CN104655519B - A kind of free water content assay method - Google Patents
A kind of free water content assay method Download PDFInfo
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Abstract
The present invention provides a kind of free water content assay method, and this method includes:Under constant temperature or Elevated Temperature Conditions, the mass value of different time sample is determined, wherein the constant temperature or the temperature range of heating are 20 DEG C~50 DEG C;Weight-loss curve is generated according to the mass value of measure, wherein, the abscissa of weight-loss curve is that time, ordinate are mass value;Moisture loss rate profile is obtained according to weight-loss curve, and obtains from moisture loss rate profile the peak value corresponding time;Mass value according to corresponding to weight-loss curve obtains the peak value correspondence time, the difference of mass value corresponding to the peak value correspondence time and the mass value corresponding to initial time in the weight-loss curve obtains the quality of Free water in sample, the method that the present invention is provided solves that determination data Stability and veracity when existing Abbe refractometer method is determined is poor and technical problem of the inapplicable relatively low sample of free water content, it can ensure that sample is determined in time simultaneously, and testing cost is low.
Description
Technical field
The present invention relates to a kind of detection technique, more particularly to a kind of free water content assay method.
Background technology
Free water, also known as unbound water, are primarily referred to as, in organism or the intracellular water that can be moved freely, being characterized in
It is more liquid, organism or cell can be left faster.
At present, the measure of free water content mainly has Abbe refractometer method and nuclear magnetic resonance method.Abbe refractometer method is base
The characteristics of Free water is more liquid, in the sucrose solution that sample is immersed to high concentration, Free water is gradually diffused into sample
In sucrose solution, the quantity reduced according to sucrose concentration calculates the quality of Free water in sample, the advantage of this method is operation letter
Single, measure expense is relatively low;Nuclear magnetic resonance method be with sample the H atom nuclear magnetic moment relaxation behavior of Free water with other hydrones
Based on difference, by monitoring the precession signal intensity that H atom nuclear magnetic moment in sample is produced, containing for Free water in sample is calculated
Amount, this method detection speed is fast, result is reliable and stable.
However, when determining free water content by Abbe refractometer method, it is impossible to which what is avoided is by sample and sucrose solution
Separation is weighed or determined, and the influence of micro Free water to sucrose solution is minimum, and small evaluated error will be significantly affected
Measurement result, therefore the Stability and veracity that this method is determined is poor;On the other hand, the concentration of sucrose solution is used in this method
Generally 40%~60%, then be inapplicable for the sample that moisture is less than 40%, because in sucrose solution
Water can infiltrate into sample;NMR belongs to large scale equipment, and most of research unit or enterprise set without such detection
It is standby to be measured, it is necessary to be sent to professional institution, it is difficult to ensure the promptness determined.Therefore, detected freely using nuclear magnetic resonance method
The problem of water content is present is to be difficult to detect sample in time, while detection is costly.
The content of the invention
The present invention provides a kind of free water content assay method, solves existing Abbe refractometer method measurement result accuracy
With stability is poor and the problem of inapplicable free water content relatively low sample, while the present invention can also ensure that sample is surveyed in time
Fixed, testing cost is low.
The present invention provides a kind of free water content assay method, and methods described includes:
Under constant temperature or Elevated Temperature Conditions, the mass value of different time sample is determined, wherein the constant temperature or heating
Temperature range is 20 DEG C~50 DEG C;
Weight-loss curve is generated according to the mass value of measure, wherein, the abscissa of the weight-loss curve is that time, ordinate are
Mass value;
Moisture loss rate profile is obtained according to the weight-loss curve, and from the moisture loss rate profile
It is middle to obtain the peak value corresponding time;
Mass value according to corresponding to the weight-loss curve obtains the peak value correspondence time, when according to the peak value to correspondence
Between corresponding mass value and the mass value corresponding to initial time in the weight-loss curve difference obtain in the sample from
By the quality of water.
In one concrete scheme, when determining free water content, it can be surveyed under any thermostat temperature in 20 DEG C~50 DEG C
Determine the mass value of different time sample, weight-loss curve is generated according to the mass value of different time sample, wherein, the horizontal stroke of weight-loss curve
The reduction of free water content in the change that coordinate is the time, ordinate is quality in mass value, weight-loss curve as sample;May be used also
With under any Elevated Temperature Conditions in 20 DEG C~50 DEG C, for example, temperature can from 20 DEG C rise to 40 DEG C during determine not
It is corresponding in different time from determination sample under 30 DEG C of Elevated Temperature Conditions for rising to 50 DEG C with the mass value of time sample, or temperature
Mass value, weight-loss curve is generated according to the mass value of the sample of measure, abscissa is that time, ordinate are matter in weight-loss curve
Value.
In one concrete scheme, when obtaining moisture loss rate profile according to the weight-loss curve, specifically, to institute
State weight-loss curve and carry out second order derivation, obtain the second order derived function of Mass versus Time, the second order derived function is moisture loss
Rate profile, when moisture loss rate profile reclaimed water disperses stall rate generation significant changes, that is, thinks in sample
Free water evaporating completely comes out, and shows as crest occur in moisture loss rate profile, the peak value corresponding time
Free water as in sample lost time point completely, then according to corresponding to weight-loss curve obtains the peak value corresponding time
The difference of mass value in mass value, the mass value and weight-loss curve corresponding to initial time is the matter of Free water in the sample
The quality of Free water obtains the free water content of sample, it is necessary to say compared with the mass value corresponding to initial time in amount, sample
It is bright, when finding multiple peak values in moisture loss rate profile, choose and lean in multiple peak values corresponding time point
Nearly weight-loss curve tends to constant time point, and the time point, corresponding peak value came out to characterize Free water evaporating completely.
In one concrete scheme, the determination sample mass value corresponding in different time under constant temperature or Elevated Temperature Conditions
When, the mass value of thermogravimetric analyzer determination sample can be specifically used, while being purged in continuous mode using nitrogen, purging speed
Rate is 5-40ml/min, by purging of the nitrogen to the sample surfaces, makes the rapid solvent evaporation in sample, separates, so that
Sample anaerobic purpose is reached, keeps sample purer, it is necessary to which explanation, thermogravimetric analyzer is a kind of existing equipment, therefore
Sample preparation, assay method in continuous mode may refer to not limited in existing thermogravimetric analyzer operation standard, the present embodiment
System.
In one concrete scheme, the determination sample mass value corresponding in different time under constant temperature or Elevated Temperature Conditions
When, minute with the mass value of sample reach it is constant untill, i.e., when the mass value of sample is constant described in continuous mode, stop
To the measure of the sample.
The present invention provides a kind of free water content assay method, by under constant temperature or Elevated Temperature Conditions, when determining different
Between sample mass value, according to the mass value of measure generate weight-loss curve, according to the weight-loss curve obtain moisture loss speed
Change curve, and the peak value corresponding time is obtained from the moisture loss rate profile, obtained according to the weight-loss curve
Obtain the mass value corresponding to the peak value correspondence time, mass value and the weight-loss curve corresponding to the peak value correspondence time
The difference of mass value corresponding to middle initial time is the quality of Free water in the sample, the free water content that the present invention is provided
Assay method solves that determination data Stability and veracity when existing Abbe refractometer method is determined is poor and inapplicable Free water
The problem of content relatively low sample, and the present invention can also ensure that sample is determined in time, and testing cost is low.
It can be used for index determining and the monitoring of various product using the inventive method, such as daily food, fruits and vegetables are former
Material and product, fast realize Quality Detection and the tracking to product, with very wide in range application field exactly.
Brief description of the drawings
Fig. 1 is the schematic diagram of ham weight-loss curve and moisture loss rate profile under 20 DEG C of constant temperatures;
Fig. 2 is the schematic diagram of wild cabbage weight-loss curve and moisture loss rate profile under 40 DEG C of constant temperatures;
Fig. 3 is the schematic diagram of Paeonia suffruticosa seed weight-loss curve and moisture loss rate profile under 30 DEG C of constant temperatures;
Fig. 4 is the schematic diagram of carrot weight-loss curve and moisture loss rate profile under 20~40 DEG C of Elevated Temperature Conditions.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is
A part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art
The every other embodiment obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
Embodiment 1
Weigh 5~35mg of sample, and be put into ceramic crucible, sample is respectively ham, purple potato, green pepper in the present embodiment
And running water, using thermogravimetric analyzer (TGA/DSC1, Mettler Toledo, Switzerland) determination sample in 20 DEG C of perseverances
Purged under the conditions of temperature in the corresponding mass value of different time, continuous mode using nitrogen, purge rates 20ml/min, minute
With sample quality reach it is constant untill, according to the mass value of measure generate weight-loss curve, second dervative is asked to weight-loss curve, two are asked
Order derivative obtain curve be moisture loss rate profile, found from moisture loss rate profile crest (see
Arrow in Fig. 1), the crest value corresponding time is the time point that Free water is all scattered and disappeared, the time point corresponding quality
The difference of value mass value corresponding with initial time in weight-loss curve (0min) be in the quality of Free water in sample, sample from
The free water content of sample is obtained compared with the corresponding mass value of initial time in weight-loss curve (0min) by the quality of water, together
When, in the present embodiment, the moisture of determination sample is (in the total moisture and weight-loss curve of sample just under the conditions of 105 DEG C of constant weights
Time beginning, corresponding mass value was compared), the measurement result of sample is as shown in table 1 and Fig. 1 in the present embodiment, and Fig. 1 is ham 20
The schematic diagram of weight-loss curve and moisture loss rate profile under DEG C constant temperature.
The measurement result of sample free water content under 1 20 DEG C of constant temperatures of table
When measure ham, purple potato, the free water content of green pepper under 20 DEG C of constant temperatures are can be seen that in table 1, in ham
Free water account for total moisture ratio be in 22.4%, i.e. ham free water content well below combining water content, purple potato and green grass or young crops
The ratio that Free water accounts for total moisture in green pepper is respectively 62.9% and 77.9%, in ham, purple potato, green pepper, the freedom in green pepper
At most, during to originally aquametry, as shown in table 1, Free water accounts for total moisture ratio to be all in 100%, i.e. running water water content
Free water.
In Fig. 1, dotted line is that abscissa is the time in weight-loss curve, weight-loss curve, and ordinate is quality, and solid line dissipates for moisture
It is the time to lose abscissa in rate profile, moisture loss rate profile, and ordinate is led for the second order of Mass versus Time
Numerical value, it will be seen from figure 1 that Free water is constantly scattered and disappeared in change over time, ham, the quality of ham tapers off trend,
In 60-80min, quality tends to be constant, and moisture loss rate profile occurs two in 0-20min and 60-80min
Crest, through analysis, when in the range of 0-20min, weight-loss curve does not tend to be constant, i.e., still contain Free water in sample, and
When in the range of 60-80min, weight-loss curve tends to be constant, so the crest value (as shown by arrows) in the range of 60-80min
Corresponding time point is only time when Free water is all scattered and disappeared in sample, and the time point corresponding matter is obtained from weight-loss curve
Amount, the quality and time in weight-loss curve are quality that the difference of the corresponding mass values of 0min is Free water in ham.Therefore,
When there are multiple peak values in moisture loss rate profile, multiple peak values should be chosen in corresponding time point close to weightless bent
Time point when line tends to be constant.
As a comparison, the purple potato (moisture 66.1%) in embodiment 1 is determined respectively according to the method for embodiment 1
7 times, measurement result shows that the ratio that Free water accounts for total moisture in purple potato is respectively 62.9%, 61.8%, 61.6%, 62.7%,
61.6%th, 63.2% and 63.8%, so the ratio that the Free water in purple potato accounts for total moisture is (62.5 ± 0.865) %, relatively
Standard deviation is 1.38%, that is, the data determined have higher stability, therefore, and the free water content that the present invention is provided is determined
Method solves the technical problem of determination data Stability and veracity difference when existing Abbe refractometer method is determined, and the present invention
NMR is not needed to use, so testing cost is low.
Embodiment 2
Weigh 5~35mg of sample, and be put into ceramic crucible, in the present embodiment sample be respectively pleurotus eryngii, wild cabbage and
Cotton candy, using thermogravimetric analyzer (TGA/DSC1, Mettler Toledo, Switzerland) determination sample in 40 DEG C of constant temperature
Under the conditions of the corresponding mass value of different time, purged using nitrogen in continuous mode, purge rates 20ml/min, minute with
Sample quality reach it is constant untill, according to the mass value of measure generate weight-loss curve, second dervative is asked to weight-loss curve, second order is sought
The curve that derivative is obtained is moisture loss rate profile, finds crest from moisture loss rate profile, the ripple
The peak value corresponding time is the time point that Free water is all scattered and disappeared, and the time point, corresponding mass value was corresponding with initial time
The difference of mass value be Free water in the quality of Free water in sample, sample quality and weight-loss curve in initial time
(0min) corresponding mass value compares the free water content for obtaining sample, meanwhile, in the present embodiment, under the conditions of 105 DEG C of constant weights
The measurement result of sample is as shown in table 2 and Fig. 2 in the moisture of determination sample, the present embodiment, and Fig. 2 is wild cabbage in 40 DEG C of constant temperature
Under the conditions of weight-loss curve and moisture loss rate profile schematic diagram.
The measurement result of sample free water content under 2 40 DEG C of constant temperatures of table
When the free water content that pleurotus eryngii, wild cabbage and cotton candy are determined under 40 DEG C of constant temperatures is can be seen that in table 2,
Free water content is respectively that free water content in 56.5% and 68.0%, i.e. wild cabbage is more than in pleurotus eryngii in pleurotus eryngii and wild cabbage
Free water content, and free water content is relatively low for the free water content in 0.371%, i.e. cotton candy in cotton candy, therefore, this hair
The free water content assay method of bright offer can be relatively low to free water content under 40 DEG C of constant temperatures sample can also carry out
Determine, so as to solve the technical problem of inapplicable free water content relatively low sample when existing Abbe refractometer method is determined.
In Fig. 2, dotted line is that abscissa is the time in weight-loss curve, weight-loss curve, and ordinate is quality, and solid line dissipates for moisture
It is the time to lose abscissa in rate profile, moisture loss rate profile, and ordinate is led for the second order of Mass versus Time
Numerical value, figure it is seen that Free water is constantly scattered and disappeared in change over time, wild cabbage, quality tapers off trend, in 50-
In 70min, quality tends to be constant, corresponding, and peak value occurs in 50-70min in moisture loss rate profile, the peak value pair
The time when time point answered all scatters and disappears for Free water in sample, the time point corresponding quality is obtained from weight-loss curve,
The quality and time are that the difference of the corresponding quality of 0min is the quality of Free water in wild cabbage.
Embodiment 3
Weigh 5~35mg of sample, and be put into ceramic crucible, in the present embodiment sample is the sample of low moisture content,
Respectively white sugar, sesame cream, honey and Paeonia suffruticosa seed, using thermogravimetric analyzer (TGA/DSC1, Mettler Toledo,
Switzerland) determination sample is blown under 30 DEG C of constant temperatures in the corresponding mass value of different time, continuous mode using nitrogen
Sweep, purge rates 20ml/min, minute with sample quality reach it is constant untill, generated according to the mass value of measure weightless bent
Line, second dervative is sought to weight-loss curve, finds the peak value corresponding time, the time point, corresponding mass value was corresponding with initial time
Mass value difference be sample Free water quality, meanwhile, in the present embodiment, the determination sample under the conditions of 105 DEG C of constant weights
Moisture, the measurement result of sample is as shown in table 3 and Fig. 3 in the present embodiment, and Fig. 3 is Paeonia suffruticosa seed in 30 DEG C of constant temperatures
The schematic diagram of lower weight-loss curve and moisture loss rate profile.
The measurement result of the sample of table 3 sample free water content under the conditions of 30 DEG C
As can be seen that determining the Free water of white sugar, sesame cream, honey and Paeonia suffruticosa seed under 30 DEG C of constant temperatures in table 3
During content, white sugar, sesame cream, the free water content of honey and Paeonia suffruticosa seed are 0, i.e. white sugar, sesame cream, honey and Paeonia suffruticosa seed
The moisture contained is all to combine water, wherein, the moisture of white sugar is minimum.
In Fig. 3, dotted line is that abscissa is the time in weight-loss curve, weight-loss curve, and ordinate is quality, and solid line dissipates for moisture
It is the time to lose abscissa in rate profile, moisture loss rate profile, and ordinate is led for the second order of Mass versus Time
Numerical value, from figure 3, it can be seen that do not occur peak value in moisture loss rate profile, i.e. freedom in the Paeonia suffruticosa seed
Water content is 0.
Embodiment 4
Weigh 5~35mg of sample, and be put into ceramic crucible, in the present embodiment sample is toothpaste, carrot, wild cabbage, ox
In jerky and dried meat floss, using thermogravimetric analyzer (TGA/DSC1, Mettler Toledo, Switzerland) determination sample 20
Determination sample was determined in the corresponding mass value of different time under the conditions of~40 DEG C of temperature programmings (0.1 DEG C/min of heating rate)
Purged in journey using nitrogen, purge rates 20ml/min, minute with sample quality reach it is constant untill, according to the matter of measure
Value generates weight-loss curve, seeks second dervative to weight-loss curve, finds peak value corresponding time, the time point corresponding mass value
The difference of mass value corresponding with initial time is the quality of Free water in sample, meanwhile, in the present embodiment, in 105 DEG C of perseverances
The measurement result of sample is as shown in table 4 and Fig. 4 in the moisture of determination sample, the present embodiment under the conditions of weight, and Fig. 4 is carrot
The schematic diagram of weight-loss curve and moisture loss rate profile under 20~40 DEG C of Elevated Temperature Conditions.
The measurement result of the sample of table 4 sample free water content under 20~40 DEG C of Elevated Temperature Conditions
As can be seen that determining toothpaste, carrot, wild cabbage, dried beef and dried meat floss under 20~40 DEG C of Elevated Temperature Conditions in table 4
In free water content when, the free water content in dried meat floss be free water content in 0, carrot at most, the Free water in toothpaste
Content is 1.09%, and the free water content in dried beef is 1.98%, therefore, the free water content assay method that the present invention is provided
Under 20~40 DEG C of Elevated Temperature Conditions also can the sample relatively low to free water content be measured, so solving existing Abbe folding
Penetrate the technical problem of inapplicable free water content relatively low sample when instrument method is determined.
In Fig. 4, dotted line is that abscissa is the time in weight-loss curve, weight-loss curve, and ordinate is quality, and solid line dissipates for moisture
It is the time to lose abscissa in rate profile, moisture loss rate profile, and ordinate is led for the second order of Mass versus Time
Numerical value, from fig. 4, it can be seen that change over time, the quality of carrot decreases, weight-loss curve tapers off trend,
In 100-160min, quality tends to be constant, corresponding, and peak value occurs in 100-110min in moisture loss rate profile,
The peak value corresponding time is free water content whole lost time points in carrot, and the time is obtained from weight-loss curve
The difference of the initial mass of the corresponding quality of point, the quality and carrot is the quality of the Free water in the carrot.
To sum up, from above-described embodiment 1 as can be seen that the data that the free water content assay method that the present invention is provided is determined
With higher stability, the technology of determination data Stability and veracity difference when existing Abbe refractometer method is determined can solve the problem that
Problem, and the present invention does not need to use NMR, so testing cost is low, while the assay method of the present invention is simple
And required equipment is common equipment, so the present invention can also ensure that sample is determined in time.
As can be seen that free water content is 0.371% in cotton candy from above-described embodiment 2 and 4, Free water contains in toothpaste
Measure as 1.09%, the free water content in dried beef is 1.98%, i.e. cotton candy, in toothpaste and dried beef free water content compared with
It is low, i.e., the free water content assay method that provides of the present invention can the sample relatively low to free water content can also determine its Free water
Content, therefore, the free water content assay method that the present invention is provided can solve inapplicable when existing Abbe refractometer method is determined
The technical problem of the relatively low sample of free water content, meanwhile, the free water content assay method that the present invention is provided is in continuous mode
Measure expense is relatively low.
Finally it should be noted that:Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations;To the greatest extent
The present invention is described in detail with reference to foregoing embodiments for pipe, it will be understood by those within the art that:Its according to
The technical scheme described in foregoing embodiments can so be modified, or which part or all technical characteristic are entered
Row equivalent substitution;And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme.
Claims (4)
1. a kind of free water content assay method, it is characterised in that methods described includes:
Under constant temperature or Elevated Temperature Conditions, the mass value of different time sample is determined, wherein the constant temperature or the temperature of heating
Scope is 20 DEG C~50 DEG C;
Weight-loss curve is generated according to the mass value of measure, wherein, the abscissa of the weight-loss curve is that time, ordinate are quality
Value;
Moisture loss rate profile is obtained according to the weight-loss curve, and obtained from the moisture loss rate profile
Obtain the peak value corresponding time;
Mass value according to corresponding to the weight-loss curve obtains the peak value correspondence time, according to peak value correspondence time institute
The difference of corresponding mass value and the mass value corresponding to initial time in the weight-loss curve obtains Free water in the sample
Quality;
The mass value that different time sample is determined under constant temperature or Elevated Temperature Conditions, including:
Under any thermostat temperature in 20 DEG C~50 DEG C, the mass value of different time sample is determined;Or
Under any Elevated Temperature Conditions in 20 DEG C~50 DEG C, the mass value of different time sample is determined;
It is described that moisture loss rate profile is obtained according to the weight-loss curve, including:
Second dervative is sought the weight-loss curve, and the second dervative is used as the moisture loss rate profile.
2. according to the method described in claim 1, it is characterised in that surveyed using thermogravimetric analyzer under constant temperature or Elevated Temperature Conditions
Determine the mass value of sample described in different time.
3. method according to claim 2, it is characterised in that the use thermogravimetric analyzer determines the quality of the sample
During value, purged in continuous mode using nitrogen, purge rates are 5-40ml/min.
4. according to the method described in claim 1, it is characterised in that the mass value of determination sample under constant temperature or Elevated Temperature Conditions
Until when constant, stopping the measure to the sample.
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