CN109580576A - The detection method of potassium ferrocyanide in a kind of salt - Google Patents
The detection method of potassium ferrocyanide in a kind of salt Download PDFInfo
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- CN109580576A CN109580576A CN201810818649.2A CN201810818649A CN109580576A CN 109580576 A CN109580576 A CN 109580576A CN 201810818649 A CN201810818649 A CN 201810818649A CN 109580576 A CN109580576 A CN 109580576A
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- potassium ferrocyanide
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- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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Abstract
The invention discloses a kind of detection methods of potassium ferrocyanide in salt, comprising the following steps: 1) sample treatment: weighing appropriate salt in sample cell, highly polar solution is added and extracts, stands, supernatant is spare as prepare liquid；2) Raman detection: taking appropriate metal-sol in Raman sample pool, and suitable prepare liquid is added and mixes, and is then placed on Raman spectrometer detection interior and is detected.The present invention has consumption of organic solvent few, green non-poisonous, the short advantage of detection time.
Description
Technical field
The present invention relates to a kind of detection methods of potassium ferrocyanide in salt.
Background technique
Potassium ferrocyanide chemical formula is K4[Fe(CN)6]·3H2O, scientific name three is hydrated six cyanogen and closes iron (II) sour potassium, light yellow
Crystal.For the complex that iron and cyanogen are formed, it is commonly called as potassium ferrocyanide, 69 DEG C~71 DEG C of fusing point, density 1.85g/cm3, readily soluble
Yu Shui dissociates into K in aqueous solution+[Fe (CN)6]4-.Potassium ferrocyanide is stable in the air, is heated to 70 DEG C and loses crystallization
Water decomposes after heat-flash.Iron (III) salting liquid and ferrocyanide nak response, obtain the Prussian blue precipitating of blue, this reaction is used for
Examine Fe3+.Potassium ferrocyanide is for manufacturing blue pigment, dyestuff, blue printing paper, the quenching medium as steel production.With strong acid and
Strong oxidizer reaction, is released hydrogen cyanide (HCN), has hypotoxicity.Potassium ferrocyanide is added to salt as a kind of anticaking agent
In, it can prevent salt from agglomerating because of water content height.In standard GB/T 2760-2014 " national food safety standard food
Additive uses standard " in salt the limitation of potassium ferrocyanide be 10ppm.The standard of detection foundation is mainly GBT at present
5009.42-2003 " analysis method of salt hygienic standard ", principle be potassium ferrocyanide in acid condition with ferrous sulfate
Blue double salt is generated, it is quantitative compared with standard items by ultraviolet test, but the reagent of sulfuric acid ferrous iron that the method uses is unstable, pole
It is vulnerable.Yan Jidong is at " potassium ferrocyanide in acid iron ammonium sulfate spectrophotometry measurement salt " by standard GBT
Reducing agent ferrous sulfate in 5009.42-2003 replaces with iron ammonium sulfate, and a left side is splashed in " pyridine --- pyrazolone measurement food
With potassium ferrocyanide method micro in salt " report pyridine --- pyrazolone development process, according to potassium ferrocyanide in acidity
Under the conditions of through distillation decomposite cyanide, react with toluene-sodium-sulfonchloramide, generation cyanogen chloride (CNCI), then with pyrrole heavy stone used as an anchor --- pyrazolone
Generate blue dyes.Extremely toxic substance cyanide, cyanogen chloride are produced in the method detection process, there is very big risk, it is uncomfortable
In popularization and use.Liu Yong is reported in an acidic solution, iron ion in " research of Resonance Light Scattering Method measurement potassium ferrocyanide "
Prussian blue, resonant light scattering enhanced strength, which is generated, with ferrocyanide nak response obtains one at λ ex=λ em=315nm
Resonance scattering peak, intensity are directly proportional to the concentration of potassium ferrocyanide.
Summary of the invention
The object of the present invention is to provide it is a kind of it is simple and efficient to handle, low-cost, national standard can be met limit the quantity and realize scene
The detection method of potassium ferrocyanide in the salt used.
Technical scheme is as follows:
The detection method of potassium ferrocyanide in a kind of salt, comprising the following steps:
1) sample treatment: weighing appropriate salt in sample cell, and highly polar solution is added and extracts, salt and highly polar solution
Mass volume ratio be 1:0.2~1:50g/ml；It stands, supernatant is spare as prepare liquid；The highly polar solution is strong
The aqueous solution of polar organic solvent；
2) Raman detection: taking appropriate metal-sol in Raman sample pool, and suitable prepare liquid is added and mixes, metal-sol
Volume ratio with prepare liquid is 10:1~1:20, is then placed on Raman spectrometer detection interior and is detected；
Preferably, the highly polar organic solvent is dimethyl sulfoxide, dimethylformamide, methanol, ethyl alcohol, acetonitrile, third
Ketone, ethylene glycol or its mixed liquor.
Preferably, in the aqueous solution of the highly polar organic solvent, by volume, organic solvent is aqueous solution total volume
1% to 99%.Extractant of the present invention is the aqueous solution of organic solvent, and the excess chlorination sodium that can forgo is dry in Raman detection
It disturbs.But if being lower than 1%, organic solvent content is very few, is unfavorable for excluding interference of the excess chlorination sodium in Raman detection, if
Higher than 99%, it is unfavorable for dissolving salt.It is further preferred that the intensive polar solvent is 10%-99% aqueous solutions of organic solvent.Further
It is preferred that the intensive polar solvent is 20%-90% aqueous solutions of organic solvent.
In the present invention, the mass volume ratio of salt and extractant is 1:0.2~1:50g/ml, if being lower than 1:0.2g/
Ml can not effectively dissolve potassium ferrocyanide, if be higher than 1:50g/ml, can dilute sample concentration, cause detection limit inclined
It is high.The mass volume ratio of salt and extractant is more preferably 1:0.5~1:5g/ml.
Preferably, prepare liquid use, which takes a step forward, dilutes 1-100 times with secondary distilled water.It is further preferred that for dilution 10-100
Times.
Preferably, the metal-sol is nanogold or nano silver.
Preferably, the volume ratio of metal-sol and prepare liquid is 10:1~1:20, if will lead to sample lower than 10:1
Amount is very little, influences detection limit；If being higher than 1:20, metal-sol is very little, and signal enhancing efficiency is insufficient.
Preferably, if necessary to quantitative, it by characteristic peak is 501cm that the present invention, which further comprises step 3),-1Or 2082cm-1
It detects obtained numerical value to compare with standard curve, obtains the quantitative detection result of the potassium ferrocyanide in salt.
Preferably, the preparation method of standard curve described in step 3) is as follows, the ferrous cyanogen of mark-on various concentration in salt
Change potassium, scanning feature peak 501cm-1Or 2082cm-1, the feature peak intensity that spiked levels and scanning obtain is drawn into standard curve.
The present invention extracts and deficiency present in detection method, entire detection process for potassium ferrocyanide in existing salt
Consumption of organic solvent is few, green non-poisonous, can exclude influence of the excessive salt in Raman detection；Agents useful for same is stablized, and can grow
Phase saves；Detection time is short, and detection can be completed in 5min.Using the method for Surface enhanced Raman spectroscopy, can be realized to food
Quantitative detection may be implemented by built-in standard curve in the quick detection at potassium ferrocyanide scene in salt.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Attached drawing 1 is 10ppm potassium ferrocyanide Surface enhanced Raman spectroscopy；
Attached drawing 2 is that salt mark-on 20ppm potassium ferrocyanide difference extractant extracts Surface enhanced Raman spectroscopy；
Attached drawing 3 is salt mark-on various concentration potassium ferrocyanide Surface enhanced Raman spectroscopy.
Attached drawing 4 is the 2082cm of salt mark-on various concentration potassium ferrocyanide-1The linearity curve of signal strength and concentration
Specific embodiment
Nanogold synthesis: 100mL is first contained to 0.01% HAuCl4Solution is heated to boiling, and is rapidly added 1% lemon of 1mL
Lemon three sodium water solutions of acid, are heated to reflux 1h, are cooled to room temperature.
Nano silver synthesis: first the silver nitrate solution by 100mL containing 1mM is heated to boiling, and is rapidly added 1% citric acid of 1mL
Three sodium water solutions, are heated to reflux 1h, are cooled to room temperature.
Embodiment 1: taking 4 portions of 1g salt, and mark-on 20ppm potassium ferrocyanide is separately added into 90% acetonitrile of 5ml, 20% diformazan
Sulfoxide, 70% methanol, 60% acetone ultrasonic extraction 2 minutes, stand to supernatant and clarify, take supernatant spare as prepare liquid.
It takes 200 μ l nano silvers in Raman sample pool, 100 μ l prepare liquids is added and mix, are then placed on portable Raman spectrometer sensing chamber
Inside detected.The Surface enhanced Raman spectroscopy such as attached drawing 2 is obtained, as seen from the figure, the method can detecte mark-on in salt
The signal of 20ppm potassium ferrocyanide.
Embodiment 2: taking 4 portions of 0.5g salt, successively mark-on 0ppm, 5ppm, 10ppm, 20ppm potassium ferrocyanide, respectively plus
Enter 60% ethylene glycol ultrasonic extraction of 2mL 1 minute, stand to supernatant and clarify, it is standby as prepare liquid to take out 10 times of supernatant dilution
With.It takes 200 μ l nanogold in Raman sample pool, 100 μ l prepare liquids is added and mix, be then placed on portable Raman spectrometer detection
It is detected interior.The Surface enhanced Raman spectroscopy such as attached drawing 3 and Fig. 4 is obtained, as seen from the figure, the method can detecte salt
The signal of middle mark-on various concentration potassium ferrocyanide.
Claims (9)
1. the detection method of potassium ferrocyanide in a kind of salt, comprising the following steps:
1) sample treatment: weighing appropriate salt in sample cell, and highly polar solution is added and extracts, the matter of salt and highly polar solution
Amount volume ratio is 1:0.2~1:50g/ml；It stands, supernatant is spare as prepare liquid；The highly polar solution is highly polar
The aqueous solution of organic solvent；
2) Raman detection: taking appropriate metal-sol in Raman sample pool, and suitable prepare liquid is added and mixes, metal-sol and to
The volume ratio for surveying liquid is 10:1~1:20, is then placed on Raman spectrometer detection interior and is detected.
2. the detection method of potassium ferrocyanide in salt as described in claim 1, which is characterized in that described is highly polar organic
Solvent is or mixtures thereof at least one of dimethyl sulfoxide, dimethylformamide, methanol, acetonitrile, acetone, ethyl alcohol, ethylene glycol.
3. the detection method of potassium ferrocyanide in salt as claimed in claim 2, which is characterized in that described is highly polar organic
In the aqueous solution of solvent, by volume, organic solvent is the 1% to 99% of aqueous solution total volume.
4. the detection method of potassium ferrocyanide in salt as claimed in claim 3, which is characterized in that by volume, You Jirong
Agent is the 10% to 9% of aqueous solution total volume.
5. the detection method of potassium ferrocyanide in the salt as described in claims 1 or 2 or 3, which is characterized in that salt and strong pole
Property solution mass volume ratio be 1:0.2-1:50g/ml.
6. the detection method of potassium ferrocyanide in the salt as described in claims 1 or 2 or 3, which is characterized in that step 1) is described
Prepare liquid, be diluted with water 1-100 times before use and enter back into step 2).
7. the detection method of potassium ferrocyanide in salt as described in claim 1, which is characterized in that the metal-sol is
Nanogold or nano silver.
8. the detection method of potassium ferrocyanide in salt as described in claim 1, which is characterized in that further include step
It 3) is 501cm by characteristic peak-1Or 2082cm-1It detects obtained numerical value to compare with standard curve, obtain in salt
The quantitative detection result of potassium ferrocyanide.
9. the detection method of potassium ferrocyanide in salt as described in claim 8, which is characterized in that mark described in step 3)
The preparation method of directrix curve is as follows, the potassium ferrocyanide of mark-on various concentration in salt, scanning feature peak 501cm-1Or 2082cm-1, the feature peak intensity that spiked levels and scanning obtain is drawn into standard curve.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111044512A (en) * | 2019-12-17 | 2020-04-21 | 谱尼测试集团股份有限公司 | Method for rapidly detecting potassium ferrocyanide in salt |
| CN112834494A (en) * | 2021-01-05 | 2021-05-25 | 中国石油化工股份有限公司 | Method for determining cyanide and total cyanide in soil |
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| CN1159576A (en) * | 1996-03-11 | 1997-09-17 | 株式会社京都第一科学 | Method of measuring enzyme reaction by raman |
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| CN1159576A (en) * | 1996-03-11 | 1997-09-17 | 株式会社京都第一科学 | Method of measuring enzyme reaction by raman |
| CN103901015A (en) * | 2014-03-25 | 2014-07-02 | 长春中元仪器有限公司 | Method for simultaneously detecting thiocyanate radical and melamine in dairy products |
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| HO SOO LIM ET AL.: "Assessment of ferrocyanide intake from food-grade salt in the Korean population", 《LWT-FOOD SCIENCE AND TECHNOLOGY》 * |
| M. FLEISCHMANN ET AL.: "The raman spectroscopy of the ferricyanide/ferrocyanide system at gold, β-palladium hydride and platinum electrodes", 《JOURNAL OF ELECTROANALYTICAL CHEMISTRY AND INTERFACIAL ELECTROCHEMISTRY》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111044512A (en) * | 2019-12-17 | 2020-04-21 | 谱尼测试集团股份有限公司 | Method for rapidly detecting potassium ferrocyanide in salt |
| CN112834494A (en) * | 2021-01-05 | 2021-05-25 | 中国石油化工股份有限公司 | Method for determining cyanide and total cyanide in soil |
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