CN112345518B - Method for measuring thiocyanate in ferricyanide complex water quality in gold cyanidation process - Google Patents
Method for measuring thiocyanate in ferricyanide complex water quality in gold cyanidation process Download PDFInfo
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- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 title claims abstract description 113
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 title claims abstract description 111
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 38
- YAGKRVSRTSUGEY-UHFFFAOYSA-N ferricyanide Chemical compound [Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] YAGKRVSRTSUGEY-UHFFFAOYSA-N 0.000 title claims abstract description 16
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 16
- 239000010931 gold Substances 0.000 title claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 32
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 31
- 230000000873 masking effect Effects 0.000 claims abstract description 19
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 9
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 9
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 8
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 8
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 8
- 238000005259 measurement Methods 0.000 claims abstract description 8
- 239000000523 sample Substances 0.000 claims description 50
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 44
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 26
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 26
- 238000002835 absorbance Methods 0.000 claims description 22
- 239000000706 filtrate Substances 0.000 claims description 18
- PANJMBIFGCKWBY-UHFFFAOYSA-N iron tricyanide Chemical compound N#C[Fe](C#N)C#N PANJMBIFGCKWBY-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 12
- 239000012496 blank sample Substances 0.000 claims description 11
- 238000007865 diluting Methods 0.000 claims description 11
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 8
- 238000011088 calibration curve Methods 0.000 claims description 7
- 239000003153 chemical reaction reagent Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 239000012086 standard solution Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 abstract description 10
- 239000002351 wastewater Substances 0.000 abstract description 5
- 238000004737 colorimetric analysis Methods 0.000 abstract description 3
- 238000005562 fading Methods 0.000 abstract description 3
- 230000002378 acidificating effect Effects 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract 2
- 150000002505 iron Chemical class 0.000 abstract 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 abstract 1
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 abstract 1
- 239000012488 sample solution Substances 0.000 abstract 1
- 239000012085 test solution Substances 0.000 abstract 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000011084 recovery Methods 0.000 description 3
- 238000002798 spectrophotometry method Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000004811 liquid chromatography Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N2021/775—Indicator and selective membrane
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- Pathology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
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- General Physics & Mathematics (AREA)
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention relates to a method for measuring thiocyanate in ferricyanide complex water quality in a gold cyanidation process, and belongs to the technical field of thiocyanate measurement. The sample solution is regulated to be acidic, 0.1g of ferrous sulfate is added to form ferric ferrocyanide precipitate, the solution is regulated to be alkaline, 0.1g of zinc sulfate is added to flocculate the precipitate, the solution is heated and boiled for 20min, the solution is taken down to be cooled, the solution is taken down to a volumetric flask with a volume of 100mL, the solution is filtered in a dry mode, a proper volume of test solution is taken, and the thiocyanate content is measured by adopting an iron salt colorimetric method. Aiming at the water quality containing high-content ferricyanide complex, the invention successfully finds out a combined masking agent for masking the ferricyanide complex, and finds out an organic solvent which can inhibit the fading of thiocyanate, thereby solving the problem that the thiocyanate in the wastewater containing the ferricyanide complex can not be accurately measured.
Description
Technical Field
The invention belongs to the technical field of determination of thiocyanate in water quality, and particularly relates to an accurate determination method of thiocyanate in iron-cyanide-containing complex water quality in a gold cyanidation process.
Background
At present, 80% of gold yield in China is derived from gold cyanidation technology, in the cyanidation process, because the pyrite content in ores and gold ores is relatively high, a large amount of cyanide can react with iron and sulfur respectively to generate thiocyanate and ferricyanide complex in water quality after the cyanidation technology, the generation of the thiocyanate directly influences cyanidation efficiency in the technology, meanwhile, serious interference can be generated on cyanide determination in subsequent water quality innocuous treatment processes, and the thiocyanate in water is partially converted into cyanide due to the influence of oxidizing substances, so that great urgent demands are provided for accurate determination of the thiocyanate in enterprises or environmental supervision departments.
The existing measurement method of thiocyanate includes gas chromatography, liquid chromatography, spectrophotometry, etc.; the spectrophotometry is suitable for the sample with higher thiocyanate content, and the operation is simple, quick and accurate. However, most spectrophotometry uses ferric salt colorimetry. However, for the waste water which is produced by the gold cyanidation technology and contains thiocyanate and a large amount of ferricyanide complex, ferric salt added during the determination of the thiocyanate can firstly react with the ferricyanide complex contained in the waste water to produce ferricyanide blue precipitate and then convert ferricyanide, the precipitate granularity is extremely fine and cannot be filtered and removed, so that the content of the thiocyanate cannot be accurately determined, in addition, the ferric salt colorimetric method also has the defect of unstable color development, the color can fade quickly in a short time, and the high-content thiocyanate waste water cannot be accurately determined by adopting gas chromatography and liquid chromatography.
Disclosure of Invention
The invention provides a combined masking agent and a stabilizer to solve the interference problem of ferricyanide complex and the problem of unstable color development of thiocyanate.
The technical scheme adopted by the invention is that the method comprises the following steps:
step one, measuring volume V 1 Placing a water sample of 100mL thiocyanate in a 250mL beaker, adding hydrochloric acid to adjust the pH value to 3-5, adding 0.1g of masking agent 1, shaking uniformly, adding sodium hydroxide to adjust the pH value of a solution to 7-8, adding 0.1g of masking agent 2, heating and boiling for 20min, taking down and cooling, and fixing the volume to a 100mL volumetric flask;
step two, taking a 100mL beaker, filtering the solution by quantitative filter paper, and discarding the primary filtrate;
drawing a standard curve
Adding 0mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL of standard thiocyanate use solution into six 50mL colorimetric tubes with plugs, adding 5mL of ferric chloride color reagent into the six 50mL colorimetric tubes with plugs, adding 1mL of ethanol, diluting to mark lines with water, shaking uniformly, and placing in a dark place for 5 minutes for measurement, wherein the content of thiocyanate in the six 50mL colorimetric tubes with plugs is 0 mug, 50 mug, 100 mug, 200 mug, 300 mug and 500 mug respectively, and a standard curve of the quality of thiocyanate versus absorbance is drawn by taking the quality of thiocyanate as an abscissa and the absorbance as an ordinate;
step four, measuring the sample
The filtrate obtained in the step two with the volume V is put into a 50mL brown colorimetric tube, 5mL ferric chloride color developing agent is added, 1mL ethanol is added, the mixture is diluted to a marked line by water and is uniformly shaken, the mixture is placed in a dark place for color development for 5 minutes, a 10mm cuvette is used as a reference with a blank tube with zero concentration at the wavelength of 460nm, the absorbance is measured, and the content of thiocyanate is detected from a calibration curve;
step five, making a full-program blank along with the sample;
step six, calculating the concentration of thiocyanate in the water sample according to the following formula:
wherein: c, the concentration of thiocyanate in the water sample, mg/L;
m-check out the quality of thiocyanate and μg in water sample from standard curve
m 0 -determining the quality of thiocyanate in the blank sample, μg, from the standard curve;
v-the volume mL of the constant volume sample in the step one is separated and taken during color development.
In the first step of the invention, the volume ratio of hydrochloric acid is 1:1, a preparation method of hydrochloric acid: 25mL of concentrated hydrochloric acid with the concentration of 12mol/L is taken, 25mL of water is added, and the mixture is uniformly shaken;
in the first step of the invention, the concentration of sodium hydroxide is 2%, and the preparation method is to take 2g of sodium hydroxide to be dissolved in 100mL of water and shake uniformly.
In the first step of the invention, the masking agent 1 is: ferrous sulfate, analytically pure ferrous sulfate heptahydrate, masking agent 2 is: zinc sulfate, analytically pure.
In the second step of the invention, the small beaker is washed with deionized water and then dried.
In the third step of the invention, the preparation method of the ferric chloride color developing agent comprises the following steps: 50g of ferric chloride was weighed and dissolved in 500mL of water, 25mL of concentrated hydrochloric acid with a concentration of 12mol/L was added, and diluted with water to 1000mL.
In the third step of the invention, the standard thiocyanate use solution can be obtained by purchasing a commercially available standard solution, and the diluted solution with the concentration of 1.00mL contains CNS - 1.00mg of the solution was used as a standard.
The preparation method of the ferric chloride color developing agent in the fourth step comprises the following steps: 50g of ferric chloride was weighed and dissolved in 500mL of water, 25mL of concentrated hydrochloric acid with a concentration of 12mol/L was added, and diluted with water to 1000mL.
The invention has the beneficial effects that:
1. the invention solves the problem that a large amount of ferric cyanide precipitates are generated when a color developing agent is added during ferric salt color comparison, and the ferric cyanide precipitates are difficult to filter and remove because the ferric cyanide precipitates are thinner, and the ferric cyanide complex can be quickly formed into the ferrous cyanide precipitates by adding ferrous sulfate under the acidic condition, and then the precipitates are flocculated by adding zinc sulfate under the weak alkaline condition, so that large-granularity precipitates are formed and are easy to filter and remove.
2. Experiments show that part of thiocyanate can be adsorbed in the process of forming flocculation precipitation with zinc sulfate, the method avoids the adsorption of thiocyanate in a heating and boiling mode, and compared with the experiment, the flocculation precipitation can lose 20% when the thiocyanate is not heated, and the recovery rate of the thiocyanate can reach more than 99% after 20 minutes of heating.
3. The invention solves the problems of unstable color development and serious color fading in a short time by using a brown colorimetric tube and adding ethanol as a stabilizer, and overcomes the defect of obvious method.
4. The absorbance value at the time of color development is improved after ethanol is added.
Aiming at the water quality containing high-content ferricyanide complex, the invention successfully finds out a combined masking agent for masking the ferricyanide complex, and finds out an organic solvent which can inhibit the fading of thiocyanate, thereby solving the problem that the thiocyanate in the wastewater containing the ferricyanide complex can not be accurately measured.
Detailed Description
Example 1
Comprises the following steps:
step one, measuring volume V 1 Placing a water sample of 100mL thiocyanate in a 250mL beaker, adding hydrochloric acid to adjust the pH value to 3, adding 0.1g of masking agent 1, shaking uniformly, adding sodium hydroxide to adjust the pH value to 7, adding 0.1g of masking agent 2, heating and boiling for 20min, taking down and cooling, and fixing the volume to a 100mL volumetric flask;
step two, taking a 100mL beaker, filtering the solution by quantitative filter paper, and discarding the primary filtrate;
drawing a standard curve
Adding 0mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL of standard thiocyanate use solution into six 50mL colorimetric tubes with plugs, adding 5mL of ferric chloride color reagent into the six 50mL colorimetric tubes with plugs, adding 1mL of ethanol, diluting to mark lines with water, shaking uniformly, and placing in a dark place for 5 minutes for measurement, wherein the content of thiocyanate in the six 50mL colorimetric tubes with plugs is 0 mug, 50 mug, 100 mug, 200 mug, 300 mug and 500 mug respectively, and a standard curve of the quality of thiocyanate versus absorbance is drawn by taking the quality of thiocyanate as an abscissa and the absorbance as an ordinate;
step four, measuring the sample
Separating 10mL of filtrate from the second step, placing the filtrate into a 50mL brown color comparison tube, adding 5mL ferric chloride color developing agent, adding 1mL of ethanol, diluting with water to a marked line, shaking uniformly, placing the mixture in a dark place for developing for 5 minutes, using a 10mm cuvette at a wavelength of 460nm, taking a blank tube with zero concentration as a reference, measuring absorbance, finding out the thiocyanate content of 153.2 mug from a calibration curve, and measuring the mass m of the blank sample 0 2.00 μg;
step five, making a full-program blank along with the sample;
step six, calculating the concentration of thiocyanate in the water sample according to the following formula:
wherein: c, the concentration of thiocyanate in the water sample, mg/L;
m-checking the quality of thiocyanate in the water sample, mug according to a standard curve;
m 0 -determining the quality of thiocyanate in the blank sample, μg, from the standard curve;
v-dividing the volume mL of the constant volume sample in the first step during color development;
the calculated thiocyanate concentration was 15.1mg/L.
Example 2
Comprises the following steps:
step one, measuring volume V 1 Placing a water sample of 100mL thiocyanate in a 250mL beaker, adding hydrochloric acid to adjust the pH value to 5, adding 0.1g of ferrous sulfate, shaking uniformly, adding sodium hydroxide to adjust the pH value to 8, adding 0.1g of zinc sulfate, heating and boiling for 20min, taking down and cooling, and fixing the volume to a 100mL volumetric flask;
step two, taking a 100mL beaker, filtering the solution by quantitative filter paper, and discarding the primary filtrate;
drawing a standard curve
Adding 0mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL of standard thiocyanate use solution into six 50mL colorimetric tubes with plugs, adding 5mL of ferric chloride color reagent into the six 50mL colorimetric tubes with plugs, adding 1mL of ethanol, diluting to mark lines with water, shaking uniformly, and placing in a dark place for 5 minutes for measurement, wherein the content of thiocyanate in the six 50mL colorimetric tubes with plugs is 0 mug, 50 mug, 100 mug, 200 mug, 300 mug and 500 mug respectively, and a standard curve of the quality of thiocyanate versus absorbance is drawn by taking the quality of thiocyanate as an abscissa and the absorbance as an ordinate;
step four, measuring the sample
Separating filtrate in the second step with volume of 5mL, placing the filtrate in a 50mL brown colorimetric tube, adding 5mL ferric chloride color-developing agent, adding 1mL ethanol, diluting with water to mark line, shaking, placing in dark for color development for 5 min, using a 10mm cuvette at wavelength of 460nm, taking a blank tube with zero concentration as reference, measuring absorbance, finding out thiocyanate content of 325.5 μg from the calibration curve, and measuring mass m of the blank sample 0 2.00 μg;
step five, making a full-program blank along with the sample;
step six, calculating the concentration of thiocyanate in the water sample according to the following formula:
wherein: c, the concentration of thiocyanate in the water sample, mg/L;
m-checking the quality of thiocyanate in the water sample, mug according to a standard curve;
m 0 -determining the quality of thiocyanate in the blank sample, μg, from the standard curve;
v-dividing the volume mL of the constant volume sample in the first step during color development;
the concentration of thiocyanate was calculated to be 64.7mg/L.
Example 3
The method comprises the following steps:
step one, measuring volume V 1 Placing a water sample of 100mL thiocyanate in a 250mL beaker, adding hydrochloric acid to adjust the pH to 4, adding 0.1g of masking agent 1, shaking uniformly, adding sodium hydroxide to adjust the pH to 7.5, adding 0.1g of masking agent 2, heating and boiling for 20min, taking down and cooling, and fixing the volume to a 100mL volumetric flask;
step two, taking a 100mL beaker, filtering the solution by quantitative filter paper, and discarding the primary filtrate;
drawing a standard curve
Adding 0mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL of standard thiocyanate use solution into six 50mL colorimetric tubes with plugs, adding 5mL of ferric chloride color reagent into the six 50mL colorimetric tubes with plugs, adding 1mL of ethanol, diluting to mark lines with water, shaking uniformly, and placing in a dark place for 5 minutes for measurement, wherein the content of thiocyanate in the six 50mL colorimetric tubes with plugs is 0 mug, 50 mug, 100 mug, 200 mug, 300 mug and 500 mug respectively, and a standard curve of the quality of thiocyanate versus absorbance is drawn by taking the quality of thiocyanate as an abscissa and the absorbance as an ordinate;
step four, measuring the sample
The filtrate obtained in the step two with the volume V is put into a 50mL brown colorimetric tube, 5mL ferric chloride color developing agent is added, 1mL ethanol is added, the mixture is diluted to a marked line by water and is uniformly shaken, the mixture is placed in a dark place for color development for 5 minutes, a 10mm cuvette is used as a reference with a blank tube with zero concentration at the wavelength of 460nm, the absorbance is measured, and the content of thiocyanate is detected from a calibration curve;
step five, making a full-program blank along with the sample;
step six, calculating the concentration of thiocyanate in the water sample according to the following formula:
wherein: c, the concentration of thiocyanate in the water sample, mg/L;
m-checking the quality of thiocyanate in the water sample by a standard curve, ug;
m 0 -checking the quality of thiocyanate in the blank sample, ug, from the standard curve;
v-the volume mL of the constant volume sample in the step one is separated and taken during color development.
In the above examples 1 to 3:
in the first step, hydrochloric acid is in a volume ratio of 1:1, a preparation method of hydrochloric acid: 25mL of concentrated hydrochloric acid with the concentration of 12mol/L is taken, 25mL of water is added, and the mixture is uniformly shaken;
in the first step, the concentration of sodium hydroxide is 2%, and the preparation method is that 2g of sodium hydroxide is dissolved in 100mL of water and uniformly shaken;
in the first step, the masking agent 1 is: ferrous sulfate, analytically pure ferrous sulfate heptahydrate, masking agent 2 is: zinc sulfate, analytically pure.
In the second step, the beaker is washed by deionized water and then dried.
The preparation method of the ferric chloride color developing agent in the step three comprises the following steps: 50g of ferric chloride was weighed and dissolved in 500mL of water, 25mL of concentrated hydrochloric acid with a concentration of 12mol/L was added, and diluted with water to 1000mL.
In the third step, the standard thiocyanate use solution can be purchasedCommercially available standard solutions are available and have a concentration of CNS in 1.00mL of solution after dilution - 1.00mg of the solution was used as a standard.
The preparation method of the ferric chloride color developing agent in the step four comprises the following steps: 50g of ferric chloride was weighed and dissolved in 500mL of water, 25mL of concentrated hydrochloric acid with a concentration of 12mol/L was added, and diluted with water to 1000mL.
The invention is further illustrated by the following experimental examples.
Experimental example 1
Step one, measuring the sample volume V with the thiocyanate content of 15.1mg/L 1 100mL, placing in a 250mL beaker, adding 1.50mg of thiocyanate standard solution, adding hydrochloric acid to adjust the acidity to pH3, adding 0.1g of ferrous sulfate, shaking uniformly, adding sodium hydroxide to adjust the acidity of the solution to 7, adding 0.1g of zinc sulfate, heating and boiling for 20min, taking down and cooling, and fixing the volume to a 100mL volumetric flask;
step two, taking a 100mL beaker, filtering the solution by quantitative filter paper, and discarding the primary filtrate;
drawing a standard curve
Adding 0mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL of standard thiocyanate use solution into six 50mL colorimetric tubes with plugs, adding 5mL of ferric chloride color reagent into the six 50mL colorimetric tubes with plugs, adding 1mL of ethanol, diluting to mark lines with water, shaking uniformly, and placing in a dark place for 5 minutes for measurement, wherein the content of thiocyanate in the six 50mL colorimetric tubes with plugs is 0 mug, 50 mug, 100 mug, 200 mug, 300 mug and 500 mug respectively, and a standard curve of the quality of thiocyanate versus absorbance is drawn by taking the quality of thiocyanate as an abscissa and the absorbance as an ordinate;
step four, measuring the sample
Separating 10mL of filtrate from the second step, placing the filtrate into a 50mL brown color comparison tube, adding 5mL ferric chloride color developing agent, adding 1mL of ethanol, diluting with water to a marked line, shaking uniformly, placing the mixture in a dark place for developing for 5 minutes, using a 10mm cuvette at a wavelength of 460nm, taking a blank tube with zero concentration as a reference, measuring absorbance, finding out the thiocyanate content of 302.5 mug from a calibration curve, and measuring the mass m of the blank sample 0 2.00 μg;
step five, making a full-program blank along with the sample;
step six, calculating the concentration of thiocyanate in the water sample according to the following formula:
wherein: c, the concentration of thiocyanate in the water sample, mg/L;
m-checking the quality of thiocyanate in the water sample, mug according to a standard curve;
m 0 -determining the quality of thiocyanate in the blank sample, μg, from the standard curve;
v-dividing the volume mL of the constant volume sample in the first step during color development;
the calculated concentration of thiocyanate radical is 30.0mg/L, and the standard recovery rate is as follows: 99.33%.
Experimental example 2
Step one, measuring the sample volume V with the thiocyanate content of 64.7mg/L 1 100mL, placing in a 250mL beaker, adding 6.5mg of thiocyanate standard solution, adding hydrochloric acid to adjust the acidity to pH5, adding 0.1g of ferrous sulfate, shaking uniformly, adding sodium hydroxide to adjust the acidity of the solution to 8, adding 0.1g of zinc sulfate, heating and boiling for 20min, taking down and cooling, and fixing the volume to a 100mL volumetric flask;
step two, taking a 100mL beaker, filtering the solution by quantitative filter paper, and discarding the primary filtrate;
drawing a standard curve
Adding 0mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL of thiocyanate standard use solution into six 50mL brown color comparison tubes with plugs, adding 5mL of ferric chloride color reagent into the six 50mL color comparison tubes with plugs, adding 1mL of ethanol, diluting to the marked line with water, shaking uniformly, and placing in a dark place for 5 minutes for measurement, wherein the thiocyanate content in the six 50mL color comparison tubes with plugs is 0 mug; 50 μg;100 μg;200 μg;300 μg;500 μg, drawing a standard curve of thiocyanate mass to absorbance by taking thiocyanate mass as an abscissa and absorbance as an ordinate;
step four, measuring the sample
Separating 2mL of filtrate from the second step, placing the filtrate into a 50mL brown color comparison tube, adding 5mL ferric chloride color developing agent, adding 1mL of ethanol, diluting with water to a marked line, shaking uniformly, placing the mixture in a dark place for developing for 5 minutes, using a 10mm cuvette at a wavelength of 460nm, taking a blank tube with zero concentration as a reference, measuring absorbance, detecting that the thiocyanate content is 260.2 mug from a calibration curve, and measuring the mass m of the blank sample 0 2.00 μg;
step five, making a full-program blank along with the sample;
step six, calculating the concentration of thiocyanate in the water sample according to the following formula:
wherein: c, the concentration of thiocyanate in the water sample, mg/L;
m-checking the quality of thiocyanate in the water sample, mug according to a standard curve;
m 0 -determining the quality of thiocyanate in the blank sample, μg, from the standard curve;
v-dividing the volume mL of the constant volume sample in the first step during color development;
the calculated concentration of thiocyanate radical is 129.1mg/L, and the standard recovery rate is as follows: 99.08%.
Claims (8)
1. The method for measuring thiocyanate in the water containing the ferricyanide complex in the gold cyanidation process is characterized by comprising the following steps of:
step one, measuring volume V 1 Placing a water sample of 100mL thiocyanate in a 250mL beaker, adding hydrochloric acid to adjust the pH value to 3-5, adding 0.1g of masking agent 1, shaking uniformly, adding sodium hydroxide to adjust the pH value of a solution to 7-8, adding 0.1g of masking agent 2, heating and boiling for 20min, taking down and cooling, and fixing the volume to a 100mL volumetric flask;
step two, taking a 100mL beaker, filtering the solution by quantitative filter paper, and discarding the primary filtrate;
drawing a standard curve
Adding 0mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL of standard thiocyanate use solution into six 50mL colorimetric tubes with plugs, adding 5mL of ferric chloride color reagent into the six 50mL colorimetric tubes with plugs, adding 1mL of ethanol, diluting to mark lines with water, shaking uniformly, and placing in a dark place for 5 minutes for measurement, wherein the content of thiocyanate in the six 50mL colorimetric tubes with plugs is 0 mug, 50 mug, 100 mug, 200 mug, 300 mug and 500 mug respectively, and a standard curve of the quality of thiocyanate versus absorbance is drawn by taking the quality of thiocyanate as an abscissa and the absorbance as an ordinate;
step four, measuring the sample
The filtrate obtained in the step two with the volume V is put into a 50mL brown colorimetric tube, 5mL ferric chloride color developing agent is added, 1mL ethanol is added, the mixture is diluted to a marked line by water and is uniformly shaken, the mixture is placed in a dark place for color development for 5 minutes, a 10mm cuvette is used as a reference with a blank tube with zero concentration at the wavelength of 460nm, the absorbance is measured, and the content of thiocyanate is detected from a calibration curve;
step five, making a full-program blank along with the sample;
step six, calculating the concentration of thiocyanate in the water sample according to the following formula:
wherein: c, the concentration of thiocyanate in the water sample, mg/L;
m-check out the quality of thiocyanate and μg in water sample from standard curve
m 0 -determining the quality of thiocyanate in the blank sample, μg, from the standard curve;
v-the volume mL of the constant volume sample in the step one is separated and taken during color development.
2. The method for determining thiocyanate in water containing iron cyanide complex in gold cyanidation process according to claim 1, wherein the method comprises the following steps: in the first step, hydrochloric acid is in a volume ratio of 1:1, a preparation method of hydrochloric acid: 25mL of concentrated hydrochloric acid with the concentration of 12mol/L is taken, 25mL of water is added, and the mixture is shaken well.
3. The method for determining thiocyanate in water containing iron cyanide complex in gold cyanidation process according to claim 1, wherein the method comprises the following steps: in the first step, the concentration of sodium hydroxide is 2%, and the preparation method is to take 2g of sodium hydroxide to dissolve in 100mL of water and shake uniformly.
4. The method for determining thiocyanate in water containing iron cyanide complex in gold cyanidation process according to claim 1, wherein the method comprises the following steps: in the first step, the masking agent 1 is: ferrous sulfate, analytically pure ferrous sulfate heptahydrate, masking agent 2 is: zinc sulfate, analytically pure.
5. The method for determining thiocyanate in water containing iron cyanide complex in gold cyanidation process according to claim 1, wherein the method comprises the following steps: in the second step, the beaker is washed by deionized water and then dried.
6. The method for determining thiocyanate in water containing iron cyanide complex in gold cyanidation process according to claim 1, wherein the method comprises the following steps: in the third step, the preparation method of the ferric chloride color developing agent comprises the following steps: 50g of ferric chloride was weighed and dissolved in 500mL of water, 25mL of concentrated hydrochloric acid with a concentration of 12mol/L was added, and diluted with water to 1000mL.
7. The method for determining thiocyanate in water containing iron cyanide complex in gold cyanidation process according to claim 1, wherein the method comprises the following steps: in the third step, the standard thiocyanate use solution can be obtained by purchasing a commercially available standard solution, and the diluted solution with the concentration of 1.00mL contains CNS - 1.00mg of the solution was used as a standard.
8. The method for determining thiocyanate in water containing iron cyanide complex in gold cyanidation process according to claim 1, wherein the method comprises the following steps: the preparation method of the ferric chloride color developing agent in the step four comprises the following steps: 50g of ferric chloride was weighed and dissolved in 500mL of water, 25mL of concentrated hydrochloric acid with a concentration of 12mol/L was added, and diluted with water to 1000mL.
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