CN104345055A - Mixed indicator, utilization and rapid detection method for grease acid value - Google Patents
Mixed indicator, utilization and rapid detection method for grease acid value Download PDFInfo
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- CN104345055A CN104345055A CN201310321186.6A CN201310321186A CN104345055A CN 104345055 A CN104345055 A CN 104345055A CN 201310321186 A CN201310321186 A CN 201310321186A CN 104345055 A CN104345055 A CN 104345055A
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Abstract
The invention provides a mixed indicator. The indicator component of the mixed indicator provided by the invention is basically composed of bromothymol blue, methyl red and phenolphthalein. Detection of grease acid value with the mixed indicator provided by the invention has the characteristics of: convenience and speediness, and high stability detection result. Distinguishing can be realized easily only by visual inspection; operation can be carried out of a laboratory, and the detection process requires only a small amount of organic solvents, thus facilitating detection of a large number of samples. The mixed indicator can be used for dark color grease detection.
Description
Technical field
The present invention relates to a kind of mixed indicator and a kind of method detecting acid value, concrete, relate to a kind of method utilizing mixed indicator to detect acid value of lipids fast.
Background technology
Acid value is the mark of fatty Free Fat acid content, and fat is in long term storage process, and slowly hydrolysis occurs the effect due to microorganism, enzyme and heat, produces free fatty acid.And the quality of fat is relevant with the content of its free fatty acid.General conventional acid value is as one of criterion.Under the condition that fat is produced, acid value can be used as the index of hydrolysis degree, under the condition of its preservation, then can be used as the index of becoming sour.Acid value is less, illustrates that oil quality is better, freshness and refinement better.
Its size weighs an important indicator of crude oil quality, it is crucial transaction index in the trade flows of crude oil, because can calculate refining loss-rate by acid value, instructing oil refining workshop to calculate caustic dosage, concentration of lye in alkali refining operating process, is the foundation of main economic and technical indices.
Indonesia and Malaysia are palmitic Liang great producing countries, total production accounts for 80% of the whole world, it is reported that Indonesia's palm oil export volume in August in this year just reaches 1,410,000 tons, one of them important mainstay industry of palm oil Indonesia, the acid value related to evaluates an important indicator of reddish brown oil quality, is also the important indicator of trade flows, replaces traditional titration method with detecting acid value fast, can can improve the palmitic efficiency of purchase and accuracy widely simultaneously, also can save testing cost simultaneously.
One, the relevant prior art about titration measuring acid value of lipids is as follows:
According to Standard, what the mensuration of acid value of lipids adopted is titrimetry, the method belongs to a kind of assay method of subjectivity, GB/T-5530-2005 defines the method measuring animal and plant fat acidity and comprises hot ethanol determination method, cold solvent determination method and potentiometric titration, wherein hot ethanol determination method is normative reference method, cold solvent method is only applicable to light grease, and potentiometric titration utilizes pH meter to judge titration end-point, and then needed for titration, the gauge of potassium hydroxide calculates acid value of oil and fat.The advantage of this titrimetry is simple, easy, and without the need to special instrument and equipment and chemical reagent, but the method has following limitation:
(1) be difficult to differentiate the faint change of indicator color and the error at measurment that causes is large, especially in the darker or muddy grease of color, between individuality, endpoint difference increases;
(2) required oil sample quantity is large, and spent by acid-base titration, the time is long;
(3) mostly need to carry out in laboratory, checkout procedure is away from scene, and operation link is many, and required chemical reagent is many with medicine, needs loaded down with trivial details solution preparation, acid base titration program, samples, sample presentation is cumbersome.
Generally speaking, have and require operating personnel high, testing process is complicated, and sense cycle is long, needs by features such as chemical reagent, is unfavorable for the foreign trade of crude oil product and produces real-time online and detect and regulate and control.Therefore realize acid value in the urgent need to a kind of new method to detect fast.
The people such as Wang Sumin (Heilungkiang science and technology of grain and oil, 2001, (4) thymol blue: 25-27) is adopted to replace phenolphthalein indicator that the judgement of dark grease titration end-point is improved, but because the color change interval (by Huang Zhilan) of thymol blue indicator is near some dark grease itself, still there is the problem that titration end-point is difficult to judge.
Two, test paper method
In order to improve the detection efficiency of the acid value of edible oil and realize Site Detection, range estimation test paper (Authorization Notice No. CN2335142Y) this ratio juris that Guilin Zhong Hui biotech company has developed for Fast Measurement edible oil acid value is the medicament generation chromogenic reaction utilizing edible oil to become sour on produced free fatty acid and test paper, then compare with the comparator block of standard according to the color situation of change of test paper, thus determine the degree that edible oil sample is become sour.
Poplar drench etc. (edible oil acid value analysis and detection technology progress [J]. oil and foodstuffs science and technology, 2008, 6 (13): 31-33) develop a kind of test paper colorimetric express method and measure edible oil acid value, the pH reagent generation chromogenic reaction that this method utilizes edible oil and fat to become sour in produced free fatty acid and test paper, the color change of test paper reflects the acid value change of edible oil, the degree that its intensity of variation and edible oil become sour is linear, and have studied temperature, time, the kind of oil and the impact of Color pair measurement result, its result shows that acid value test paper color between 0 ~ 5.0 changes quite greatly, with the naked eye colorimetric is easy to distinguish, and this test paper is to temperature, reaction time, the kind of oil sample and color are all insensitive, but this test paper method existence and stability is poor, the shortcoming that error is slightly large, so also need to carry out studying and improving in the homogeneity improving acid value test paper and stability.
Three, near infrared spectroscopy
Publication number is the edible oil fatty acid value detection method that application discloses based on near-infrared spectrum analysis of CN101504363, collect representational sample, scan in 780 ~ 2500nm Spectral range, pre-service is carried out to sample set spectrum, here the methods such as level and smooth, differential, differentiate or Wavelet Denoising Method are adopted, to offset background interference, improve the resolution of spectrum.The standard spectrum of calibration samples collection, and same sample needs repeatedly duplicate measurements, using averaged spectrum as the standard spectrum of this sample.The grease must getting known acid value, as checking collection, is used spectrum scanning optical spectrum under the same conditions, is calculated acid value value according to the model set up, need repeatedly, until obtain satisfied model.Although near infrared determination method has plurality of advantages, but instrument price is expensive, need the spectral signature using chemometrics method Criterion sample and the mathematical model measured between component content, continuous supplementary model data are needed to calibrate, need a large amount of sample messages, this method is in the mensuration of edible oil acid value at present, and application document is less.
Four, self-made Instrument method
CN101097210 discloses a grain and oil automatic detector of acid value, but this kind of equipment does not have commercialization at present.
According to actual conditions, when pension parachute crude oil, the galley proof sample of a lot of tank wagon, barge, ship transport can be received every day.Every day all can be a large amount of sample up to a hundred that exceedes need to detect.And it is also different that the height of acid value determines its purchasing price, when the content of free acid is 10 higher than 5%(acid value) time, the price comparison of purchase is low, the content of the free acid in crude oil is different, also this crude oil is determined for which kind of purposes, be 7 as the content from fatty acid in crude oil is less than 3.5%(acid value) time, generally as inner wrapping edible oil, be generally used for preparing special oil product at 3.5-5% with when being greater than 5%.Therefore the result detected directly determines the economic benefit of an enterprise, if resolved detection can go out the acid value of grease fast and accurately, also indirectly can bring economic benefit to enterprise.
Therefore how determining the acid value of these oil samples fast and accurately, is the pressing issues faced in actual production.
Summary of the invention
A first aspect of the present invention is to provide a kind of mixed indicator.Mixed indicator disclosed in this invention has very sensitive chromogenic reaction, and the colour developing that can suddenly change within the scope of very narrow acid value, therefore can be used for carrying out the detection of acid value.In addition this mixed indicator is when carrying out oil acid value detection, has extraordinary portability, therefore can simplify process and the operation steps of oil acid value detection.
In order to realize this goal of the invention, the indicator composition of mixed indicator disclosed by the invention is made up of Bromothymol blue, methyl red and phenolphthalein substantially.
Preferably, the indicator composition of described mixed indicator is made up of Bromothymol blue 25 ~ 55 weight portion, methyl red 3 ~ 25 weight portion and phenolphthalein 25 ~ 80 weight portion substantially, preferred, the indicator composition of described mixed indicator is made up of Bromothymol blue 30 ~ 50 weight portion, methyl red 5 ~ 20 weight portion and phenolphthalein 30 ~ 70 weight portion substantially.
Mixed indicator as above is dissolved in the solvent of lower alcohol and/water, and described lower alcohol is selected from methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, butanols.Described mixed indicator concentration is in a solvent 1 ~ 9g/L.
A second aspect of the present invention discloses a kind of method of quick detection acid value of lipids, and wherein said method comprises the following steps:
(1) by oil sample, alkali lye and mixed indicator mixing as above;
(2) described oil sample color is observed to change;
(3) acid value is determined:
(3-1) when described oil sample is turquoise, grass green or dark green, according to described alkali lye consumption and oil sample color, acid value is determined; Or
(3-2) when described oil sample is sky blue, reduce alkali lye consumption, and repeat step (1)-(3); Or
(3-3) when described oil sample is yellow, increase alkali lye consumption, and repeat step (1)-(3).
Method as above, in wherein said alkali lye, the mole dosage of alkali and the ratio of grease weight to be measured are 0.96 × 10
-4~ 6.27 × 10
-4mol/g, the consumption of mixed indicator is every 100mg grease 100ul ~ 150ul.
Method as above, wherein in step (3-1), acid value is determined by colorimetric card or alkali lye consumption-oil sample color-acid value table.
Method as above, wherein said testing sample carried out desolventing technology before step (1).
Method as above, wherein said desolventing technology comprises adsorbent decolouring and/or extraction decolouring.
As above method, wherein said extraction desolventing technology comprises and the oil sample to be measured of unknown acid value is added polar organic solvent and non-polar organic solvent mixes, the two-phase of non-polar solvent and polar solvent layering is obtained respectively after layering, the polar solvent, layer obtained is decoloring layer, described polar solvent comprises alcohols, amide-type, organic solvent of ketone, and described non-polar solvent comprises ethers, sherwood oil, alkanes, based organic solvent.
Method as above, described desolventing technology comprises the decolouring of employing adsorbent, and preferred adsorbent is activated charcoal, silica gel, carclazyte, molecular sieve or silicate, and the amount of adsorbent is 20 ~ 70% of testing sample.
Method as above, the acid value of wherein said grease is 4-36, is preferably 4 ~ 12, is more preferably 7 ~ 11.
Method as above, wherein in the front step also comprising the acid value scope determining described grease of step (1).
Method as above, the fat type of wherein said oil sample to be measured is: Rice oil, sunflower oil, palm oil, palm-kernel oil, peanut oil, rapeseed oil, soybean oil, linseed oil, cottonseed oil, safflower seed oil, Purple Perilla Seed Oil, tea-seed oil, Castor oil, palm fruit oil, olive oil, oleum theobromatis, tallowseed oil, almond oil, apricot kernel oil, bancoul nuts oil, rubber seed oil, rice bran oil, maize germ, wheat germ oil, sesame seed oil, oenothera seed oil, hazelnut oil, pumpkin seed oil, nut oil, grape-kernel oil, linseed oil, borage seed oil, Seabuckthorm Seed Oil, tomato seed oil, macadimia nut oil, coconut oil, cocoa butter, algae wet goods.
A third aspect of the present invention, provide described mixing instruction and detecting the application in acid value of lipids, the acid value of lipids scope wherein detected is 4 ~ 36, is preferably 4 ~ 12, is more preferably 7 ~ 11.
A fourth aspect of the present invention, disclose a kind of product detecting acid value of lipids, wherein said product comprises mixed indicator as above, and preferably, described product also comprises the known standard sample of acid value, colorimetric card and/or alkali lye consumption-oil sample color-acid value table.
The present inventor is through extensive and deep research, by improving the detection method of acid value of lipids,, time length, inconvenient operation high for current oil acid value detection method cost, and the problem that testing result accuracy rate is not high, the present invention aims to provide a kind of oil acid value detection method of convenient, fast, low cost.Complete the present invention on this basis.
Technical conceive of the present invention is as follows:
Instant invention overcomes the defect of prior art, propose a kind of method of quick detection of acid value of lipids, this technique is in conjunction with the advantage of conventional colorimetric method, the basis of colourimetry is improved, have employed the indicator that variable color is sensitiveer, decrease due to less due to the difference of color in colourimetry and metrical error that is that cause to a greater extent, improve the accuracy of oil acid value detection result, significantly improve convenience and the agility of testing process, make it have environmental protection, fast, the advantage such as convenience, low cost.In the method for optimizing simultaneously improved, before carrying out acid value detection, carry out pre-service, decrease the impact that the color in raw material crude oil is brought, achieve the acid value utilizing human eye just accurately can detect grease, making the acid value of grease detect disengaging laboratory to operate separately, therefore have more standby practicality, being particularly suitable for for needing the instant occasion detecting acid value result.Further, in testing process, can use and body effect or the less solvent of harm are detected, achieve safety detection.
In the present invention, term " contains " or " comprising " represents that various composition can be applied in potpourri of the present invention or composition together.Therefore, term " primarily of ... composition " and " by ... form " be included in term and " contain " or in " comprising "." substantially by ... composition " represents the key component in potpourri or composition, does not get rid of other auxiliary material, as solvent or thinning agent etc.
Below describe in detail to various aspects of the present invention:
The kind of grease to be measured
In the present invention, the type of grease to be measured can be the crude oil of the grease of any kind, its nonrestrictive example comprises: Rice oil, sunflower oil, palm oil, palm-kernel oil, peanut oil, rapeseed oil, soybean oil, linseed oil, cottonseed oil, safflower seed oil, Purple Perilla Seed Oil, tea-seed oil, Castor oil, palm fruit oil, olive oil, oleum theobromatis, tallowseed oil, almond oil, apricot kernel oil, bancoul nuts oil, rubber seed oil, rice bran oil, maize germ, wheat germ oil, sesame seed oil, oenothera seed oil, hazelnut oil, pumpkin seed oil, nut oil, grape-kernel oil, linseed oil, borage seed oil, Seabuckthorm Seed Oil, tomato seed oil, macadimia nut oil, coconut oil, cocoa butter, algae oil.Because these crude oils are with many impurity, therefore adopt colourimetry carry out acid number detect time, can bring certain error, and long between saltation zone due to color, the result accuracy rate therefore detected is lower.Adopt the detection method described in the present invention, can be easy to avoid this technical matters, the interference making the detection of acid value overcome color to bring.Especially, in a specific embodiment of the present invention, make the reddish brown oil (red palm oil crude oil) of color serious interference as detected object.
Mixed indicator
The indicator composition of mixed indicator disclosed in the present invention is made up of Bromothymol blue, methyl red and phenolphthalein substantially.
In a preferred embodiment of the invention, in described indicator composition, comprise Bromothymol blue 25 ~ 55 weight portion, methyl red 3 ~ 25 weight portion and phenolphthalein 25 ~ 80 weight portion,
In another preferred embodiment of the invention, described indicator composition comprises Bromothymol blue 30 ~ 50 weight portion, methyl red 5 ~ 20 weight portion and phenolphthalein 30 ~ 70 weight portion.
Here " substantially by ... composition " to refer in mixed indicator not containing or indicator at the most containing other a small amount of or micro-type.But do not get rid of adding of other non-indicator composition in this mixed indicator, as adding of solvent or thinning agent.
Described bromthymol blue, also referred to as bromothymol blue, or 3 ', 3 "-dibromo Thymol Blues.Described methyl red, also referred to as butter yellow o-carboxylic acid, methane is red or alkane is red.The mixed indicator used in the present invention, the change of its color has very narrow visual range, namely when each acid value of lipids integer figure change, also obvious change can be there is in color, therefore, according to the principle of this colour developing, the acid value numerical value in grease determines the acid value of grease easily via the change of color.
At mixed indicator of the present invention, can be dissolved in solvent and use, the solvent adopted can be single solvent, also can be the solvent of mixing, as water or the organic solvent that dissolves each other with water.The preferred lower alcohol of described organic solvent, described lower alcohol is at normal temperatures for liquid carbon number is the hydroxyl compound solvent of 1 to 8.Concrete, the non-limitative example of lower alcohol comprises: methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutyl alcohol, the tert-butyl alcohol, amylalcohol etc.
Mixed indicator in the present invention has narrower variable color difference, and when acid number or acid value are changed to 1, the result developed the color by this mixed indicator, range estimation has obviously to be distinguished.Therefore, color change interval is narrow, and when detecting the oil sample of the unknown, employing colourimetry just can distinguish the acid value representated by often kind of color easily.
Described mixed indicator in use, can be carry out mixture with arbitrary proportion and solvent, those skilled in the art are appreciated that, the addition of indicator is little on the impact of colour developing, can realize the addition of the object of the invention, all in scope disclosed by the invention.The amount of the indicator added is every 100mg grease 100 ~ 150ul.
The method of oil acid value detection
For the oil kind that the color of crude oil to be detected is more shallow, can not desolventing technology be carried out, directly carry out fatty acid detection method as described below and carry out.
But for the grease to be measured that color is darker, because its color is comparatively dark, directly carries out testing result and have certain error.Detect in acid value of lipids in traditional titrimetry, because dark color with oil color is comparatively dark, the interference of grease intrinsic colour and be difficult to the variable color observing indicator, is namely difficult to judge titration end-point.Although can by materialsing less and adding the judgement that solvent improves titration end-point, when oil sample color is pitch black, very few sample can strengthen error at measurment, and too much solvent load can cause waste of solvent and increase the judgement difficulty of titration end-point.
Present invention employs two approach to address this problem, Article 1 approach is by decolouring reddish brown crude oil adsorbent; Article 2 approach, by extraction desolventing technology, reaches the effect of decolouring.Two kinds of methods all reach the acid value that both can not change sample itself, can reduce tested number again, provide a kind of fast, convenient, save money and the portable method of environmental protection.
Before detecting, oil sample (being called for short oil sample to be measured or testing sample) to be detected can carry out adsorbent desolventing technology, described desolventing technology, can comprise conventional grease-decolor process.Comprise and adopt adsorbent to decolour, as activated charcoal, silica gel, carclazyte, molecular sieve or silicate decolour etc.
In a specific embodiment of the present invention, oil sample to be measured and activated charcoal are refluxed when organic solvent exists, except the dark impurity in degrease, therefore when carrying out colour developing and judging, interference by color is smaller, is therefore conducive to adopting colourimetry to carry out the detection of acid value.
In another one embodiment of the present invention, described grease is by extraction decolouring, concrete, described testing sample and polar organic solvent and non-polar organic solvent are carried out mixing rear table and leaves standstill the two-phase obtaining layering, then this potpourri is mixed with alkali lye.In the mixed solution obtained, add mixed indicator as above, the color of polar solvent, layer and colorimetric card are compared, the acid value result of the testing sample of unknown acid value can be obtained.
In a specific embodiment of the present invention, described detection method may be used for the acid value detecting acid value 4 ~ 36, comprises the following steps:
A method for quick detection acid value of lipids, is characterized in that, described method comprises the following steps:
(1) by oil sample, alkali lye and mixed indicator mixing as mentioned above;
(2) described oil sample color is observed to change;
(3) acid value is determined:
(3-1) when described oil sample is turquoise, grass green or dark green, according to described alkali lye consumption and oil sample color, acid value is determined; Or
(3-2) when described oil sample is sky blue, reduce alkali lye consumption, and repeat step (1)-(3); Or
(3-3) when described oil sample is yellow, increase alkali lye consumption, and repeat step (1)-(3).
In described alkali lye, the mole dosage of alkali and the ratio of grease weight to be measured are 0.96 × 10-4 ~ 6.27 × 10-4mol/g, and the consumption of mixed indicator is every 100mg grease 100ul ~ 150ul.
In step (3-1), acid value is determined by colorimetric card or alkali lye consumption-oil sample color-acid value table.Described colorimetric card or alkali lye consumption-oil sample color-acid value table, refer to the consumption according to alkali lye, within the scope of certain acid value, there is the colour developing of sudden change, concrete, can according to following formula, calculate the consumption (error for ± 35ul) of the required alkali lye added when indicator is shown as grass green, accordingly, also according to the amount of added alkali lye, the acid value of colour developing can be calculated:
V represents the volume adding KOH, and unit is ul
C=0.03289 mol/L
AV is middle acid value value (I)
Therefore, according to which, can calculate the form of alkali lye consumption-oil sample color-acid value, preferably, often group comprises five samples.
Also can making corresponding colorimetric card, described colorimetric card, referring to the color shown adding certain alkali lye amount in the grease of standard acid value and the card be made into.When the sample of unknown acid value adds equal or almost equal alkali lye, and the color demonstrated is identical with the color of the grease of standard acid value, so can confirm that the acid value of this unknown acid value sample is close or identical with this standard acid value.The grease of described colorimetric card employing standard acid value adds mixed indicator of the present invention to carry out developing the color and obtaining, and because its color color change interval is narrow, therefore can carry out colour developing reading quickly and easily, and then measure the acid value of grease.
Colorimetric card described in the present invention can be various color board, also can be the solution with respective color.Not being particularly limited, the colorimetric card described in the present invention, can be the card of answering with caustic dosage, acid number and Color pair, also can contain other various carrier of corresponding relation, as plastic cards, be with coloured test tube, beaker etc.
The preparation method of described colorimetric card, adopt the oil sample with standard acid value or known acid value as handling object, process color is identical with the disposal route of above-mentioned unknown grease or substantially identical, and the molal quantity of the alkali in wherein added alkali lye is identical or substantially identical.
Do not do special restriction, the colorimetric card that any method is made can as the colorimetric card described in the present invention.Especially, colorimetric card in the present invention, refers to the color manifested through above-mentioned indicator after the known sample of certain acid value is added alkali lye.The amount of the alkali lye added is identical or substantially identical with the amount of the alkali lye added in the oil sample of unknown acid value.
In a specific embodiment of the present invention, in the process preparing colorimetric card, especially, using 5 adjacent integer acid values as one group, then add alkali lye and neutralize, make the chromatic zones of each oil sample separately.
In a preferred embodiment of the present invention, decoloured before step (1) to described oil sample, preferably, described decolouring is extraction decolouring; Preferred extraction decolouring comprises and grease to be measured is added polar organic solvent and non-polar organic solvent mixes, and collects polar solvent, layer; Described polar organic solvent refers to the polar organic solvent not occurring to ionize, and its non-limitative example comprises: alcohols, amide-type, ketone etc.Wherein alcohols comprises methyl alcohol, ethanol, propyl alcohol, butanols, amylalcohol etc., and described ketone comprises acetone, MEK, butanone etc.Non-polar organic solvent refers to various little polar organic solvent, its non-limitative example comprises the organic solvents such as ethers, sherwood oil, alkanes, ester class, concrete, alkanes comprises propane, butane, n-pentane, isopentane, isopropyl alkane, isobutane, new butane, hexane, isohexane, isooctane etc., and ethers comprises methyl ether, ether, ethyl methyl ether, propyl ether etc.
Can layering interfaces be formed between the polar organic solvent that the present invention is above-mentioned and non-polar organic solvent, thus be conducive to the interference color in grease being carried out extraction decolouring.
In a preferred embodiment of the present invention, before step (1), described oil sample is decoloured, preferably carry out adsorbent decolouring, preferred adsorbent is activated charcoal, silica gel, carclazyte, molecular sieve or silicate, and the amount of preferred adsorbent is 20 ~ 70% of testing sample.
Described adsorbent decolouring comprises and grease to be measured is added the decolorant such as activated charcoal, silicon dioxide carries out reflux decolour.The ratio of the adsorbent added is the adsorbent of 20 ~ 70% grease weight.The solvent added is alcohols solvent, is selected from methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, butanols etc.
Utilize method disclosed in the present invention, the scope of the acid value of detection can be 4 ~ 36, preferably 4 ~ 12, more preferably 7 ~ 11.Along with the rising of the acid value of oil sample, the amount of the alkali lye added also increases.Develop the color to make the grease of often kind of acid value and differentiate, those skilled in the art suitably can increase and decrease the alkali lye amount added, and the colour developing in certain area is made a distinction as far as possible.
In one embodiment of the invention, the acid value of detection is 35 ~ 36, its result and true value close.In another embodiment of the present invention, the acid value of detection is 32 ~ 33, its result and true value close.In another embodiment of the present invention, the acid value of detection is 24 ~ 25, its result and true value close.
The ratio of the alkali in alkali lye in the present invention and grease to be measured is 0.96 × 10
-4~ 6.27 × 10
-4mol/g.
In a specific embodiment of the present invention, its non-limitative example is: when detection acid value is the grease of 4 ~ 12, in the alkali lye added, the molal quantity of alkali and the ratio of grease weight are 0.96 × 10
-4~ 1.79 × 10
- 4mol/g, when detection acid value is 12 ~ 20, this ratio is 2.50 × 10
-4~ 3.21 × 10
-4mol/g, when detection acid value is the grease of 20 ~ 36, this ratio is 3.93 × 10
-4~ 6.15 × 10
-4mol/g.Concrete, the consumption of the alkali lye added can be calculated by above-mentioned formula (I).
In testing process, the amount of the indicator added has no particular limits, and those skilled in the art, according to routine operation, can determine the consumption of the indicator added in process color.In the specific embodiment of the present invention, the amount of the mixed indicator solvent that every 100mg oil sample to be measured adds is 100ul ~ 150ul.
As previously mentioned, mixed indicator of the present invention, when the grease that detection color with oil color is more shallow, does not need to carry out desolventing technology.Contrast with colorimetric card after directly can being developed the color by above-mentioned method, obtain the acid value scope of grease.Thus reach the object detecting acid value fast.
Detect the product of acid value of lipids
As mentioned above, oil acid value detection method disclosed by the invention, comprises mixed indicator as above, and in the present invention's embodiment, described product also comprises the known standard sample of acid value, colorimetric card and/or alkali lye consumption-oil sample color-acid value table.
Summary
The method for quick of acid value of the present invention can comprise:
(1) oil sample, alkali lye and described mixed indicator are mixed;
(2) described oil sample color is observed to change;
(3) acid value is determined:
(3-1) when described oil sample is turquoise, grass green or dark green, according to described alkali lye consumption and oil sample color, acid value is determined; Or
(3-2) when described oil sample is sky blue, reduce alkali lye consumption, and repeat step (1)-(3); Or
(3-3) when described oil sample is yellow, increase alkali lye consumption, and repeat step (1)-(3).
Advantage:
Adopt the mixed indicator in the present invention to carry out the detection of acid value of lipids, compared to traditional colourimetry, there is following characteristics:
(1) survey the same convenient and swift of acid value with test paper method, but testing result has very high stability simultaneously;
(2) do not need the color of instrument to grease to detect, only need with the naked eye to estimate the acid value just easily can offering an explanation out oil sample to be measured;
(3) laboratory can be departed to operate, and only need a small amount of organic solvent in testing process, facilitate the detection of a large amount of sample.
(4) can be used for the darker grease of color to detect.
Accompanying drawing explanation
Fig. 1 is the acid value of preparation in embodiment 1 is the schematic diagram of the colorimetric card of 4-8.
Fig. 2 is the colour developing result schematic diagram of unknown grease 1 in embodiment 1.
Fig. 3 is the acid value of preparation in embodiment 2 is the schematic diagram of the colorimetric card of 5-10.
Fig. 4 is the schematic diagram of the colour developing result of unknown grease 2 in embodiment 2.
Embodiment
As no specific instructions, various raw material of the present invention all can be obtained by commercially available; Or prepare according to the conventional method of this area.Unless otherwise defined or described herein, all specialties used herein and scientific words and those skilled in the art the meaning be familiar with identical.In addition any method similar or impartial to described content and material all can be applicable in the inventive method.
Other aspects of the present invention, due to disclosure herein, are apparent to those skilled in the art.
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.The experimental technique of unreceipted actual conditions in the following example, measures according to national standard usually.If there is no corresponding national standard, then according to general international standard, normal condition or carry out according to the condition that manufacturer advises.Unless otherwise indicated, otherwise all numbers are weight portion, and all number percent is weight percentage.
Unless otherwise defined or described herein, all specialties used herein and scientific words and those skilled in the art the meaning be familiar with identical.In addition any method similar or impartial to described content and material all can be applicable in the inventive method.
Unknown grease 1-4 used by detection method in the present invention, as the testing sample in the present invention or oil sample to be measured, the true value adopting American Oil examination criteria AOCS Ca5a – 40 to survey its acid value is:
| Oil sample to be measured | Grease 1 | Grease 2 | Grease 3 | Grease 4 |
| Acid value true value | 6.34 | 7.00 | 8.97 | 14.22 |
The concentration of alkali lye C used in embodiment is below 0.03289mol/L.
At following various reagent, be analysis pure.
| Title | Supplier | Article No./lot number/specification |
| Methyl red | Shanghai Ai Bi chemical reagent company limited | Lot number F20090319 |
| Bromcresol green | Shanghai Ai Bi chemical reagent company limited | Lot number F20090319 |
| Thymol blue | Chemical Reagent Co., Ltd., Sinopharm Group | Article No. 71040754 |
| Methyl orange | Shanghai Ai Bi chemical reagent company limited | Lot number F20090325 |
| Dimethyl diaminophenazine chloride | Aladdin reagent (Shanghai) Co., Ltd. | Article No. 1095584 |
| Bromothymol blue | Chemical Reagent Co., Ltd., Sinopharm Group | Article No. 71008460 |
| Phenolphthalein | Chemical Reagent Co., Ltd., Sinopharm Group | P108715 |
| Thymolphthalein | ACROS | Lot number A0272373 |
| Normal hexane | Shanghai Ling Feng chemical reagent company limited | AR500G |
| Methyl alcohol | Chemical Reagent Co., Ltd., Sinopharm Group | AR500G |
| Absolute ethyl alcohol | Chemical Reagent Co., Ltd., Sinopharm Group | AR500G |
| Potassium hydroxide | Yixing City Chemical Reagent Plant No.2 | AR500G |
One, the choice experiment of indicator:
Need the indicator selected must have between very sharp saltation zone during change due to acid value.The indicator adopted is as follows:
When adopting thymol blue to make indicator, be designated as indicator one;
Adopt methyl red (20mg)+bromcresol green (20mg)+thymol blue (50mg), be designated as mixed indicator two;
Adopt methyl orange (15mg)+dimethyl diaminophenazine chloride (20mg)+Bromothymol blue (50mg), be designated as mixed indicator three;
Adopt 30mg Bromothymol blue+20mg methyl red+40mg phenolphthalein+20mg thymolphthalein, be designated as mixed indicator four;
Adopt 20mg Bromothymol blue+20mg methyl red+10mg phenolphthalein+100mg thymolphthalein, be designated as mixed indicator five;
Adopt 20mg Bromothymol blue+40mg methyl red+100mg phenolphthalein+100mg thymolphthalein, be designated as mixed indicator six;
Adopt 30mg Bromothymol blue+20mg methyl red+40mg phenolphthalein, be designated as mixed indicator seven;
Adopt 30mg Bromothymol blue+30mg methyl red+30mg phenolphthalein, be designated as mixed indicator eight;
Adopt 50mg Bromothymol blue+30mg methyl red+30mg phenolphthalein, be designated as mixed indicator nine;
Adopt 20mg Bromothymol blue+5mg methyl red+20mg phenolphthalein, be designated as mixed indicator ten;
Adopt 20mg Bromothymol blue+20mg methyl red+20mg phenolphthalein, be designated as mixed indicator 11;
Adopt 20mg Bromothymol blue+20mg methyl red+20mg phenolphthalein, be designated as mixed indicator 12;
Adopt 40mg Bromothymol blue+40mg methyl red+30mg phenolphthalein, be designated as mixed indicator 13;
Adopt 40mg Bromothymol blue+40mg methyl red+70mg phenolphthalein, be designated as mixed indicator 14.
Table 1 adopts the color change after various indicator interval
| AV value | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | |
| One | Color | Blue | Blue | Blue | Light blue | Light blue | ||||
| Two | Color | Dark blue | Blue | Yellow | Yellow | |||||
| Three | Color | Blue | Blue | Blue | Grass green | Dark green | ||||
| Four | Color | Blue | Blue | Grass green | Dark green | Yellow | ||||
| Five | Color | Blue | Pale blue | Grass green | Dark green | Dark green | ||||
| Six | Color | Blue | Blue | Blue | Grass green | Dark green | ||||
| Seven | Color | Sky blue | Acid blue | Grass green | Dark green | Yellow | ||||
| Eight | Color | Sky blue | Acid blue | Grass green | Dark green | Yellow | ||||
| Nine | Color | Sky blue | Acid blue | Grass green | Dark green | Yellow |
| Ten | Color | Sky blue | Acid blue | Grass green | Dark green | Yellow | ||||
| 11 | Color | Sky blue | Acid blue | Grass green | Dark green | Yellow | ||||
| 12 | Color | Sky blue | Acid blue | Grass green | Dark green | Yellow | ||||
| 13 | Color | Sky blue | Acid blue | Grass green | Dark green | Yellow | ||||
| 14 | Color | Sky blue | Acid blue | Grass green | Dark green | Yellow |
Note: the definition of above-mentioned color and change judge to draw to the more sensitive professional person of color by three jointly.
Corresponding colour developing result, be the grease of standard acid value (4,5,6,7,8,9,10,11,12) 100mg, add containing above-mentioned 120ul indicator (ethanol: heat up in a steamer the mixed indicator that water volume ratio is the solubilize of 3:2), slowly drip alkali lye C(concentration 0.03289mol/L simultaneously), make the colour developing of the grease of the various standard acid values adding same indicator have obvious difference.When the first six group mixed indicator reaches best colour developing, in the grease of every 100mg, add 500-600ul aqueous slkali C.When mixed indicator seven to ten four, when adding the alkali lye of 360ul, its color discrimination is the highest.
As can be seen from the colour developing result in table 1, adopt indicator one, its color change interval is wider, cannot distinguish the sample of each standard acid value.
After adopting indicator two, three mixed indicator, it all narrows than the color range of mixed indicator one, but this combination colour developing result is undesirable, cannot separate concrete acid value scope according to chromatic zones.
After adopting indicator four, five, six, all narrow than indicator color range above, but still color developing effect is not obvious.
Adopt indicator seven ~ indicator 14, visually can distinguish significantly.
Sense organ evaluation and test experiment:
Adopt respectively mixed indicator two, three, four, seven and ten several samples of carrying out developing the color carry out subjective appreciation (develop the color except adopting indicator two have 4 samples except, what use other indicator to develop the color has 5 samples), valuation officer is 10 is the people to the general sensitivity of color, evaluates and tests as follows.
Method one (adopting " two-three-point assay method "): repeat to make two groups of experimental results and (take 100mg standard acid value oil in indicator mix proportion scheme of the same race, add 120ul indicator and 500-600ul aqueous slkali C), two standard acid values are selected respectively identical in two groups, with the grease (i.e. different acid value) of the immediate acid value of another one, thus obtain one group of three sample, require that valuation officer chooses color that single sample differentiated, repeat three experiments.
Method two (adopting " ranking method "): make one group of experimental result and (take 100mg standard acid value oil in indicator mix proportion scheme of the same race, add 120ul indicator and 500-600ul aqueous slkali C), prompting evaluation personnel color trends is changed to: blue-green-yellow, require valuation officer by acid value from small to large, i.e. color change putting in order and arrange from deep to shallow.Repeat three experiments.
Subjective appreciation the results are shown in following table:
The results of sensory evaluation of the different indicator of table 2
| Indicator | Method one (error rate) | Method two (error rate) |
| Two | 100% | 100% |
| Three | 100% | 100% |
| Four | 100% | 100% |
| Seven | 0% | 0% |
| Ten | 0% | 0% |
Two, oil acid value detection embodiment:
Embodiment 1:
The preparation of starting material and reagent:
(1) solution and indicator is configured
1. saturated normal hexane and methanol solution: analytically pure methyl alcohol and normal hexane are poured in separating funnel respectively, fully vibrates, stratification; Getting upper strata is saturated hexane solution A, and taking off layer is saturated methanol solution B, carries out airtight preservation respectively, stand-by.
2. the mixed liquor of second alcohol and water: ethanol (analyzing pure) is mixed with the ratio of 3:2 with distilled water, airtight preservation, stand-by.
3. aqueous slkali: the mixed liquor adding second alcohol and water in potassium hydroxide, fully carry out demarcation after mixing and obtain alkali lye C, its alkali concn numerical value (0.03289moL/L), keeps in Dark Place, stand-by.
4. indicator: the mixed liquor adding 20ml second alcohol and water in mixed indicator seven (Bromothymol blue 30mg+ methyl red 20mg+ phenolphthalein 40mg), airtight preservation, stand-by.
(2) preparation of colorimetric card:
1. purified soyabean oil and palmitic acid (analyzing pure) configuration acid value is used to be respectively 4,5,6,7, the standard acid value oil of 8: measure purified soyabean oil and palmitic acid acid value is respectively AVa and AVb, Refined Soybean oil quality is m1, and palmitic acid quality is m2, carries out the configuration of standard acid value oil according to formula m1 × AVa+m2 × AVb=acid value × (m1+m2).
2. take the standard acid value oil of about 100mg → add 4ml solution A to carry out dissolving → accurately add 360ul aqueous slkali C and fully shake up mixed indicator seven that 4ml solution B of vibrating → add carries out extracting → get subnatant → add 120ul and carry out chromogenic reaction → as one of standard colorimetric.
3. standard acid value oil content acid value being respectively 4-8 does not carry out reaction solution, the standard color comparison card that the 5 kinds of chromogenic reaction results obtained are answered as an acid value and Color pair according to above process 2..
(3) chromogenic reaction:
Take the reddish brown grease 1 of about 100mg → add 4ml solution A to carry out dissolving → accurately add 360ul aqueous slkali C and fully shake up mixed indicator seven that 4ml solution B of vibrating → add carries out extracting → adding 120ul and carry out chromogenic reaction → contrast with standard color comparison card (Fig. 1) according to the colour developing result (Fig. 2) of lower floor's solution, reading acid value is 6-7, and testing result and true value close.
Use mixed indicator eight ~ 14 to replace mixed indicator seven respectively, repeat above-mentioned test, result is similar to using the result of mixed indicator seven.
Embodiment 2:
(1) decolouring of grease
Take the reddish brown oil of about 200mg, then add the activated charcoal of 8ml isopropyl alcohol (analyzing pure) and about 100mg, heating reflux decolour 15min, solution E after obtaining after filtration decolouring.
(2) solution and indicator is configured
1. aqueous slkali: the mixed liquor adding second alcohol and water in potassium hydroxide, fully demarcates after mixing, writes down numerical value (0.03289moL/L) and be recorded as alkali lye C, keeping in Dark Place, stand-by.
2. indicator: the mixed liquor adding 20ml second alcohol and water in mixed indicator eight, airtight preservation, stand-by.
(3). the preparation of standard color comparison card
1. the grease of the standard acid value in embodiment 1 is adopted;
2. the mixed indicator eight → fully shake up vibration → colour developing result as standard color comparison card of solution → add aqueous slkali C and 120ul of 470ul after accurately pipetting 4ml decolouring.
3. do not reacted according to above process 2. by the standard acid value oil content of 7-11, the 5 kinds of chromogenic reaction results obtained are as a standard color comparison card.
(4). chromogenic reaction:
The mixed indicator eight of solution after the reddish brown grease 2 taking about 100mg accurately pipettes 4ml decolouring → add aqueous slkali C and 120ul of 470ul → fully shake up vibration → colour developing result (Fig. 3) to contrast with standard color comparison card (Fig. 4), reading acid value scope is 7-8, testing result and true value close.
Use mixed indicator seven, nine ~ 14 to replace mixed indicator eight respectively, repeat above-mentioned test, result is similar to using the result of mixed indicator eight.
Activated carbon decolorizing and conventional titration contrast (adopting GB/T5530-2005 method to detect)
| Reddish brown oil samples to be measured | Conventional titration | Titration after activated carbon decolorizing | Relative error |
| Grease 1 | 7.15 | 7.18 | -0.42% |
| Grease 2 | 7.62 | 7.83 | -2.76% |
| Grease 3 | 9.27 | 9.19 | 0.86% |
| Grease 4 | 14.42 | 14.48 | 0.42% |
As can be seen from the content of upper table, the acid value in grease substantially not sorbent suspension decolouring impact, decolouring process in, only have the pigment impurity in grease to be tightly held by activated carbon, and free fatty acid does not change significantly.Therefore can illustrate, the accuracy that desolventing technology can not have influence on the acid value testing result of grease is carried out to crude oil.
Three, stability experiment
3 experimental implementation persons test following three kinds of greases repeatedly according to the step of embodiment 1 and embodiment 2, and stability and repeatability are all good, rate of accuracy reached 100%.
Embodiment 3:(is identical with the method for operating in embodiment 1, but the alkali lye amount added is not identical, and preparing colorimetric card accepted standard acid value grease is 12-16):
Take the reddish brown grease 4 of about 100mg → add 4ml solution A to carry out dissolving → accurately add 760ul aqueous slkali C and fully shake up mixed indicator nine that 4ml solution B of vibrating → add carries out extracting → adding 120ul and carry out chromogenic reaction → contrast with standard color comparison card with the colour developing result of lower floor's solution, reading acid value is 14-15, testing result and true value close.
Embodiment 4:(is identical with the method for operating in embodiment 1, but the alkali lye added is different, and preparing colorimetric card accepted standard acid value grease is 8-12)
Take the reddish brown grease 3 of about 100mg → add 4ml solution A to carry out dissolving → accurately add 543ul aqueous slkali C and fully shake up mixed indicator ten that 4ml solution B of vibrating → add carries out extracting → adding 120ul and carry out chromogenic reaction → contrast with standard color comparison card with the colour developing result of lower floor's solution, reading acid value is 8-9, testing result and true value close.
Embodiment 5:(is identical with the method in embodiment 2):
Reddish brown grease 2 is added 4ml isopropyl alcohol adopt the decolouring of the method in embodiment 2 after the mixed indicator 11 → fully shake up vibration → colour developing result to contrast with standard color comparison card of solution → add aqueous slkali C and 120ul of 470ul, reading acid value scope is 7-8, close with true value.
Four, the method in employing the present invention detects colorimetric card preparation method when acid value is the grease of 4-36
The method in embodiment 1 or embodiment 2 is adopted to carry out developing the color and judge the acid value of crude oil.
When preparing colorimetric card used in the present invention, 5 groups of standard acid value greases are one group, get the addition that middle acid value value is criterion calculation alkali lye.
The computing formula of the amount of the alkali lye added in the grease of every 100ml is:
V represents the volume adding KOH, and unit is ul
C=0.03289 mol/L
AV is middle acid value value
The concentration preparing the alkali lye C that colorimetric card adopts is:
For the oil sample of a unknown acid value, when its acid value is in 4-36, this colorimetric card can be pursuant to and detects.
Chromogenic reaction 1: unknown grease 4 is detected, the method in embodiment 1 is adopted to process, first compare by the method for the colorimetric card of 4-8, find that its colour developing result is for yellow, infer that its acid number should more than 8, therefore, use the colorimetric card of 8-12 instead, adopt the method in embodiment 4 to process unknown grease 4, its colour developing result is yellow, infers that its acid number should more than 12.After adopting the method in embodiment 3 to process, when comparing with the colorimetric card of 12-16, its colour developing result is between 14-15, and therefore can determine that the acid number of unknown grease 4 is 14-15, the true valency of this result and acid value of lipids is close.
For disclosed several detection method in detection method disclosed in this patent and prior art, its relative merits are than as follows:
The foregoing is only preferred embodiment of the present invention, and be not used to limit substantial technological context of the present invention, substantial technological content of the present invention is broadly defined in the right of application, any technology entities that other people complete or method, if with application right define identical, also or a kind of change of equivalence, be all covered by being regarded as among this right.
The all documents mentioned in the present invention are quoted as a reference all in this application, are just quoted separately as a reference as each section of document.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read foregoing of the present invention, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (10)
1. a mixed indicator, is characterized in that, the indicator composition of described mixed indicator is made up of Bromothymol blue, methyl red and phenolphthalein substantially.
2. mixed indicator as claimed in claim 1, it is characterized in that, substantially be made up of Bromothymol blue 25 ~ 55 weight portion, methyl red 3 ~ 25 weight portion and phenolphthalein 25 ~ 80 weight portion in described indicator composition, preferably, described indicator composition is made up of Bromothymol blue 30 ~ 50 weight portion, methyl red 5 ~ 20 weight portion and phenolphthalein 30 ~ 70 weight portion substantially.
3. mixed indicator as claimed in claim 1 or 2, it is characterized in that, the solvent of described mixed indicator is selected from water or lower alcohol, described lower alcohol be preferably in methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, butanols one or more.
4. detect a method for acid value of lipids fast, it is characterized in that, described method comprises the following steps:
(1) by mixed indicator mixing according to any one of oil sample, alkali lye and claim 1-3;
(2) described oil sample color is observed to change;
(3) acid value is determined:
(3-1) when described oil sample is turquoise, grass green or dark green, according to described alkali lye consumption and oil sample color, acid value is determined; Or
(3-2) when described oil sample is sky blue, reduce alkali lye consumption, and repeat step (1)-(3); Or
(3-3) when described oil sample is yellow, increase alkali lye consumption, and repeat step (1)-(3).
5. method as claimed in claim 4, it is characterized in that, in described alkali lye, the mole dosage of alkali and the ratio of grease weight to be measured are 0.96 × 10
-4~ 6.27 × 10
-4mol/g, the consumption of mixed indicator is every 100mg grease 100ul ~ 150ul.
6. method as claimed in claim 4, is characterized in that, in step (3-1), acid value is determined by colorimetric card or alkali lye consumption-oil sample color-acid value table.
7. method as claimed in claim 4, it is characterized in that, step (1) front also comprise the acid value scope determining described grease step and/or, before step (1), also comprise the step that described oil sample is decoloured, preferably, described decolouring is adsorbent decolouring and/or extraction decolouring;
Preferred extraction decolouring comprises and grease to be measured is added polar organic solvent and non-polar organic solvent mixes, collect polar solvent, layer, preferred polar solvent comprises alcohols, amide-type, organic solvent of ketone, and preferred non-polar solvent comprises ethers, sherwood oil, alkanes, based organic solvent;
Preferred adsorbent is activated charcoal, silica gel, carclazyte, molecular sieve or silicate, and/or the amount of preferred adsorbent is 20 ~ 70% of testing sample.
8. method as claimed in claim 4, it is characterized in that, the acid value of described grease is 4-36, is preferably 4 ~ 12, is more preferably 7 ~ 11.
9. the mixed indicator according to any one of claim 1-3 is detecting the application in acid value of lipids.
10. one kind is detected the product of acid value of lipids, it is characterized in that, described product comprises the mixed indicator according to any one of claim 1-3, and preferably, described product also comprises the known standard sample of acid value, colorimetric card and/or alkali lye consumption-oil sample color-acid value table.
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| CN106338512A (en) * | 2016-09-18 | 2017-01-18 | 国网福建省电力有限公司 | Acid content measurement device for insulating paper for electric power high voltage oil-filled equipment and implementation method of acid content measurement device |
| CN107389669A (en) * | 2017-06-22 | 2017-11-24 | 湖北富邦科技股份有限公司 | A kind of dark oil anti-caking agent acid number content assaying method |
| CN107677534A (en) * | 2017-09-08 | 2018-02-09 | 广东宝华农业科技股份有限公司 | A kind of rapid extraction grease from oil plant is used for the method for acid value detection |
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| CN108020547A (en) * | 2017-12-17 | 2018-05-11 | 沧州普瑞东方科技有限公司 | A kind of method for measuring organic three potassium fluoborates salt content |
| CN108072651A (en) * | 2016-11-28 | 2018-05-25 | 上海泓宝绿色水产股份有限公司 | A kind of total alkalinity detecting system and its application method for being used to detect that total alkalinity is 0-300mg/L |
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| CN110736742A (en) * | 2018-07-18 | 2020-01-31 | 郑州科技学院 | fried vegetable oil quality identification color developing agent and preparation method and application thereof |
| CN110736743A (en) * | 2018-07-18 | 2020-01-31 | 郑州科技学院 | fried corn oil quality identification color developing agent and preparation method and application thereof |
| CN111289508A (en) * | 2018-12-07 | 2020-06-16 | 云南商测质量检验技术服务有限公司 | Acid value rapid test paper and detection method thereof |
| CN113533628A (en) * | 2021-07-19 | 2021-10-22 | 西安热工研究院有限公司 | Method for detecting acid value of synthetic lubricating oil |
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| CN113533628B (en) * | 2021-07-19 | 2023-09-29 | 西安热工研究院有限公司 | Method for detecting acid value of synthetic lubricating oil |
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