CN106383119A - Spectrophotometry of rapidly detecting concentration of peroxide in edible oil - Google Patents
Spectrophotometry of rapidly detecting concentration of peroxide in edible oil Download PDFInfo
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- CN106383119A CN106383119A CN201610982392.5A CN201610982392A CN106383119A CN 106383119 A CN106383119 A CN 106383119A CN 201610982392 A CN201610982392 A CN 201610982392A CN 106383119 A CN106383119 A CN 106383119A
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- solution
- colour developing
- methanol
- agent
- butanol
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- 150000002978 peroxides Chemical class 0.000 title claims abstract description 56
- 239000008157 edible vegetable oil Substances 0.000 title claims abstract description 21
- 238000002798 spectrophotometry method Methods 0.000 title abstract description 7
- 239000000243 solution Substances 0.000 claims abstract description 110
- 239000003921 oil Substances 0.000 claims abstract description 58
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 56
- 239000003381 stabilizer Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 189
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 132
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 55
- 239000003795 chemical substances by application Substances 0.000 claims description 48
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 20
- 238000001514 detection method Methods 0.000 claims description 19
- 238000005375 photometry Methods 0.000 claims description 17
- 239000002738 chelating agent Substances 0.000 claims description 15
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical group [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 claims description 14
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims description 14
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 13
- 229930003268 Vitamin C Natural products 0.000 claims description 13
- 235000019154 vitamin C Nutrition 0.000 claims description 13
- 239000011718 vitamin C Substances 0.000 claims description 13
- -1 hydroxylamine compound Chemical class 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 11
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 10
- 150000002440 hydroxy compounds Chemical class 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 7
- VGYYSIDKAKXZEE-UHFFFAOYSA-L hydroxylammonium sulfate Chemical compound O[NH3+].O[NH3+].[O-]S([O-])(=O)=O VGYYSIDKAKXZEE-UHFFFAOYSA-L 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical group [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- 230000000717 retained effect Effects 0.000 claims description 3
- 239000001119 stannous chloride Substances 0.000 claims description 3
- 235000011150 stannous chloride Nutrition 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims 1
- 230000031700 light absorption Effects 0.000 abstract description 35
- 239000002699 waste material Substances 0.000 abstract description 5
- 239000012496 blank sample Substances 0.000 abstract description 3
- 239000008139 complexing agent Substances 0.000 abstract 3
- ZWLQACFYTXLLEJ-UHFFFAOYSA-N butan-1-ol;methanol Chemical compound OC.CCCCO ZWLQACFYTXLLEJ-UHFFFAOYSA-N 0.000 description 44
- 238000000034 method Methods 0.000 description 41
- 239000003153 chemical reaction reagent Substances 0.000 description 31
- 150000001875 compounds Chemical class 0.000 description 28
- 239000011521 glass Substances 0.000 description 28
- 239000007787 solid Substances 0.000 description 28
- 239000012046 mixed solvent Substances 0.000 description 24
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 description 23
- 238000004458 analytical method Methods 0.000 description 21
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 13
- 239000000523 sample Substances 0.000 description 11
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 229910001448 ferrous ion Inorganic materials 0.000 description 8
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 7
- 229910001447 ferric ion Inorganic materials 0.000 description 6
- 238000004401 flow injection analysis Methods 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000019197 fats Nutrition 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 235000016709 nutrition Nutrition 0.000 description 2
- 230000035764 nutrition Effects 0.000 description 2
- 235000014593 oils and fats Nutrition 0.000 description 2
- 238000012803 optimization experiment Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 1
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 210000000577 adipose tissue Anatomy 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- NXPHCVPFHOVZBC-UHFFFAOYSA-N hydroxylamine;sulfuric acid Chemical compound ON.OS(O)(=O)=O NXPHCVPFHOVZBC-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 206010040882 skin lesion Diseases 0.000 description 1
- 231100000444 skin lesion Toxicity 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Engineering & Computer Science (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a spectrophotometry of rapidly detecting the concentration of peroxide in edible oil. The spectrophotometry adopts the following components including a reducing agent solution and a color development complexing agent and is characterized in that a stabilizer is added in the reducing agent solution and/or the color development complexing agent or in a mixed solution of the reducing agent solution and the color development complexing agent. According to the spectrophotometry, the background value of a blank sample is lowered to enable color reaction not to be interfered, a light absorption value is stable enough to enable the spectrophotometry to be combined with the existing spectrophotometric determination instrument to accurately determine the concentration of the peroxide, and poor quality oil and waste oils are effectively distinguished.
Description
Technical field
The present invention relates to a kind of photometry, particularly to a kind of luminosity of peroxide concentrations in quick detection edible oil
Method.
Background technology
Fat is the Main Ingredients and Appearance of edible oil, is also the basic nutrition material required for human normal vital movement, to people
The operation of body normal physiological function is most important.The fatty acid producing after steatolysiss is the most direct energy source of human body.Remove
Outside storage and supplying energy, multiple fatty acids that oils and fatss provide, including Oleic acid, linoleic acid, alpha-linolenic acid etc., are body structures
Important component, oils and fatss lack and poor growth even stagnation, skin lesion etc. will occur.Research shows, the human body fat of one day
Fat acid source about 50% is obtained by edible oil.Therefore edible oil, for supplementing human nutrition in time, safeguards that health is must
Indispensable.
Unsaturated lipid compound in oil product can occur redox reaction to produce peroxide with the oxygen of in the air.With
Peroxide concentrations to raise, in oil product, various harmful substance contents also can accordingly increase, and eventually results under oil quality
Fall, or even oil product Kazakhstan is smelly, becomes sour, and goes bad.Peroxide value is one of international important indicator of measurement edible oil quality, it
Directly reflect the quality of oil quality.Peroxide in oil product is also a kind of harmful substance being detrimental to health in itself,
Excess intake lipid peroxide, may lead to cardiovascular disease, accelerate the aging of human organ.
At present, the commonly used traditional standard method of the determination of POV in food oil, i.e. iodometry.The method
Although not needing special instruments and equipment, existence and stability and poor reproducibility, time-consuming, and operation requires intrinsic the lacking such as strict
Point.Except iodimetric titration, also various instrument analytical methods, including fluorophotometric, chemiluminescence is it is seen that spectrophotometric, liquid phase color
Spectrum, liquid matter is online, and chromaticness is online, Flow Injection Analysis etc..These methods respectively have feature, such as, the flowing note that Japanese proposes
Penetrate-fluorimetry, sensitivity, selectivity are all very high, but the response time requiring is long, under conditions of heating, flow injection
The reacting ring length of analysis system remains a need for more than 80 meters and just can complete chromogenic reaction, and this is to the anti-pressure ability of whole system and defeated
Send the requirement of pump all very high.Chemiluminescence is very sensitive, but needs special and expensive fluorometric reagent, and this reagent is at present also
The not marketization.In oil product, the content of peroxide is higher, does not need method to have very high sensitivity during practical application.Here
Afterwards, American scholar proposes the flow injection-analytical photometry of peroxide for 1999.This Flow Injection Analysis System reacts
Circle length only needs 20 cm, so that the pressure of mobile phase induction system returns normal pressure, system is simplified, analyze speed
Also very fast.
Liquid matter is online, and the online required equipment of chromaticness is relatively expensive, and analyze speed is slower, and needs complexity, consumption
When sample pre-treatments.
It is the more method of current application with the peroxide in spectrophotometric determination oil product.Spectrophotometer with respect to
Gas chromatogram, liquid chromatograph, infrared spectrometer, liquid matter is online, and chromaticness is online etc., have more economical, the features such as simple to operate.
But this instrumental method generally deposits weakness at present is that sample pre-treatments are complicated, such as mostly needs to extract, separates, heating waited
Journey, wastes time and energy, and analyze speed is slower.
In addition these methods are mostly used only to measure the peroxide value in normal oil product, can not be applied directly to poor quality
Oil, the discriminating of waste oil and monitoring.Main cause is existing method is to divide just for the relatively simple Normal Goods oil of composition
Analysis object is set up, and waste oil (including swill oil, reclaim frying oil an etc.) class complex sample is difficult to be suitable for.This kind of multiple
There is more impurity in miscellaneous sample, easily cause severe jamming, leads to method to lose efficacy.
Present patent application inventor cooperated with P.K.Dasgupta, proposed a kind of flow injection-photometry in 1999
Peroxide in analysis oil product.The method detects that the principles of chemistry of peroxide in oil product are:
Fe2++ROOH+H+→RO·+Fe3++H2O (1)
RO·+Fe2++H+→ROH+Fe3+(2)
Fe3++n(SCN-)→Fe(SCN)n (3-n)+(3)
ROOH in reaction equation:Represent the lipid peroxide in food oil.
This method solvent for use is methanol or butanol or methanol and butanol mixed liquid;Reducing agent is ferrous salt;Colour developing complexation
Agent is rhodanate.
Ferrous ion generates ferric ion (see reaction equation (1)) with peroxide reactions in a solvent.Chemical reaction
The oxygen radical of one of the product in formula (1) also can react generation ferric ion (see reaction equation with ferrous ion
(2)).Ferric ion forms red complex with thiocyanate ion, thus the content with spectrphotometric method for measuring red complex.
Experiment shows, the concentration of peroxide and the red complex content being formed have quantitative correspondingly closing under given conditions
System, and response speed is fast, and sample pre-treatments are simple.Measure in oil product using above-mentioned chemical reaction and with reference to flow injection system
Peroxide concentrations achieve preferable effect.Flow injection system automaticity is higher, but equipment is costly.
If using the above-mentioned principles of chemistry and peroxide concentrations in photometer combination mensuration edible oil, it will significantly reduce
Instrument and equipment cost, instrumentation is also simpler, beneficial to penetration and promotion.If however, directly utilizing the above-mentioned principles of chemistry to prepare
Analysis sample, measures peroxide concentrations with photometer and can face following problem:In order to test the peroxidating of variable concentrations scope
Thing, reagent ferrous ions and colour developing chelating agent must be all excessive, but ferrous ion is in the presence of excessive colour developing chelating agent,
Its electrode potentialBecome very low, reducing power is extremely strong, easily by the dissolved oxygen Quick Oxidation in solution, this will
Lead to following serious problems:(1) background value of blank sample is too high;(2) normal chromogenic reaction is heavily disturbed, light absorption value
Extremely unstable.This two factors meeting severe jamming measurement results, lead to analysis result inaccurate, or even detect unsuccessfully.This is mesh
Chromogenic reaction in front above-mentioned system is difficult to combine with photometer and carries out the main cause of detection by quantitative peroxide.
Content of the invention
For existing problem, it is an object of the invention to provide peroxide concentrations in a kind of quick detection edible oil
Photometry, reduces the background value of blank sample, makes chromogenic reaction interference-free, light absorption value is sufficiently stable, make it with existing
Photometric instrument combines the Accurate Determining carrying out peroxide concentrations, effectively differentiates poor oil and waste oil.
To achieve these goals, the technical scheme is that:Peroxide concentrations in a kind of quick detection edible oil
Photometry, including reductant solution and colour developing enveloping agent solution it is characterised in that:In described reductant solution and/or colour developing
Add stabilizer in enveloping agent solution;Or add stabilizer in the mixed solution of reductant solution and colour developing enveloping agent solution.
Specifically detecting step is:
(1), respectively reducing agent and colour developing chelating agent solvent are prepared solution, and be retained separately;
(2), in reductant solution or/and colour developing enveloping agent solution, add stabilizer, then before the reaction by reducing agent
Solution and colour developing enveloping agent solution mixing;
Or the reducing agent of stabilizer and the chelating agent mixing that develops the color will be not added with before the reaction, directly it is not added with stablizing above-mentioned
Add stabilizer in the reductant solution of agent and colour developing chelating agent mixed liquor;
(3), in the mixed solution of the reductant solution having stabilizer and colour developing enveloping agent solution, add oil samples, mix
Even, react 10-50s, reacted sample is transferred in photometer and carries out detecting the content obtaining peroxide.
First colour developing enveloping agent solution and reductant solution are retained separately, carry out again when carrying out sample detection mutually
Mixing, so can avoid two kinds of solution to mix the ferrous ion causing too early and be dissolved oxygen fast oxidative problem in a large number.Plus
Enter stabilizer and suppress dissolved oxygen iron protoxide ion further, make normal chromogenic reaction from interference, so that system
Light absorption value is sufficiently stable in the range of certain time, and abundant satisfaction accurately carries out the basic demand of photometric detection.
In such scheme:Described stabilizer is iron powder, reproducibility hydroxy compounds, reproducibility hydroxylamine compound and tin salt
In at least one.
In such scheme:Described stabilizer is iron powder, and the mass concentration of described iron powder is 0.0001-5.0g/L.
In such scheme, described stabilizer is reproducibility hydroxy compounds, and the concentration of described reproducibility hydroxy compounds is
0.0001-30.0mmol/L.
In such scheme, described reproducibility hydroxy compounds are vitamin C.
In such scheme, described stabilizer is reproducibility hydroxylamine compound, and the concentration of described reproducibility hydroxylamine compound is
0.0002-50mmol/L.
Preferably:Described reproducibility hydroxylamine compound is oxammonium sulfate., at least one in oxammonium hydrochloride..
In such scheme:Described stabilizer is tin salt, and the concentration of described tin salt is 0.0001-100mmol/L.
Preferably:Described tin salt is stannous sulfate, at least one in stannous chloride.
In such scheme:Reducing agent is ferrous salt;Colour developing chelating agent is rhodanate, and the concentration of reducing agent is 0.5-
50mmol/L, the concentration of colour developing chelating agent is 0.5-40mmol/L, and described solvent is methanol or butanol, or described solvent is methanol
The mixed solution prepared according to arbitrary proportion with butanol.
Experiment shows, the stabilizer concentration size of addition is particularly significant to the stability of chromogenic reaction.Concentration is too low cannot
Reach the rapid oxidation of suppression ferrous ion, do not reach the purpose of stable chromogenic reaction;Excessive concentration can lead to ferrous ion with
The ferric ion that peroxide produces is reduced rapidly, does not equally reach the purpose of stable chromogenic reaction.Through repetition test, I
Have found various stabilizers in reductant solution, or simultaneously colour developing enveloping agent solution and reductant solution in optimal
Concentration range.Under this concentration conditions, the stabilization time scope of chromogenic reaction was up to 30~50 minutes.This time be enough to complete oil
The photometry detection of peroxide in product.
Due to using said method it is ensured that the low latitude white background value of sample and the high stability of chromogenic reaction, fully full
The foot basic demand of Instrument measuring, overcome in this system due to ferrous ion being difficult to of being dissolved that oxygen Quick Oxidation leads to and
Photometer combines the difficult problem carrying out that in oil product, determining of peroxide value is surveyed.Fig. 1 is under the conditions of identical optimization experiment, dense with peroxide
Spend fast detector when adding moderate amount of sulfuric acid azanol and stannous sulfate complex stabilizer and being added without stabilizer, to same oil sample
Product are analyzed measuring the light absorption value obtaining -- time curve.As shown by data adds the light absorption value of stabilizer post analysis sample
Stability significantly improves.
Fig. 2 is the representative standard curve obtaining under the conditions of one group of optimization experiment.As shown by data, this system is in finite concentration
In the range of, light absorption value and peroxide concentrations have good linear relationship (R2=0.9925).
The invention has the beneficial effects as follows:The present invention proposes a kind of brand-new intelligence measuring lipid peroxide in oil product
Change rapid detection system, have that analyze speed is fast, accuracy rate is high, the features such as good stability, simple to operate, low cost.
Brief description
Fig. 1 is light absorption value and peroxide concentrations standard curve.
Fig. 2 is the graph of a relation of time and light absorption value.
Specific embodiment
The present invention will be further described with specific embodiment below in conjunction with the accompanying drawings:
Embodiment 1
Colour developing enveloping agent solution is prepared:36mmol NH4Methanol butanol mixed liquid (the methanol of SCN:Butanol=7: 3, V/V).
Compound method:Weigh 18mmol NH4In SCN to 500 milliliter of beaker, measure 500 ml methanol butanol mixed solvents with graduated cylinder
(methanol:Butanol=7: 3, V/V) in this 500 milliliters of beakers, stirred to solid dissolving with glass rod.
Reductant solution is prepared:20mmol(NH4)Fe(SO4), the methanol butanol mixed solution of 2.8mmol vitamin C
(methanol:Butanol=99:1,V/V).Compound method:Weigh 10mmol (NH4)Fe(SO4), 1.4mmol vitamin C is to 500 millis
Rise in beaker, measure 500 ml methanol butanol mixed solvent (methanol with graduated cylinder:Butanol=99:1, V/V) this 500 milliliters burnings are arrived
In cup, stirred to solid dissolving with glass rod.
10.0 milliliters of reductant solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor during mensure
In milliliter reagent bottle, then pipette 0.5 milliliter of oil samples in reagent bottle, cover tightly the equal power of bottle cap and shake 10-20 second, stand solution
The 20-30 second can measure its light absorption value on photometer, according to the standard curve of Fig. 2, obtains the concentration of peroxide.We are right
Instrument adds software and data is processed and analyzes, and this software is this area conventional meanses, and this software is by the extinction measuring
Value is analyzed with the corresponding data of standard specimen automatically, provides the identification result of oil quality, result and actual samples taken
It is consistent.
Embodiment 2
Colour developing chelating agent agent solution is prepared:50mmol NH4Methanol butanol mixed liquid (the methanol of SCN:Butanol=7:3,V/
V).Compound method:Weigh 25mmol NH4In SCN to 500 milliliter of beaker, measure 500 ml methanol to this 500 milliliters with graduated cylinder
In beaker, stirred to solid dissolving with glass rod.
Reductant solution is prepared:40mmol(NH4)Fe(SO4), the methanol of 30mmol vitamin C.Compound method:Weigh
20mmol(NH4)Fe(SO4), 15mmol vitamin C, in 500 milliliters of beakers, measures 500 ml methanol butanol with graduated cylinder and mixes
Bonding solvent (methanol:Butanol=99:1, V/V) in this 500 milliliters of beakers, stirred to solid dissolving with glass rod.
10.0 milliliters of reductant solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor during mensure
In milliliter reagent bottle, then pipette 0.5 milliliter of oil samples in reagent bottle, cover tightly the equal power of bottle cap and shake 10-20 second, stand solution
The 20-30 second can measure its light absorption value on photometer, according to the standard curve of Fig. 2, obtains the concentration of peroxide.We are right
Instrument adds software and data is processed and analyzes, and this software will be entered the light absorption value measuring automatically with the corresponding data of standard specimen
Row relative analyses, provide the identification result of oil quality, and result is consistent with actual samples taken.
Embodiment 3
Colour developing chelating agent agent solution is prepared:Methanol butanol mixed liquid (the methanol of 0.5mmol NH4SCN:Butanol=7: 3, V/
V).Compound method:Weigh in 0.025mmol NH4SCN to 500 milliliter of beaker, measure 500 ml methanol butanol mixing with graduated cylinder
Solvent (methanol:Butanol=7:3, V/V) in this 500 milliliters of beakers, stirred to solid dissolving with glass rod.
Reductant solution is prepared:0.5mmol (NH4) Fe (SO4), the methanol butanol mixing of 0.0001mmol vitamin C
Solution (methanol:Butanol=99: 1, V/V).Compound method:Weigh 0.025mmol (NH4) Fe (SO4), third kind of 0.00005mmol
Vitamin, in 500 milliliters of beakers, measures 500 ml methanol butanol mixed solvent (methanol with graduated cylinder:Butanol=99: 1, V/V)
To in this 500 milliliters of beakers, stirred to solid dissolving with glass rod.
10.0 milliliters of reductant solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor during mensure
In milliliter reagent bottle, then pipette 0.5 milliliter of oil samples in reagent bottle, cover tightly the equal power of bottle cap and shake 10-20 second, stand solution
The 20-30 second can measure its light absorption value on photometer, according to the standard curve of Fig. 2, obtains the concentration of peroxide.We are right
Instrument adds software and data is processed and analyzes, and this software will be entered the light absorption value measuring automatically with the corresponding data of standard specimen
Row relative analyses, provide the identification result of oil quality, and result is consistent with actual samples taken.
Embodiment 4
Colour developing enveloping agent solution is prepared:36mmol NH4Methanol butanol mixed liquid (the methanol of SCN, 0.2g/L iron powder:Butanol
=6:4,V/V).Compound method:Weigh 18mmol NH4SCN, 0.1g iron powder, in 500 milliliters of beakers, measures 500 millis with graduated cylinder
Rise methanol butanol mixed solvent (methanol:Butanol=6:4, V/V) in this 500 milliliters of beakers, stirred to white with glass rod
NH4SCN solid dissolving.
Reductant solution is prepared:20mmol(NH4)Fe(SO4), the methanol butanol mixed solution (methanol of 0.2g/L iron powder:Fourth
Alcohol=99: 1, V/V).Compound method:Weigh 10mmol (NH4)Fe(SO4), in iron powder 0.1g/L to 500 milliliter of beaker, use graduated cylinder
Measure 500 ml methanol butanol mixed solvent (methanol:Butanol=99: 1, V/V) in this 500 milliliters of beakers, stirred with glass rod
(NH to white4)Fe(SO4) solid dissolving.
10.0 milliliters of reductant solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor during mensure
In milliliter reagent bottle, then pipette 0.5 milliliter of oil samples in reagent bottle, cover tightly the equal power of bottle cap and shake 10-20 second, stand solution
The 20-30 second can measure its light absorption value on photometer, according to the standard curve of Fig. 2, obtains the concentration of peroxide.We are right
Instrument adds software and data is processed and analyzes, and this software will be entered the light absorption value measuring automatically with the corresponding data of standard specimen
Row relative analyses, provide the identification result of oil quality, and result is consistent with actual samples taken.
Embodiment 5
Colour developing enveloping agent solution is prepared:2.0mmol NH4Methanol butanol mixed liquid (the methanol of SCN, 0.0001g/L iron powder:
Butanol=6:4,V/V).Compound method:Weigh 1.0mmol NH4SCN, 0.00005g iron powder, in 500 milliliters of beakers, uses graduated cylinder
Measure 500 ml methanol butanol mixed solvent (methanol:Butanol=6:4, V/V) in this 500 milliliters of beakers, with glass rod stir to
The NH of white4SCN solid dissolving.
Reductant solution is prepared:0.8mmol(NH4)Fe(SO4), the methanol butanol mixed solution (first of 0.0001g/L iron powder
Alcohol:Butanol=99: 1, V/V).Compound method:Weigh 0.4mmol (NH4)Fe(SO4), iron powder 0.00005g to 500 milliliter of beaker
In, measure 500 ml methanol butanol mixed solvent (methanol with graduated cylinder:Butanol=99:1, V/V) in this 500 milliliters of beakers, use
Glass rod stirs to white (NH4)Fe(SO4) solid dissolving.
10.0 milliliters of reductant solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor during mensure
In milliliter reagent bottle, then pipette 0.5 milliliter of oil samples in reagent bottle, cover tightly the equal power of bottle cap and shake 10-20 second, stand solution
The 20-30 second can measure its light absorption value on photometer, according to the standard curve of Fig. 2, obtains the concentration of peroxide.We are right
Instrument adds software and data is processed and analyzes, and this software will be entered the light absorption value measuring automatically with the corresponding data of standard specimen
Row relative analyses, provide the identification result of oil quality, and result is consistent with actual samples taken.
Embodiment 6
Colour developing enveloping agent solution is prepared:36mmol NH4Methanol butanol mixed liquid (the methanol of SCN, 5.0g/L iron powder:Butanol
=6: 4, V/V).Compound method:Weigh 18mmol NH4SCN, 2.5g iron powder, in 500 milliliters of beakers, measures 500 millis with graduated cylinder
Rise methanol butanol mixed solvent (methanol:Butanol=6:4, V/V) in this 500 milliliters of beakers, stirred to white with glass rod
NH4SCN solid dissolving.
Reductant solution is prepared:20mmol(NH4)Fe(SO4), the methanol butanol mixed solution (methanol of 5.0g/L iron powder:Fourth
Alcohol=99: 1, V/V).Compound method:Weigh 10mmol (NH4)Fe(SO4), in iron powder 2.5g to 500 milliliter of beaker, use graduated cylinder amount
Take 500 ml methanol butanol mixed solvent (methanol:Butanol=99:1, V/V) in this 500 milliliters of beakers, with glass rod stir to
(the NH of white4)Fe(SO4) solid dissolving.
10.0 milliliters of reductant solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor during mensure
In milliliter reagent bottle, then pipette 0.5 milliliter of oil samples in reagent bottle, cover tightly the equal power of bottle cap and shake 10-20 second, stand solution
The 20-30 second can measure its light absorption value on photometer, according to the standard curve of Fig. 2, obtains the concentration of peroxide.We are right
Instrument adds software and data is processed and analyzes, and this software will be entered the light absorption value measuring automatically with the corresponding data of standard specimen
Row relative analyses, provide the identification result of oil quality, and result is consistent with actual samples taken.
Embodiment 7
Colour developing enveloping agent solution is prepared:36mmol NH4Methanol butanol mixed liquid (the methanol of SCN:Butanol=5:5,V/V).
Compound method:Weigh 18mmol NH4In SCN to 500 milliliter of beaker, measure 500 ml methanol butanol mixed solvents with graduated cylinder
(methanol:Butanol=5:5, V/V) in this 500 milliliters of beakers, stirred to white NH with glass rod4SCN solid dissolving.
Reductant solution is prepared:28mmol(NH4)Fe(SO4), the methanol butanol mixed solution (first of 30mmol stannous sulfate
Alcohol:Butanol=99:1,V/V).Compound method:Weigh 14mmol (NH4)Fe(SO4), 15mmol stannous sulfate is to 500 milliliters of beakers
In, measure 500 ml methanol butanol mixed solvent (methanol with graduated cylinder:Butanol=99:1, V/V) in this 500 milliliters of beakers, use
Glass rod stirs to white (NH4)Fe(SO4) solid dissolving.
10.0 milliliters of reductant solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor during mensure
In milliliter reagent bottle, then pipette 0.5 milliliter of oil samples in reagent bottle, cover tightly the equal power of bottle cap and shake 10-20 second, stand solution
The 20-30 second can measure its light absorption value on photometer, according to the standard curve of Fig. 2, obtains the concentration of peroxide.We are right
Instrument adds software and data is processed and analyzes, and this software will be entered the light absorption value measuring automatically with the corresponding data of standard specimen
Row relative analyses, provide the identification result of oil quality, and result is consistent with actual samples taken.
Embodiment 8
Colour developing enveloping agent solution is prepared:36mmol NH4SCN, 2mmol stannous sulfate, the methanol of 14mmol vitamin C
Butanol mixed liquid (methanol:Butanol=7: 3, V/V).Compound method:Weigh 18mmol NH4SCN, 1mmol stannous sulfate, 7mmol
Vitamin C, in 500 milliliters of beakers, measures 500 ml methanol butanol mixed solvent (methanol with graduated cylinder:Butanol=7: 3, V/
V) in this 500 milliliters of beakers, stirred to solid dissolving with glass rod.
Reductant solution is prepared:20mmol(NH4)Fe(SO4), 4mmol stannous sulfate, the methanol of 14mmol vitamin C
Butanol mixed solution (methanol:Butanol=99:1,V/V).Compound method:Weigh 10mmol (NH4)Fe(SO4), 2mmol sulphuric acid is sub-
Stannum, 7mmol vitamin C, in 500 milliliters of beakers, measures 500 ml methanol butanol mixed solvent (methanol with graduated cylinder:Butanol
=99:1, V/V) in this 500 milliliters of beakers, stirred to solid dissolving with glass rod.
10.0 milliliters of reductant solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor during mensure
In milliliter reagent bottle, then pipette 0.5 milliliter of oil samples in reagent bottle, cover tightly the equal power of bottle cap and shake 10-20 second, stand solution
The 20-30 second can measure its light absorption value on photometer, according to the standard curve of Fig. 2, obtains the concentration of peroxide.We are right
Instrument adds software and data is processed and analyzes, and this software will be entered the light absorption value measuring automatically with the corresponding data of standard specimen
Row relative analyses, provide the identification result of oil quality, and result is consistent with actual samples taken.
Embodiment 9
Colour developing enveloping agent solution is prepared:Methanol butanol mixed liquid (the methanol of 45mmol NH4SCN:Butanol=7:3,V/V).
Compound method:Weigh in 22.5mmol NH4SCN to 500 milliliter of beaker, measure 500 ml methanol butanol mixed solvents with graduated cylinder
(methanol:Butanol=7: 3, V/V) in this 500 milliliters of beakers, stirred to solid dissolving with glass rod.
Reductant solution is prepared:3mmol (NH4) Fe (SO4), the methanol butanol mixed solution (first of 100mmol stannous sulfate
Alcohol:Butanol=99:1,V/V).Compound method:Weigh 1.5mmol (NH4) Fe (SO4), 50mmol stannous sulfate to 500 milliliters burns
In cup, measure 500 ml methanol butanol mixed solvent (methanol with graduated cylinder:Butanol=99:1, V/V) in this 500 milliliters of beakers,
Stirred to solid dissolving with glass rod.
10.0 milliliters of reductant solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor during mensure
In milliliter reagent bottle, then pipette 0.5 milliliter of oil samples in reagent bottle, cover tightly the equal power of bottle cap and shake 10-20 second, stand solution
The 20-30 second can measure its light absorption value on photometer, according to the standard curve of Fig. 2, obtains the concentration of peroxide.We are right
Instrument adds software and data is processed and analyzes, and this software will be entered the light absorption value measuring automatically with the corresponding data of standard specimen
Row relative analyses, provide the identification result of oil quality, and result is consistent with actual samples taken.
Embodiment 10
Colour developing enveloping agent solution is prepared:Methanol butanol mixed liquid (the methanol of 4mmol NH4SCN:Butanol=5:5,V/V).
Compound method:Weigh in 2mmol NH4SCN to 500 milliliter of beaker, measure 500 ml methanol butanol mixed solvent (first with graduated cylinder
Alcohol:Butanol=5: 5, V/V) in this 500 milliliters of beakers, stirred to white NH4SCN solid dissolving with glass rod.
Reductant solution is prepared:2mmol (NH4) Fe (SO4), 0.0001mmol stannous sulfate, 12mmol oxammonium hydrochloride.
Methanol butanol mixed solution (methanol:Butanol=99:1,V/V).Compound method:Weigh 1mmol (NH4) Fe (SO4),
0.00005mmol stannous sulfate, 6mmol oxammonium hydrochloride., in 500 milliliters of beakers, measures 500 ml methanol butanol with graduated cylinder and mixes
Bonding solvent (methanol:Butanol=99: 1, V/V) in this 500 milliliters of beakers, stirred solid to white (NH4) Fe (SO4) with glass rod
Body dissolves.
10.0 milliliters of reductant solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor during mensure
In milliliter reagent bottle, then pipette 0.5 milliliter of oil samples in reagent bottle, cover tightly the equal power of bottle cap and shake 10-20 second, stand solution
The 20-30 second can measure its light absorption value on photometer, according to the standard curve of Fig. 2, obtains the concentration of peroxide.We are right
Instrument adds software and data is processed and analyzes, and this software will be entered the light absorption value measuring automatically with the corresponding data of standard specimen
Row relative analyses, provide the identification result of oil quality, and result is consistent with actual samples taken.
Embodiment 11
Colour developing enveloping agent solution is prepared:Methanol butanol mixed liquid (the methanol of 40mmol NH4SCN, 50mmol oxammonium hydrochloride.:
Butanol=5:5,V/V).Compound method:Weigh 2mmol NH4SCN, 25mmol oxammonium hydrochloride., in 500 milliliters of beakers, uses graduated cylinder
Measure 500 ml methanol butanol mixed solvent (methanol:Butanol=1: 9, V/V) in this 500 milliliters of beakers, with glass rod stir to
The NH4SCN solid dissolving of white.
Reductant solution is prepared:32mmol (NH4) Fe (SO4), the methanol butanol mixed solution (first of 50mmol oxammonium hydrochloride.
Alcohol:Butanol=99: 1, V/V).Compound method:Weigh 16mmol (NH4) Fe (SO4), 25mmol oxammonium hydrochloride. to 500 milliliters burns
In cup, measure 500 ml methanol butanol mixed solvent (methanol with graduated cylinder:Butanol=99:1, V/V) in this 500 milliliters of beakers,
Stirred to white (NH4) Fe (SO4) solid dissolving with glass rod.
10.0 milliliters of reductant solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor during mensure
In milliliter reagent bottle, then pipette 0.5 milliliter of oil samples in reagent bottle, cover tightly the equal power of bottle cap and shake 10-20 second, stand solution
The 20-30 second can measure its light absorption value on photometer, according to the standard curve of Fig. 2, obtains the concentration of peroxide.We are right
Instrument adds software and data is processed and analyzes, and this software will be entered the light absorption value measuring automatically with the corresponding data of standard specimen
Row relative analyses, provide the identification result of oil quality, and result is consistent with actual samples taken.
Embodiment 12
Colour developing enveloping agent solution is prepared:Methanol butanol mixed liquid (the methanol of 4mmol NH4SCN:Butanol=5:5,V/V).
Compound method:Weigh in 2mmol NH4SCN to 500 milliliter of beaker, measure 500 ml methanol butanol mixed solvent (first with graduated cylinder
Alcohol:Butanol=5: 5, V/V) in this 500 milliliters of beakers, stirred to white NH4SCN solid dissolving with glass rod.
Reductant solution is prepared:2mmol (NH4) Fe (SO4), 4.0mmol stannous sulfate, 0.0001mmol oxammonium hydrochloride.
Methanol butanol mixed solution (methanol:Butanol=99:1,V/V).Compound method:Weigh 1mmol (NH4) Fe (SO4), 2.0mmol
Stannous sulfate, 0.00005mmol oxammonium hydrochloride., in 500 milliliters of beakers, measures 500 ml methanol butanol mixed solvents with graduated cylinder
(methanol:Butanol=99: 1, V/V) in this 500 milliliters of beakers, stirred molten to white (NH4) Fe (SO4) solid with glass rod
Solution.
10.0 milliliters of reductant solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor during mensure
In milliliter reagent bottle, then pipette 0.5 milliliter of oil samples in reagent bottle, cover tightly the equal power of bottle cap and shake 10-20 second, stand solution
The 20-30 second can measure its light absorption value on photometer, according to the standard curve of Fig. 2, obtains the concentration of peroxide.We are right
Instrument adds software and data is processed and analyzes, and this software will be entered the light absorption value measuring automatically with the corresponding data of standard specimen
Row relative analyses, provide the identification result of oil quality, and result is consistent with actual samples taken.
Embodiment 13
Colour developing enveloping agent solution is prepared:Methanol butanol mixed liquid (the methanol of 30mmol NH4SCN:Butanol=5:5,V/V).
Compound method:Weigh in 15mmol NH4SCN to 500 milliliter of beaker, measure 500 ml methanol butanol mixed solvents with graduated cylinder
(methanol:Butanol=5:5, V/V) in this 500 milliliters of beakers, stirred to white NH4SCN solid dissolving with glass rod.
Reductant solution is prepared:18mmol (NH4) Fe (SO4), 40mmol stannous chloride, the first of 0.02mmol oxammonium sulfate.
Alcohol butanol mixed solution (methanol:Butanol=99: 1, V/V).Compound method:Weigh 9mmol (NH4) Fe (SO4), 20mmol chlorination
Stannous, 0.01mmol oxammonium sulfate., in 500 milliliters of beakers, measures 500 ml methanol butanol mixed solvent (methanol with graduated cylinder:
Butanol=99:1, V/V) in this 500 milliliters of beakers, stirred to white (NH4) Fe (SO4) solid dissolving with glass rod.
10.0 milliliters of reductant solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor during mensure
In milliliter reagent bottle, then pipette 0.5 milliliter of oil samples in reagent bottle, cover tightly the equal power of bottle cap and shake 10-20 second, stand solution
The 20-30 second can measure its light absorption value on photometer, according to the standard curve of Fig. 2, obtains the concentration of peroxide.We are right
Instrument adds software and data is processed and analyzes, and this software will be entered the light absorption value measuring automatically with the corresponding data of standard specimen
Row relative analyses, provide the identification result of oil quality, and result is consistent with actual samples taken.
Embodiment 14
Colour developing enveloping agent solution is prepared:36mmol NH4Methanol butanol mixed liquid (the methanol of SCN:Butanol=7: 3, V/V).
Compound method:Weigh 18mmol NH4In SCN to 500 milliliter of beaker, measure 500 ml methanol butanol mixed solvents with graduated cylinder
(methanol:Butanol=7:3, V/V) in this 500 milliliters of beakers, stirred to solid dissolving with glass rod.
Reductant solution is prepared:20mmol(NH4)Fe(SO4), compound method:Weigh 10mmol (NH4)Fe(SO4), consumption
Cylinder measures 500 ml methanol butanol mixed solvent (methanol:Butanol=99:1, V/V) in this 500 milliliters of beakers, stirred with glass rod
Mix to solid dissolving.
10.0 milliliters of reductant solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor during mensure
In milliliter reagent bottle, add vitamin C, the concentration of vitamin C is 4.8mmol/L.Pipette 0.5 milliliter of oil samples again
To in reagent bottle, cover tightly the equal power of bottle cap and shake 10-20 second, the standing solution 20-30 second can measure its extinction on photometer
Value, according to the standard curve of Fig. 2, obtains the concentration of peroxide.We add software and data are processed and is divided to instrument
Analysis, this software will be analyzed the light absorption value measuring automatically with the corresponding data of standard specimen, provides the discriminating of oil quality
As a result, result is consistent with actual samples taken.
The present invention is not limited to above-described embodiment it will be appreciated that those of ordinary skill in the art is without creative work
Just many modifications and variations can be made according to the design of the present invention.Therefore, all technical staff in the art are according to the present invention
Design on the basis of existing technology pass through the available technical scheme of logical analysis, reasoning, or a limited experiment, all
Should be in the protection domain being defined in the patent claims.
Claims (10)
1. in a kind of quick detection edible oil peroxide concentrations photometry, including reductant solution and colour developing chelating agent molten
Liquid it is characterised in that:Add stabilizer in described reductant solution and/or colour developing enveloping agent solution;Or in reductant solution
With interpolation stabilizer in the mixed solution of colour developing enveloping agent solution.
2. according to claim 1 in quick detection edible oil peroxide concentrations photometry it is characterised in that:Specifically
Detecting step is:
(1), respectively reducing agent and colour developing chelating agent solvent are prepared solution, and be retained separately;
(2), in reductant solution or/and colour developing enveloping agent solution, add stabilizer, then before the reaction by reductant solution
With colour developing enveloping agent solution mixing;
Or reducing agent and the colour developing chelating agent mixing of stabilizer will be not added with before the reaction, directly in the above-mentioned stabilizer of being not added with
Add stabilizer in reductant solution and colour developing chelating agent mixed liquor;
(3), in the mixed solution of the reductant solution having stabilizer and colour developing enveloping agent solution, add oil samples, mix, instead
Answer 10-50s, reacted sample is transferred in photometer and carries out detecting the content obtaining peroxide.
3. in quick detection edible oil according to claim 1 or claim 2 peroxide concentrations photometry it is characterised in that:Institute
State at least one that stabilizer is in iron powder, reproducibility hydroxy compounds, reproducibility hydroxylamine compound and tin salt.
4. according to claim 3 in quick detection edible oil peroxide concentrations photometry it is characterised in that:Described steady
Determining agent is iron powder, and the mass concentration of described iron powder is 0.0001-5.0g/L.
5. according to claim 3 in quick detection edible oil peroxide concentrations photometry it is characterised in that:Described steady
Determining agent is reproducibility hydroxy compounds, and described reproducibility hydroxy compounds are vitamin C, described reproducibility hydroxy compounds
Concentration be 0.0001-30.0mmol/L.
6. according to claim 3 in quick detection edible oil peroxide concentrations photometry it is characterised in that:Described steady
Determining agent is reproducibility hydroxylamine compound, and the concentration of described reproducibility hydroxylamine compound is 0.0002-50mmol/L.
7. according to claim 6 in quick detection edible oil peroxide concentrations photometry it is characterised in that:Described also
Originality hydroxylamine compound is oxammonium sulfate., at least one in oxammonium hydrochloride..
8. according to claim 3 in quick detection edible oil peroxide concentrations photometry it is characterised in that:Described steady
Determining agent is tin salt, and the concentration of described tin salt is 0.0001-100mmol/L.
9. according to claim 8 in quick detection edible oil peroxide concentrations photometry it is characterised in that:Described Asia
Pink salt is stannous sulfate, at least one in stannous chloride.
10. according to claim 3 in quick detection edible oil peroxide concentrations photometry it is characterised in that:Reduction
Agent is ferrous salt;Colour developing chelating agent is rhodanate, and the concentration of reducing agent is 0.5-50mmol/L, and the concentration of colour developing chelating agent is
0.5-40mmol/L, described solvent is methanol or butanol, or described solvent is methanol and butanol according to mixing that arbitrary proportion is prepared
Close solution.
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CN108802342A (en) * | 2017-05-04 | 2018-11-13 | 陈锡秋 | Oil product detects and application |
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