CN109001367A - A method of utilizing ion chromatography cyanide ion - Google Patents
A method of utilizing ion chromatography cyanide ion Download PDFInfo
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- CN109001367A CN109001367A CN201810970572.0A CN201810970572A CN109001367A CN 109001367 A CN109001367 A CN 109001367A CN 201810970572 A CN201810970572 A CN 201810970572A CN 109001367 A CN109001367 A CN 109001367A
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- Prior art keywords
- ion
- cyanogen root
- sample
- solution
- standard solution
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
Abstract
The present invention discloses a kind of method using ion-chromatographic determination trace cyanide ion, comprising the following steps: prepares the leacheate containing NaOH, NaOAc, ethylenediamine, mass concentration is the cyanogen root standard solution of 1.0ug/ml and the sample solution of drug to be determined；It is analyzed respectively into ion chromatograph, spectrogram is integrated, cyanogen root residual quantity is calculated further according to formula.With method of the invention, it is not necessarily to configuration instruction agent in advance and a variety of titrant, a large amount of time can be saved；That sample introduction is analyzed is easy to operate for ion chromatography, simplifies the complex operations process of titration；The accuracy of testing result is improved, and greatly reduces detection limit, overcomes the subjectivity of titration end-point judgement；Avoid the spectrophotometry defect bigger by matrix interference；Avoid the defect that eye-observation subjectivity is strong in colorimetric method.
Description
Technical field
The present invention relates to Pharmaceutical Analysis method, in particular to a kind of side using ion-chromatographic determination trace cyanide ion
Method.
Background technique
Due to cyanogen root have excellent complexing power, be widely used in coking, ore dressing, non-ferrous metal metallurgy and processing,
The industry such as plating, process hides, electronics and instrument and meter, therefore the above every profession and trade is also the main source of the waste liquid containing cyanogen root.Due to cyanogen
Root directly generates mortality gas hydrogen cyanide under acidic environment, so the monitoring and control to the waste liquid containing cyanogen root are environmental protections
With the key means of personal safety.
Currently, the determination of trace method of cyanide ion is mainly titration, spectrophotometry and test paper colorimetric method.Titration
It is that zinc nitrate, tartaric acid and methyl orange are added in the sample, the sodium hydroxide solution of rear addition 0.1% adds 1 drop phenolphthalein to indicate
Color developing agent is added after adding potassium dihydrogen phosphate and toluene-sodium-sulfonchloramide with glacial acetic acid tune pH to faintly acid in agent.The shortcomings that titration is to need
Manual configuration indicator and a variety of titrant are wanted, pre-treatment operation is more, and process is complicated, and time-consuming, and titration end-point judges bad standard
Really grasp.Spectrophotometry is bigger by matrix interference, and application range is narrow.Test paper colorimetric method is by dipping the examination after solution
Paper is compared with standard color card, it the shortcomings that be human eye judgement, subjective consciousness is stronger.
Summary of the invention
Technical problem to be solved by the present invention lies in provide a kind of using ion-chromatographic determination trace cyanide ion
Method can reduce operation, the simple flow, the master for avoiding matrix interference, overcoming endpoint and human eye colorimetric of prewired solvent
The property seen.
In order to solve the above technical problems, the technical solution adopted by the present invention are as follows: a kind of to utilize ion-chromatographic determination trace
The method of cyanide ion, comprising the following steps:
Prepare the leacheate containing NaOH, NaOAc, ethylenediamine, mass concentration be 1.0ug/ml cyanogen root standard solution and
The sample solution of drug to be determined；It is analyzed respectively into ion chromatograph, spectrogram is integrated, calculated further according to formula
To cyanogen root residual quantity:
Wherein:
CSTD 01: the concentration of cyanogen root in standard solution；
ASTD 01: the peak area of cyanogen root in standard solution；
WS: the quality of sample；
VS: the dilution volume of sample；
AS: the peak area of cyanogen root in sample solution.
In a kind of specific embodiment, chromatographic column is Dionex IonPac AS7,4*250mm.
In a kind of specific embodiment, column temperature (Column Temperature) is 30 DEG C, detection cell temperature (Cell
It Temperature) is 35 DEG C.
In a specific embodiment, detection mode (Detection Mode) uses Electrochemical Detection
(Electrochemistry Detection)。
In a specific embodiment, mobile phase be sodium hydroxide containing 0.05-0.2M, 0.25-1.0M sodium acetate,
The aqueous solution of 0.25%-1.0% ethylenediamine.
In a specific embodiment, flow velocity 1.0mL/min, sample volume are 25 μ L.
In a specific embodiment, working electrode is Ag electrode, and reference electrode is Ag/AgCl electrode.
The detection of cyanogen root mainly has titration, but since titration needs to configure a variety of solution and color developing agent, titration end-point
In the presence of personal subjective judgement, the accuracy of result is influenced, and time-consuming, complicated for operation for entire titration process.Using the present invention
Method, be not necessarily to configuration instruction agent in advance and a variety of titrant, a large amount of time can be saved；The ion chromatography behaviour that sample introduction is analyzed
Make simply, to simplify the complex operations process of titration；The accuracy for improving testing result overcomes the master of titration end-point judgement
The property seen；Greatly reduce detection limit, detection limit 10ppm；Avoid spectrophotometry by matrix interference it is bigger lack
It falls into；Avoid the defect that eye-observation subjectivity is strong in colorimetric method.
Detailed description of the invention
Fig. 1 is the chromatography of ions figure of 1.0ug/ml cyanogen root standard solution in one specific embodiment of method of the invention.
Fig. 2 is the chromatography of ions figure of sample to be tested in one specific embodiment of method of the invention.
Specific embodiment
Clear, complete description will be carried out to technical solution of the present invention below, it is clear that described embodiment is this hair
Bright a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art exist
Every other embodiment obtained under the premise of creative work is not made, shall fall within the protection scope of the present invention.
Embodiment 1
Required instrument: Thermo ICS 5000+ equivalent or more；Ten a ten thousandth balance equivalents or more.
Reagent: 50% sodium hydrate aqueous solution, sodium acetate, ethylenediamine
Required experimental method parameter:
The residual of cyanogen root is calculated further according to formula:
Wherein: CSTD 01For the concentration of cyanogen root in standard solution, ASTD 01For the peak area of cyanogen root in standard solution, WSFor sample
The quality of product, VSFor the dilution volume of sample, ASFor the peak area of cyanogen root in sample solution.
For the remaining detection of cyanogen root in laboratory research and development sample sample, WSFor 204.47mg, VSFor 10ml, cyanogen root standard
Solution is 1.0ug/ml, and the condition detected is as follows:
Test map is as shown in Figure 2.It is as follows to calculate cyanogen root residual quantity result:
In conclusion the various embodiments described above are only presently preferred embodiments of the present invention, it is not of the invention to limit
Protection scope, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be all included in
In protection scope of the present invention.
Claims (7)
1. a kind of method using ion-chromatographic determination trace cyanide ion, which comprises the following steps:
Prepare the leacheate containing NaOH, NaOAc, ethylenediamine, mass concentration is the cyanogen root standard solution of 1.0ug/ml and to be measured
Determine the sample solution of drug；
It is analyzed respectively into ion chromatograph, spectrogram is integrated, cyanogen root residual quantity is calculated further according to formula；
Wherein:
CSTD 01: the concentration of cyanogen root in standard solution；
ASTD 01: the peak area of cyanogen root in standard solution；
WS: the quality of sample；
VS: the dilution volume of sample；
AS: the peak area of cyanogen root in sample solution.
2. the method as described in claim 1, which is characterized in that the chromatographic column that the method uses is Dionex IonPac
AS7,4*250mm。
3. the method as described in claim 1, which is characterized in that it is 30 DEG C that column temperature is arranged in the method, and detection cell temperature is 35
℃。
4. the method as described in claim 1, which is characterized in that detection pattern uses Electrochemical Detection in the method.
5. the method as described in claim 1, which is characterized in that in the method leacheate be sodium hydroxide containing 0.05-0.2M,
The aqueous solution of 0.25-1.0M sodium acetate, 0.25%-1.0% ethylenediamine.
6. the method as described in claim 1, which is characterized in that flow velocity is 1.0mL/min in the method, and sample volume is 25 μ
L。
7. the method as described in claim 1, which is characterized in that working electrode is Ag electrode in the method, and reference electrode is
Ag/AgCl electrode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810970572.0A CN109001367A (en) | 2018-08-24 | 2018-08-24 | A method of utilizing ion chromatography cyanide ion |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810970572.0A CN109001367A (en) | 2018-08-24 | 2018-08-24 | A method of utilizing ion chromatography cyanide ion |
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| CN109001367A true CN109001367A (en) | 2018-12-14 |
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| CN201810970572.0A Pending CN109001367A (en) | 2018-08-24 | 2018-08-24 | A method of utilizing ion chromatography cyanide ion |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103616452A (en) * | 2013-12-06 | 2014-03-05 | 中国烟草总公司郑州烟草研究院 | Determination method for experiment of simulating cigarette burning for generating hydrogen cyanide |
| CN104280509A (en) * | 2014-09-26 | 2015-01-14 | 中国石油化工股份有限公司 | Device and method for detecting total cyanide and sulfide in water solution by employing direct conversion |
| CN104297367A (en) * | 2014-09-26 | 2015-01-21 | 中国石油化工股份有限公司 | Device and method for amperometric detection of total cyanide and sulfide of wastewater by online photolysis dialysis/chromatographic separation |
-
2018
- 2018-08-24 CN CN201810970572.0A patent/CN109001367A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103616452A (en) * | 2013-12-06 | 2014-03-05 | 中国烟草总公司郑州烟草研究院 | Determination method for experiment of simulating cigarette burning for generating hydrogen cyanide |
| CN104280509A (en) * | 2014-09-26 | 2015-01-14 | 中国石油化工股份有限公司 | Device and method for detecting total cyanide and sulfide in water solution by employing direct conversion |
| CN104297367A (en) * | 2014-09-26 | 2015-01-21 | 中国石油化工股份有限公司 | Device and method for amperometric detection of total cyanide and sulfide of wastewater by online photolysis dialysis/chromatographic separation |
Non-Patent Citations (2)
| Title |
|---|
| 李美君 等: "离子色谱法测定厄贝沙坦中氰化物", 《中南药学》 * |
| 王勇 等: "离子色谱法检验血液中氰化物", 《现代科学仪器》 * |
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