CN112285270A - Method for determining total cyanide in water containing hydrogen peroxide - Google Patents
Method for determining total cyanide in water containing hydrogen peroxide Download PDFInfo
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- CN112285270A CN112285270A CN202010928074.7A CN202010928074A CN112285270A CN 112285270 A CN112285270 A CN 112285270A CN 202010928074 A CN202010928074 A CN 202010928074A CN 112285270 A CN112285270 A CN 112285270A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
Abstract
The invention belongs to the technical field of cyanide determination, and particularly relates to a method for determining total cyanide in hydrogen peroxide-containing water; the interference of hydrogen peroxide on results is eliminated in a skillful manner by using a combined masking agent, wherein the masking agent combines manganese dioxide and copper chloride, the manganese dioxide is used as a catalyst to decompose excessive hydrogen peroxide in a sample, the copper chloride can accelerate the catalytic effect of the manganese dioxide and shorten the reaction time, and the manganese dioxide is not dissolved under an alkaline condition, so that the manganese dioxide can be repeatedly used; the second masking agent is silver nitrate, and because chloride ions are introduced into the sample, the interference is removed by using the silver nitrate, and meanwhile, the interference of sulfides and thiocyanate contained in the sample can be masked by the silver nitrate; and the third masking agent is EDTA, and because copper ions are introduced to influence the determination result, the EDTA is added to mask the interference of the copper ions, so that the problem of low determination result in the determination process of the total cyanide containing hydrogen peroxide is solved, and the content of the total cyanide in the sample is accurately determined.
Description
Technical Field
The invention belongs to the technical field of cyanide determination, and particularly relates to a method for determining total cyanide in hydrogen peroxide-containing water.
Background
Cyanide-containing water is ubiquitous in many enterprises, cyanide belongs to a highly toxic substance, and accurate detection of cyanide is very important, for example, in a gold production process, a cyaniding gold leaching process is one of very important means, while water in the cyaniding gold leaching process contains higher total cyanide, hydrogen peroxide is usually used when cyanide is treated, and the hydrogen peroxide is usually used in an excessive amount, so that the water contains excessive hydrogen peroxide, and the hydrogen peroxide reacts with the cyanide in a distillation process to enable the total cyanide measurement result to be lower, and the influence of the hydrogen peroxide is not considered in the existing standards and documents.
Disclosure of Invention
In order to overcome the problems, the invention provides a method for measuring total cyanide in water containing hydrogen peroxide, which solves the problem of low measurement result when the total cyanide in the water containing hydrogen peroxide is measured by adding a masking agent.
A method for measuring total cyanide in water containing hydrogen peroxide comprises the following steps:
step one, measuring a sample with the volume V of 200mL, transferring the sample into a 250mL beaker, and adding Na into the beaker if the pH value of the sample is less than 72CO3Adjusting the pH of the solution to between 8 and 8.5, and adding 1mL of Na to the beaker2CO3Adding hydrochloric acid into the beaker to adjust the pH value to 8-8.5 if the pH value of the sample is more than 10, and adding 1mL of Na into the beaker2CO3Adding 0.2g of manganese dioxide and 1mL of copper chloride solution into the beaker, covering the surface dish, and standing for 40 minutes;
step two, filtering the solution, transferring the filtrate into a distillation flask, washing the precipitate and filter paper for 2 times respectively, transferring all washing liquid into the distillation flask, sequentially adding glass beads into the distillation flask, 10mL of silver nitrate solution with the concentration of 0.100mol/L and 10mL of EDTA-2Na solution with the concentration of 100g/L are shaken up and kept still for 10min, then 10-15 mL of EDTA-2Na solution with the concentration of 100g/L and 15-20 mL of phosphoric acid solution with the mass concentration of more than or equal to 85% are added into a distillation flask, the distillation flask is evenly shaken up, the distillation flask is connected with a distillation device, a 100mL receiving tube is taken, 10mL of 40g/L sodium hydroxide solution is added into the receiving tube to be used as absorption liquid, the upper end of a distillate guide pipe is connected with the outlet of a condensation tube, the lower end of the distillate guide pipe is inserted into the absorption liquid of the receiving tube, the connection part is checked and is tight, and distillation is started;
stopping distillation when the volume of the solution in the receiving pipe is 80-85mL, flushing the distillate guide pipe with water, adding the flushing liquid into the receiving pipe, and taking down the receiving pipe;
adding water into the receiving pipe, diluting to a scale, and shaking up to obtain an alkaline sample A to be detected, wherein the volume is recorded as V1；
Fifthly, making a full procedure blank along with the sample to obtain an alkaline blank sample B to be detected;
step six, determination of sample
The volume of the fraction is V2Placing the alkaline sample A to be detected in a conical flask, adding 0.2mL of a silver test reagent indicator into the conical flask, shaking uniformly, titrating with a silver nitrate standard solution under continuous rotary shaking until the solution is changed from yellow to orange red, and recording the volume of the consumed silver nitrate standard solution as Va；
Step seven, calculating the mass concentration of the total cyanide in the sample according to the following formula, wherein the mass concentration is calculated by cyanide ions:
in the formula: rho1-mass concentration of total cyanide, mg/L;
c is the molar concentration of the silver nitrate standard solution, mol/L;
Vathe amount of the silver nitrate standard solution is mL when the sample is titrated;
V0titrating the amount of the silver nitrate standard solution in the blank test, wherein the amount is mL;
v-volume of sample, mL;
V1obtaining the volume, mL, of the alkaline sample A to be detected;
V2the volume of the alkaline sample A to be detected is divided into mL;
26.02-molar mass of cyanide ions, g/mol.
Na used in the first step2CO3The solution concentration is 100g/L, and the preparation method comprises the following steps: weighing 10.0g of sodium carbonate, dissolving in water, diluting to 100mL, and shaking up.
The concentration of the copper chloride solution used in the first step is 10g/L, and the preparation method comprises the following steps: weighing 1.00g of copper chloride, dissolving in water, diluting to 100mL, and shaking up.
The preparation method of the silver nitrate solution with the concentration of 0.100mol/L in the second step comprises the following steps: 16.987g of analytically pure silver nitrate is weighed, dissolved in water, diluted to a constant volume of 1000mL, shaken up and stored in a brown reagent bottle.
The preparation method of the EDTA-2Na solution with the concentration of 100g/L in the second step comprises the following steps: 10.0g of disodium ethylenediamine tetraacetate is weighed and dissolved in water, diluted to 100mL and shaken up.
The preparation method of the sodium hydroxide solution with the concentration of 40g/L used in the step two comprises the following steps: 40g of sodium hydroxide is weighed, dissolved in water, diluted to 1000mL, shaken up and stored in a polyethylene plastic container.
The concentration of the silver nitrate standard solution used in the sixth step is 0.01mol/L, and the preparation method comprises the following steps: weighing 1.6987g of reference silver nitrate, dissolving in water, diluting to a constant volume of 1000mL, shaking up, and storing in a brown reagent bottle;
the preparation method of the Yinling indicator comprises the following steps: 0.02g of p-dimethylaminobenzylidene rhodanine is dissolved in acetone, diluted to 100mL with acetone, stored in a brown bottle and stabilized in the dark for one month before use.
The invention has the beneficial effects that:
the method selects a reasonable mode, and solves the problem of low measurement result in the measurement process of the total cyanide in the water containing hydrogen peroxide; the interference of hydrogen peroxide is eliminated, and the total cyanide content in the sample is accurately determined. The interference of hydrogen peroxide on a result is eliminated in a skillful mode of using a combined masking agent, wherein the masking agent is composed of manganese dioxide and copper chloride, the manganese dioxide is insoluble under an alkaline condition, the manganese dioxide can be repeatedly used as a catalyst to eliminate the interference of hydrogen peroxide in a sample, and the masking agent is silver nitrate. And the third masking agent is EDTA, and because the introduced copper ions have influence on the measurement result, the EDTA is added to mask the interference of the copper ions.
Detailed Description
A method for measuring total cyanide in water containing hydrogen peroxide comprises the following steps:
step one, a sample with the volume V of 200mL is measured by using a measuring cylinder and transferred into a 250mL beaker, and Na is added into the beaker if the pH value of the sample is less than 72CO3Adjusting the pH of the solution to between 8 and 8.5, and adding 1mL of Na to the beaker2CO3Adding hydrochloric acid into the beaker to adjust the pH value to 8-8.5 if the pH value of the sample is more than 10, and adding 1mL of Na into the beaker2CO3Adding 0.2g of manganese dioxide and 1mL of copper chloride solution into the beaker, covering the surface dish, and standing for 40 minutes;
step two, transferring the filtered solution into a distillation flask, washing the precipitate and filter paper for 2 times respectively, transferring all washing liquid into the distillation flask, sequentially adding glass beads into the distillation flask, 10mL of silver nitrate solution with the concentration of 0.100mol/L and 10mL of EDTA-2Na solution with the concentration of 100g/L are shaken up and kept still for 10min, then 10-15 mL of EDTA-2Na solution with the concentration of 100g/L and 15-20 mL of phosphoric acid solution with the mass concentration of more than or equal to 85% are added into a distillation flask, the distillation flask is evenly shaken up, the distillation flask is connected with a distillation device, a 100mL receiving tube is taken, 10mL of 40g/L sodium hydroxide solution is added into the receiving tube to be used as absorption liquid, the upper end of a distillate guide pipe is connected with the outlet of a condensation tube, the lower end of the distillate guide pipe is inserted into the absorption liquid of the receiving tube, the connection part is checked and is tight, and distillation is started;
stopping distillation when the volume of the solution in the receiving pipe is 80-85mL, flushing the distillate guide pipe with water, adding the flushing liquid into the receiving pipe, and taking down the receiving pipe;
adding water into the receiving pipe, diluting to a scale, and shaking up to obtain an alkaline sample A to be detected, wherein the volume is recorded as V1；
Fifthly, making a full procedure blank along with the sample to obtain an alkaline blank sample B to be detected;
step six, determination of sample
The volume of the fraction is V2Placing the alkaline sample A to be detected in a conical flask, adding 0.2mL of a silver test reagent indicator into the conical flask, shaking uniformly, titrating with a silver nitrate standard solution under continuous rotary shaking until the solution is changed from yellow to orange red, and recording the volume of the consumed silver nitrate standard solution as Va；
Step seven, calculating the mass concentration of the total cyanide in the sample according to the following formula, wherein the mass concentration is calculated by cyanide ions:
in the formula: rho1-mass concentration of total cyanide, mg/L;
c is the molar concentration of the silver nitrate standard solution, mol/L;
Vathe amount of the silver nitrate standard solution is mL when the sample is titrated;
V0titrating the amount of the silver nitrate standard solution in the blank test, wherein the amount is mL;
v-volume of sample, mL;
V1obtaining the volume, mL, of the alkaline sample A to be detected;
V2the volume of the alkaline sample A to be detected is divided into mL;
26.02-molar mass of cyanide ions, g/mol.
Na used in the first step2CO3The solution concentration is 100g/L, and the preparation method comprises the following steps: weighing 10.0g of sodium carbonate, dissolving in water, diluting to 100mL, and shaking up.
The volume ratio of hydrochloric acid to water in the hydrochloric acid used in the first step is 1:2, and the preparation method comprises the following steps: 25mL of concentrated hydrochloric acid with the mass fraction of more than 20% is measured, diluted by distilled water and added into a 50mL colorimetric tube, and the mixture is shaken up.
The concentration of the copper chloride solution used in the first step is 10g/L, and the preparation method comprises the following steps: weighing 1.00g of copper chloride, dissolving in water, diluting to 100mL, and shaking up.
The preparation method of the silver nitrate solution with the concentration of 0.100mol/L in the second step comprises the following steps: 16.987g of analytically pure silver nitrate is weighed, dissolved in water, diluted to a constant volume of 1000mL, shaken up and stored in a brown reagent bottle.
The preparation method of the EDTA-2Na solution with the concentration of 100g/L in the second step comprises the following steps: 10.0g of disodium ethylenediamine tetraacetate is weighed and dissolved in water, diluted to 100mL and shaken up.
The preparation method of the sodium hydroxide solution with the concentration of 40g/L used in the step two comprises the following steps: 40g of sodium hydroxide is weighed, dissolved in water, diluted to 1000mL, shaken up and stored in a polyethylene plastic container.
The concentration of the silver nitrate standard solution used in the sixth step is 0.01mol/L, and the preparation method comprises the following steps: weighing 1.6987g of reference silver nitrate, dissolving in water, diluting to a constant volume of 1000mL, shaking up, and storing in a brown reagent bottle;
the preparation method of the Yinling indicator comprises the following steps: 0.02g of p-dimethylaminobenzylidene rhodanine is dissolved in acetone, diluted to 100mL with acetone, stored in a brown bottle and stabilized in the dark for one month before use.
Example 1
The method for determining the total cyanide in the water containing hydrogen peroxide is operated according to the method, wherein the volume V is extracted in the sixth step2Putting 100mL of an alkaline sample A to be detected into an erlenmeyer flask, adding 0.2mL of a silver test reagent into the erlenmeyer flask, shaking uniformly, titrating with a silver nitrate standard solution under continuous rotary shaking until the solution changes from yellow to orange red, and recording a reading Va5.00mL, and calculating the mass concentration of total cyanide in the sample:
the total cyanide mass concentration in the sample was calculated to be 12.9 mg/L.
Example 2
Total cyanidation in water containing hydrogen peroxideThe method of measuring the substance is carried out as described above, wherein in step six the volume V is taken2Putting 100mL of an alkaline sample A to be detected into an erlenmeyer flask, adding 0.2mL of a silver test reagent into the erlenmeyer flask, shaking uniformly, titrating with a silver nitrate standard solution under continuous rotary shaking until the solution changes from yellow to orange red, and recording a reading Va12.05mL, and calculating the mass concentration of total cyanide in the sample:
the calculated total cyanide mass concentration in the sample was 31.2 mg/L.
Experimental example 1
The sample of example 1 was subjected to the standard addition recovery test by adding 27.44mg of potassium ferricyanide (containing 13mg of cyanide ion) to 1L of the sample of example 1, mixing them, and taking 200ml of the mixture as a sample to conduct the standard addition recovery test according to the above method, wherein the volume V was taken in the sixth step2Putting 100mL of an alkaline sample A to be detected into an erlenmeyer flask, adding 0.2mL of a silver test reagent into the erlenmeyer flask, shaking uniformly, titrating with a silver nitrate standard solution under continuous rotary shaking until the solution changes from yellow to orange red, and recording a reading Va9.95mL, and the mass concentration of total cyanide in the sample was calculated:
the calculated total cyanide mass concentration in the sample was 25.8mg/L, and the recovery rate of the spiked standard was 99.2%.
Experimental example 2
The sample in example 2 was subjected to the spiking recovery test, wherein sample 1L of example 2 was subjected to cyanation and mixing with 66.48mg of potassium ferricyanide (containing 31.5mg of cyanide ion), 200ml of the mixture was used as a sample to conduct the spiking recovery test according to the above method, wherein volume V was taken in step six2100mL of the alkaline sample A to be tested is placed in an erlenmeyer flask, 0.2mL of the reagent silver is added into the erlenmeyer flask, and the erlenmeyer flask is shakenHomogenizing, continuously shaking, titrating with silver nitrate standard solution until the solution changes from yellow to orange red, and recording reading Va9.95mL, and the mass concentration of total cyanide in the sample was calculated:
the calculated total cyanide mass concentration in the sample was 62.7mg/L, and the recovery rate of the spiked standard was 100.0%.
The recovery rate of the added standard reaches more than 99 percent, and the method is proved to be accurate and feasible.
Claims (7)
1. A method for measuring total cyanide in water containing hydrogen peroxide is characterized by comprising the following steps:
step one, measuring a sample with the volume V of 200mL, transferring the sample into a 250mL beaker, and adding Na into the beaker if the pH value of the sample is less than 72CO3Adjusting the pH of the solution to between 8 and 8.5, and adding 1mL of Na to the beaker2CO3Adding hydrochloric acid into the beaker to adjust the pH value to 8-8.5 if the pH value of the sample is more than 10, and adding 1mL of Na into the beaker2CO3Adding 0.2g of manganese dioxide and 1mL of copper chloride solution into the beaker, covering the surface dish, and standing for 40 minutes;
step two, filtering the solution, transferring the filtrate into a distillation flask, washing the precipitate and filter paper for 2 times respectively, transferring all washing liquid into the distillation flask, sequentially adding glass beads into the distillation flask, 10mL of silver nitrate solution with the concentration of 0.100mol/L and 10mL of EDTA-2Na solution with the concentration of 100g/L are shaken up and kept still for 10min, then 10-15 mL of EDTA-2Na solution with the concentration of 100g/L and 15-20 mL of phosphoric acid solution with the mass concentration of more than or equal to 85% are added into a distillation flask, the distillation flask is evenly shaken up, the distillation flask is connected with a distillation device, a 100mL receiving tube is taken, 10mL of 40g/L sodium hydroxide solution is added into the receiving tube to be used as absorption liquid, the upper end of a distillate guide pipe is connected with the outlet of a condensation tube, the lower end of the distillate guide pipe is inserted into the absorption liquid of the receiving tube, the connection part is checked and is tight, and distillation is started;
stopping distillation when the volume of the solution in the receiving pipe is 80-85mL, flushing the distillate guide pipe with water, adding the flushing liquid into the receiving pipe, and taking down the receiving pipe;
adding water into the receiving pipe, diluting to a scale, and shaking up to obtain an alkaline sample A to be detected, wherein the volume is recorded as V1；
Fifthly, making a full procedure blank along with the sample to obtain an alkaline blank sample B to be detected;
step six, determination of sample
The volume of the fraction is V2Placing the alkaline sample A to be detected in a conical flask, adding 0.2mL of a silver test reagent indicator into the conical flask, shaking uniformly, titrating with a silver nitrate standard solution under continuous rotary shaking until the solution is changed from yellow to orange red, and recording the volume of the consumed silver nitrate standard solution as Va；
Step seven, calculating the mass concentration of the total cyanide in the sample according to the following formula, wherein the mass concentration is calculated by cyanide ions:
in the formula: rho1-mass concentration of total cyanide, mg/L;
c is the molar concentration of the silver nitrate standard solution, mol/L;
Vathe amount of the silver nitrate standard solution is mL when the sample is titrated;
V0titrating the amount of the silver nitrate standard solution in the blank test, wherein the amount is mL;
v-volume of sample, mL;
V1obtaining the volume, mL, of the alkaline sample A to be detected;
V2the volume of the alkaline sample A to be detected is divided into mL;
26.02-molar mass of cyanide ions, g/mol.
2. The method according to claim 1 for treating an aqueous medium containing hydrogen peroxideMethod for determining cyanide, characterized in that Na is used in the first step2CO3The solution concentration is 100g/L, and the preparation method comprises the following steps: weighing 10.0g of sodium carbonate, dissolving in water, diluting to 100mL, and shaking up.
3. The method for determining total cyanide in water containing hydrogen peroxide as claimed in claim 2, wherein the concentration of the copper chloride solution used in the first step is 10g/L, and the preparation method comprises: weighing 1.00g of copper chloride, dissolving in water, diluting to 100mL, and shaking up.
4. The method for determining total cyanide in an aqueous solution containing hydrogen peroxide according to claim 3, wherein the silver nitrate solution with a concentration of 0.100mol/L in the second step is prepared by the following method: 16.987g of analytically pure silver nitrate is weighed, dissolved in water, diluted to a constant volume of 1000mL, shaken up and stored in a brown reagent bottle.
5. The method for determining total cyanide in water containing hydrogen peroxide according to claim 4, wherein the preparation method of EDTA-2Na solution with concentration of 100g/L in the second step comprises: 10.0g of disodium ethylenediamine tetraacetate is weighed and dissolved in water, diluted to 100mL and shaken up.
6. The method for determining total cyanide in an aqueous solution containing hydrogen peroxide according to claim 5, wherein the sodium hydroxide solution with a concentration of 40g/L used in the second step is prepared by the following steps: 40g of sodium hydroxide is weighed, dissolved in water, diluted to 1000mL, shaken up and stored in a polyethylene plastic container.
7. The method for determining total cyanide in water containing hydrogen peroxide as claimed in claim 6, wherein the silver nitrate standard solution used in the sixth step has a concentration of 0.01mol/L, and the preparation method comprises: weighing 1.6987g of reference silver nitrate, dissolving in water, diluting to a constant volume of 1000mL, shaking up, and storing in a brown reagent bottle;
the preparation method of the Yinling indicator comprises the following steps: 0.02g of p-dimethylaminobenzylidene rhodanine is dissolved in acetone, diluted to 100mL with acetone, stored in a brown bottle and stabilized in the dark for one month before use.
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