CN108490061A - A kind of detection method of detection hydrogen cyanide and cyanide content - Google Patents
A kind of detection method of detection hydrogen cyanide and cyanide content Download PDFInfo
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Abstract
The invention discloses a kind of detection methods of detection hydrogen cyanide and cyanide content, establish the cyclic voltammetry (CV) of concentration of cyanide in direct determination sample, then Differential Pulse Voltammetry, it is detected under the three-electrode system that it is auxiliary electrode to be complex film modified glass-carbon electrode as working electrode, platinum electrode, saturated calomel electrode is reference electrode, quantitative analysis is carried out using calibration curve method to sample to obtain a result, it is characterized in that, detection method comprises the following steps：（1）Sample preparation steps；（2）The preparation process of standard solution；（3）Detecting step.This method detection is easy to operate, accuracy is high, high sensitivity, high specificity.
Description
Technical field
The present invention relates to cyanide detection technique field more particularly to a kind of detections of detection hydrogen cyanide and cyanide content
Method.
Background technology
Cyanide category extremely toxic substance can be entered in human body by respiratory tract, alimentary canal and skin, in cell mitochondrial
The ferric iron of oxidized form cytochrome oxidase combines, and prevents the ferric iron back in oxidizing ferment, interferes cell eupnea, makes
At body anoxic so that generating poisoning effect.In addition, cyanide is also possible to form other hazardous compounds under certain condition,
There are security risks in food, beverage.Due to the fast development of modern industry, many cyanides by plating, paint, dyestuff,
The sewage of the industries such as rubber discharge enters in natural water, seriously endangers the health of the mankind.So far from 2009, China oneself
Through a lot of cyanide poisoning events occur, health of the masses has been seriously affected.
Currently, the assay method about cyanide has very much.Such as colorimetric, titration, isotopic dilution, gas-chromatography, original
Sub- absorption spectrum and infrared absorption spectrum etc..Most widely used is spectrophotometry, electrochemical assay, gas chromatography.
Although these methods there are a large amount of reports at home, still have that cumbersome, time-consuming and quality efficiency is not high to ask in its method
Topic.
Based on this, exploitation it is a kind of can it is easy, quick and sensitively detection hydrogen cyanide and cyanide detection method urgently
It is to be solved.
Invention content
To solve not easy enough to the detection of hydrogen cyanide and cyanide, quick in the prior art, the inadequate technology of sensitivity
Problem, the present invention provide a kind of detection method, reach content that is easy to operate, can quickly detecting hydrogen cyanide and cyanide.
In order to achieve the above objectives, it is achieved by following technical solution：
A kind of detection method of detection hydrogen cyanide and cyanide content, establishes the cycle volt of concentration of cyanide in direct determination sample
Peace method (CV), then Differential Pulse Voltammetry, is with the three-electrode system of working electrode, auxiliary electrode, reference electrode
Under be detected, using calibration curve method to sample carry out quantitative analysis obtain a result, detection method comprises the following steps：
（1）Sample preparation：10 ~ 20min of appropriate sodium hydroxide alkaline hydrolysis is added in various concentration cyanide solution or hydrogen cyanide, then
100g/L ~ 300g/L acetic acid zinc solutions, and saturation tartaric acid solution is added, additive amount is sample：Acetic acid zinc solution volume ratio etc.
In 1：4 ~ 5, sample：It is saturated tartaric acid solution volume ratio and is equal to 1：2~3；
（2）The preparation of standard solution：The potassium cyanide standard items storing solution for being configured to 10mg/L is diluted to a series of standard of concentration
Solution, same to step（1）Same procedure handles sample；
（3）Detection：For complex film modified glass-carbon electrode as working electrode, reference electrode is saturated calomel electrode, and auxiliary electrode is
Platinum electrode forms three-electrode system；The three-electrode system is placed in the sample or standard solution handled well, uses phosphate
PH to 4.0 ~ 8.0, current potential is adjusted to carry out Differential Pulse Voltammetry, record electricity later from -0.6~0.8 V cyclic voltammetry scans
Stream-potential curve establishes electric current and concentration of cyanide curve.
Preferably, the preparation method of complex film modified glassy carbon electrode comprises the following steps：
（1）Glassy carbon electrode is put into containing 20 ~ 50g/L of taurine, 2,3- naphthalene, two acetal（NDA）40 ~ 60g/L, cobalt acetate are water-soluble
The solution of 0.01 ~ 0.08mol/L of liquid, 1 ~ 3g/L of graphene oxide solution, immersion 8 ~ for 24 hours, then it is dried in vacuo 5 ~ 8h；
（2）By palladium bichloride and sodium chloride according to 1：3 ~ 4 molar ratio is add to deionized water, and 5 ~ 6h of magnetic agitation is made mixed
Solution is closed, a concentration of 1.3 ~ 2.0mmol/L of palladium bichloride in mixed solution；
（3）By step（1）Treated, and glassy carbon electrode is that cathode is put into step（2）The palladium chloride solution of preparation, platinum electrode are sun
Pole is 1.2 ~ 2.0mA/cm in electric current2 , depositing temperature deposit 1 ~ 3h under the conditions of being 30 ~ 38 DEG C, obtain complex film modified glass carbon electricity
Pole.
Preferably, step（1）The soaking time is 12h.
Preferably, step（2）A concentration of 1.4 ~ 1.6 mmol/L of the palladium bichloride.
Preferably, step（2）A concentration of 1.5mmol/L of the palladium bichloride.
Preferably, step（3）The sedimentation time is 1.5h.
Preferably, step（3）The electric current is 1.3 mA/cm2 。
Preferably, step（2）Described in buffer solution be phosphate buffer.
Preferably, the detection of the detection method is limited to 1nmol/L.
Preferably, the cyanide is one kind in hydrogen cyanide, Cymag, potassium cyanide, cyanogen chloride, acrylonitrile, positive fourth eyeball
Or it is a variety of.
Advantageous effect：
（1）It may be implemented in high specific under low-detection lower limit, with sensitivity to the quick detection of cyanide；
（2）In the case of the concentration decades of times at concentrations up to cyanide to be checked of chaff interferent, still can efficiently it realize to cyanogen to be checked
The detection of compound；
（3）Detection method rapid sensitive detection cyanide easy to operate, at low cost, achievable；
（4）The detection method is good to measuring samples adaptability, is substantially not present any restrictions, easy to utilize；
（5）The detection method can be realized to being detected while a variety of cyanides.
Description of the drawings
2 linear graph of Fig. 1 embodiments.
Specific embodiment
A kind of detection method of detection cyanide content of embodiment 1
A kind of detection method of detection cyanide content, establishes the cyclic voltammetry (CV of concentration of cyanide in direct determination sample
), be with working electrode, auxiliary electrode, reference electrode three-electrode system under be detected, using calibration curve method to sample into
Row quantitative analysis is obtained a result, and detection method comprises the following steps：
（1）Sample preparation：Appropriate sodium hydroxide alkaline hydrolysis 10min is added in various concentration hydrogen cyanide, Cymag, is then added
100g/L acetic acid zinc solutions, and saturation tartaric acid solution, additive amount is sample：Acetic acid zinc solution volume ratio is equal to 1：4, sample：
It is saturated tartaric acid solution volume ratio and is equal to 1：2；
（2）The preparation of standard solution：The potassium cyanide standard items storing solution for being configured to 10mg/L is diluted to a series of standard of concentration
Solution, same to step（1）Same procedure handles sample；
（3）Detection：For complex film modified glass-carbon electrode as working electrode, reference electrode is saturated calomel electrode, and auxiliary electrode is
Platinum electrode forms three-electrode system；The three-electrode system is placed in the sample or standard solution handled well, uses phosphate
PH to 4.0, current potential is adjusted to carry out Differential Pulse Voltammetry, record current later from -0.6~0.8 V cyclic voltammetry scans
Potential curve establishes electric current and concentration of cyanide curve.
The preparation method of the complex film modified glassy carbon electrode comprises the following steps：
（1）Glassy carbon electrode is put into 20g/L containing taurine, 2,3- naphthalene, two acetal（NDA）40g/L, cobalt acetate aqueous solution
The solution of 0.01mol/L, graphene oxide solution 1g/L impregnate 8h, are then dried in vacuo 5h；
（2）By palladium bichloride and sodium chloride according to 1：3 molar ratio is add to deionized water, magnetic agitation 5h, and it is molten that mixing is made
Liquid, a concentration of 1.3mmol/L of palladium bichloride in mixed solution；
（3）By step（1）Treated, and glassy carbon electrode is that cathode is put into step（2）The palladium chloride solution of preparation, platinum electrode are sun
Pole is 1.2mA/cm in electric current2 , depositing temperature be 30 DEG C under the conditions of deposit 1h, obtain complex film modified glass-carbon electrode.
Experimental result：
Specificity：Other interfering ions are added into the cryanide ion aqueous solution of the various concentration of configuration in the present embodiment（F-, Cl-,
Br-, I-, NO3-, NO2-, CO3 2-, SCN-, S2-, SO4 2-）It (is added in the form of salts, the total concentration of interfering substance be added is 10 μ
Mol/L), the method used in embodiment 1 is repeated to measure the solution of known concentration of cyanide.The experimental results showed that is,
Make there are a large amount of interfering substances, gained testing result is still very accurate, with 1 gained testing result phase of embodiment
Difference is also little, shows the strong antijamming capability of the method for the present invention, has very strong specificity.
The range of linearity and detection limit：It uses complex film modified electrode to be detected and recycles volt from -0.6 ~ 0.8 V for current potential
Peace scanning, carries out Differential Pulse Voltammetry, record current-potential curve, according to pair of electric current and concentration of cyanide later
It should be related to, establish standard curve, electric current（I, μ A）With the concentration of cyanide（C, μm ol/L）2.0 × 10-6~0.8×10-3
In a linear relationship within the scope of mmol/L, equation of linear regression is：I = 17.64c + 1.52（R2=0.9999, n=5）.Base
In the signal-to-noise ratio of three times（S/N = 3）, obtain the modified electrode and 4 × 10 be limited to the detection of cyanide-6 mmol/L。
The cyanide content measured using this method, the rate of recovery are 96.8% ~ 101.3%, and relative standard deviation is：1.4%.
A kind of detection method of detection cyanide content of embodiment 2
A kind of detection method of detection cyanide content, establishes the cyclic voltammetry (CV of concentration of cyanide in direct determination sample
), be with working electrode, auxiliary electrode, reference electrode three-electrode system under be detected, using calibration curve method to sample into
Row quantitative analysis is obtained a result, and detection method comprises the following steps：
（1）Sample preparation：Appropriate sodium hydroxide alkaline hydrolysis 15min is added in various concentration potassium cyanide, cyanogen chloride, is then added
200g/L acetic acid zinc solutions, and saturation tartaric acid solution, additive amount is sample：Acetic acid zinc solution volume ratio is equal to 1：4.5, sample
Product：It is saturated tartaric acid solution volume ratio and is equal to 1：2.5；
（2）The preparation of standard solution：The potassium cyanide standard items storing solution for being configured to 10mg/L is diluted to a series of standard of concentration
Solution, same to step（1）Same procedure handles sample；
（3）Detection：For complex film modified glass-carbon electrode as working electrode, reference electrode is saturated calomel electrode, and auxiliary electrode is
Platinum electrode forms three-electrode system；The three-electrode system is placed in the sample or standard solution handled well, uses phosphate
PH to 6.5, current potential is adjusted to carry out Differential Pulse Voltammetry, record current later from -0.6~0.8 V cyclic voltammetry scans
Potential curve establishes electric current and concentration of cyanide curve.
Preferably, the preparation method of complex film modified glassy carbon electrode comprises the following steps：
（1）Glassy carbon electrode is put into 40g/L containing taurine, 2,3- naphthalene, two acetal（NDA）50g/L, cobalt acetate aqueous solution
The solution of 0.05mol/L, graphene oxide solution 2g/L impregnate 12h, are then dried in vacuo 6h；
（2）By palladium bichloride and sodium chloride according to 1：3.5 molar ratio is add to deionized water, and magnetic agitation 5.5h is made mixed
Solution is closed, a concentration of 1.5mmol/L of palladium bichloride in mixed solution；
（3）By step（1）Treated, and glassy carbon electrode is that cathode is put into step（2）The palladium chloride solution of preparation, platinum electrode are sun
Pole is 1.3mA/cm in electric current2 , depositing temperature be 35 DEG C under the conditions of deposit 1.5h, obtain complex film modified glass-carbon electrode.
Experimental result：
Specificity：Other interfering ions are added into the cryanide ion aqueous solution of the various concentration of configuration in the present embodiment（F-, Cl-,
Br-, I-, NO3-, NO2-, CO3 2-, SCN-, S2-, SO4 2-）It (is added in the form of salts, the total concentration of interfering substance be added is 15 μ
Mol/L), the method used in embodiment 2 is repeated to measure the solution of known concentration of cyanide.The experimental results showed that is,
Make there are a large amount of interfering substances, gained testing result is still very accurate, with 2 gained testing result phase of embodiment
Difference is also little, shows the strong antijamming capability of the method for the present invention, has very strong specificity.
The range of linearity and detection limit：It uses complex film modified electrode to be detected and recycles volt from -0.6 ~ 0.8 V for current potential
Peace scanning, carries out Differential Pulse Voltammetry, record current-potential curve, according to pair of electric current and concentration of cyanide later
It should be related to, establish standard curve, electric current（I, μ A）With the concentration of cyanide（C, μm ol/L）1.0 × 10-6~1.2×10-3
In a linear relationship within the scope of mmol/L, equation of linear regression is：I = 22.45c +2.24（R2=1, n=5）.Based on three times
Signal-to-noise ratio（S/N = 3）, obtain the modified electrode and 1.0 × 10 be limited to the detection of cyanide-6 mmol/L。
The cyanide content measured using this method, the rate of recovery are 98.0% ~ 100.8%, and relative standard deviation is：0.6%.
A kind of detection method of detection cyanide content of embodiment 3
A kind of detection method of detection cyanide content, establishes the cyclic voltammetry (CV of concentration of cyanide in direct determination sample
), be with working electrode, auxiliary electrode, reference electrode three-electrode system under be detected, using calibration curve method to sample into
Row quantitative analysis is obtained a result, and detection method comprises the following steps：
（1）Sample preparation：Appropriate sodium hydroxide alkaline hydrolysis 20min is added in various concentration acrylonitrile, n-Butyronitrile, is then added
300g/L acetic acid zinc solutions, and saturation tartaric acid solution, additive amount is sample：Acetic acid zinc solution volume ratio is equal to 1：5, sample：
It is saturated tartaric acid solution volume ratio and is equal to 1：3；
（2）The preparation of standard solution：The potassium cyanide standard items storing solution for being configured to 10mg/L is diluted to a series of standard of concentration
Solution, same to step（1）Same procedure handles sample；
（3）Detection：For complex film modified glass-carbon electrode as working electrode, reference electrode is saturated calomel electrode, and auxiliary electrode is
Platinum electrode forms three-electrode system；The three-electrode system is placed in the sample or standard solution handled well, uses phosphate
PH to 8, current potential is adjusted to carry out Differential Pulse Voltammetry, record current electricity later from -0.6~0.8 V cyclic voltammetry scans
Position curve, establishes electric current and concentration of cyanide curve.
Preferably, the preparation method of complex film modified glassy carbon electrode comprises the following steps：
（1）Glassy carbon electrode is put into 50g/L containing taurine, 2,3- naphthalene, two acetal（NDA）60g/L, cobalt acetate aqueous solution
The solution of 0.08mol/L, graphene oxide solution 3g/L impregnate for 24 hours, are then dried in vacuo 8h；
（2）By palladium bichloride and sodium chloride according to 1：4 molar ratio is add to deionized water, magnetic agitation 6h, and it is molten that mixing is made
Liquid, a concentration of 2.0mmol/L of palladium bichloride in mixed solution；
（3）By step（1）Treated, and glassy carbon electrode is that cathode is put into step（2）The palladium chloride solution of preparation, platinum electrode are sun
Pole is 2.0mA/cm in electric current2 , depositing temperature be 38 DEG C under the conditions of deposit 3h, obtain complex film modified glass-carbon electrode.
Experimental result：
Specificity：Other interfering ions are added into the cryanide ion aqueous solution of the various concentration of configuration in the present embodiment（F-, Cl-,
Br-, I-, NO3-, NO2-, CO3 2-, SCN-, S2-, SO4 2-）（It is added in the form of salts, the total concentration of interfering substance be added is 20 μ
mol/L）, repeat the method used in embodiment 3 and the solution of known concentration of cyanide measured.The experimental results showed that is,
Make there are a large amount of interfering substances, gained testing result is still very accurate, with 3 gained testing result phase of embodiment
Difference is also little, shows the strong antijamming capability of the method for the present invention, has very strong specificity.
The range of linearity and detection limit：It uses complex film modified electrode to be detected and recycles volt from -0.6 ~ 0.8 V for current potential
Peace scanning, carries out Differential Pulse Voltammetry, record current-potential curve, according to pair of electric current and concentration of cyanide later
It should be related to, establish standard curve, electric current（I, μ A）With the concentration of cyanide（C, μm ol/L）6.0 × 10-6~0.6×10-3
In a linear relationship within the scope of mmol/L, equation of linear regression is：I = 18.96c + 3.42（R2=0.9999, n=5）.Base
In the signal-to-noise ratio of three times（S/N = 3）, obtain the modified electrode and 3.0 × 10 be limited to the detection of cyanide-6 mmol/L。
The cyanide content measured using this method, the rate of recovery are 97.2% ~ 103.2%, and relative standard deviation is：1.8%.
Claims (10)
1. a kind of detection method of detection hydrogen cyanide and cyanide content, establishes the cycle of concentration of cyanide in direct determination sample
Voltammetry (CV), then Differential Pulse Voltammetry, is with three electrode bodies of working electrode, auxiliary electrode, reference electrode
It is detected under system, carrying out quantitative analysis to sample using calibration curve method obtains a result, which is characterized in that detection method includes
Following steps：
（1）Sample preparation：10 ~ 20min of appropriate sodium hydroxide alkaline hydrolysis is added in various concentration cyanide solution or hydrogen cyanide, then
100g/L ~ 300g/L acetic acid zinc solutions, and saturation tartaric acid solution is added, additive amount is sample：Acetic acid zinc solution volume ratio etc.
In 1：4 ~ 5, sample：It is saturated tartaric acid solution volume ratio and is equal to 1：2~3；
（2）The preparation of standard solution：The potassium cyanide standard items storing solution for being configured to 10mg/L is diluted to a series of standard of concentration
Solution, same to step（1）Same procedure handles sample；
（3）Detection：For complex film modified glass-carbon electrode as working electrode, reference electrode is saturated calomel electrode, and auxiliary electrode is
Platinum electrode forms three-electrode system；The three-electrode system is placed in the sample or standard solution handled well, uses phosphate
PH to 4.0 ~ 8.0, current potential is adjusted to carry out Differential Pulse Voltammetry, record electricity later from -0.6~0.8 V cyclic voltammetry scans
Stream-potential curve establishes electric current and concentration of cyanide curve.
2. detection method according to claim 1, which is characterized in that the preparation method of complex film modified glassy carbon electrode includes such as
Lower step：
（1）Glassy carbon electrode is put into containing 20 ~ 50g/L of taurine, 2,3- naphthalene, two acetal（NDA）40 ~ 60g/L, cobalt acetate are water-soluble
The solution of 0.01 ~ 0.08mol/L of liquid, 1 ~ 3g/L of graphene oxide solution, immersion 8 ~ for 24 hours, then it is dried in vacuo 5 ~ 8h；
（2）By palladium bichloride and sodium chloride according to 1：3 ~ 4 molar ratio is add to deionized water, and 5 ~ 6h of magnetic agitation is made mixed
Solution is closed, a concentration of 1.3 ~ 2.0mmol/L of palladium bichloride in mixed solution；
（3）By step（1）Treated, and glassy carbon electrode is that cathode is put into step（2）The palladium chloride solution of preparation, platinum electrode are sun
Pole is 1.2 ~ 2.0mA/cm in electric current2 , depositing temperature deposit 1 ~ 3h under the conditions of being 30 ~ 38 DEG C, obtain complex film modified glass carbon electricity
Pole.
3. detection method according to claim 2, which is characterized in that step（1）The soaking time is 12h.
4. detection method according to claim 2, which is characterized in that step（2）A concentration of the 1.4 of the palladium bichloride ~
1.6 mmol/L。
5. detection method according to claim 4, which is characterized in that step（2）The palladium bichloride it is a concentration of
1.5mmol/L。
6. detection method according to claim 2, which is characterized in that step（3）The sedimentation time is 1.5h.
7. detection method according to claim 2, which is characterized in that step（3）The electric current is 1.3 mA/cm2 。
8. detection method according to claim 1, which is characterized in that step（2）Described in buffer solution be phosphate-buffered
Liquid.
9. detection method according to claim 1, which is characterized in that the detection of the detection method is limited to 1nmol/L.
10. detection method according to claim 1, which is characterized in that the cyanide is hydrogen cyanide, Cymag, cyaniding
It is one or more in potassium, cyanogen chloride, acrylonitrile, n-Butyronitrile.
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