CN104849273A - Method for rapidly testing thiocyanate ions in coking desulfurization liquid - Google Patents
Method for rapidly testing thiocyanate ions in coking desulfurization liquid Download PDFInfo
- Publication number
- CN104849273A CN104849273A CN201510303798.1A CN201510303798A CN104849273A CN 104849273 A CN104849273 A CN 104849273A CN 201510303798 A CN201510303798 A CN 201510303798A CN 104849273 A CN104849273 A CN 104849273A
- Authority
- CN
- China
- Prior art keywords
- thiocyanate
- coking
- thiocyanate ion
- desulfurization liquid
- coking desulfurization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a technology for analyzing thiocyanate ions in an aqueous solution. The technology can be widely used for testing thiocyanate ions in industrial water in the fields of steel, coking and chemical engineering, and is also suitable for testing the thiocyanate ions in normal domestic water. A method comprises the following steps: according to a principle that CNS<-> and metal ions Fe<3+> can react to produce color development, adding excess metal ions Fe<3+> into a to-be-detected aqueous solution, then measuring the absorbance of reaction liquid under a maximum absorption wavelength by using a 723 type spectrophotometer, and then calculating the thiocyanate ion content of the to-be-detected solution according to a light absorption curve of a standard solution. The method disclosed by the invention is simple and convenient, and also ensures that the generation of a toxic substance namely cyanogen bromide in an original analysis method can be avoided, and the use of toxic medicines namely phenol and bromine water can be reduced; a new path for testing the thiocyanate ions in the aqueous solution can be provided, the cleaning property of a coking laboratory can be improved, and the safety of a laboratory environment can be increased; and the method disclosed by the invention is novel in idea, convenient to operate and wide in application scope, and has relatively good environmental protection benefits and social benefits.
Description
Technical field
The invention provides a kind of inspection being widely used in Thiocyanate ion in iron and steel, coking, chemical industry process water, be also applicable to the inspection of normal life water Thiocyanate ion, be specially Thiocyanate ion method for quickly detecting in a kind of aqueous solution.
Background technology
At metallurgy industry especially coking industry, generally containing thiocyanate in the process waters such as doctor solution, this material not only has a strong impact on catalyst regeneration, sulphur flotation and catalyst effect in doctor solution, in order to ensure desulfurized effect, needs the content of Accurate Determining thiocyanate.In traditional detection method, detect thiocyanate content and must use bromine and phenol.And these two kinds of medicines are all highly volatiles, and skin and mucous membrane are had to the noxious material of intense stimulus and corrosive attack, danger is very high, has very large safety management risk, is not suitable for using in enterprise laboratory.And traditional analysis is checked and is needed nearly half an hour at every turn.Therefore, one determination method is safely and efficiently badly in need of.
Summary of the invention
For above-mentioned situation, the present invention aims to provide a kind of new sulfur cyanate radical inspection technology, and it not only effectively can avoid using and generating of toxic pharmaceuticals, greatly increases work efficiency simultaneously.And principle is simple and easy, easy to operate, operating cost is low, is worth universal and promotes.
For achieving the above object, the method for the invention is solved by following technical scheme:
Thiocyanate ion method for quickly detecting in a kind of coking desulfurization liquid, comprises the steps:
(1) Thiocyanate ion concentration standard curve is drawn;
(2) content of the Thiocyanate ion in sample is measured.
The feature of the method for inspection of the present invention also has:
Method of the present invention is according to CNS
-with Fe
3+ the principle of ionic reaction colour developing, adds excessive Fe in aqueous solution to be measured
3+ metallic ion, then uses the absorbance of 723 type spectrophotometers assaying reaction liquid under maximum absorption wavelength, then calculates molten sulfur cyanide ion content to be measured according to the absorption curve of standard solution.
Described maximum absorption wavelength is 460nm.
Method detailed of the present invention is:
Thiocyanate ion method for quickly detecting in a kind of coking desulfurization liquid, according to the actual conditions of thiocyanate in coking desulfurization liquid, preparation ammonium thiocyanate standard solution, its concentration is followed successively by 50g/L, 100g/L, 150g/L, 200g/L, 300g/L; Draw 1ml in 500mL volumetric flask, add excessive Fe
3+ with distilled water diluting to scale, then pipette the solution 1mL after dilution in 50mL volumetric flask, with distilled water diluting to scale, under 460nm wavelength, use 1cm cuvette, with FeCl
3 make reference liquid, read absorbance, and drawing standard curve;
Regression equation is the corresponding coefficient R of C=466.50A+1.65
2=0.9997; Wherein, C represents ammonium thiocyanate concentration, and A represents absorbance, and R is related coefficient;
Shake up after fetching sample, filter, draw 1ml filtrate in 500mL volumetric flask, add excessive Fe
3+ with distilled water diluting to scale, then pipette the solution 1mL after dilution in 50mL volumetric flask, with distilled water diluting to scale, under 460nm wavelength, use 1cm cuvette, with FeCl
3 make reference liquid, read absorbance, calculate thiocyanate content according to typical curve.
Coking desulfurization liquid of the present invention refers to the coke-oven gas that high-temperature coking produces, in purification process, and the absorbing liquid of desulfurization process.
Method for quickly detecting of the present invention can be widely used in the inspection of Thiocyanate ion in analytical industry water, is iron and steel, coking, chemical industry process water as preferably described process water.
Method for quickly detecting of the present invention can be widely used in the inspection of normal life water Thiocyanate ion.
Beneficial effect of the present invention is: method for quickly detecting of the present invention, and tool has the following advantages:
(I) adopt spectrocolorimetry to analyze thiocyanate content, use instrument and medicine comparatively universal, there is outfit in most laboratory.
(II) generation of cyanogen bromide can effectively be avoided when analyzing sample.
(III) use of toxic pharmaceuticals phenol and bromine water is saved.
(IV) colourimetry is simple, nontoxic, environmentally safe, greatly increases work efficiency simultaneously.
The inspection technology of a kind of new sulfur cyanic acid ion provided by the invention, the core technology of this analytical approach adopts Fe
3+ with CNS
- the principle of reaction solution, and by preferred extinction wavelength, change reactant liquor absorbance.This can be widely used in the inspection of Thiocyanate ion in iron and steel, coking, chemical industry process water, is also applicable to the inspection of normal life water Thiocyanate ion, has good environmental benefit and social benefit.
In a word, the present invention is simple and convenient, and avoids the generation of noxious material cyanogen bromide in original analysis method, decreases the use of toxic pharmaceuticals phenol, bromine water.New approach opened to the inspection of Thiocyanate ion in aqueous solution, improves the spatter property in coking laboratory, improve the security of chemically examining environment.Thinking of the present invention is novel, easy to operate, and wide accommodation, has good environmental benefit and social benefit.
Accompanying drawing explanation
Fig. 1 is the impact of absorbing wavelength on absorbance;
Fig. 2 standard solution absorbance curve;
Fig. 3 inspection process figure.
Embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention is described in detail.
Test example 1 describes the Selection experiment to extinction wavelength.
Configuration standard solution, the absorbance respectively after the measurement of 420nm, 430nm, 440nm, 450nm, 460nm, 470nm, 480nm, 490nm place adds excessive iron solion.
Concrete outcome is shown in Fig. 1, and when visible wavelength is 460nm, effect is best.
The plot step of test example 2 typical curve.
Preparation ammonium thiocyanate standard solution, its concentration is followed successively by 50g/L, 100g/L, 150g/L, 200g/L, 300g/L; Draw 1ml in 500mL volumetric flask, add excessive Fe
3+ with distilled water diluting to scale, then pipette the solution 1mL after dilution in 50mL volumetric flask, with distilled water diluting to scale, under 460nm wavelength, use 1cm cuvette, with FeCl
3 make reference liquid, read absorbance, and drawing standard curve;
Concrete outcome is shown in Fig. 2, is standard solution absorbance curve.
The testing procedure of certain concrete sample of test example 3 and method.
The sample fetched is shaken up, filters, draw 1ml filtrate in 500mL volumetric flask, add excessive Fe
3+ with distilled water diluting to scale, then pipette the solution 1mL after dilution in 50mL volumetric flask, with distilled water diluting to scale, under 460nm wavelength, use 1cm cuvette, with FeCl
3 make reference liquid, reading absorbance is 0.402.Thiocyanate content is calculated: 466.50*0.402+1.65=189.18g/L according to typical curve
Concrete analysis process of the present invention is as follows:
The sample fetched is shaken up, filters, draw 1ml filtrate in 500mL volumetric flask, add excessive Fe
3+ with distilled water diluting to scale, then pipette the solution 1mL after dilution in 50mL volumetric flask, with distilled water diluting to scale, under 460nm wavelength, use 1cm cuvette, with FeCl
3 make reference liquid, read absorbance.Thiocyanate content is calculated according to typical curve.
Claims (8)
1. a Thiocyanate ion method for quickly detecting in coking desulfurization liquid, comprises the steps:
(1) Thiocyanate ion concentration standard curve is drawn;
(2) content of the Thiocyanate ion in sample is measured.
2. Thiocyanate ion method for quickly detecting in coking desulfurization liquid according to claim 1, it is characterized in that, the method is according to CNS
-with Fe
3+ the principle of ionic reaction colour developing, adds excessive Fe in aqueous solution to be measured
3+ metallic ion, then uses the absorbance of 723 type spectrophotometers assaying reaction liquid under maximum absorption wavelength, then calculates molten sulfur cyanide ion content to be measured according to the absorption curve of standard solution.
3. Thiocyanate ion method for quickly detecting in coking desulfurization liquid according to claim 2, is characterized in that, described maximum absorption wavelength is 460nm.
4. Thiocyanate ion method for quickly detecting in coking desulfurization liquid according to claim 3, is characterized in that, according to the actual conditions of thiocyanate in coking desulfurization liquid, preparation ammonium thiocyanate standard solution, its concentration is followed successively by 50g/L, 100g/L, 150g/L, 200g/L, 300g/L; Draw 1ml in 500mL volumetric flask, add excessive Fe
3+ with distilled water diluting to scale, then pipette the solution 1mL after dilution in 50mL volumetric flask, with distilled water diluting to scale, under 460nm wavelength, use 1cm cuvette, with FeCl
3 make reference liquid, read absorbance, and drawing standard curve;
Regression equation is the corresponding coefficient R of C=466.50A+1.65
2=0.9997; Wherein, C represents ammonium thiocyanate concentration, and A represents absorbance, and R is related coefficient;
Shake up after fetching sample, filter, draw 1ml filtrate in 500mL volumetric flask, add excessive Fe
3+ with distilled water diluting to scale, then pipette the solution 1mL after dilution in 50mL volumetric flask, with distilled water diluting to scale, under 460nm wavelength, use 1cm cuvette, with FeCl
3 make reference liquid, read absorbance, calculate thiocyanate content according to typical curve.
5. Thiocyanate ion method for quickly detecting in coking desulfurization liquid according to claim 4, is characterized in that, described coking desulfurization liquid refers to the coke-oven gas that high-temperature coking produces, in purification process, and the absorbing liquid of desulfurization process.
6. Thiocyanate ion method for quickly detecting in coking desulfurization liquid according to claim 1, it is characterized in that, the method is applied to the inspection of Thiocyanate ion in analytical industry water.
7. Thiocyanate ion method for quickly detecting in coking desulfurization liquid according to claim 6, is characterized in that, described process water is iron and steel, coking, chemical industry process water.
8. Thiocyanate ion method for quickly detecting in coking desulfurization liquid according to claim 1, it is characterized in that, the method is applied to the inspection of normal life water Thiocyanate ion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510303798.1A CN104849273A (en) | 2015-06-04 | 2015-06-04 | Method for rapidly testing thiocyanate ions in coking desulfurization liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510303798.1A CN104849273A (en) | 2015-06-04 | 2015-06-04 | Method for rapidly testing thiocyanate ions in coking desulfurization liquid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104849273A true CN104849273A (en) | 2015-08-19 |
Family
ID=53849079
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510303798.1A Pending CN104849273A (en) | 2015-06-04 | 2015-06-04 | Method for rapidly testing thiocyanate ions in coking desulfurization liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104849273A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106483157A (en) * | 2016-10-09 | 2017-03-08 | 中国石油化工股份有限公司 | The determination method of total chlorine in a kind of doctor solution |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201382930Y (en) * | 2009-02-27 | 2010-01-13 | 陕西出入境检验检疫局检验检疫技术中心 | Rapid testing kit for sodium sulfocyanate in liquid milk |
| CN101825575A (en) * | 2009-03-06 | 2010-09-08 | 陕西出入境检验检疫局检验检疫技术中心 | Method for quickly detecting thiocyanate in liquid milk and detection test paper thereof |
| CN102608109A (en) * | 2012-03-03 | 2012-07-25 | 河北省科学院生物研究所 | Thiocyanate radical detecting kit and application thereof |
| CN103323412A (en) * | 2013-05-30 | 2013-09-25 | 攀钢集团江油长城特殊钢有限公司 | Thiocyanate spectrophotometry method for detecting iron content of high-temperature alloy |
| CN104406960A (en) * | 2014-10-30 | 2015-03-11 | 黑龙江省兽药饲料监察所 | Kit for rapid detection and quantification of thiocyanate radicals in raw fresh milk, and its application |
-
2015
- 2015-06-04 CN CN201510303798.1A patent/CN104849273A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201382930Y (en) * | 2009-02-27 | 2010-01-13 | 陕西出入境检验检疫局检验检疫技术中心 | Rapid testing kit for sodium sulfocyanate in liquid milk |
| CN101825575A (en) * | 2009-03-06 | 2010-09-08 | 陕西出入境检验检疫局检验检疫技术中心 | Method for quickly detecting thiocyanate in liquid milk and detection test paper thereof |
| CN102608109A (en) * | 2012-03-03 | 2012-07-25 | 河北省科学院生物研究所 | Thiocyanate radical detecting kit and application thereof |
| CN103323412A (en) * | 2013-05-30 | 2013-09-25 | 攀钢集团江油长城特殊钢有限公司 | Thiocyanate spectrophotometry method for detecting iron content of high-temperature alloy |
| CN104406960A (en) * | 2014-10-30 | 2015-03-11 | 黑龙江省兽药饲料监察所 | Kit for rapid detection and quantification of thiocyanate radicals in raw fresh milk, and its application |
Non-Patent Citations (1)
| Title |
|---|
| 潘霞霞等: "焦化废水中硫氰化物的快速检测方法", 《煤化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106483157A (en) * | 2016-10-09 | 2017-03-08 | 中国石油化工股份有限公司 | The determination method of total chlorine in a kind of doctor solution |
| CN106483157B (en) * | 2016-10-09 | 2021-12-28 | 中国石油化工股份有限公司 | Method for measuring total chlorine in desulfurization solution |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103048287B (en) | Sulfur ion measurement method based on gold nanoparticles as simulated peroxidase | |
| CN103364352B (en) | Method for rapid determination of sulphur ions with nanogold as logic gate color developing probe | |
| CN101614719B (en) | Method for measuring content of vanadium by potassium permanganate oxidation-ferrous ammonium sulphate titrating method | |
| CN103926300A (en) | Improved method for determining free chlorine ions in cement paste or mortar | |
| CN108318618A (en) | One kind being suitable for the high chlorine root sanitary sewage COD rapid detection methods of production platform | |
| CN103645186A (en) | Method for analyzing content of COD (chemical oxygen demand) in sewage with high chloride ion concentration | |
| CN104034683A (en) | Method for measuring chlorine content of vanadium battery electrolyte solution | |
| Jermak et al. | Headspace single‐drop microextraction with in‐drop derivatization and capillary electrophoretic determination for free cyanide analysis | |
| CN103712981A (en) | Method for detecting content of nitrogen in denitrified fly ash | |
| CN105203475A (en) | Method of determining chemical oxygen demand in chlorine-containing water sample | |
| CN101825579A (en) | Method for measuring concentration of polyacrylamide solution | |
| CN101839901A (en) | Digestion solution formula for fast determining chemical oxygen demand | |
| CN102768191B (en) | Method for easily detecting trace thallium in water | |
| CN102830116B (en) | Detection device and detection method for continuous flow of total cyanide in water | |
| CN110057896A (en) | The analysis method of content of fluoride in a kind of hazardous waste | |
| CN104849273A (en) | Method for rapidly testing thiocyanate ions in coking desulfurization liquid | |
| CN204649628U (en) | Reductive agent addition pick-up unit and analyser | |
| CN106546696A (en) | The analysis method of chloride content in a kind of sulfur Gas Fields output water | |
| CN105911009A (en) | Method for performing chemical oxygen demand testing by means of gaseous phase molecular absorption spectroscopy | |
| CN102175746B (en) | Analytical reagent and method for analyzing content of sulfuric acid and ferric irons | |
| CN102590317B (en) | PH composite electrode method for measuring content of nitrite ions in solution | |
| Urban | Colorimetry of sulphur anions: Part II A specific colorimetric method for the determination of trithionate | |
| JP2019113357A (en) | Analysis method and analysis device | |
| CN209014454U (en) | Flow Injection Analysis measures the device of volatile phenol in underground water | |
| KR101362110B1 (en) | A circular type analytical device for cyanide ion analysis |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150819 |