CN109342433B - A kind of tartar potassium hydrogen phthalate Detection of Stability method - Google Patents
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Abstract
The present invention relates to a kind of tartar potassium hydrogen phthalate Detection of Stability methods, are characterized in that, step includes: S1, takes refrigerated cylinder wine to be detected in container；S2, container is placed under -4.5 DEG C of environment standing sedimentation 5-10 hours；S3, wine sample supernatant is taken, poured into clean triangular flask, triangular flask merging filled in the plastic beaker of -5 DEG C of brine ices, filtering, filtrate is injected in Clear glass bottles and jars；S4, wine to be frozen is kept into icing condition 7h under the conditions of -10 DEG C；S5, freezing wine liquid is placed in tap water at normal temperature and is thawed to no ice, be placed under the conditions of -4.5 DEG C of temperature, standing sedimentation 30min；S6, it is irradiated into darkroom with glare light electric torch, the wine body from all directions.Accuracy of the present invention is higher；Low with equipment input cost, achievable Multi-example detects simultaneously, the high advantage of detection efficiency.
Description
Technical field
The present invention relates to grape wine detection technique fields, specifically, being a kind of tartar potassium hydrogen phthalate stability inspection
Survey method.
Background technique
Biatrate is the highest salt of content in grape wine, and hypersaturated state is typically exhibited in grape wine, is being store
Biatrate will be slow crystallization and be precipitated during depositing, and occur often to make after grape wine bottling if this crystallization is precipitated
Consumer misunderstands.Therefore, the biatrate in grape wine is removed in advance in process of production, prevents from producing after bottling
Raw crystal settling is a very important wine production technology, and the hydrogen tartrate salt-stable of grape wine also becomes one
Important quality control index.
Because of the standard detecting method that tartar acid hydrogen salt stability is not unified, Production of Wine enterprise is taken all
It is respective empirical method.It the use of two kinds of more tartar acid hydrogen salt Detection of Stability methods is respectively at present freezing
With conductivity saturation temperature method.
Freezing principle: tartrate supersaturation is the reason of causing tartar to precipitate, to be dissolved according to tartrate
The characteristics of degree is reduced with the decline of temperature, whether there is or not crystalline deposits for observation after grape wine to be handled to a period of time at low temperature, come
Detect the tartar stability of grape wine.
Freezing operating process: after grape wine to be measured is taken advantage of cold filtering using 0.45um filter membrane or filter plate, -18 DEG C are placed in
In refrigerator, continue to be kept for icing condition 5 hours after wine liquid freezes completely, room temperature water-bath is thawed after taking-up, is existed immediately after defrosting
Whether electric torch for black room observation bottom of bottle has crystalloid precipitating, if determining tartar acid hydrogen salt without crystal settling
Qualified stability.
Conductivity saturation temperature method principle: the conductivity reflection unit volume grape wine effects of ion sum of grape wine
How much, and crystallizing can be such that conductive ion is precipitated from solution and conductivity is caused to decline, therefore can be with grape wine conductivity come body
Existing biatrate dissolves situation.Saturation temperature refers to corresponding temperature when liquid is in a saturated state, when fluid temperature is greater than
When saturation temperature, liquid unsaturation is stablized；When fluid temperature is lower than saturation temperature, liquid supersaturation, that is, unstable.Grape
The suitable storage temperature of wine national Specification grape wine is 5~25 DEG C, if stored according to national standard temperature requirement, as long as guaranteeing grape
Wine biatrate saturation temperature can guarantee that grape wine does not occur winestone precipitating on the market less than 5 DEG C.Potassium hydrogen tartrate is full
It is 5 DEG C with temperature setting, i.e., when the saturation temperature of grape wine is 5 DEG C and is following, then grape wine stablizes shape in biatrate
State.
Conductivity saturation temperature method operating process: after grape wine to be measured is taken advantage of cold filtering using 0.45um filter membrane or filter plate,
Conductivity, the every raising Conductivity Results of 0.5 DEG C of record of temperature are measured within the scope of 0~30 DEG C；Sample is dropped again
Temperature is added excessive potassium hydrogen tartrate and maintains -5 DEG C of stirring 1h, measure sample conductance within the scope of 0~30 DEG C again to -5 DEG C
Rate, the every raising Conductivity Results of 0.5 DEG C of record of temperature；Draw two within the scope of 0~30 DEG C conductance profiles, curve phase
Intersection point is saturation temperature, the then tartar acid hydrogen salt qualified stability when saturation temperature≤0 DEG C.
Freezing and conductivity saturation temperature method used at present respectively has advantage and disadvantage.Freezing advantage: detection device is simple,
Occupy it is artificial few, can multiple samples detect simultaneously；Disadvantage: detecting step is more, high to the skill requirement of reviewer, as a result by
Environment and operating process influence greatly, and accuracy rate is low.Conductivity saturation temperature method advantage: equipment reads data, detection by environment and
Operating process influence is small, can really reflect the tartar stability of wine；Disadvantage: detection device price is high, and an equipment is once only capable of
A sample is detected, detection efficiency is low.
Summary of the invention
The present invention is parameter and process optimization to be carried out on the basis of existing freezing, and then propose a kind of high accuracy Portugal
Grape wine biatrate Detection of Stability method, the detection method are more quasi- for the detection of tartar acid hydrogen salt stability
Really, guarantee wine product quality.
The technical solution adopted by the invention is as follows:
A kind of tartar potassium hydrogen phthalate Detection of Stability method, is characterized in that,
Its specific steps includes:
S1, take refrigerated cylinder wine to be detected in container；
S2, container is placed in -4.5 DEG C of temperature environments, standing sedimentation 5-10 hours；
S3, wine sample supernatant is taken, poured into clean triangular flask, the plastics that triangular flask merging fills -5 DEG C of brine ices are burnt
In cup, filter type when using production is filtered, and filtrate is injected in Clear glass bottles and jars；
S4, wine to be frozen is put into freezer compartment of refrigerator, icing condition 7h is kept under the conditions of -10 DEG C；
S5, freezing wine liquid is placed in tap water at normal temperature and is thawed to no ice, be placed under the conditions of -4.5 DEG C of temperature, it is heavy to stand
30min drops；
S6, it is irradiated into darkroom with glare light electric torch, the wine body from all directions has crystalloid precipitating, then determines Portugal
Grape wine hydrogen tartrate salt-stable is unqualified；There is no crystal settling, then determines tartar acid hydrogen salt qualified stability.
During the step S1 to step S2, if you need to transport wine liquid, it is used as and is turned using the incubator for being built-in with ice bag
Case is transported, the plastic bottle equipped with wine liquid is placed in the transport box and carries out transfer.
In the step S4, the timing starting point of the 7h is when freezing completely from wine sample.
In order to avoid being put into the vial of freezer compartment of refrigerator because frequently using bottom of bottle accumulation hydrogen tartrate k particle and impurity
Precipitating observation and result judgement are influenced, the vial for freezing has used every time first to be cleaned up with clear water, is subsequently poured into few
Dipping by lye bottom of bottle 5min is measured, places into ultrasonic cleaner and cleans up.
A kind of tartar potassium hydrogen phthalate Detection of Stability method of the invention, passes through the parameter and mistake to existing freezing
Cheng Youhua provides a set of more scientific accurate detection method, and this method is compared with traditional freezing, by grape wine cool stable
Accuracy rate of testing result is increased to 92.5% by 75%, and accuracy is higher；Compared with conductivity saturation temperature method, there is equipment investment
At low cost, achievable Multi-example detects simultaneously, the high advantage of detection efficiency.
Detailed description of the invention
Fig. 1: the conductance profile figure of sample 1；
Sequence 1: conductivity varies with temperature curve before wine sample addition potassium hydrogen tartrate (crystal seed)；Sequence 2: wine sample adds wine
Conductivity varies with temperature curve to stone potassium hydrogen phthalate (crystal seed) afterwards；
Fig. 2: the conductance profile figure of sample 9；
Sequence 1: conductivity varies with temperature curve before wine sample addition potassium hydrogen tartrate (crystal seed)；Sequence 2: wine sample adds wine
Conductivity varies with temperature curve to stone potassium hydrogen phthalate (crystal seed) afterwards；
Fig. 3: the conductance profile figure of sample 31；
Sequence 1: conductivity varies with temperature curve before wine sample addition potassium hydrogen tartrate (crystal seed)；Sequence 2: wine sample adds wine
Conductivity varies with temperature curve to stone potassium hydrogen phthalate (crystal seed) afterwards；
The Poreto figure of Fig. 4: 40 sample False Rates；
Fig. 5: cryogenic temperature X1 testing result residual plot；
Fig. 6: the interval graph (95% confidence interval of mean value) of testing result and cryogenic temperature；
Fig. 7: cooling time X2 testing result residual plot；
Fig. 8: the chart for individual values of testing result and cooling time；
Fig. 9: the box traction substation of testing result；
Figure 10: the interval graph of testing result and thawing mode；
Figure 11: the interval graph of testing result and wine sample temperature to be filtered；
Figure 12: refrigerating liquor sample volume X5 testing result residual plot；
Figure 13: cryogenic temperature X1 and cooling time X2 carries out the factor interactive analysis figure (Pareto of standardization effect
Figure responds and determines concordance rate, α=0.05 for Y)；
Figure 14: the response optimization analysis chart under conductivity Qualification；
Figure 15: the response optimization analysis chart in the unqualified situation of conductivity；
Figure 16: accuracy rate mean analysis result figure；
Figure 17: accuracy rate dispersion analysis result figure.
Specific embodiment
Specifically detecting for tartar potassium hydrogen phthalate Detection of Stability method of the present invention is provided below in conjunction with various charts
Journey, to there is more deep understanding to testing principle of the invention.
S1, it takes refrigerated cylinder wine to be detected in 350ml plastic bottle, is placed in the incubator of ice bag；
S2, it grape wine to be detected is placed in -4.5 DEG C of refrigerators carries out standing sedimentation, the time controlled at 5-10 hours；
S3, wine sample supernatant is poured into clean triangular flask, triangular flask is placed on to the plastics for filling -5 DEG C of brine ices
It in beaker, is operated according to Lange peristaltic pump operation sequence, was carried out with such as 606 filter plates of the filter plate with workshop same model
Filter, is injected into the Clear glass bottles and jars of 200ml；
S4, wine to be frozen is put into freezer compartment of refrigerator, icing condition 7h is kept under the conditions of -10 DEG C of temperature, it is described
The timing starting point of 7h is when freezing completely from wine sample；
S5, be placed in tap water at normal temperature thaw without ice after, take out under -4.5 DEG C of temperature environments, standing sedimentation 30min；
S6, it is irradiated into darkroom with glare light electric torch, the wine body from all directions.There is crystalloid precipitating, then determines Portugal
Grape wine hydrogen tartrate salt-stable is unqualified；There is no crystal settling, then determines tartar acid hydrogen salt qualified stability.
A kind of tartar potassium hydrogen phthalate Detection of Stability method of high accuracy provided in this embodiment, the shape of scheme
At mainly being realized by following process:
1, using the conductivity saturation temperature method testing result of high accuracy as true value, the accurate of existing freezing is determined
Rate is 75%.
2,25 impact factors for influencing freezing accuracy are obtained by IPO process analysis, are analyzed by causality matrix
Determine 6 important factors (cryogenic temperature, cooling time, frozen samples bottle cleanliness, defreezing method, wine sample temperature control to be filtered
System, wine sample volume), by quantitative screening determine 5 key factors (cryogenic temperature, cooling time, frozen samples bottle cleanliness,
Defreezing method, wine sample temperature to be filtered control), wherein key factor " frozen samples bottle cleanliness " is real by winning improvement means fastly
It is existing.The fast improvement means of winning refer to: in order to avoid being put into the vial of freezer compartment of refrigerator because frequently gathering winestone using bottom of bottle
Potassium hydrogen phthalate particle and the observation of impurity effect precipitating and result judgement, the vial for freezing has used every time first to be cleaned with clear water
Completely, it is subsequently poured into a small amount of dipping by lye bottom of bottle 5min, places into ultrasonic cleaner and cleans up.
3, DOE test is carried out to key factor " cryogenic temperature " and " cooling time ", determines that optimum combination parameter is " -10
DEG C, 7 hours "；Determine that thawing mode is " after water-bath is thawed after -4.5 DEG C of standing 30min by standard testing matrix preferred embodiment
Observation ", wine sample temperature control mode to be filtered are " sample to be filtered to be placed on -5 DEG C of brine bath heat preservations, filter process medium temperature
﹤ -3 DEG C of degree ".
4, freezing after improving is determined using the conductivity saturation temperature method testing result of high accuracy as true value again
Accuracy rate be 97.5%.
It is divided into several parts below, specifically introduces and probe into the detailed process to form detection method:
One, to the assessment of existing freezing
Because of the authenticity and accuracy of the testing result of conductivity saturation temperature method, the application is as testing result
True value is assessed and is optimized to existing method.
1, the definition of grape wine cool stable accuracy rate of testing result
Grape wine cool stable accuracy rate of testing result is set as Y；
The ratio that qualification is judged to unqualified (i.e. class Ⅰ malocclusion mistake) is set as y1;
The unqualified ratio for being mistaken for qualified (class Ⅱ malocclusion mistake) is set as y2.
Then: the total batch number of batch number/detection of Y=freezing and conductivity saturation temperature method testing result judgement consistency
×100%。
40 samples are chosen, carry out determination of stability with freezing and conductivity saturation temperature method respectively, as a result such as 1 institute of table
Show.In table, g: nodeless mesh precipitating；F: there is a small amount of crystalline deposit；Ff: there is moderate quatity crystalline deposit；Fff: there is mass crystallization heavy
It forms sediment.
Conclusion: 40 samples carry out determination of stability with freezing and conductivity saturation temperature method respectively, the results showed that,
In 30 pattern detection results it is consistent, 10 pattern detection results are inconsistent, wherein qualification is judged to unqualified (i.e. class Ⅰ malocclusion mistake)
7, qualification (i.e. class Ⅱ malocclusion mistake) 3 is mistaken for by unqualified.
It applies formula and obtains following data:
Y = 30/40 ×100% = 75%
y1 = 7/40 ×100% = 17.5%
y2 = 3/40 ×100% = 7.5%
It is using the testing result of the conductivity saturation temperature method of high accuracy as true value above, it is determined that existing freezing
The Detection accuracy of method is only 75%.
2, to the analysis of grape wine cool stable accuracy rate of testing result
From the testing result of 40 samples, the detection process of sample drawn 1, sample 9 and sample 31 carries out specific respectively
Analysis, and the conductivity detection data for providing above three sample changes and corresponding conductance profile figure.
The conductivity saturation temperature method testing result of sample 1 is as shown in table 2, and the conductance profile of sample 1 is as shown in Figure 1；
The result shows that the cold stabilization result of sample 1 is g, the judgement result of freezing and conductivity saturation temperature method is
Qualification, as a result unanimously, the biatrate test result of sample 1 are to stablize.
The conductivity saturation temperature method testing result of sample 9 is as shown in table 3, and the conductance profile of sample 9 is as shown in Figure 2；
The result shows that the cold stabilization result of sample 9 is g, freezing testing result is determined as qualification, conductivity saturation temperature
Method testing result is determined as unqualified, and as a result inconsistent, the biatrate test result of sample 9 is unstable.
The conductivity saturation temperature method testing result of sample 31 is as shown in table 4, the conductance profile of sample 31 such as Fig. 3 institute
Show；
The result shows that the cold stabilization result of sample 31 is fff, the testing result of freezing and conductivity saturation temperature method is equal
It is determined as unqualified, as a result unanimously, the biatrate test result of sample 31 is unstable.
Graphic analyses is carried out to the False Rate of 40 samples, the Poreto figure of False Rate refers to Fig. 4, available conclusion
Be: the erroneous judgement of cold stability inspection result concentrate on freezing testing result be f and g when, therefore, the main base of the analysis in later period
It is carried out in the vinosity of the state.
Two, the factor for influencing freezing testing result is explored
Based on the detection method of existing freezing, IPO flowsheet simulation is carried out to its process, and combine the factorial analysis side 5M1E
Method finds 25 controllable factors according to testing result effect, as listed in table 5:
Above-mentioned 25 factors are filtered out into 6 important factors and 5 key factors, 5 key factors by causality matrix
It is cryogenic temperature X1, cooling time X2, defreezing method X3, wine sample temperature X4 to be filtered, refrigerating liquor sample volume X5 respectively.
This influence of 5 key factors to testing result is made a concrete analysis of below by way of experiment.
1, influence of the cryogenic temperature X1 to testing result
Measurement index: x1(-10 DEG C, -20 DEG C, -30 DEG C)
Carry out the date: in September, 2017 20-25 days
[sample size]: totally 10
[measurer]: cold stability is examined
[measurement method]: freezing detection, range estimation precipitation capacity provide judgement result
Testing result residual plot is shown in Fig. 5, and the interval graph of testing result and cryogenic temperature is shown in Fig. 6；
[measurement conclusion]: cryogenic temperature X1 has a significant impact testing result, and X1 cryogenic temperature is key factor.
2, influence of the cooling time X2 to testing result
Measurement index: x2(3h, 5h, 8h, 16h)
Carry out the date: in September, 2017 12-16 days
[sample size]: totally 10
[measurer]: cold stability is examined
[measurement method]: freezing detection, range estimation precipitation capacity provide judgement result
Testing result residual plot is shown in Fig. 7, and the chart for individual values of testing result and cooling time is shown in Fig. 8, the box traction substation of testing result
See Fig. 9；
[measurement conclusion]: cooling time X2 has a significant impact testing result, and X2 cooling time is key factor.
3, influence of the thawing mode X3 to testing result
Measurement index: x3(water-bath is observed immediately after thawing, and is observed after -4.5 DEG C of placement 30min after water-bath is thawed, 10 DEG C
12h observation is placed after refrigerator defrosting)
Carry out the date: 9 days 27-10 months of in September, 2017
[sample size]: totally 10
[measurer]: cold stability is examined
[measurement method]: freezing detection, range estimation precipitation capacity provide judgement result
The interval graph of testing result and thawing mode is shown in Figure 10
[measurement conclusion]: thawing mode X3 has a significant impact testing result, and X3 thawing mode is key factor.
4, influence of the wine sample temperature X4 to be filtered to testing result
Measurement index: x4(-4.5 DEG C, 0 DEG C, 4.5 DEG C)
Carry out the date: 9 days 27-10 months of in September, 2017
[sample size]: totally 10
[measurer]: cold stability is examined
[measurement method]: freezing detection, range estimation precipitation capacity provide judgement result
The interval graph of testing result and wine sample temperature to be filtered is shown in Figure 11
[measurement conclusion]: wine sample temperature X4 to be filtered has a significant impact testing result, and X4 wine sample temperature to be filtered is to close
The key factor.
5, influence of the refrigerating liquor sample volume X5 to testing result
Measurement index: x5(100ml, 200ml, 400ml)；
Carry out the date: 10-15 days in October, 2017；
[sample size]: totally 10；
[measurer]: cold stability is examined；
[measurement method]: freezing detection, range estimation precipitation capacity provide judgement result；
Testing result residual plot is shown in Figure 12；
[measurement conclusion]: for refrigerating liquor sample volume X5 on testing result without influence, X5 refrigerating liquor sample volume is not key factor.
So far, the key factor for screening four influence testing results is cryogenic temperature X1, cooling time X2, solution respectively
Jelly mode X3 and wine sample temperature X4 to be filtered.
The present invention is by carrying out cryogenic temperature and cooling time excellent to cryogenic temperature, cooling time DOE experimental design
Change, determines reasonable parameter.Using standard testing matrix to thawing mode and the temperature controlled corrective measure of wine sample to be filtered into
Row scoring, chooses optimal case.
1, DOE experimental design is carried out to cryogenic temperature X1, cooling time X2, factorial experiment is horizontally disposed to be shown in Table 6, runs sequence
7 are shown in Table with test structure.
Factor interactive analysis is carried out to cryogenic temperature X1 and cooling time X2, analyzes the result is shown in Figure 13, as the result is shown
X1 cryogenic temperature acts on significantly result accuracy, and X2 cooling time is to the effect of result accuracy also close to significant, Ke Yijin
One step optimizes.
For carrying out response optimization analysis, response optimization device the result is shown in Figure 14 and Figure 15 under conductivity Qualification, as a result
Display cryogenic temperature is spent for -10, cooling time cold stable judgement accuracy highest when being 3 hours, but the condition is for conductivity
Then accuracy is very poor for unqualified situation, and global optimization effect is shown, cryogenic temperature is -10 DEG C, and cooling time detects when being 7h
Determine accuracy highest.Further progress mean value and dispersion analysis, analyze the result is shown in Figure 16 and Figure 17, and analysis freezes as the result is shown
Temperature is -10 DEG C, and cooling time is best when being 7h, is determined as optimal conditions.
2, it is scored using standard testing matrix the corrective measure of thawing mode X3 and wine sample temperature X4 to be filtered, is selected
Optimal case is taken, is shown in Table 8.
Determine that thawing mode preferred plan is to observe after -4.5 DEG C of placement 30min after water-bath is thawed by preferred embodiment, to
Filtering wine sample temperature control preferred plan is that sample to be filtered is placed on to -5 DEG C of brine bath heat preservations, temperature ﹤ -3 in filter process
℃。
Three, improvement project is determined
Cryogenic temperature X1---- cryogenic temperature is set as -10 DEG C；
Cooling time X2---- timing since wine sample freezes completely freezes 7h；
It is observed after -4.5 DEG C of placement 30min after thawing mode X3---- water-bath is thawed；
Sample to be filtered is placed in -5 DEG C of brine baths by wine sample temperature control X4---- to be filtered to be kept the temperature, wine sample temperature
< -3 DEG C.
Four, improvement effect is verified
Show that grape wine cool stable accuracy rate of testing result Y is increased to improved by 75% before improving by comparison
97.5%；The ratio y1 that qualification is judged to unqualified (i.e. class Ⅰ malocclusion mistake) is reduced to 2.5% by 17.5% before improving；It is unqualified to be mistaken for
The ratio y2 of qualified (class Ⅱ malocclusion mistake) is reduced to 0% by 7.5% before improving.
A kind of tartar potassium hydrogen phthalate Detection of Stability method of the invention, has the characteristics that following:
1, simple and easy, cost input is low；
2, it is verified using second method, can really reflect hydrogen tartrate salt-stable；
3, using analysis tools such as IPO process analysis, C & E matrix, quantitative screening and DOE tests to checkout procedure and inspection
It tests result to be analysed scientifically, detection method is more scientific, and inspection result accuracy is effectively ensured；
4, detection method gropes the analysis with science tools, the more scientific system of method by test data；
5, accuracy is higher compared with traditional freezing；
6, equipment input cost is low, it can be achieved that Multi-example detects simultaneously compared with conductivity saturation temperature method, detection efficiency
It is high.
Claims (4)
1. a kind of tartar potassium hydrogen phthalate Detection of Stability method, is characterized in that:
Its specific steps includes:
S1, take refrigerated cylinder wine to be detected in container；
S2, container is placed in -4.5 DEG C of temperature environments, standing sedimentation 5-10 hours；
S3, wine sample supernatant is taken, poured into clean triangular flask, triangular flask merging is filled to the plastic beaker of -5 DEG C of brine ices
In, it is filtered using with filter plate when Workshop Production with model, filtrate is injected in Clear glass bottles and jars；
S4, wine to be frozen is put into freezer compartment of refrigerator, icing condition 7h is kept under the conditions of -10 DEG C；
S5, freezing wine liquid is placed in tap water at normal temperature and is thawed to no ice, be placed under the conditions of -4.5 DEG C of temperature, standing sedimentation
30min；
S6, it is irradiated into darkroom with glare light electric torch, the wine body from all directions has crystalloid precipitating, then determines grape wine
Hydrogen tartrate salt-stable is unqualified；There is no crystal settling, then determines tartar acid hydrogen salt qualified stability.
2. a kind of tartar potassium hydrogen phthalate Detection of Stability method as described in claim 1, is characterized in that:
During the step S1 to step S2, using the incubator for being built-in with ice bag as transport box, wine liquid will be housed
Container, which is placed in the transport box, carries out transfer.
3. a kind of tartar potassium hydrogen phthalate Detection of Stability method as described in claim 1, is characterized in that:
In the step S4, the timing starting point of the 7h is when freezing completely from wine sample.
4. a kind of tartar potassium hydrogen phthalate Detection of Stability method as described in claim 1, is characterized in that:
Vial for freezing has used every time first to be cleaned up with clear water, and a small amount of dipping by lye bottom of bottle 5min is subsequently poured into,
It places into ultrasonic cleaner and cleans up.
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