2) in described mixed liquor I, add developer to obtain mixed liquor I I; (3) will after the I of mixed liquor I described in step 2 colour developing, carry out chromatography, observe ferric ion colour developing band, according to ferric ion colour developing strip length, calculate iron ion content.
Preferably, described chromatography is polymeric adsorbent column chromatography, and described polymeric adsorbent column chromatography resin used is the selective adsorption resin of grain diameter 1-100 micron.
Preferably, stabilizing agent comprises 0.005g/L-50g/L EDTA, 0.005g/L-100g/L aluminium salt, 0.005g/L-50g/L nitrogen-containing compound, 0.005g/L-50g/L jelling agent and pH adjusting agent.Wherein aluminium salt is selected from least one in aluminium bromide, aluminium sulphate, aluminum chloride, aluminium nitrate, aluminum fluoride; Hydrazine class compound is selected from least one in the alkyl derivative, phenylhydrazine, paranitrophenylhydrazine, dinitrophenylhydrazine of hydrazine, hydrazine; Containing amino/amine compound, be selected from fatty amine and the homologs thereof such as carbamic acid, carbamate and homolog thereof, aminobenzoic acid, anthranilate and homolog thereof, ethylenediamine and homolog thereof, amino-antipyrine and homolog thereof, methylamine, ethamine, propylamine, comprise monoamine, diamine, tertiary amine simultaneously; Described nitrogen-containing heterocycle compound is selected from the double heteroatoms heterogeneous ring compounds such as single heteroatoms heterogeneous ring compound such as pyrroles, furans, thiophene or azole.Jelling agent is selected from least one of Arabic gum, sodium alginate, sucrose fatty acid ester, gelatin, silica gel, polyvinylpyrrolidone.
Preferably, developer is 0.005g/L-50g/L Phen, 0.005g/L-50g/L vitamin c and damping fluid or 0.005g/L-50g/L thiocyanate, 0.005g/L-50g/L persulfate and pH adjusting agent.The pH value adjustable damping fluid of pH adjusting agent for coexisting with other materials arbitrarily, as the mixed solution of weak acid and salt thereof (HAc and NaAc), the mixed solution (NH of weak base and salt thereof
3h
2o and NH
4cl), the pH value of developer is 1-13, and preferably pH value is 6-8.
Preferably, also can will add in the sample impouring polymeric adsorbent chromatographic column to be checked of described stabilizing agent and developer, observe ferric ion colour developing band, according to colour developing strip length, calculate iron ion content in red wine.Described iron ion content height is linear positive correlation with variable color strip length, and national standard is limited the quantity of as 8ppm to the highest of ferric ion in grape wine, and the present invention has measured the working curve of the corresponding variable color strip length of 1-12ppm iron ion content c l relation, as shown in Figure 1.
More preferably, choose known iron concentration and be 8ppm red wine sample according to the present invention operation steps, according to test result, on resin column, delimit acceptance line.Whether the iron ion content that the method can detect red wine sample quickly and efficiently meets national standard restriction, has widespread use and is worth.
Similarly, the method of the invention can be different according to selected chromatography method, further optimize and have paper chromatography fast detection method, thin-layer chromatography detection method etc., described method all can be delimited acceptance line according to national standard, prepare corresponding device for fast detecting, be applied to field quick detection, there is widespread use value and great economy and be worth.
By a plurality of embodiment, the present invention is described further below, wherein red wine sample is stochastic buying gained on the market, is labeled as sample A, sample B, sample C.
S11: the preparation of stabilizing agent
Get EDTA0.25mg, aluminium nitrate 5mg, phenylhydrazine 5mg, Arabic gum 25mg join in the damping fluid of 5mL, regulate pH=7.0;
S12: the preparation of developer
Get Phen 1mg, vitamin c 0.5mg and join in the damping fluid of 5mL, regulate pH=7.0;
S13: iron ion content detects
Get 5mL red wine sample to be measured A, add wherein the stabilizing agent of S11 preparation gained, add the developer of S12 preparation gained after shaking up again, after shaking up, add resin column, measure the length of resin column variable color part, this length is directly proportional to iron content.Through contrasting with working curve, the iron ion content obtaining in red wine sample A is 2.5ppm.
S21: the preparation of stabilizing agent
Get EDTA15mg, aluminium nitrate 30mg, antipyrine 5mg, Arabic gum 30mg join in the damping fluid of 3mL, regulate pH=6.0;
S22: the preparation of developer
Get Phen 1mg, vitamin c 0.5mg and join in the damping fluid of 3mL, regulate pH=6.0;
S23: iron ion content detects
Get 5mL red wine sample to be measured B, add wherein the stabilizing agent of S21 preparation gained, add the developer of S22 preparation gained after shaking up again, after shaking up, add resin column, measure the length of resin column variable color part, this length is directly proportional to iron content.Through contrasting with working curve, the iron ion content obtaining in red wine sample B is 6.2ppm.
S31: the preparation of stabilizing agent
Get EDTA15mg, aluminium nitrate 30mg, phenylhydrazine 30mg, ethylenediamine 30mg, gelatin 30mg joins in the damping fluid of 3mL, regulates pH=8;
S32: the preparation of developer
Get potassium rhodanide 30mg, potassium persulfate 30mg and join in the damping fluid of 3mL, regulate pH=8;
S33: iron ion content detects
Get 5mL red wine sample to be measured B, add wherein the stabilizing agent of S31 preparation gained, add the developer of S32 preparation gained after shaking up again, after shaking up, add resin column, measure the length of resin column variable color part, this length is directly proportional to iron content.Through contrasting with working curve, the iron ion content obtaining in red wine sample B is 10.9ppm.
Comparative example 1 testing result accuracy comparison
Get red wine sample A, B, the C censorship identical with embodiment, censorship test result is respectively: 2.4ppm, 6.3ppm, 10.8ppm.To sum up, testing result deviation of the present invention is less than 3%, meets the actual needs that detect completely.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a method for iron ion content in fast detecting red wine, comprises the following steps: (1) is got sample to be checked and added stabilizing agent to obtain mixed liquor I, and described stabilizing agent comprises EDTA, pH adjusting agent, aluminium salt, nitrogen-containing compound, jelling agent; Described nitrogen-containing compound is selected from hydrazine class compound, contains amino-compound, amino-contained compound or nitrogen-containing heterocycle compound; (2) in described mixed liquor I, add developer to obtain mixed liquor I I; (3) will after the I of mixed liquor I described in step 2 colour developing, carry out chromatography, observe ferric ion colour developing band, according to ferric ion colour developing strip length, calculate iron ion content.
2. method according to claim 1, is characterized in that, described chromatography is polymeric adsorbent column chromatography, and described polymeric adsorbent column chromatography resin used is the selective adsorption resin of grain diameter 1-100 micron.
3. method according to claim 1, is characterized in that, described stabilizing agent comprises 0.005g/L-50g/LEDTA, 0.005g/L-100g/L aluminium salt, 0.005g/L-50g/L nitrogen-containing compound, 0.005g/L-50g/L jelling agent and pH adjusting agent.
4. method according to claim 1, is characterized in that, described developer is 0.005g/L-50g/L Phen, 0.005g/L-50g/L vitamin c and pH adjusting agent, and pH value is 6-8.
5. method according to claim 1, is characterized in that, described developer is 0.005g/L-50g/L thiocyanate, 0.005g/L-50g/L persulfate and pH adjusting agent, and pH value is 6-8.
6. method according to claim 1, is characterized in that, described aluminium salt is selected from least one in aluminium bromide, aluminium sulphate, aluminum chloride, aluminium nitrate, aluminum fluoride.
7. according to the method described in any one in claims 1 to 3, it is characterized in that, described hydrazine class compound is selected from least one in the alkyl derivative, phenylhydrazine, paranitrophenylhydrazine, dinitrophenylhydrazine of hydrazine, hydrazine.
8. according to the method described in any one in claims 1 to 3, it is characterized in that, the described amino/amine compound that contains is selected from carbamic acid, carbamate and homolog thereof, aminobenzoic acid, anthranilate and homolog thereof, ethylenediamine and homolog thereof, amino-antipyrine and homolog thereof, fatty amine and homolog thereof.
9. according to the method described in any one in claims 1 to 3, it is characterized in that, described nitrogen-containing heterocycle compound is selected from pyrroles, furans, thiophene, azole.
10. according to the method described in any one in claims 1 to 3, it is characterized in that, described jelling agent is selected from least one of Arabic gum, sodium alginate, sucrose fatty acid ester, gelatin, silica gel, polyvinylpyrrolidone, and the total concentration of described jelling agent is controlled at 0.005g/L-50g/L.
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| CN104792717A (en) * | 2015-05-05 | 2015-07-22 | 梧州市产品质量检验所 | Method of detecting iron content in metallic ores |
| CN109400756A (en) * | 2018-11-26 | 2019-03-01 | 广州大学 | A kind of hydroxyl radical reaction system prepares the preparation method of agaropectin oligose |
| CN109557016A (en) * | 2017-09-25 | 2019-04-02 | 上海梅山钢铁股份有限公司 | Reagent is used in a kind of low tin amount cold rolling electroplating tin steel plate surface corrosion active site detection |
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| CN112014386A (en) * | 2020-08-14 | 2020-12-01 | 湘潭华辰仪器有限公司 | Method for detecting content of trace iron in quartz sand |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104792717A (en) * | 2015-05-05 | 2015-07-22 | 梧州市产品质量检验所 | Method of detecting iron content in metallic ores |
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| CN109557016B (en) * | 2017-09-25 | 2021-07-09 | 上海梅山钢铁股份有限公司 | Method for detecting surface corrosion active points of low-tin-content cold-rolled electrolytic tin-plated steel plate |
| CN109400756A (en) * | 2018-11-26 | 2019-03-01 | 广州大学 | A kind of hydroxyl radical reaction system prepares the preparation method of agaropectin oligose |
| CN110865075A (en) * | 2019-12-31 | 2020-03-06 | 南通大学 | Conventional urinary iron detection kit and detection method thereof |
| CN112014386A (en) * | 2020-08-14 | 2020-12-01 | 湘潭华辰仪器有限公司 | Method for detecting content of trace iron in quartz sand |
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