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Overview of methods for determination of free sulfur dioxide in wine
When the concentration of sulfur dioxide in wine is high, it can be used as a bacteriostatic agent. However, if the content of sulfur dioxide in wine is too high, sulfur odor will be produced on the one hand. On the other hand, modern clinical medicine believes that excessive free sulfur dioxide can induce asthma in some people. And other allergic reactions. The relevant national standards stipulate that the residual amount of sulfur dioxide in fermented wine should be less than or equal to 0.01g/kg.
At present, the determination of sulfur dioxide in China mainly uses iodometric method, alkali titration method and colorimetric method. New detection methods such as fluorescence method, chemiluminescence method, electrochemistry and enzymatic method are also applied, and some new separation detection technologies, such as flow Injection, intermittent chemical analysis techniques, ion chromatography, gas diffusion membrane separation, capillary electrophoresis, and various types of sensors have developed rapidly.
The traditional manual analysis technology not only has high labor intensity, long analysis time, but also the result is easily affected by the analyst, and the error is large. At the same time, due to the use of toxic and harmful solution in the operation process, it is easy to cause great pollution to the environment. The manual photometric method and the discontinuous chemical analyzer method are compared below.
(1) Manual photometry:
Experimental principle: The sulfite (sulphur dioxide standard solution) forms a complex with the sodium tetrachloromercury absorbing solution, and the complex produces a color reaction in the color developing body system.
Instrument used: 721 domestic photometer
Experimental procedure: firstly prepare a sulfur dioxide standard solution, using n-hexanol as a defoaming agent, and adding 6 different concentrations of sulfur dioxide standard use liquid to the cold undegassed wine (prepared by adding a mercury stabilizer through a sulfur dioxide stock solution) Then add the pararosaniline hydrochloride solution separately, rotate and mix, then add formaldehyde solution to make up the volume. After the incubation for a period of time, the colorimetric solution without the standard solution was used as a reference, and the absorbance was measured at 550 nm to prepare a regression equation of the calibration curve. The sample blank was used as a reference. The absorbance of the sample was determined by the same method, and the sulfur dioxide content was calculated by linear regression equation of the calibration curve.
(2) Intermittent chemical analyzer method
Experimental principle: The sulfur dioxide standard solution and the color developer are added into the cuvette through the sampling needle to produce a color reaction, and the light transmission intensity is detected by a colorimeter, and the corresponding absorbance value is obtained, and the corresponding concentration is automatically calculated. All steps are controlled by computer to fully realize the mechanization and intelligence of the experimental process.
Intermittent chemical analyzer schematic
Instrument used: German CleverChem200 automatic interrupted chemical analyzer
Experimental procedure: The standard mother liquor, samples and reagents prepared in advance are placed in the corresponding standard position, sample position, reagent position, edit the work list, start the analysis, realize one-button start, no manual operation is required in the whole process, and the result is finally obtained.
Intermittent chemical analyzer working simulation diagram
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Combining the above two methods, we found that the discontinuous chemical analyzer method has advantages in terms of high degree of automation, low sample consumption, and low environmental pollution. The following table compares and summarizes the discontinuous chemical analyzer method and manual photometric method:
Comparison
Intermittent chemical analyzer
Manual photometry
Sample and reagent consumption
Only a small amount of sample and reagents (saving 90-99%) greatly reduces sample consumption, which means that the initial equipment cost can be compensated in a very short time.
Need to consume a lot of chemical reagents and laboratory water resources, high cost per analysis
Environmental hazard
Containing special equipment, it can reduce the harm of reagents to the environment, and use NaOH as the absorption liquid to reduce the harm to the environment.
The operation process uses toxic mercury tetrachloride, which is easy to cause mercury pollution to the environment.
Analysis speed
Up to 60 samples can be analyzed per hour, the measurement efficiency is obviously improved, the sample can be fully automated in large quantities, and no intervention by the operator is required during the analysis, completely eliminating the cumbersome chemical treatment process in the past.
The analysis speed is slow, and batch sample analysis cannot be realized. The analysis process is cumbersome and requires complicated chemical processing.
Accuracy and accuracy
The test results are more accurate, repeatable, and reduce human error because the sample uses the same mechanical transport process.
Detection accuracy and accuracy are greatly influenced by human factors, and different operators may produce different analysis results.
Detection limit
Thanks to the 24-bit digital detector, the detection limit is greatly reduced (ppb can be detected) and the measurement accuracy is higher.
With an ordinary optical detector, the resolution is greatly affected, and the detection limit of the instrument is high.
Automated operation
(1) It is equipped with an automatic liquid picker for automatic sampling.
(2) Automatically take reagents, realized by peristaltic pump or robot
(3) Automatic dilution, including automatic preparation of standard curve, analysis after automatic dilution of excess sample, can be realized by automatic diluter
(4) Automatic mixing of reagents or samples
(5) Automatic heating and guarantee constant temperature reaction
(6) Centralized control of data, including result printing, data calibration, and data storage.
(1) by manual sampling, taking reagents, and mixing reagents with samples
(2) The standard curve needs to be manually prepared. The sample exceeding the standard needs to be identified by the experimenter.
(3) The reaction cannot be controlled under constant temperature conditions.
(4) need to artificially digest and distill samples
(5) Data is calculated manually or by means of office software.