CN104597079B - The assay method of palm oil iodine number - Google Patents
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Abstract
The present invention relates to a kind of assay method of palm oil iodine number.The iodine number of palm oil is higher, and its degree of saturation is lower, and degree of unsaturation is higher, thus the corresponding fusing point of palm oil is lower, and the crystallization temperature corresponding to its decrease temperature crystalline process is lower.The temperature of peak crystallization and the iodine number of sample are associated in the palm oil crystallization process exotherm that differential scanning calorimetry is obtained, and fisheye temperature T is then fitted out respectivelyon, peak temperature Tpeak, crystallization complete temperature ToffWith the relation of iodine number；For analyzing a series of follow-up palm oil samples, without the analysis newly-built vertical standard control curve of counterpoise and its respective associated formula every time.A kind of assay method of the new palm oil iodine number provided using the present invention, can determine the palm oil samples iodine number in the range of different iodine numbers.Safe operation of the present invention is simple, and measuring speed is fast, and measurement result accurately and reliably, improves the security and efficiency of oil sample measure.
Description
Technical field
The invention belongs to Chemical Engineering industrial crystallization technical field, and in particular to a kind of assay method of palm oil iodine number.
Background technology
Palm oil is to squeeze out from the brown pulp on oil palm tree, and predominantly (mass fraction is about triglycerides
, and a small amount of diglyceride and monoglyceride 98%).Triglycerides is formed by glycerine and long chain fatty acids, its long chain fatty acids
Mainly include：Palmitic acid mass fraction is about 45%, and oleic acid and linoleic mass fraction are about 40%.Different long-chain fats
Acid can form different triglycerides.The degree of saturation of palm oil is about 50%, because it is free of cholesterol, rich in vitamin
E and carrotene, and it is cheap, therefore at home and abroad it is widely used in culinary art and food manufacturing.Current palm oil is the world
One important component in grease market, its ratio in world's grease total output is more than 30%.
The refined processing method of the greases such as palm oil mainly includes refining and modified, wherein the purpose refined is to remove raw material
Grease color, flavour, the other than triglycerides component of quality are influenceed in palm oil；And modification is to remove part higher melt
Triglycerides, improves the degree of unsaturation of grease, widens the application of grease.In palm oil futures exchange typically with " degree " come
Represent palm oil classification, " degree " is that the fusing point of grease contained by is named, reaction be grease degree of unsaturation.But by
In general palm oil with modified progress, fusing point is gradually reduced, after fusing point is less than 15 degree, and detection fusing point refers under room temperature condition
Mark is more and more difficult, then product is identified using iodine number, and the fusing point of grease will no longer be important indicator in this case, then
The classification of palm oil is identified using iodine number.Iodine number is represents a kind of index of degree of unsaturation in organic compound, and it refers to
The grams of (addition) iodine can be absorbed in 100g materials.This method is mainly used in the materials such as grease, aliphatic acid, wax and polyesters
Determine.The iodine number of grease is higher, and its degree of unsaturation is higher, and fusing point is lower.Therefore the measure of iodine number has especially in oils industry
For consequence.
At present, the method general in the world that determines of iodine number is American Oil association Cd 1-25 Webster determination methods, this
Sample is dissolved in carbon tetrachloride by method first, adds Wijs reagent, 20~25 DEG C of 30min of keeping temperature；Iodine is added afterwards
Change potassium solution [15% (quality)] and water, titrated, referred to starch solution (10%) for indicator with 0.1mol/L sodium thiosulfate
Show titration end-point.This method is determined accurately and reliably, low for equipment requirements, but usually uses poisonous reagent, such as tetrachloro
Change carbon etc., easily laboratory technician is caused harm with environment, and titration operation requires higher, complex operation to laboratory technician, artificially
Factor is influenceed than larger.Chinese patent CN102262067A have studied determines edible oil using the In situ ATR-FTIR method that decays
Iodine number, it is compared using the peak area of infrared spectrogram with standard curve, draws sample iodine number.This method avoid using having
The reagent of poison, determines sample safer, but this method is higher to equipment requirement, and sample treatment and minute compare
It is long, more than more than ten minutes time are totally needed, and the consummate degree of experimental implementation is had higher requirements.In addition, experiment is built every time
The standard curve of vertical sample more takes, and is unfavorable for improving determination efficiency.External scientific research personnel Haryati and Che Man
(Haryati,T.,Man,Y.C.,Ghazali,H.,Asbi,B.,&Buana,L,Determination of iodine
value of palm oil based on triglyceride composition,Journal of the American
Oil Chemists'Society, (1998), 75 (7), 789-792.) invent triglycerides in utilization chromatography determination grease
Composition, and then calculate the iodine number of grease.This method test safety, and it is simple to operate, be conducive to a large amount of measure；But
This method needs the triglycerides of a large amount of species in quantitative, qualitative analysis grease, and preliminary preparation amount is huge, in addition the party
Method model only considers the higher several main content of triglyceride of content in palm oil, therefore this method lacks generally applicable
Property, application is restricted.
Therefore, it is necessary to set up a kind of measure new method of the oily iodine number of quick, safe and reliable palmitic acid.
The content of the invention
In order to overcome prior art not enough, the present invention provides a kind of assay method of new palm oil iodine number, this method solution
The current palm oil iodine number of having determined determines complex operation, the problem of reagent poisons larger, and the inventive method is quick, safe and reliable.
The present invention establishes a kind of quick palm oil iodine number assay method using differential scanning calorimetry.The method is according to iodine
Value it is higher, unsaturated triglyceride content is higher in grease, and the fusing point of corresponding grease is lower, crystallization peak temperature it is lower this
General principle, quick, accurate, the easy advantage possessed using differential scanning calorimetry develops fat crystals process heat
Change and oil iv relation curve.
Technical scheme is as follows：
A kind of assay method of palm oil iodine number；It is to utilize differential scanning calorimetry.
Differential scanning calorimetry step is as follows：
(1) a series of palm oil samples of known iodine number are heated in the case of stirring, makes the solid in palm oil complete
Portion dissolves, and eliminates influence of the history crystallization process to measurement result；
(2) the palm oil samples after being dissolved in (1) are taken into differential scanning calorimeter crucible, sealing is put into differential scanning
Calorimeter；
(3) crucible is warming up to 60-75 DEG C of simultaneously constant temperature 20-40 minutes, then cooling to is fully crystallized palm oil, determines
During palm oil crystallization process thermal change；Obtain peak crystallization in palm oil crystallization process exotherm.
(4) crystallization peak temperature data in obtained palm oil crystallization process exotherm are closed with known iodine number
Connection, obtains the standard control curve and incidence formula of palm oil iodine number and its crystallization peak temperature；Palm oil iodine number and its peak crystallization
There is this linear relationships of Y=AX+B between temperature, wherein Y is palm oil iodine number, and X is palm oil crystallization peak temperature, calculates A
And B；
(5) by differential scanning calorimetry, using method and parameter same in the step of above-mentioned (1)-(3), determine and treat point
The crystallization peak temperature of palm oil samples is analysed, the standard control curve and incidence formula for then utilizing (4) to obtain, by crystallization peak temperature
Obtain the iodine number of palm oil samples to be analyzed.
Described crystallization peak temperature is fisheye temperature Ton, peak temperature TpeakOr crystallization completes temperature Toff。
A series of palm oil sample sizes are preferably 20-35 in described step (1).
Known iodine number is preferably 60-75 in described step (1).
The solution temperature of palm oil samples is preferably 60-75 DEG C in described step (1)；It is preferred that constant temperature 20-40 minutes.
The cooling of palm oil samples is preferably to -40 DEG C~-50 DEG C in described step (3).
Described heating or rate of temperature fall is preferably 5 DEG C/min.
The present invention new method description and and be described as follows：
The iodine number of palm oil is higher, and its degree of saturation is lower, and degree of unsaturation is higher, thus the corresponding fusing point of palm oil is got over
Low, the crystallization temperature corresponding to its decrease temperature crystalline process is lower.The palm oil crystallization process that differential scanning calorimetry is obtained is put
Peak crystallization 1 goes out fisheye temperature T in heating curveon, peak temperature TpeakTemperature T is completed with crystallizationoffClosed with the iodine number of sample
Connection, then fits out fisheye temperature T respectivelyon, peak temperature Tpeak, crystallization complete temperature ToffWith the relation of iodine number；Palm oil
There is this linear relationships of Y=AX+B between iodine number and its crystallization peak temperature, wherein Y is palm oil iodine number；X crystallizes for palm oil
Peak temperature；Crystallization peak temperature includes fisheye temperature Ton, peak temperature TpeakOr crystallization completes temperature Toff；These three temperature
Someone's peak value in the characteristic temperature of peak crystallization, different documents is belonged to, someone is with fisheye temperature is gone out, in our methods
In, with these three temperature it is any can, and from embodiment it can also be seen that, the experimental precision base obtained with three kinds of temperature
Originally be it is the same, with three temperature can, do not influence measurement accuracy；A and B is constant, is surveyed using known iodine number and experiment
Crystallization peak temperature data calculate constant A and B, its computational methods has many kinds, can also use excel, origin,
The softwares such as matlab are handled, and these methods can be used, and without specificity, the selections of distinct methods is not interfered with accurately yet
Degree.Constant A and B determination after, it is possible to according in palm oil products this iodine number-crystallization peak temperature linear pass
System, the crystallization peak temperature of the palm oil crystallization process obtained using differential scanning calorimetry sets up palm oil crystallization peak temperature and palm fibre
Standard control curve and corresponding incidence formula between palmitic acid oil iodine number；
In methods described above, step (1)-(4) are palm oil iodine number and the standard pair of crystallization peak temperature in this method
Process is set up according to curve and respective associated formula；Step (5) is the analysis process of palm oil samples to be measured.Standard control curve
, can be for analyzing a series of follow-up palm oil samples, without analysis every time again with corresponding incidence formula once setting up
Set up standard control curve and its respective associated formula.
In methods described above step 1, to ensure the representativeness of sample and the application of standard control curve, simultaneously
Time of measuring and its convenience are taken into account, the iodine number of palm oil samples known to iodine number is between 60-75, more preferably 70.
In methods described above step 1, to ensure that the accuracy and representativeness of standard curve take into account time of measuring simultaneously
And its convenience, the quantity of palm oil samples is between 20-35, and preferably 30.
In methods described above step 1, to ensure that solid is completely dissolved so as to ensure to sample homogeneity, palm in sample
The thermostat temperature of oil samples is between 60-75 DEG C, more preferably 70 DEG C.
In methods described above step 1, to ensure that solid is completely dissolved while take into account time of measuring in sample, palm oil
The constant temperature time of sample is between 20-40 minutes, more preferably 30 minutes.
In methods described above step 2, to ensure that the repeatability of measurement is taken into account used in thermal analyzer with the degree of accuracy simultaneously
Crucible volume, palm oil sample size is 3-10 milligrams, more preferably 5 milligrams.
In methods described above step 3, to ensure that measurement reproducibility takes into account time of measuring, the heating of palm oil samples simultaneously
Speed is 5 DEG C/min.
In methods described above step 3, it is completely dissolved to ensure that cooling starts solid in preceding sample, palm oil samples liter
Between warm to 60-75 DEG C, more preferably 70 DEG C.
In methods described above step 3, it is completely dissolved to ensure that cooling starts solid in preceding sample while taking into account measurement
Time, the constant temperature time of palm oil samples is between 20-40 minutes, more preferably 30 minutes.
In methods described above step 3, to ensure experiment crystallization process repeatability, palm oil samples rate of temperature fall is 5
℃/min。
In methods described above step 3, to ensure palm oil sample crystallization completely, palm oil samples are cooled to -40 DEG C
To -50 DEG C, more preferably -45 DEG C.
Compared with prior art, outstanding feature of the invention is：1. safety, any added regent is not used；2. convenience, sample
Product do not need advanced processing, can direct measurement；3. quick, the whole time-consuming more conventional titration of experiment shortens more than 50%；4. it is accurate
Really, interference from human factor is removed, relative deviation is less than 1.00%.
A kind of assay method of the new palm oil iodine number provided using the present invention, can be determined in the range of different iodine numbers
Palm oil samples iodine number.Safe operation of the present invention is simple, and measuring speed is fast, and measurement result accurately and reliably, improves grease
Security and efficiency that sample is determined.
Brief description of the drawings
Different palm oil samples decrease temperature crystalline process heat release spectrograms in Fig. 1 embodiments 1
Fig. 2：T used in embodiment 2on(Y is iodine number to-iodine number standard control curve figure in formula in figure, and X is fisheye temperature
Degree)；
Fig. 3：T used in embodiment 3peak(Y is iodine number to-iodine number standard control curve figure in formula in figure, and X is peak value temperature
Degree)；
Fig. 4：T used in embodiment 4off(Y is iodine number to-iodine number standard control curve figure in formula in figure, and X is brilliant completion temperature
Degree)；
Embodiment
The present invention will be described in detail for following embodiments：
Embodiment 1：The foundation of standard control curve between palm oil samples iodine number and crystalline exotherm peak.
30 different brackets palm oil products that iodine number known to iodine number is 65-75 are taken, by these samples in stirring action
Under, heated under the conditions of temperature 70 C, all dissolving, constant temperature 30min；Palm oil samples 5mg is taken to differential scanning calorimeter crucible
In, sealed with supporting crucible cover, be put into differential scanning calorimeter.Crucible is warming up to 70 DEG C with 5 DEG C/min, constant temperature 30min, it
- 45 DEG C are cooled to 5 DEG C/min afterwards, palm oil crystallization process thermal change is determined.The heat release spectrogram of obtained different samples is such as
Shown in Fig. 1.
Different temperatures (goes out in the fat crystals peak 1 that above-mentioned oil sample iodine number is determined with differential scanning calorimetry respectively
Fisheye temperature Ton, peak temperature Tpeak, crystallization complete temperature Toff) be associated, obtain Ton- iodine number, Tpeak- iodine number, Toff- iodine
Three standard control curves of value are respectively such as Fig. 2 to Fig. 4.From this figure, it can be seen that palm oil iodine number and its crystallization peak temperature are present
Obvious linear relationship.Using data shown in Fig. 2 to Fig. 4, pass through matlab softwares and palmitic acid oil iodine number Y and its crystallization peak temperature X
Between this linear relationships of Y=AX+B that exist, fitted by parameter and respectively obtain Ton- iodine number, Tpeak- iodine number, Toff- iodine number
The value of parameter A and B in three relational expressions simultaneously and then obtains TonThe relational expression of-iodine number is Y=-0.6203X+68.2912；
TpeakThe relational expression of-iodine number is Y=-0.6093X+68.0120；ToffThe relational expression of-iodine number is Y=-0.5937X+67.7043.
Embodiment 2：Utilize differential scanning calorimetry Ton- iodine number standard control curve determines the iodine number of palm oil.
The iodine number of palm oil samples to be analyzed is determined using differential scanning calorimetry, takes palm oil samples 10mg to add first
Into differential scanning calorimeter crucible, sealed with supporting crucible cover, be put into differential scanning calorimeter.By crucible with 5 DEG C/min liters
Temperature is to 70 DEG C, and constant temperature 30min cools to -45 DEG C with 5 DEG C/min afterwards, determines palm oil crystallization process thermal change.By this
Method, the peak crystallization 1 for determining this sample goes out fisheye temperature TonFor -12.03 DEG C, by this numerical value and the T fittedon- iodine number
Standard curve (result is as shown in Figure 2) is compareed and calculated using the incidence formula Y=-0.6203X+68.2912 in figure
It is 75.7534 to go out sample iodine number result.To verify the accuracy of this method, using the iodine of the standard Webster titration measuring sample
It is worth for 75.5013.Found by the contrast of two methods measurement result, this method determines the iodine number and standard Wei of obtained grease
The absolute relative error of family name's titration is 0.333%, and the result that this explanation the inventive method is obtained is accurately and reliably.
Embodiment 3：Utilize differential scanning calorimetry Ton- iodine number standard control curve determines the iodine number of palm oil.
The iodine number of palm oil samples to be analyzed is determined using differential scanning calorimetry, takes palm oil samples 5mg to add first
Into differential scanning calorimeter crucible, sealed with supporting crucible cover, be put into differential scanning calorimeter.By crucible with 5 DEG C/min liters
Temperature is to 60 DEG C, and constant temperature 40min cools to -50 DEG C with 5 DEG C/min afterwards, determines palm oil crystallization process thermal change.By this
Method, the peak crystallization 1 for determining this sample goes out fisheye temperature TonFor -10.03 DEG C, by this numerical value and the T fittedon- iodine number
Standard curve (result is as shown in Figure 2) is compareed and calculated using the incidence formula Y=-0.6203X+68.2912 in figure
It is 74.5128 to go out sample iodine number result.To verify the accuracy of this method, using the iodine of the standard Webster titration measuring sample
It is worth for 73.8024.Found by the contrast of two methods measurement result, this method determines the iodine number and standard Wei of obtained grease
The absolute relative error of family name's titration is 0.953%, and the result that this explanation the inventive method is obtained is accurately and reliably.
Embodiment 4：Utilize differential scanning calorimetry Tpeak- iodine number standard control curve determines the iodine number of grease.
The iodine number of palm oil samples to be analyzed is determined using differential scanning calorimetry, takes oil sample 5mg to be added to first
In differential scanning calorimeter crucible, sealed with supporting crucible cover, be put into differential scanning calorimeter.Crucible is heated up with 5 DEG C/min
To 70 DEG C, constant temperature 30min cools to -45 DEG C with 5 DEG C/min afterwards, determines palm oil crystallization process thermal change.Pass through this side
Method, the peak temperature Tpeak for determining the peak crystallization 1 of this sample is -3.69 DEG C, by this numerical value and the T fittedpeak- iodine number
Standard curve (result is as shown in Figure 3) is compareed and calculated using the incidence formula Y=-0.6093X+68.0120 in figure
It is 70.2603 to go out sample iodine number result.To verify the accuracy of this method, using the iodine of the standard Webster titration measuring sample
It is worth for 70.5056.Found by the contrast of two methods measurement result, this method determines the iodine number and standard Wei of obtained grease
The absolute relative error of family name's titration is 0.349%, and the result that this explanation the inventive method is obtained is accurately and reliably.
Embodiment 5：Utilize differential scanning calorimetry Tpeak- iodine number standard control curve determines the iodine number of grease.
The iodine number of palm oil samples to be analyzed is determined using differential scanning calorimetry, takes oil sample 10mg to be added to first
In differential scanning calorimeter crucible, sealed with supporting crucible cover, be put into differential scanning calorimeter.Crucible is heated up with 5 DEG C/min
To 75 DEG C, constant temperature 20min cools to -40 DEG C with 5 DEG C/min afterwards, determines palm oil crystallization process thermal change.Pass through this side
Method, the peak temperature Tpeak for determining the peak crystallization 1 of this sample is -3.20 DEG C, by this numerical value and the T fittedpeak- iodine number
Standard curve (result is as shown in Figure 3) is compareed and calculated using the incidence formula Y=-0.6093X+68.0120 in figure
It is 69.9618 to go out sample iodine number result.To verify the accuracy of this method, using the iodine of the standard Webster titration measuring sample
It is worth for 70.6321.Found by the contrast of two methods measurement result, this method determines the iodine number and standard Wei of obtained grease
The absolute relative error of family name's titration is 0.958%, and the result that this explanation the inventive method is obtained is accurately and reliably.
Embodiment 6：Utilize differential scanning calorimetry Toff- iodine number standard control curve determines the iodine number of grease.
The iodine number of palm oil samples to be analyzed is determined using differential scanning calorimetry, takes oil sample 5mg to be added to first
In differential scanning calorimeter crucible, sealed with supporting crucible cover, be put into differential scanning calorimeter.Crucible is heated up with 5 DEG C/min
To 70 DEG C, constant temperature 30min cools to -45 DEG C with 5 DEG C/min afterwards, determines palm oil crystallization process thermal change.Pass through this side
Method, the crystallization for determining the peak crystallization 1 of this sample completes temperature ToffFor -10.09 DEG C, by this numerical value and the T fittedoff- iodine
Value standard curve (result is as shown in Figure 4) is compareed and calculated using the incidence formula Y=-0.5937X+67.7043 in figure
It is 73.6947 to draw sample iodine number result.To verify the accuracy of this method, using the standard Webster titration measuring sample
Iodine number is 73.5402.Found by the contrast of two methods measurement result, this method determines the iodine number and standard of obtained grease
The absolute relative error of Webster titration is 0.210%, and the result that this explanation the inventive method is obtained is accurately and reliably.
Embodiment 7：Utilize differential scanning calorimetry Toff- iodine number standard control curve determines the iodine number of grease.
The iodine number of palm oil samples to be analyzed is determined using differential scanning calorimetry, takes oil sample 3mg to be added to first
In differential scanning calorimeter crucible, sealed with supporting crucible cover, be put into differential scanning calorimeter.Crucible is heated up with 5 DEG C/min
To 65 DEG C, constant temperature 25min cools to -45 DEG C with 5 DEG C/min afterwards, determines palm oil crystallization process thermal change.Pass through this side
Method, the crystallization for determining the peak crystallization 1 of this sample completes temperature ToffFor -11.20 DEG C, by this numerical value and the T fittedoff- iodine
Value standard curve (result is as shown in Figure 4) is compareed and calculated using the incidence formula Y=-0.5937X+67.7043 in figure
It is 74.3537 to draw sample iodine number result.To verify the accuracy of this method, using the standard Webster titration measuring sample
Iodine number is 74.8014.Found by the contrast of two methods measurement result, this method determines the iodine number and standard of obtained grease
The absolute relative error of Webster titration is 0.602%, and the result that this explanation the inventive method is obtained is accurately and reliably.
A kind of assay method of new palm oil iodine number proposed by the present invention, is retouched by preferred embodiment
State, person skilled substantially can be not departing from present invention, in spirit and scope to structure as described herein and preparation side
Method is modified or suitably change is with combining, to realize the technology of the present invention.In particular, all similar replacements
Apparent to those skilled in the art with changing, they are considered as being included in spiritual, scope of the invention and interior
Rong Zhong.
Claims (3)
1. a kind of assay method of palm oil iodine number, it is characterized in that using differential scanning calorimetry, step is as follows：
(1) a series of palm oil samples of known iodine number are heated in the case of stirring, makes the solid in palm oil all molten
Solution, eliminates influence of the history crystallization process to measurement result；
(2) the palm oil samples after being dissolved in (1) are taken into differential scanning calorimeter crucible, sealing is put into means of differential scanning calorimetry
Instrument；
(3) crucible is warming up to 60-75 DEG C of simultaneously constant temperature 20-40 minutes, then cooling to is fully crystallized palm oil, continuous mode
The thermal change of middle palm oil crystallization process；Obtain peak crystallization in palm oil crystallization process exotherm；
(4) crystallization peak temperature data in obtained palm oil crystallization process exotherm are associated with known iodine number, obtained
To palm oil iodine number and its standard control curve and incidence formula of crystallization peak temperature；Palm oil iodine number and its crystallization peak temperature it
Between there is this linear relationships of Y=AX+B, wherein Y is palm oil iodine number, and X is palm oil crystallization peak temperature, calculates A and B；
(5) by differential scanning calorimetry, using method and parameter same in the step of above-mentioned (1)-(3), palm fibre to be analyzed is determined
The crystallization peak temperature of palmitic acid oil samples, the standard control curve and incidence formula for then utilizing (4) to obtain, is obtained by crystallization peak temperature
The iodine number of palm oil samples to be analyzed；
Described crystallization peak temperature is fisheye temperature Ton, peak temperature TpeakOr crystallization completes temperature Toff；Described step
(1) a series of palm oil sample sizes are 20-35 in；Known iodine number is 60-75 in described step (1).
2. the method as described in claim 1, it is characterized in that palm oil samples are cooled to -40 DEG C~-50 in described step (3)
℃。
3. the method as described in claim 1, it is characterized in that described heating or rate of temperature fall are 5 DEG C/min.
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Address after: 300350 District, Jinnan District, Tianjin Haihe Education Park, 135 beautiful road, Beiyang campus of Tianjin University Patentee after: Tianjin University Address before: 300072 Tianjin City, Nankai District Wei Jin Road No. 92, Tianjin University Patentee before: Tianjin University |