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
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- 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
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- 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
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000004939 coking Methods 0.000 title claims abstract description 26
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 title claims abstract description 15
- -1 thiocyanate ions Chemical class 0.000 title claims abstract description 10
- 239000007788 liquid Substances 0.000 title claims description 25
- 238000006477 desulfuration reaction Methods 0.000 title claims description 18
- 230000023556 desulfurization Effects 0.000 title claims description 18
- 238000012360 testing method Methods 0.000 title abstract description 7
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000002835 absorbance Methods 0.000 claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 11
- 239000012086 standard solution Substances 0.000 claims abstract description 9
- 238000010521 absorption reaction Methods 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 5
- 239000010959 steel Substances 0.000 claims abstract description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 22
- 238000007865 diluting Methods 0.000 claims description 14
- 239000012153 distilled water Substances 0.000 claims description 14
- 238000007689 inspection Methods 0.000 claims description 13
- 238000010790 dilution Methods 0.000 claims description 7
- 239000012895 dilution Substances 0.000 claims description 7
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- RFMQOHXWHFHOJF-UHFFFAOYSA-N cyano thiocyanate Chemical compound N#CSC#N RFMQOHXWHFHOJF-UHFFFAOYSA-N 0.000 claims description 2
- 150000001455 metallic ions Chemical class 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 7
- 239000003814 drug Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 4
- 231100000331 toxic Toxicity 0.000 abstract description 4
- 230000002588 toxic effect Effects 0.000 abstract description 4
- ATDGTVJJHBUTRL-UHFFFAOYSA-N cyanogen bromide Chemical compound BrC#N ATDGTVJJHBUTRL-UHFFFAOYSA-N 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- JGJLWPGRMCADHB-UHFFFAOYSA-N hypobromite Inorganic materials Br[O-] JGJLWPGRMCADHB-UHFFFAOYSA-N 0.000 abstract description 3
- 229940079593 drug Drugs 0.000 abstract description 2
- 229910021645 metal ion Inorganic materials 0.000 abstract 2
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 239000008235 industrial water Substances 0.000 abstract 1
- 230000031700 light absorption Effects 0.000 abstract 1
- 231100000167 toxic agent Toxicity 0.000 abstract 1
- 239000003440 toxic substance Substances 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000013459 approach Methods 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000001473 noxious effect Effects 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 230000004308 accommodation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000012956 testing procedure Methods 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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 |
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|---|---|---|---|
| CN201510303798.1A CN104849273A (en) | 2015-06-04 | 2015-06-04 | Method for rapidly testing thiocyanate ions in coking desulfurization liquid |
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| CN104849273A true CN104849273A (en) | 2015-08-19 |
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| CN201510303798.1A Pending CN104849273A (en) | 2015-06-04 | 2015-06-04 | Method for rapidly testing thiocyanate ions in coking desulfurization liquid |
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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 |
| CN112782107A (en) * | 2020-12-25 | 2021-05-11 | 河北旭阳能源有限公司 | Method for determining ammonium thiocyanate in desulfurization solution |
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| 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 |
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2015
- 2015-06-04 CN CN201510303798.1A patent/CN104849273A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| 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 |
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| 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 (3)
| 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 |
| CN112782107A (en) * | 2020-12-25 | 2021-05-11 | 河北旭阳能源有限公司 | Method for determining ammonium thiocyanate in desulfurization solution |
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Application publication date: 20150819 |