CN103163098A - Pit mud chromaticity measuring method - Google Patents
Pit mud chromaticity measuring method Download PDFInfo
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- CN103163098A CN103163098A CN2013100437004A CN201310043700A CN103163098A CN 103163098 A CN103163098 A CN 103163098A CN 2013100437004 A CN2013100437004 A CN 2013100437004A CN 201310043700 A CN201310043700 A CN 201310043700A CN 103163098 A CN103163098 A CN 103163098A
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Abstract
The invention relates to a pit mud chromaticity measuring method and belongs to the field of analysis and detection. The pit mud chromaticity measuring method comprises the following steps: a, at least three groups of standard solutions with different chromaticity values used for a colorimetric method are prepared, an absorbance value of each group of the standard solution is measured by adopting the colorimetric method on a portion with 280-330nm wave length, a standard curve is made, an equation of the standard curve is Y=k*X+g, wherein the k and the g are factors of the equation of the standard curve, Y is the chromaticity value, and X is the absorbance value; b, Mg pit mud is put in an Nm 1 solvent in a static state and filtered, filter liquor is diluted until the chromaticity value is smaller than 100 degrees, the dilution ratio is counted as J, the absorbance value of the filter liquor is measured by adopting the colorimetric method under 280-330nm wave length, according to the standard curve equation in the step a, and the chromaticity value of the filter liquor is counted as D. The pit mud chromaticity measuring method can accurately measure the chromaticity of the pit mud, the cost is low, and the measuring speed is high.
Description
Technical field
The present invention relates to store the assay method of mud colourity, belong to the analyzing and testing field.
Background technology
Mud cellar for storing things fermentation is one of characteristic of brewageing of aromatic Chinese spirit.Cellar for storing things mud forms certain organoleptic feature through long-term microbial action and Metabolite Accumulation, rubs the aspect such as ripe degree from color, smell and feel and can tentatively pass judgment on pit mud quality.Along with the cellar for storing things growth in age, cellar for storing things mud color is deepened gradually, and in the mud of cellar for storing things, the composition of microorganism also affects the color of cellar for storing things mud, so stores the performance that the mud color can embody cellar for storing things mud, is the important indicator of pit mud quality.The method of passing judgment at present cellar for storing things mud color is mainly by observing, and this method easily is subjected to the interference of human factor, and color can not well be distinguished when close.
At present, still do not have a kind of can Accurate Determining the relevant report of method of cellar for storing things mud colourity.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of method that can measure exactly cellar for storing things mud colourity.
Technical scheme of the present invention is:
The invention provides a kind of assay method of storing mud colourity, comprise the steps:
A, the known colourimetry standard solution of the different chromatic values of preparation at least three groups, absorbance in 280nm～every group of standard solution of 330nm wavelength place's employing colorimetric method for determining, make typical curve, the typical curve equation is Y=k * X+g (being Y=k*X+g), wherein, k, g are the coefficient in the typical curve equation, and Y is chromatic value, and X is absorbance; Thereby determine k, g value;
B, M g cellar for storing things mud is standing in N ml solvent, filter, gained filtrate is diluted to its chromatic value＜100 degree, extension rate is counted J, filtrate after dilution is adopted its absorbance of colorimetric method for determining under 280nm～320nm wavelength, the chromatic value that calculates filtrate according to the typical curve equation of a step is designated as D, so
Cellar for storing things mud chromatic value unit Wei Du ﹒ ml/g.
Preferably, the standard solution of seven groups of different chromatic values of preparation in a step, the preparation method is: first prepare chromatic value and be 500 titer, then dilution is 10,20,40,60,80, the 100 series standard solution of spending for chromatic value.
Preferably, the standard solution described in a step is platinum-cobalt titer or chromium-cobalt titer.
Preferred, the standard solution described in a step is chromium-cobalt titer.
Preferably, adopt 290nm～320nm wavelength in a step.
Preferably, the solvent described in the b step is water, toluene, ethanolic solution, acetone or sherwood oil.
Preferred, solvent described in the b step is that concentration is the acetone soln of 70～90wt%.
Preferably, in step b, the solid-to-liquid ratio of cellar for storing things mud and solvent is 1:7～9.
Preferably, in step b, cellar for storing things mud is standing front first with its fragmentation in solvent, and time of repose is 30～35min.
Preferably, in step b, gained filtrate is carried out the front process of colorimetric method for determining centrifugal treating, and the rotating speed of centrifugal treating is 4500-5500rmp, and centrifugation time is 10-15min.
Beneficial effect of the present invention:
The inventive method can be measured the colourity of cellar for storing things mud comparatively accurately, can be because of the different measurement results that affect of technician's sense organ.The inventive method operation steps is simple, and cost is lower, and finding speed is very fast.The present invention stores mud colourity for research a kind of new selection is provided, and has broad application prospects.
Embodiment
The method that the present invention measures cellar for storing things mud colourity can adopt following steps:
The titer of colourity (chromatic value is different) is determined in a, preparation, then dilution is the serial solution of different colourities, measure the absorbance of the serial solution of this difference colourity in 280nm～330nm wavelength place, make typical curve, the typical curve equation is Y=k*X+g, and wherein, k, g are the coefficient in the typical curve equation, Y is chromatic value, and X is absorbance;
B, with Mg store mud standing in the Nml solvent, filter, gained filtrate is diluted to its chromatic value＜100 degree, extension rate is counted J, filtrate after dilution is adopted its absorbance of colorimetric method for determining under 280nm～320nm wavelength, the chromatic value that calculates filtrate according to the typical curve equation of a step is designated as D, so
Cellar for storing things mud chromatic value unit Wei Du ﹒ ml/g.
In the present invention, filtrate colourity is not diluted with interior the needs at 100 degree, and surpassing 100 degree needs according to 2
nDilute, make the filtrate chromaticity range in 100 degree, with interior suitable with chromium cobalt typical curve, the gained test result is more accurate at 100 degree.
Preferably, the standard solution of seven groups of different chromatic values of preparation in a step, the preparation method is: first prepare chromatic value and be 500 titer, then dilution is 10,20,40,60,80, the 100 series standard solution of spending for chromatic value.A step standard solution can adopt colourimetry titer commonly used, as: platinum-cobalt titer or chromium-cobalt titer.Generally the colourity of titer is 500 degree.
Preferably, the standard solution in described a step is platinum-cobalt titer or chromium-cobalt titer.Chromium-cobalt titer more preferably.This is mainly because platinum-cobalt standard solution is not suitable for quantitative measurement in 10 °～100 ° scopes, so the described titer of a step is preferably chromium-cobalt titer.
Preferably, adopt 290nm～320nm wavelength in a step.
Preferably, the solvent described in the b step is water, toluene, ethanolic solution, acetone or sherwood oil.
Preferred, solvent described in the b step is that concentration is the acetone soln of 70～90wt%, because acetone is best to the extracting effect of cellar for storing things mud.
Preferably, in step b, the solid-to-liquid ratio of cellar for storing things mud and solvent is 1:7～9.
Preferably, in step b, cellar for storing things mud is standing front first with its fragmentation in solvent, and time of repose is 30～35min.
Preferably, in step b, gained filtrate is carried out the front process of colorimetric method for determining centrifugal treating, and the rotating speed of centrifugal treating is 4500-5500 (being preferably 5000) rmp, and centrifugation time is 10-15min.
The proposition of technical solution of the present invention is based on following principle: show certain color and luster on the mud sense organ of cellar for storing things, because in the mud of cellar for storing things, matter interaction, soil ulmin accumulation and microorganism long term Metabolite Accumulation form, select effective solvent that it is extracted, by measuring the colourity of leaching liquor, be converted into again at last cellar for storing things mud average chrominance.The determination of colority of cellar for storing things mud leaching liquor is based on ultraviolet/visible spectrophotometer method, by selecting best wavelength, makes the typical curve of colourity and absorbance, just can determine the colourity of leaching liquor.Ultraviolet/visible spectrophotometer method is to utilize the molecule of material or the Optical Absorption effect of a certain wavelength coverage of ion pair, material is carried out qualitative analysis, quantitative test and structure analysis, and the spectrum of institute's foundation is the light of specific wavelength in molecule or Ions Absorption incident light and the absorption spectrum that produces.Secondly, material has selectivity to Optical Absorption, utilizes measured matter the Optical Absorption of certain wavelength to be understood the characteristic of material, the basis of Here it is spectroscopic methodology.By measuring measured matter to the absorption intensity (absorbance) of different wave length, select optimal wavelength, under this wavelength condition, set up the typical curve of colourity and absorbance.
Below in conjunction with embodiment, the specific embodiment of the present invention is further described, does not therefore limit the present invention among described scope of embodiments.
The selection that test example 1 is soaked solvent
Respectively take 5.00g and store mud, adding respectively 25mL concentration is ethanol, distilled water, acetone, sherwood oil, the toluene immersion 10min of 95wt%, measures the dissolving situation of cellar for storing things mud pigment, as shown in table 1.
Table 1 cellar for storing things mud pigment solubility test result
As shown in Table 1, acetone lixiviate cellar for storing things mud pigment effect is best.
The selection of test example 2 time of repose
Respectively take 5.00g and store mud in the conical flask of 5 250mL, get 25mL acetone in four conical flasks with transfer pipet, set different soak time (20min, 25min, 30min, 35min, 40min), then filter, filtrate adopts ultraviolet/visible spectrophotometer to scan detection, and testing conditions is: reference liquid: acetone, wavelength coverage: 200nm～600nm, wavelength interval: 1nm, multiplicity: 1, Abs scope: 0.000nm～3.000nm.All-wave is grown the scope scanning result and is shown, soak time is 30min～35min, and it is maximum that the colourity in female poor leaching liquor reaches, and quite approaching, and the pigment of namely storing in mud is dissolved in solvent basically, therefore, chooses 30min～35min as cellar for storing things mud extraction time.
The selection of test example 3 leaching liquor treatment conditions
Get A, two parts of dissimilar cellar for storing things mud of B, respectively take 5.00g cellar for storing things mud in the conical flask of 4 250mL, respectively add acetone 25mL, aly in every type stir with glass bar, another part is not stirred (namely standing).Extraction time is 35min, filters; Measure respectively absorbance, result is as shown in table 2.
As can be seen from Table 2, stirring has larger broken ring effect to cellar for storing things mud pigment, therefore need not stir when lixiviate, only needs and will store the less of mud particle disposal, and standing extraction gets final product.
Respectively take in addition the dissimilar vinasse of 10.00g in the conical flask of 2 250mL, respectively add acetone 25mL, after stirring, extraction time is 35min.Two portions of leaching liquors of gained are respectively got half carry out respectively centrifugal treating, centrifugal condition is: the time: 10min～15min, rotating speed: 5000rpm.Measure respectively the absorbance of leaching liquor before and after centrifugal treating, result is as shown in table 2.
As can be seen from Table 2, centrifugal absorbance later increases.Reason is to contain the suspension granule in the mud leaching liquor of cellar for storing things, affects absorbance.Therefore, the absorbance of leaching liquor after centrifugal treating more can its absorbance of actual response.
The impact of table 2 leaching liquor treatment conditions on the leaching liquor absorbance
The selection of test example 4 solvent strengths
Respectively take 5.00g and store mud in the conical flask of 5 250mL, add respectively the acetone soln of 25mL variable concentrations (50,60,70,80,90,99.9wt%), soak time is 35min, after filtration, centrifugal treating (method of test example 3), measure absorbance, result is as shown in table 3.As can be seen from Table 3: concentration is that the acetone extracting effect of 70～90wt% is better.
The acetone solution of table 3 variable concentrations is stored mud pigment test findings
The selection of test example 5 wavelength
Preparation 500 degree color standard storing solutions: 500 ° of chromium cobalt standard solutions: accurately take potassium dichromate 0.0437g and cobaltous sulphate (CoSO
47H
2O) 1.000g is dissolved in a small amount of water, adds concentrated sulphuric acid 0.5mL, is diluted with water to 500mL.
Get respectively 500 ° of chromium cobalt standard solutions 0,0.5,1,2,4,6,8,10mL is in the 25mL color comparison tube, be diluted to scale with the optics purified water, shake up, the colourity of each pipe is respectively 10 °, 20 °, 40 °, 60 °, 80 °, 100 °, in 290～320 wavelength places, take pure water as blank, measure absorbance, drawing standard curve with the 1cm quartz colorimetric utensil.
Choose the optimal wavelength of the absorbance of measuring different colourity liquid, method is: the fixing cuvette that uses 1cm, the solution that employing ultraviolet/visible spectrophotometer is 10 °, 20 °, 40 °, 60 °, 80 °, 100 ° degree to the colourity that is diluted to chromium-cobalt standard solution in the scope of 200nm～600nm scans, analyze the linear relationship of colourity and absorbance, the final top condition of determining to measure colourity.Result shows that the absorption peak of two appears in the chromium/cobalt liquor of different colourities in the scope of 250nm～330nm, be two characteristic absorption peaks of potassium dichromate.Therefore near 260nm absorption peak is unstable, is chosen in the absorption peak at 280nm～330nm place.For determining the optimal wavelength condition, be 280nm～330nm in condition, the interval wavelength points is that 1nm scans, and determines that finally the determination of colority optimal wavelength is the scope of 290nm～320nm.
The selection of test example 6 solid-to-liquid ratios
Respectively take 5g cellar for storing things mud in 5 conical flasks, add respectively different volumes (be respectively 15,25,35,45,55ml) leaching liquor, leaching liquor concentration is 70～90wt%, and soak time is 30～35min.After filtration, centrifugal treating (method of test example 3), measure absorbance.Result is as shown in table 4.As can be seen from the table: solid-to-liquid ratio is that the extracting effect of 1:7～9 is best.
Table 4 different solid is than cellar for storing things mud pigment dissolving result
According to the above results, determine to measure the colourity of cellar for storing things mud, can adopt following method: take the cellar for storing things to be measured mud of 3～5g in the beaker container of 250mL, the acetone soln that adds respectively 70～90wt% of 7～9 times of volumes, vessel port seals with preservative film, shake gently every 10 during this time, soak 25～35min.Then filtration, centrifugal, leaching liquor adopts ultraviolet/spectrophotometer meter in 290nm～320nm place's survey its absorbance (acetone with 70～90wt% is done reference), (acetone of use 70～90wt% that leaching liquor colourity is larger dilutes according to 1/2n to be converted into the colourity of solution again, n is natural number, then change into corresponding colourity according to extension rate), be converted at last the colourity of storing mud.
Embodiment 1 adopts the inventive method to measure cellar for storing things mud (cellar for storing things wall mud) colourity
Preparation colourity is 500 chromium of spending-cobalt titers, then dilution is the serial solution of different colourities (colourity is 10,20,40,60,80,100 degree), measure the absorbance of the serial solution of this difference colourity in 300nm～320nm wavelength place, make typical curve, obtaining the typical curve equation is Y=k*X+g, and wherein, k, g are the coefficient in the typical curve equation, X is chromatic value, and Y is absorbance; Calculate k=0.0019, g=0.
Get cellar for storing things wall mud (cellar for storing things wall mud refers to store the cellar for storing things mud that is positioned in the pond on the perisporium of pond, cellar for storing things), be placed in sampling bag, take 5g in the 250ml conical flask, add 40ml acetone, lixiviate 30min filters that centrifugal (centrifugal condition: rotating speed is 5000rmp, and centrifugation time is 10～15min), filtrate is diluted 8 times (only needs filtrate colourity to dilute with interior the needs at 100 degree, over needing according to 2 in the present invention
nDilute, make the filtrate chromaticity range in 100 degree, spend with interior suitable with chromium cobalt typical curve 100, therefore test result is accurate), then survey light absorption value under 300nm～320nm condition, measurement result is: Y=0.180, and calculating leaching liquor colourity according to the typical curve equation is 94.74 degree (less than 100 degree), the colourity of storing wall mud is 6063.36 Du ﹒ ml/g.
Embodiment 2 adopts the inventive method to measure cellar for storing things mud (cellar for storing things bed mud) colourity
Get cellar for storing things bed mud (cellar for storing things wall mud refers to store the cellar for storing things mud that is positioned at bottom, pond, cellar for storing things in the pond), in sampling bag, take 5g in the 250ml conical flask, add 40ml acetone, lixiviate 30min, filter that centrifugal (centrifugal condition: rotating speed is 5000rmp, centrifugation time is 10～15min), dilute 8 times, survey light absorption value (acetone with 70～90wt% is done reference) under 300nm～320nm condition, measurement result is: Y=0.150, and calculating leaching liquor colourity according to the typical curve equation is 78.95 degree, the colourity of storing mud is 5052.63 Du ﹒ ml/g.
Embodiment 3 adopts the inventive method to measure cellar for storing things mud (pit skin mud) colourity
Get pit skin mud (pit skin mud refers to finish the rear cellar for storing things mud that is used for sealing Jiao Chi into the cellar for storing things), in sampling bag, take 5g in the 250ml conical flask, add 40ml acetone, lixiviate 30min, filter that centrifugal (centrifugal condition: rotating speed is 5000rmp, centrifugation time is 10～15min), dilute 8 times, survey light absorption value (acetone with 70～90wt% is done reference) under 300nm～320nm condition, measurement result is: Y=0.185, and calculating leaching liquor colourity according to the typical curve equation is 97.37 degree, the colourity of storing mud is 6231.68 Du ﹒ ml/g.
Claims (9)
1. the assay method of cellar for storing things mud colourity, is characterized in that, comprises the steps:
The colourimetry standard solution of a, the different chromatic values of preparation at least three groups, absorbance in 280nm～every group of standard solution of 330nm wavelength place's employing colorimetric method for determining, make typical curve, the typical curve equation is Y=k * X+g, wherein, k, g are the coefficient in the typical curve equation, and Y is chromatic value, and X is absorbance; Thereby determine k, g value;
B, M g cellar for storing things mud is standing in N ml solvent, filter, gained filtrate is diluted to its chromatic value＜100 degree, extension rate is counted J, filtrate after dilution is adopted its absorbance of colorimetric method for determining under 280nm～330nm wavelength, the chromatic value that calculates filtrate according to the typical curve equation of a step is designated as D, so
Cellar for storing things mud chromatic value unit Wei Du ﹒ ml/g.
2. the assay method of cellar for storing things according to claim 1 mud colourity, it is characterized in that, the standard solution of seven groups of different chromatic values of preparation in step a, the preparation method is: first preparing chromatic value is the titer of 500 degree, and then dilution is the series standard solution of 10,20,40,60,80,100 degree for chromatic value.
3. the assay method of cellar for storing things according to claim 1 and 2 mud colourity, is characterized in that, the standard solution described in step a is platinum-cobalt titer or chromium-cobalt titer.
4. the assay method of cellar for storing things according to claim 1 and 2 mud colourity, is characterized in that, adopts 290nm～320nm wavelength in a step.
5. the assay method of cellar for storing things according to claim 1 and 2 mud colourity, is characterized in that, the solvent described in step b is water, toluene, ethanolic solution, acetone or sherwood oil.
6. the assay method of cellar for storing things according to claim 5 mud colourity, is characterized in that, solvent described in step b is that concentration is the acetone of 70～90wt%.
7. the assay method of cellar for storing things according to claim 1 and 2 mud colourity, is characterized in that, in step b, the solid-to-liquid ratio of cellar for storing things mud and solvent is 1:7～9.
8. the assay method of cellar for storing things according to claim 1 and 2 mud colourity, is characterized in that, in step b, cellar for storing things mud is standing front first with its fragmentation in solvent, and time of repose is 30～35min.
9. the assay method of cellar for storing things according to claim 1 and 2 mud colourity, is characterized in that, in step b, gained filtrate is carried out before colorimetric method for determining through centrifugal treating, and the rotating speed of centrifugal treating is 4500-5500rmp, and centrifugation time is 10-15min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109916699A (en) * | 2019-03-29 | 2019-06-21 | 瓮福达州化工有限责任公司 | A kind of detection method of purifying phosphoric acid coloration |
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| EP1324016B1 (en) * | 2000-10-02 | 2007-11-14 | Jose Pascual Gracia Romeo | Colorimetric method for determining the color of wine from the grape |
| CN102095693A (en) * | 2010-12-31 | 2011-06-15 | 泸州品创科技有限公司 | Method for measuring chromaticity of vinasse |
| CN102175835A (en) * | 2011-01-26 | 2011-09-07 | 泸州品创科技有限公司 | Method for detecting pit age of strong aromatic distilled spirit pit mud |
| CN102226754A (en) * | 2011-03-29 | 2011-10-26 | 泸州品创科技有限公司 | Method for determining age of cellar mud of Luzhou-flavor liquor cellar |
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- 2013-02-01 CN CN201310043700.4A patent/CN103163098B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1324016B1 (en) * | 2000-10-02 | 2007-11-14 | Jose Pascual Gracia Romeo | Colorimetric method for determining the color of wine from the grape |
| KR20020088470A (en) * | 2001-05-17 | 2002-11-29 | 주식회사 소일테크 | Spectrophotometric determination method for residual chlorine in trap water |
| CN102095693A (en) * | 2010-12-31 | 2011-06-15 | 泸州品创科技有限公司 | Method for measuring chromaticity of vinasse |
| CN102175835A (en) * | 2011-01-26 | 2011-09-07 | 泸州品创科技有限公司 | Method for detecting pit age of strong aromatic distilled spirit pit mud |
| CN102226754A (en) * | 2011-03-29 | 2011-10-26 | 泸州品创科技有限公司 | Method for determining age of cellar mud of Luzhou-flavor liquor cellar |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109916699A (en) * | 2019-03-29 | 2019-06-21 | 瓮福达州化工有限责任公司 | A kind of detection method of purifying phosphoric acid coloration |
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