CN106383119B - Quickly detect the photometry of peroxide concentrations in edible oil - Google Patents
Quickly detect the photometry of peroxide concentrations in edible oil Download PDFInfo
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- CN106383119B CN106383119B CN201610982392.5A CN201610982392A CN106383119B CN 106383119 B CN106383119 B CN 106383119B CN 201610982392 A CN201610982392 A CN 201610982392A CN 106383119 B CN106383119 B CN 106383119B
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- 150000002978 peroxides Chemical class 0.000 title claims abstract description 53
- 239000008157 edible vegetable oil Substances 0.000 title claims abstract description 18
- 238000005375 photometry Methods 0.000 title claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 114
- 239000003921 oil Substances 0.000 claims abstract description 58
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 57
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 48
- 239000003381 stabilizer Substances 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- 238000001514 detection method Methods 0.000 claims abstract description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 169
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 120
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 55
- 239000007788 liquid Substances 0.000 claims description 20
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000008139 complexing agent Substances 0.000 claims description 16
- -1 hydroxylamine compound Chemical class 0.000 claims description 15
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims description 14
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 11
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 10
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- FHHJDRFHHWUPDG-UHFFFAOYSA-N peroxysulfuric acid Chemical compound OOS(O)(=O)=O FHHJDRFHHWUPDG-UHFFFAOYSA-N 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 compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- 239000000203 mixture Substances 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
- 239000012496 blank sample Substances 0.000 abstract description 3
- ZWLQACFYTXLLEJ-UHFFFAOYSA-N butan-1-ol;methanol Chemical compound OC.CCCCO ZWLQACFYTXLLEJ-UHFFFAOYSA-N 0.000 description 48
- 238000005259 measurement Methods 0.000 description 35
- 239000003153 chemical reaction reagent Substances 0.000 description 31
- 239000011521 glass Substances 0.000 description 28
- 238000002360 preparation method Methods 0.000 description 28
- 239000007787 solid Substances 0.000 description 27
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 24
- 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 18
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 16
- 238000000034 method Methods 0.000 description 13
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 12
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 12
- 229930003268 Vitamin C Natural products 0.000 description 12
- 238000010835 comparative analysis Methods 0.000 description 12
- 235000019154 vitamin C Nutrition 0.000 description 12
- 239000011718 vitamin C Substances 0.000 description 12
- 239000000523 sample Substances 0.000 description 11
- 238000004090 dissolution Methods 0.000 description 10
- 238000005303 weighing Methods 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 238000004458 analytical method Methods 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 7
- 238000004401 flow injection analysis Methods 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 150000002440 hydroxy compounds Chemical class 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 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
- 230000008033 biological extinction Effects 0.000 description 2
- 235000014113 dietary fatty acids 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
- 239000004519 grease Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000012803 optimization experiment Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004448 titration 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
- 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019197 fats Nutrition 0.000 description 1
- 238000004817 gas chromatography Methods 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
- 230000002401 inhibitory effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 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
- 230000004130 lipolysis Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 238000012423 maintenance Methods 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
- 235000015097 nutrients Nutrition 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 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
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 238000000159 protein binding assay Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 206010040882 skin lesion Diseases 0.000 description 1
- 231100000444 skin lesion Toxicity 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000003860 storage 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 kind of photometries of peroxide concentrations in quickly detection edible oil, including reducing agent solution and colour developing enveloping agent solution, it is characterised in that: adds stabilizer in the reducing agent solution and/or colour developing enveloping agent solution；Or stabilizer is added in the mixed solution of reducing agent solution and colour developing enveloping agent solution.The background value for reducing blank sample, makes chromogenic reaction interference-free, and light absorption value is sufficiently stable, makes it the Accurate Determining for carrying out peroxide concentrations in conjunction with existing photometric instrument, effectively identifies poor oil and gutter oil.
Description
Technical field
The present invention relates to a kind of photometry, in particular to the luminosity of peroxide concentrations in a kind of quickly detection edible oil
Method.
Background technique
Fat be edible oil main ingredient and human normal vital movement required for basic nutrients, to people
The operation of body normal physiological function is most important.The fatty acid generated after lipolysis is the most direct energy source of human body.It removes
Outside storage and supplying energy, a variety of fatty acid, including oleic acid, linoleic acid, alpha-linolenic acid etc. that grease provides, are body structures
Important component, grease shortage will will appear slow growth even stagnation, skin lesion etc..Studies have shown that one day rouge of human body
Fat acid source about 50% is obtained by edible oil.Therefore for edible oil for human nutrition is replenished in time, maintenance human health is must
Indispensable.
Unsaturated lipid compound in oil product can occur redox reaction with the oxygen in air and generate peroxide.With
Peroxide concentrations increase, various harmful substance contents can also accordingly increase in oil product, eventually result under oil quality
Drop or even oil product Kazakhstan are smelly, rancid, go bad.Peroxide value is one of the important indicator of international measurement edible oil quality, it
Directly reflect the superiority and inferiority of oil quality.Peroxide in oil product itself is also a kind of harmful substance being detrimental to health,
Excess intake lipid peroxide, may cause cardiovascular disease, accelerate the aging of human organ.
Currently, the determination of POV in food oil generallys use traditional standard method, i.e. iodometric titration.This method
Although not needing special instruments and equipment, there are stability and poor reproducibility, and time-consuming, and operation requires strictly to wait intrinsic lack
Point.In addition to iodimetric titration, there are also various instrument analytical methods, including fluorophotometric, chemiluminescences, 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, for example, the flowing note that Japanese proposes
- fluorimetry is penetrated, sensitivity, selectivity are all very high, but the desired reaction time is long, under heating conditions, flow injection
There is still a need for 80 meters or more could complete chromogenic reaction for the reacting ring length of analysis system, 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 fluorescent reagent, and this reagent is gone back at present
It is not market-oriented.The content of peroxide is higher in oil product, and when practical application does not need method with very high sensitivity.Herein
Later, flow injection-analytical photometry of peroxide is proposed within American scholar 1999.Flow Injection Analysis System reaction
Circle length only needs 20 centimetres or so, so that the pressure of mobile phase transportation system be made to return normal pressure, system is simplified, and analyzes speed
Also very fast.
Liquid matter is online, and equipment required for chromaticness is online is relatively expensive, and analysis speed is slower, and needs complicated, consumption
When sample pre-treatments.
It is at present using more method with the peroxide in spectrophotometric determination oil product.Spectrophotometer relative to
Gas-chromatography, liquid chromatogram, infrared spectrometer, liquid matter is online, and chromaticness is online etc., there is the features such as more economic, easy to operate.
But it is sample pre-treatments complexity that current this instrumental method, which generally deposits weakness, for example needs to extract mostly, is separated, and heating waited
Journey, time-consuming and laborious, analysis 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 identification and monitoring of gutter oil.It is point that main cause, which is existing method just for the relatively simple Normal Goods oil of composition,
Analysis object is set up, and is difficult to be applicable in gutter oil (including swill oil, recycling frying oil etc.) a kind of complex sample.It is this kind of multiple
Miscellaneous sample be easy to cause severe jamming there are more impurity, and method is caused to fail.
Present patent application inventor cooperates with P.K.Dasgupta, and a kind of flow injection-photometry was proposed in 1999
Analyze the peroxide in oil product.This method detects the principles of chemistry of peroxide in oil product are as follows:
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: the lipid peroxide in food oil is represented
This method solvent for use is methanol or butanol or methanol and butanol mixed liquid；Reducing agent is ferrous salt；Colour developing complexing
Agent is rhodanate.
Ferrous ion generates ferric ion with peroxide reactions in a solvent (see reaction equation (1)).Chemical reaction
The oxygen radical of one of product in formula (1) can also react with ferrous ion and generate ferric ion (see reaction equation
(2)).Ferric ion and thiocyanate ion form red complex, thus with the content of photometry measurement red complex.
Experiment shows that the concentration of peroxide and the red complex content of formation have one-to-one quantitative pass under given conditions
System, and reaction speed is fast, and sample pre-treatments are simple.Using above-mentioned chemical reaction and combine in flow injection system measurement oil product
Peroxide concentrations achieve preferable effect.Flow injection system the degree of automation is higher, but equipment is costly.
If utilizing peroxide concentrations in the above-mentioned principles of chemistry and photometer binding assay edible oil, it will significantly reduce
Instrument and equipment cost, instrumentation is also simpler, is conducive to popularize.However, if directly being prepared using the above-mentioned principles of chemistry
Sample is analyzed, following problem can be faced with photometer measurement peroxide concentrations: the peroxidating in order to test various concentration range
Object, reagent ferrous ions and colour developing complexing agent all must be it is excessive, but ferrous ion excessively develop the color complexing agent in the presence of,
Its electrode potentialBecome very low, reducing power is extremely strong, is easily quickly aoxidized by the dissolved oxygen 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
It is extremely unstable.The two factors meeting severe jamming measurement result causes to analyze result inaccuracy, or even detection failure.This is mesh
Chromogenic reaction in preceding above-mentioned system is difficult to combine the main reason for carrying out quantitative detection peroxide with photometer.
Summary of the invention
For existing problem, the purpose of the present invention is to provide peroxide concentrations in a kind of quickly detection edible oil
Photometry reduces the background value of blank sample, makes chromogenic reaction interference-free, and light absorption value is sufficiently stable, make it with it is existing
Photometric instrument combines the Accurate Determining for carrying out peroxide concentrations, effectively identifies poor oil and gutter oil.
To achieve the goals above, the technical solution of the present invention is as follows: a kind of quickly detect peroxide concentrations in edible oil
Photometry, including reducing agent solution and colour developing enveloping agent solution, it is characterised in that: in the reducing agent solution and/or colour developing
Stabilizer is added in enveloping agent solution；Or stabilizer is added in the mixed solution of reducing agent solution and colour developing enveloping agent solution.
Specific detecting step are as follows:
(1), reducing agent and colour developing complexing agent solvent are prepared into solution respectively, and are retained separately；
(2), stabilizer is added in reducing agent solution or/and colour developing enveloping agent solution, then before the reaction by reducing agent
Solution and colour developing enveloping agent solution mixing；
Or before the reaction mix the reducing agent for being not added with stabilizer and colour developing complexing agent, directly stabilization is not added with above-mentioned
Stabilizer is added in the reducing agent solution and colour developing complexing agent mixed liquor of agent；
(3), oil samples are added in the mixed solution of the reducing agent solution for having stabilizer and the enveloping agent solution that develops the color, mix
It is even, 10-50s is reacted, the sample after reaction is transferred to the content for being detected to obtain peroxide in photometer.
Colour developing enveloping agent solution and reducing agent solution are retained separately first, carried out again when carrying out sample detection mutually
Mixing, ferrous ion caused by can mixing too early to avoid two kinds of solution in this way are dissolved the problem of oxygen largely quickly aoxidizes.Add
Enter stabilizer and further suppress dissolved oxygen iron protoxide ion, makes normal chromogenic reaction from interference, to make system
Light absorption value is sufficiently stable within certain time, sufficiently meets the accurate basic demand for carrying out photometric detection.
In above scheme: the stabilizer is iron powder, reproducibility hydroxy compounds, reproducibility hydroxylamine compound and tin salt
At least one of.
In above scheme: the stabilizer is iron powder, and the mass concentration of the iron powder is 0.0001-5.0g/L.
In above scheme, the stabilizer is reproducibility hydroxy compounds, and the concentration of the reproducibility hydroxy compounds is
0.0001-30.0mmol/L。
In above scheme, the reproducibility hydroxy compounds is vitamin C.
In above scheme, the stabilizer is reproducibility hydroxylamine compound, and the concentration of the reproducibility hydroxylamine compound is
0.0002-50mmol/L。
It is preferred that: the reproducibility hydroxylamine compound is at least one of hydroxyl sulfate, hydroxylamine hydrochloride.
In above scheme: the stabilizer is tin salt, and the concentration of the tin salt is 0.0001-100mmol/L.
It is preferred that: the tin salt is at least one of stannous sulfate, stannous chloride.
In above scheme: reducing agent is ferrous salt；Colour developing complexing agent is rhodanate, and the concentration of reducing agent is 0.5-
The concentration of 50mmol/L, the complexing agent that develops the color are 0.5-40mmol/L, and the solvent is methanol or butanol or the solvent is methanol
The mixed solution prepared with butanol according to arbitrary proportion.
Experiment shows that the stabilizer concentration size of addition is particularly significant to the stability of chromogenic reaction.Concentration is too low can not
Reach the rapid oxidation for inhibiting ferrous ion, the purpose of stable chromogenic reaction is not achieved；Excessive concentration will lead to ferrous ion with
The ferric ion that peroxide generates is reduced rapidly, and the purpose of stable chromogenic reaction is equally not achieved.By repetition test, I
Have found various stabilizers in reducing agent solution, or simultaneously colour developing enveloping agent solution and reducing agent solution in it is best
Concentration range.Under this concentration conditions, the stabilization time range of chromogenic reaction was up to 30~50 minutes.The time is enough to complete oil
The photometry detection of peroxide in product.
Due to using the above method, the high stability of low latitude the white background value and chromogenic reaction of sample ensure that, sufficiently completely
The foot basic demand of Instrument measuring, overcome in the system as ferrous ion be dissolved caused by oxygen quickly aoxidize be difficult to
Photometer combines the problem for carrying out that peroxide determining value is surveyed in oil product.Fig. 1 be under identical optimization experiment condition, it is dense with peroxide
Degree fast detector is when being added moderate amount of sulfuric acid azanol and stannous sulfate compound stabilizer and being added without stabilizer, to same oil sample
Product carry out light absorption value -- the time curve that analysis measurement obtains.Statistics indicate that the light absorption value of stabilizer post analysis sample is added
Stability significantly improves.
Fig. 2 is the representative standard curve obtained under one group of optimization experiment condition.Statistics indicate that the system is in a certain concentration
In range, light absorption value and peroxide concentrations have good linear relationship (R2=0.9925).
The beneficial effects of the present invention are: the invention proposes a kind of intelligence of lipid peroxide in completely new measurement oil product
Change rapid detection system, there is the features such as analysis speed is fast, accuracy rate is high, and stability is good, easy to operate, at low cost.
Detailed description of the invention
Fig. 1 is light absorption value and peroxide concentrations standard curve.
Fig. 2 is the relational graph of time and light absorption value.
Specific embodiment
The present invention will be further described in the following with reference to the drawings and specific embodiments:
Embodiment 1
The enveloping agent solution that develops the color is prepared: 36mmol NH4Methanol butanol mixed liquid (the methanol: butanol=7: 3, V/V) of SCN.
Preparation method: 18mmol NH is weighed4In SCN to 500 milliliters of beaker, 500 ml methanol butanol mixed solvents are measured with graduated cylinder
It (methanol: butanol=7: 3, V/V) into 500 milliliters of beakers, is stirred with glass rod to solid and is dissolved.
Reducing agent solution is prepared: 20mmol (NH4)Fe(SO4), the methanol butanol mixed solution of 2.8mmol vitamin C
(methanol: butanol=99:1, V/V).Preparation method: 10mmol (NH is weighed4)Fe(SO4), 1.4mmol vitamin C to 500 millis
It rises in beaker, measures 500 ml methanol butanol mixed solvents (methanol: butanol=99:1, V/V) to this 500 milliliters burnings with graduated cylinder
In cup, is stirred with glass rod to solid and dissolved.
10.0 milliliters of reducing agent solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor when measurement
It in milliliter reagent bottle, then pipettes in 0.5 milliliter of oil samples to reagent bottle, covers tightly the equal power of bottle cap and shake 10-20 seconds, stand solution
Its light absorption value can be measured on photometer within 20-30 seconds, standard curve according to fig. 2 obtains the concentration of peroxide.We are right
Instrument addition software is handled and is analyzed to data, which is this field conventional means, which will be the extinction of measurement
Value is compared and analyzed with the corresponding data of standard specimen automatically, provides the identification result of oil quality, as a result with practical samples taken
It is consistent.
Embodiment 2
The complexing agent agent solution that develops the color is prepared: 50mmol NH4Methanol butanol mixed liquid (the methanol: butanol=7:3, V/ of SCN
V).Preparation method: 25mmol NH is weighed4In SCN to 500 milliliters of beaker, 500 ml methanols are measured to this 500 milliliters with graduated cylinder
In beaker, is stirred with glass rod to solid and dissolved.
Reducing agent solution is prepared: 40mmol (NH4)Fe(SO4), the methanol of 30mmol vitamin C.Preparation method: it weighs
20mmol(NH4)Fe(SO4), it is mixed that 15mmol vitamin C measures 500 ml methanol butanol into 500 milliliters of beakers, with graduated cylinder
Bonding solvent (methanol: butanol=99:1, V/V) is stirred to solid with glass rod and is dissolved into 500 milliliters of beakers.
10.0 milliliters of reducing agent solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor when measurement
It in milliliter reagent bottle, then pipettes in 0.5 milliliter of oil samples to reagent bottle, covers tightly the equal power of bottle cap and shake 10-20 seconds, stand solution
Its light absorption value can be measured on photometer within 20-30 seconds, standard curve according to fig. 2 obtains the concentration of peroxide.We are right
Instrument addition software data are handled and are analyzed, the software by the light absorption value of measurement automatically with the corresponding data of standard specimen into
Row comparative analysis provides the identification result of oil quality, is as a result consistent with practical samples taken.
Embodiment 3
The complexing agent agent solution that develops the color is prepared: the methanol butanol mixed liquid (methanol: butanol=7: 3, V/ of 0.5mmol NH4SCN
V).Preparation method: weighing in 0.025mmol NH4SCN to 500 milliliters of beaker, measures the mixing of 500 ml methanol butanol with graduated cylinder
Solvent (methanol: butanol=7:3, V/V) is stirred to solid with glass rod and is dissolved into 500 milliliters of beakers.
Reducing agent solution is prepared: the methanol butanol mixing of 0.5mmol (NH4) Fe (SO4), 0.0001mmol vitamin C
Solution (methanol: butanol=99: 1, V/V).Preparation method: weighing 0.025mmol (NH4) Fe (SO4), and third kind of 0.00005mmol
Vitamin measures 500 ml methanol butanol mixed solvent (methanol: butanol=99: 1, V/V) into 500 milliliters of beakers, with graduated cylinder
Into 500 milliliters of beakers, is stirred with glass rod to solid and dissolved.
10.0 milliliters of reducing agent solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor when measurement
It in milliliter reagent bottle, then pipettes in 0.5 milliliter of oil samples to reagent bottle, covers tightly the equal power of bottle cap and shake 10-20 seconds, stand solution
Its light absorption value can be measured on photometer within 20-30 seconds, standard curve according to fig. 2 obtains the concentration of peroxide.We are right
Instrument addition software data are handled and are analyzed, the software by the light absorption value of measurement automatically with the corresponding data of standard specimen into
Row comparative analysis provides the identification result of oil quality, is as a result consistent with practical samples taken.
Embodiment 4
The enveloping agent solution that develops the color is prepared: 36mmol NH4Methanol butanol mixed liquid (the methanol: butanol of SCN, 0.2g/L iron powder
=6:4, V/V).Preparation method: 18mmol NH is weighed4SCN, 0.1g iron powder measure 500 millis into 500 milliliters of beakers, with graduated cylinder
Methanol butanol mixed solvent (methanol: butanol=6:4, V/V) is risen into 500 milliliters of beakers, is stirred with glass rod to white
NH4The dissolution of SCN solid.
Reducing agent solution is prepared: 20mmol (NH4)Fe(SO4), the methanol butanol mixed solution (methanol: fourth of 0.2g/L iron powder
Alcohol=99: 1, V/V).Preparation method: 10mmol (NH is weighed4)Fe(SO4), in iron powder 0.1g/L to 500 milliliters of beaker, use graduated cylinder
500 ml methanol butanol mixed solvents are measured (methanol: butanol=99: 1, V/V) into 500 milliliters of beakers, to be stirred with glass rod
To (the NH of white4)Fe(SO4) solid dissolution.
10.0 milliliters of reducing agent solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor when measurement
It in milliliter reagent bottle, then pipettes in 0.5 milliliter of oil samples to reagent bottle, covers tightly the equal power of bottle cap and shake 10-20 seconds, stand solution
Its light absorption value can be measured on photometer within 20-30 seconds, standard curve according to fig. 2 obtains the concentration of peroxide.We are right
Instrument addition software data are handled and are analyzed, the software by the light absorption value of measurement automatically with the corresponding data of standard specimen into
Row comparative analysis provides the identification result of oil quality, is as a result consistent with practical samples taken.
Embodiment 5
The enveloping agent solution that develops the color is prepared: 2.0mmol NH4SCN, 0.0001g/L iron powder methanol butanol mixed liquid (methanol:
Butanol=6:4, V/V).Preparation method: 1.0mmol NH is weighed4SCN, 0.00005g iron powder use graduated cylinder into 500 milliliters of beakers
500 ml methanol butanol mixed solvents (methanol: butanol=6:4, V/V) are measured into 500 milliliters of beakers, with glass rod stir to
The NH of white4The dissolution of SCN solid.
Reducing agent 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).Preparation method: 0.4mmol (NH is weighed4)Fe(SO4), iron powder 0.00005g to 500 milliliters of beaker
In, 500 ml methanol butanol mixed solvents (methanol: butanol=99:1, V/V) is measured into 500 milliliters of beakers with graduated cylinder, is used
Glass rod is stirred to (the NH of white4)Fe(SO4) solid dissolution.
10.0 milliliters of reducing agent solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor when measurement
It in milliliter reagent bottle, then pipettes in 0.5 milliliter of oil samples to reagent bottle, covers tightly the equal power of bottle cap and shake 10-20 seconds, stand solution
Its light absorption value can be measured on photometer within 20-30 seconds, standard curve according to fig. 2 obtains the concentration of peroxide.We are right
Instrument addition software data are handled and are analyzed, the software by the light absorption value of measurement automatically with the corresponding data of standard specimen into
Row comparative analysis provides the identification result of oil quality, is as a result consistent with practical samples taken.
Embodiment 6
The enveloping agent solution that develops the color is prepared: 36mmol NH4Methanol butanol mixed liquid (the methanol: butanol of SCN, 5.0g/L iron powder
=6: 4, V/V).Preparation method: 18mmol NH is weighed4SCN, 2.5g iron powder measure 500 millis into 500 milliliters of beakers, with graduated cylinder
Methanol butanol mixed solvent (methanol: butanol=6:4, V/V) is risen into 500 milliliters of beakers, is stirred with glass rod to white
NH4The dissolution of SCN solid.
Reducing agent solution is prepared: 20mmol (NH4)Fe(SO4), the methanol butanol mixed solution (methanol: fourth of 5.0g/L iron powder
Alcohol=99: 1, V/V).Preparation method: 10mmol (NH is weighed4)Fe(SO4), in iron powder 2.5g to 500 milliliters of beaker, with graduated cylinder amount
Take 500 ml methanol butanol mixed solvents (methanol: butanol=99:1, V/V) into 500 milliliters of beakers, with glass rod stir to
(the NH of white4)Fe(SO4) solid dissolution.
10.0 milliliters of reducing agent solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor when measurement
It in milliliter reagent bottle, then pipettes in 0.5 milliliter of oil samples to reagent bottle, covers tightly the equal power of bottle cap and shake 10-20 seconds, stand solution
Its light absorption value can be measured on photometer within 20-30 seconds, standard curve according to fig. 2 obtains the concentration of peroxide.We are right
Instrument addition software data are handled and are analyzed, the software by the light absorption value of measurement automatically with the corresponding data of standard specimen into
Row comparative analysis provides the identification result of oil quality, is as a result consistent with practical samples taken.
Embodiment 7
The enveloping agent solution that develops the color is prepared: 36mmol NH4The methanol butanol mixed liquid (methanol: butanol=5:5, V/V) of SCN.
Preparation method: 18mmol NH is weighed4In SCN to 500 milliliters of beaker, 500 ml methanol butanol mixed solvents are measured with graduated cylinder
(methanol: butanol=5:5, V/V) is stirred with glass rod to the NH of white into 500 milliliters of beakers4The dissolution of SCN solid.
Reducing agent solution is prepared: 28mmol (NH4)Fe(SO4), the methanol butanol mixed solution (first of 30mmol stannous sulfate
Alcohol: butanol=99:1, V/V).Preparation method: 14mmol (NH is weighed4)Fe(SO4), 15mmol stannous sulfate to 500 milliliters of beakers
In, 500 ml methanol butanol mixed solvents (methanol: butanol=99:1, V/V) is measured into 500 milliliters of beakers with graduated cylinder, is used
Glass rod is stirred to (the NH of white4)Fe(SO4) solid dissolution.
10.0 milliliters of reducing agent solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor when measurement
It in milliliter reagent bottle, then pipettes in 0.5 milliliter of oil samples to reagent bottle, covers tightly the equal power of bottle cap and shake 10-20 seconds, stand solution
Its light absorption value can be measured on photometer within 20-30 seconds, standard curve according to fig. 2 obtains the concentration of peroxide.We are right
Instrument addition software data are handled and are analyzed, the software by the light absorption value of measurement automatically with the corresponding data of standard specimen into
Row comparative analysis provides the identification result of oil quality, is as a result consistent with practical samples taken.
Embodiment 8
The enveloping agent solution that develops the color is prepared: 36mmol NH4SCN, 2mmol stannous sulfate, the methanol of 14mmol vitamin C
Butanol mixed liquid (methanol: butanol=7: 3, V/V).Preparation method: 18mmol NH is weighed4SCN, 1mmol stannous sulfate, 7mmol
Vitamin C measures 500 ml methanol butanol mixed solvent (methanol: butanol=7: 3, V/ into 500 milliliters of beakers, with graduated cylinder
V it) into 500 milliliters of beakers, is stirred with glass rod to solid and is dissolved.
Reducing agent 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).Preparation method: 10mmol (NH is weighed4)Fe(SO4), 2mmol sulfuric acid is sub-
Tin, 7mmol vitamin C measure 500 ml methanol butanol mixed solvent (methanol: butanol into 500 milliliters of beakers, with graduated cylinder
=99:1, V/V) into 500 milliliters of beakers, it is stirred with glass rod to solid and is dissolved.
10.0 milliliters of reducing agent solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor when measurement
It in milliliter reagent bottle, then pipettes in 0.5 milliliter of oil samples to reagent bottle, covers tightly the equal power of bottle cap and shake 10-20 seconds, stand solution
Its light absorption value can be measured on photometer within 20-30 seconds, standard curve according to fig. 2 obtains the concentration of peroxide.We are right
Instrument addition software data are handled and are analyzed, the software by the light absorption value of measurement automatically with the corresponding data of standard specimen into
Row comparative analysis provides the identification result of oil quality, is as a result consistent with practical samples taken.
Embodiment 9
The enveloping agent solution that develops the color is prepared: the methanol butanol mixed liquid (methanol: butanol=7:3, V/V) of 45mmol NH4SCN.
Preparation method: weighing in 22.5mmol NH4SCN to 500 milliliters of beaker, measures 500 ml methanol butanol mixed solvents with graduated cylinder
It (methanol: butanol=7: 3, V/V) into 500 milliliters of beakers, is stirred with glass rod to solid and is dissolved.
Reducing agent solution is prepared: 3mmol (NH4) Fe (SO4), the methanol butanol mixed solution (first of 100mmol stannous sulfate
Alcohol: butanol=99:1, V/V).Preparation method: weighing 1.5mmol (NH4) Fe (SO4), and 50mmol stannous sulfate is burnt to 500 milliliters
In cup, 500 ml methanol butanol mixed solvents (methanol: butanol=99:1, V/V) is measured into 500 milliliters of beakers with graduated cylinder,
It is stirred with glass rod to solid and is dissolved.
10.0 milliliters of reducing agent solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor when measurement
It in milliliter reagent bottle, then pipettes in 0.5 milliliter of oil samples to reagent bottle, covers tightly the equal power of bottle cap and shake 10-20 seconds, stand solution
Its light absorption value can be measured on photometer within 20-30 seconds, standard curve according to fig. 2 obtains the concentration of peroxide.We are right
Instrument addition software data are handled and are analyzed, the software by the light absorption value of measurement automatically with the corresponding data of standard specimen into
Row comparative analysis provides the identification result of oil quality, is as a result consistent with practical samples taken.
Embodiment 10
The enveloping agent solution that develops the color is prepared: the methanol butanol mixed liquid (methanol: butanol=5:5, V/V) of 4mmol NH4SCN.
Preparation method: weighing in 2mmol NH4SCN to 500 milliliters of beaker, measures 500 ml methanol butanol mixed solvent (first with graduated cylinder
Alcohol: it butanol=5: 5, V/V) into 500 milliliters of beakers, is dissolved with the NH4SCN solid that glass rod is stirred to white.
Reducing agent solution is prepared: 2mmol (NH4) Fe (SO4), 0.0001mmol stannous sulfate, 12mmol hydroxylamine hydrochloride
Methanol butanol mixed solution (methanol: butanol=99:1, V/V).Preparation method: weighing 1mmol (NH4) Fe (SO4),
0.00005mmol stannous sulfate, it is mixed that 6mmol hydroxylamine hydrochloride measures 500 ml methanol butanol into 500 milliliters of beakers, with graduated cylinder
Bonding solvent (methanol: butanol=99: 1, V/V) into 500 milliliters of beakers, is stirred solid to white (NH4) Fe (SO4) with glass rod
Body dissolution.
10.0 milliliters of reducing agent solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor when measurement
It in milliliter reagent bottle, then pipettes in 0.5 milliliter of oil samples to reagent bottle, covers tightly the equal power of bottle cap and shake 10-20 seconds, stand solution
Its light absorption value can be measured on photometer within 20-30 seconds, standard curve according to fig. 2 obtains the concentration of peroxide.We are right
Instrument addition software data are handled and are analyzed, the software by the light absorption value of measurement automatically with the corresponding data of standard specimen into
Row comparative analysis provides the identification result of oil quality, is as a result consistent with practical samples taken.
Embodiment 11
The enveloping agent solution that develops the color is prepared: the methanol butanol mixed liquid of 40mmol NH4SCN, 50mmol hydroxylamine hydrochloride (methanol:
Butanol=5:5, V/V).Preparation method: weighing 2mmol NH4SCN, and 25mmol hydroxylamine hydrochloride uses graduated cylinder into 500 milliliters of beakers
Measure 500 ml methanol butanol mixed solvents (methanol: butanol=1: 9, V/V) into 500 milliliters of beakers, with glass rod stir to
The NH4SCN solid dissolution of white.
Reducing agent solution is prepared: 32mmol (NH4) Fe (SO4), the methanol butanol mixed solution (first of 50mmol hydroxylamine hydrochloride
Alcohol: butanol=99: 1, V/V).Preparation method: weighing 16mmol (NH4) Fe (SO4), and 25mmol hydroxylamine hydrochloride is burnt to 500 milliliters
In cup, 500 ml methanol butanol mixed solvents (methanol: butanol=99:1, V/V) is measured into 500 milliliters of beakers with graduated cylinder,
It is dissolved with (NH4) Fe (SO4) solid that glass rod is stirred to white.
10.0 milliliters of reducing agent solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor when measurement
It in milliliter reagent bottle, then pipettes in 0.5 milliliter of oil samples to reagent bottle, covers tightly the equal power of bottle cap and shake 10-20 seconds, stand solution
Its light absorption value can be measured on photometer within 20-30 seconds, standard curve according to fig. 2 obtains the concentration of peroxide.We are right
Instrument addition software data are handled and are analyzed, the software by the light absorption value of measurement automatically with the corresponding data of standard specimen into
Row comparative analysis provides the identification result of oil quality, is as a result consistent with practical samples taken.
Embodiment 12
The enveloping agent solution that develops the color is prepared: the methanol butanol mixed liquid (methanol: butanol=5:5, V/V) of 4mmol NH4SCN.
Preparation method: weighing in 2mmol NH4SCN to 500 milliliters of beaker, measures 500 ml methanol butanol mixed solvent (first with graduated cylinder
Alcohol: it butanol=5: 5, V/V) into 500 milliliters of beakers, is dissolved with the NH4SCN solid that glass rod is stirred to white.
Reducing agent solution is prepared: 2mmol (NH4) Fe (SO4), 4.0mmol stannous sulfate, 0.0001mmol hydroxylamine hydrochloride
Methanol butanol mixed solution (methanol: butanol=99:1, V/V).Preparation method: 1mmol (NH4) Fe (SO4), 2.0mmol are weighed
Stannous sulfate, 0.00005mmol hydroxylamine hydrochloride measure 500 ml methanol butanol mixed solvents into 500 milliliters of beakers, with graduated cylinder
It (methanol: butanol=99: 1, V/V) into 500 milliliters of beakers, is stirred with glass rod molten to white (NH4) Fe (SO4) solid
Solution.
10.0 milliliters of reducing agent solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor when measurement
It in milliliter reagent bottle, then pipettes in 0.5 milliliter of oil samples to reagent bottle, covers tightly the equal power of bottle cap and shake 10-20 seconds, stand solution
Its light absorption value can be measured on photometer within 20-30 seconds, standard curve according to fig. 2 obtains the concentration of peroxide.We are right
Instrument addition software data are handled and are analyzed, the software by the light absorption value of measurement automatically with the corresponding data of standard specimen into
Row comparative analysis provides the identification result of oil quality, is as a result consistent with practical samples taken.
Embodiment 13
The enveloping agent solution that develops the color is prepared: the methanol butanol mixed liquid (methanol: butanol=5:5, V/V) of 30mmol NH4SCN.
Preparation method: weighing in 15mmol NH4SCN to 500 milliliters of beaker, measures 500 ml methanol butanol mixed solvents with graduated cylinder
(methanol: butanol=5:5, V/V) is dissolved into 500 milliliters of beakers with the NH4SCN solid that glass rod is stirred to white.
Reducing agent solution is prepared: 18mmol (NH4) Fe (SO4), 40mmol stannous chloride, the first of 0.02mmol hydroxyl sulfate
Alcohol butanol mixed solution (methanol: butanol=99: 1, V/V).Preparation method: 9mmol (NH4) Fe (SO4), 20mmol chlorination are weighed
Stannous, 0.01mmol hydroxyl sulfate into 500 milliliters of beakers, with graduated cylinder measure 500 ml methanol butanol mixed solvents (methanol:
Butanol=99:1, V/V) into 500 milliliters of beakers, it is dissolved with (NH4) Fe (SO4) solid that glass rod is stirred to white.
10.0 milliliters of reducing agent solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor when measurement
It in milliliter reagent bottle, then pipettes in 0.5 milliliter of oil samples to reagent bottle, covers tightly the equal power of bottle cap and shake 10-20 seconds, stand solution
Its light absorption value can be measured on photometer within 20-30 seconds, standard curve according to fig. 2 obtains the concentration of peroxide.We are right
Instrument addition software data are handled and are analyzed, the software by the light absorption value of measurement automatically with the corresponding data of standard specimen into
Row comparative analysis provides the identification result of oil quality, is as a result consistent with practical samples taken.
Embodiment 14
The enveloping agent solution that develops the color is prepared: 36mmol NH4Methanol butanol mixed liquid (the methanol: butanol=7: 3, V/V) of SCN.
Preparation method: 18mmol NH is weighed4In SCN to 500 milliliters of beaker, 500 ml methanol butanol mixed solvents are measured with graduated cylinder
(methanol: butanol=7:3, V/V) is stirred to solid with glass rod and is dissolved into 500 milliliters of beakers.
Reducing agent solution is prepared: 20mmol (NH4)Fe(SO4), preparation method: weigh 10mmol (NH4)Fe(SO4), dosage
Cylinder measures 500 ml methanol butanol mixed solvents (methanol: butanol=99:1, V/V) into 500 milliliters of beakers, is stirred with glass rod
It mixes to solid and dissolves.
10.0 milliliters of reducing agent solutions and 10.0 milliliters of colour developing enveloping agent solutions are accurately pipetted to 25 with pipettor when measurement
In milliliter reagent bottle, vitamin C is added, the concentration of vitamin C is 4.8mmol/L.0.5 milliliter of oil samples is pipetted again
Into reagent bottle, covers tightly the equal power of bottle cap and shake 10-20 seconds, its extinction can be measured on photometer by standing solution 20-30 seconds
Value, standard curve according to fig. 2 obtain the concentration of peroxide.We handle and divide to data to instrument addition software
Analysis, the software automatically will compare and analyze the light absorption value of measurement with the corresponding data of standard specimen, provide the identification of oil quality
As a result, result is consistent with practical samples taken.
The present invention is not limited to the above embodiment, it should be understood that those skilled in the art are not necessarily to creative work
It according to the present invention can conceive and make many modifications and variations.Therefore, all technician in the art are according to the present invention
Design pass through the available technical solution of logical analysis, reasoning, or a limited experiment on the basis of existing technology, all
It should within the scope of protection determined by the claims.
Claims (7)
1. the photometry of peroxide concentrations in a kind of quickly detection edible oil, including reducing agent solution and colour developing complexing agent it is molten
Liquid, it is characterised in that: add stabilizer in the reducing agent solution and/or colour developing enveloping agent solution；Or in reducing agent solution
Stabilizer is added in the mixed solution of colour developing enveloping agent solution；Specific detecting step are as follows:
(1), reducing agent and colour developing complexing agent solvent are prepared into solution respectively, and are retained separately；
(2), stabilizer is added in reducing agent solution or/and colour developing enveloping agent solution, then before the reaction by reducing agent solution
With colour developing enveloping agent solution mixing；
Or it will be not added with the reducing agent of stabilizer before the reaction and colour developing complexing agent mixes, directly in the above-mentioned stabilizer of being not added with
Stabilizer is added in reducing agent solution and colour developing complexing agent mixed liquor；
(3), oil samples are added in the mixed solution of the reducing agent solution for having stabilizer and the enveloping agent solution that develops the color, mix, instead
10-50s is answered, the sample after reaction is transferred to the content for being detected to obtain peroxide in photometer；
The stabilizer is at least one of iron powder, reproducibility hydroxylamine compound and tin salt.
2. quickly detecting the photometry of peroxide concentrations in edible oil according to claim 1, it is characterised in that: described steady
Determining agent is iron powder, and the mass concentration of the iron powder is 0.0001-5.0g/L.
3. quickly detecting the photometry of peroxide concentrations in edible oil according to claim 1, it is characterised in that: described steady
Determining agent is reproducibility hydroxylamine compound, and the concentration of the reproducibility hydroxylamine compound is 0.0002-50mmol/L.
4. quickly detecting the photometry of peroxide concentrations in edible oil according to claim 1, it is characterised in that: described to go back
Originality hydroxylamine compound is at least one of hydroxyl sulfate, hydroxylamine hydrochloride.
5. quickly detecting the photometry of peroxide concentrations in edible oil according to claim 1, it is characterised in that: described steady
Determining agent is tin salt, and the concentration of the tin salt is 0.0001-100mmol/L.
6. quickly detecting the photometry of peroxide concentrations in edible oil according to claim 5, it is characterised in that: the Asia
Pink salt is at least one of stannous sulfate, stannous chloride.
7. quickly detecting the photometry of peroxide concentrations in edible oil according to claim 1, it is characterised in that: reducing agent
For ferrous salt；Colour developing complexing agent is rhodanate, and the concentration of reducing agent is 0.5-50mmol/L, and the concentration for the complexing agent that develops the color is
0.5-40mmol/L, the solvent is methanol or butanol or the solvent is that methanol and butanol are mixed according to what arbitrary proportion was prepared
Close solution.
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| CN106383119A (en) | 2017-02-08 |
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