CN110672540A - Method for determining hexavalent chromium in solid waste - Google Patents
Method for determining hexavalent chromium in solid waste Download PDFInfo
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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
- 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
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
The invention belongs to the technical field of determination of inorganic metal elements in solid waste, and particularly relates to a method for determining hexavalent chromium in solid waste; aiming at the problems that the measurement result of hexavalent chromium in the existing solid waste is low and the test method has defects, an ultrasonic-heating-refluxing method is adopted, so that the problems that the hexavalent chromium in the solid waste cannot be completely leached, a polyethylene film is easy to break in the heating process, the measurement of the hexavalent chromium by a sodium salt atom absorption method is unstable, oxygen-enriched flame is difficult to control and the like are solved, and the content of the hexavalent chromium in the solid waste can be accurately measured.
Description
Technical Field
The invention belongs to the technical field of determination of inorganic metal elements in solid waste, and particularly relates to a method for determining hexavalent chromium in solid waste.
Background
Hexavalent chromium has strong toxicity, generally considered 100 times higher than trivalent chromium and is easily absorbed by the human body, and is recognized as a carcinogen due to its oxidative property and high permeability to the skin, which results in great toxicity. The hexavalent chromium-containing solid waste mainly comes from the fields of fur tanning, product processing, ferroalloy smelting, processing of chromium-containing ores and the like, and the hexavalent chromium in the chromium-containing solid waste is not treated after being stacked for a long time, so that the hexavalent chromium in the solid waste is dissolved in water through rain and enters surface water or permeates into the ground, water sources and soil are polluted, farmlands are damaged, and people, livestock and other organisms are damaged. Therefore, an accurate analysis method for hexavalent chromium in the solid waste is imperative, and a powerful data guarantee is provided for harmless, quantitative reduction and resource treatment of the solid waste. The existing method HJ687-2014 has the defects that the operability is poor, the method adopts a heating and stirring method for leaching and cannot completely leach, a polyethylene film is adopted for sealing in the stirring process, the polyethylene film is easy to break in the heating process, the loss of hexavalent chromium is caused, an atomic absorption method is adopted for measuring a sample, and the atomic absorption is unstable due to the fact that a large amount of sodium salt is added into a leaching solution, and oxygen-enriched flame is needed to be difficult to control.
Disclosure of Invention
Aiming at the problems that the existing solid waste is low in hexavalent chromium measurement result and the test method has defects, the invention adopts an ultrasonic-heating-refluxing method to solve the problems that hexavalent chromium in the solid waste cannot be completely leached, a polyethylene film is easy to break in the heating process, the measurement of the hexavalent chromium in the solid waste is unstable by a sodium salt atomic absorption method, oxygen-enriched flame is difficult to control and the like, and the content of the hexavalent chromium in the solid waste can be accurately measured.
A method for determining hexavalent chromium in solid waste comprises the following steps:
step one, weighing a solid waste sample containing hexavalent chromium with the mass of 1.50g-2.00g, placing the solid waste sample into a reflux bottle, adding 50.0ml of alkaline extraction solution into the reflux bottle, and shaking up;
continuously adding 850mg of magnesium chloride hexahydrate and 0.5ml of dipotassium hydrogen phosphate-potassium dihydrogen phosphate buffer solution into the reflux bottle, and shaking up;
inserting a return pipe into the return bottle, putting the return pipe into an ultrasonic machine, starting the ultrasonic machine to carry out ultrasonic treatment for 120 minutes, and simultaneously starting the heating function of the ultrasonic machine, wherein the heating temperature is 98 +/-2 ℃, and the ultrasonic power is more than or equal to 500W;
and step four, after the ultrasonic treatment is finished, taking down the reflux bottle from the ultrasonic machine, cooling to room temperature, filtering the liquid in the reflux bottle, putting the filtrate into a 250ml conical flask, adjusting the pH value of the filtrate in the conical flask to 4.5 +/-0.5 by using concentrated sulfuric acid, transferring the solution in the conical flask into a 100ml volumetric flask, adding water to fix the volume to the marked line, shaking up, to be detected, recording the solution with the fixed volume as a sample A, and recording the volume as V0；
Step five, measuring a sample:
drawing of standard curve
Adding 0.20ml, 0.50ml, 1.00ml, 2.00ml, 4.00ml, 6.00ml, 8.00ml and 10.0ml of chromium standard use solution into eight 50m1 colorimetric tubes respectively, adding water to dilute the solutions to a marked line, adding 0.5m1 sulfuric acid (1+1) and 0.5ml phosphoric acid (1+1) into each colorimetric tube respectively, shaking the solutions evenly, adding 2ml of color developing agent into each colorimetric tube, shaking the solutions evenly, after 5-10min, using a 10 or 30mm cuvette, using water as a reference to determine absorbance at a wavelength of 540nm of a spectrophotometer, and drawing a standard curve of hexavalent chromium concentration to absorbance by using hexavalent chromium concentration as a horizontal coordinate and using absorbance as a vertical coordinate;
determination of samples
Placing a sample A with the volume V in a new 50m1 colorimetric tube, diluting the sample A to a marked line by using water, adding 0.5m1 sulfuric acid (1+1) and 0.5ml phosphoric acid (1+1) into the colorimetric tube, shaking uniformly, adding 2ml of color developing agent into the colorimetric tube, shaking uniformly, measuring absorbance at the wavelength of 540nm of a spectrophotometer by using a 10 or 30mm cuvette and using water as a reference after 5-10min, and finding out the concentration C of hexavalent chromium in the sample A from a standard curve;
step six, making a full-program blank along with the sample to obtain a blank sample B, and measuring the concentration C of the blank sample B with the volume V0；
Step seven, calculating the content of hexavalent chromium in the solid waste according to the following formula:
in the formula: w is the content of hexavalent chromium, mg/kg;
c is the concentration of hexavalent chromium in the sample A, mg/L;
C0concentration of hexavalent chromium in sample B, mg/L
50-volume of cuvette, mL;
v is the volume of the aliquot A, mL;
V0total volume of sample a, mL;
m-mass of hexavalent chromium-containing solid waste sample, g.
And in the fourth step, if a precipitate is generated in the process of adjusting the pH value, filtering the solution in the conical flask after the pH value of the filtrate in the conical flask reaches 4.5 +/-0.5, and transferring the filtered solution into a 100ml volumetric flask.
The preparation method of the alkaline extraction solution in the first step comprises the following steps: 20g of sodium hydroxide and 30g of sodium carbonate are weighed and dissolved in water, and water is added for dilution to reach the constant volume of 1L, and the solution is stored in a polyethylene bottle.
The preparation method of the dipotassium hydrogen phosphate-monopotassium phosphate buffer solution in the second step comprises the following steps: 87.1g of dipotassium hydrogen phosphate and 68.0g of monopotassium phosphate are weighed and dissolved in water, and water is added for dilution to reach the volume of 1L.
In the fifth step, firstly preparing a chromium standard stock solution: 0.2829 +/-0.0001 g of potassium dichromate dried for 2 hours at 110 ℃ is weighed, dissolved by water, transferred into a volumetric flask of 1000ml, diluted by water to a marked line and shaken up, and the solution contains 0.1mg of hexavalent chromium;
the preparation method of the chromium standard use solution comprises the following steps: sucking 5.00ml of chromium standard stock solution, placing the stock solution in a 500ml volumetric flask, diluting the stock solution with water to a marked line, shaking up, and preparing the stock solution when the stock solution is used, wherein 1ug of hexavalent chromium is contained in 1ml of chromium standard use solution;
the color developing agent is prepared by the following steps: 0.2g of diphenylcarbodihydrazide is weighed, dissolved in 50m of 1 acetone, diluted to l00ml by adding water, shaken up and stored in a brown bottle to be prepared as required.
The invention has the beneficial effects that:
1. firstly, the reflux bottle filled with the sample is heated and ultrasonically treated, so that the granularity of the sample becomes smaller, the solubility of the sample is increased, the specific surface area of the sample is increased, hexavalent chromium is easier to release, and all hexavalent chromium can be released from solid waste.
2. The reflux method is adopted, so that the loss of hexavalent chromium is avoided, and the defects of the polyethylene film are overcome.
3. The method is more stable than atomic absorption method.
Detailed Description
A method for determining hexavalent chromium in solid waste comprises the following steps:
step one, weighing a solid waste sample containing hexavalent chromium with the mass of 1.50g-2.00g by using a balance, placing the solid waste sample into a reflux bottle, adding 50.0ml of alkaline extraction solution into the reflux bottle, and shaking up;
continuously adding 850mg of magnesium chloride hexahydrate and 0.5ml of dipotassium hydrogen phosphate-potassium dihydrogen phosphate buffer solution into the reflux bottle, and shaking up;
inserting a return pipe into the return bottle, putting the return pipe into an ultrasonic machine, starting the ultrasonic machine to carry out ultrasonic treatment for 120 minutes, and simultaneously starting the heating function of the ultrasonic machine, wherein the heating temperature is 98 +/-2 ℃, and the ultrasonic power is more than or equal to 500W;
step four, after the ultrasound is finished, taking down the reflux bottle from the ultrasonic machine, cooling to room temperature, filtering the liquid in the reflux bottle by using filter paper, putting the filtrate into a 250ml conical flask, adjusting the pH value of the filtrate in the conical flask to 4.5 +/-0.5 by using concentrated sulfuric acid, transferring the solution in the conical flask into a 100ml volumetric flask, fixing the volume to the marked line by using water, shaking up, measuring, and performing ultrasonic analysis on the volume to obtain the liquidThe volume of the solution was designated as sample A and volume as V0；
Step five, measuring a sample:
drawing of standard curve
Adding 0.20ml, 0.50ml, 1.00ml, 2.00ml, 4.00ml, 6.00ml, 8.00ml and 10.0ml of chromium standard use solution into eight 50m1 colorimetric tubes respectively, adding water to dilute the solutions to a marked line, adding 0.5m1 sulfuric acid (1+1) and 0.5ml phosphoric acid (1+1) into each colorimetric tube respectively, shaking the solutions evenly, adding 2ml of color developing agent into each colorimetric tube, shaking the solutions evenly, after 5-10min, using a 10 or 30mm cuvette, using water as a reference to determine absorbance at a wavelength of 540nm of a spectrophotometer, and drawing a standard curve of hexavalent chromium concentration to absorbance by using hexavalent chromium concentration as a horizontal coordinate and using absorbance as a vertical coordinate;
determination of samples
Placing a sample A with the volume V in a new 50m1 colorimetric tube, diluting the sample A to a marked line by using water, adding 0.5m1 sulfuric acid (1+1) and 0.5ml phosphoric acid (1+1) into the colorimetric tube, shaking uniformly, adding 2ml of color developing agent into the colorimetric tube, shaking uniformly, measuring absorbance at the wavelength of 540nm of a spectrophotometer by using a 10 or 30mm cuvette and using water as a reference after 5-10min, and finding out the concentration C of hexavalent chromium in the sample A from a standard curve;
step six, making a full-program blank along with the sample to obtain a blank sample B, and measuring the concentration C of the blank sample B with the volume V0；
Step seven, calculating the content of hexavalent chromium in the solid waste according to the following formula:
in the formula: w is the content of hexavalent chromium, mg/kg;
c is the concentration of hexavalent chromium in the sample A, mg/L;
C0concentration of hexavalent chromium in sample B, mg/L
50-volume of cuvette, mL;
v is the volume of the aliquot A, mL;
V0total volume of sample a, mL;
m-mass of hexavalent chromium-containing solid waste sample, g.
And in the fourth step, if a precipitate is generated in the process of regulating the pH value, filtering the solution in the conical flask after the pH value of the filtrate in the conical flask reaches 4.5 +/-0.5, filtering the precipitate and throwing away, and transferring the filtered solution into a 100ml volumetric flask.
The preparation method of the alkaline extraction solution in the first step comprises the following steps: 20g of sodium hydroxide and 30g of sodium carbonate are weighed and dissolved in water, and water is added for dilution to reach the constant volume of 1L, and the solution is stored in a polyethylene bottle.
The preparation method of the dipotassium hydrogen phosphate-monopotassium phosphate buffer solution with the pH value of 7 in the second step comprises the following steps: 87.1g of dipotassium hydrogen phosphate and 68.0g of monopotassium phosphate are weighed and dissolved in water, and water is added for dilution to reach the volume of 1L.
In the fifth step, firstly preparing a chromium standard stock solution: weighing potassium dichromate (K) dried at 110 deg.C for 2 hr2Cr2O7Guaranteed reagent) 0.2829 +/-0.0001 g, dissolved in water, transferred into a volumetric flask of 1000ml, diluted by adding water to the marked line, shaken evenly, and the lml solution contains 0.1mg of hexavalent chromium;
the preparation method of the chromium standard use solution comprises the following steps: sucking 5.00ml of chromium standard stock solution, placing the stock solution in a 500ml volumetric flask, diluting the stock solution with water to a marked line, shaking up, and preparing the stock solution when the stock solution is used, wherein 1ug of hexavalent chromium is contained in 1ml of chromium standard use solution;
the preparation method of the used sulfuric acid (1+1) comprises the following steps: sulfuric acid (H)2SO4p is 1.849g/ml, superior pure) is slowly added into water with the same volume and evenly mixed;
the preparation method of the used phosphoric acid (1+1) comprises the following steps: phosphoric acid (H)3P04P ═ 1.699g/m1, guaranteed purity) was mixed with water in equal volume;
the color developing agent is prepared by the following steps: 0.2g of diphenylcarbodihydrazide is weighed, dissolved in 50m of 1 acetone, diluted to l00ml by adding water, shaken up and stored in a brown bottle to be prepared as required.
Example 1
The solid waste containing hexavalent chromium with the mass of 1.50g is measured by the method, and the result calculation specifically comprises the following steps:
the hexavalent chromium content of the solid waste was calculated to be 2.60 mg/kg.
Example 2
The solid waste containing hexavalent chromium with the mass of 1.75g is measured by the method, and the result calculation specifically comprises the following steps:
the hexavalent chromium content of the solid waste was calculated to be 11.5 mg/kg.
Example 3
2.00g of hexavalent chromium-containing solid waste is measured by the method, and the result calculation specifically comprises the following steps:
the hexavalent chromium content of the solid waste was calculated to be 48.5 mg/kg.
Experimental example 1
At present, the state does not have a standard sample of the hexavalent chromium-containing solid waste, and the method adopts a standard recovery rate adding method to verify the accuracy.
A balance weight is used to take 1.50g of the hexavalent chromium-containing solid waste used in the example 1 into a reflux bottle, 4.00mL of a liquid hexavalent chromium standard sample with the concentration of 1.00mg/L is added into the reflux bottle, the measurement is carried out according to the method, and the result is specifically calculated as follows:
calculating to obtain the hexavalent chromium content of 5.20mg/kg, wherein the standard addition recovery rate is as follows: 97.50%, demonstrating that the method has very good accuracy.
Experimental example 2
A balance weight is used to take 1.75g of the hexavalent chromium-containing solid waste used in the example 2 into a reflux bottle, 2.00mL of a liquid hexavalent chromium standard sample with the concentration of 10.00mg/L is added into the reflux bottle, the measurement is carried out according to the method, and the result is specifically calculated as follows:
calculating to obtain the hexavalent chromium content of 22.7mg/kg, wherein the standard addition recovery rate is as follows: 98.00%, demonstrating that the method has very good accuracy.
Claims (5)
1. A method for determining hexavalent chromium in solid waste is characterized by comprising the following steps:
step one, weighing a solid waste sample containing hexavalent chromium with the mass of 1.50g-2.00g, placing the solid waste sample into a reflux bottle, adding 50.0ml of alkaline extraction solution into the reflux bottle, and shaking up;
continuously adding 850mg of magnesium chloride hexahydrate and 0.5ml of dipotassium hydrogen phosphate-potassium dihydrogen phosphate buffer solution into the reflux bottle, and shaking up;
inserting a return pipe into the return bottle, putting the return pipe into an ultrasonic machine, starting the ultrasonic machine to carry out ultrasonic treatment for 120 minutes, and simultaneously starting the heating function of the ultrasonic machine, wherein the heating temperature is 98 +/-2 ℃, and the ultrasonic power is more than or equal to 500W;
and step four, after the ultrasonic treatment is finished, taking down the reflux bottle from the ultrasonic machine, cooling to room temperature, filtering the liquid in the reflux bottle, putting the filtrate into a 250ml conical flask, adjusting the pH value of the filtrate in the conical flask to 4.5 +/-0.5 by using concentrated sulfuric acid, transferring the solution in the conical flask into a 100ml volumetric flask, adding water to fix the volume to the marked line, shaking up, to be detected, recording the solution with the fixed volume as a sample A, and recording the volume as V0；
Step five, measuring a sample:
drawing of standard curve
Adding 0.20ml, 0.50ml, 1.00ml, 2.00ml, 4.00ml, 6.00ml, 8.00ml and 10.0ml of chromium standard use solution into eight 50m1 colorimetric tubes respectively, adding water to dilute the solutions to a marked line, adding 0.5m1 sulfuric acid (1+1) and 0.5ml phosphoric acid (1+1) into each colorimetric tube respectively, shaking the solutions evenly, adding 2ml of color developing agent into each colorimetric tube, shaking the solutions evenly, after 5-10min, using a 10 or 30mm cuvette, using water as a reference to determine absorbance at a wavelength of 540nm of a spectrophotometer, and drawing a standard curve of hexavalent chromium concentration to absorbance by using hexavalent chromium concentration as a horizontal coordinate and using absorbance as a vertical coordinate;
determination of samples
Placing a sample A with the volume V in a new 50m1 colorimetric tube, diluting the sample A to a marked line by using water, adding 0.5m1 sulfuric acid (1+1) and 0.5ml phosphoric acid (1+1) into the colorimetric tube, shaking uniformly, adding 2ml of color developing agent into the colorimetric tube, shaking uniformly, measuring absorbance at the wavelength of 540nm of a spectrophotometer by using a 10 or 30mm cuvette and using water as a reference after 5-10min, and finding out the concentration C of hexavalent chromium in the sample A from a standard curve;
step six, making a full-program blank along with the sample to obtain a blank sample B, and measuring the concentration C of the blank sample B with the volume V0；
Step seven, calculating the content of hexavalent chromium in the solid waste according to the following formula:
in the formula: w is the content of hexavalent chromium, mg/kg;
c is the concentration of hexavalent chromium in the sample A, mg/L;
C0concentration of hexavalent chromium in sample B, mg/L
50-volume of cuvette, mL;
v is the volume of the aliquot A, mL;
V0total volume of sample a, mL;
m-mass of hexavalent chromium-containing solid waste sample, g.
2. The method for measuring hexavalent chromium in solid waste according to claim 1, wherein the pH adjustment in the fourth step is performed while a precipitate is generated, after the pH of the filtrate in the erlenmeyer flask reaches 4.5 ± 0.5, the solution in the erlenmeyer flask is filtered, and the filtered solution is transferred to a 100ml volumetric flask.
3. The method for determining hexavalent chromium in the solid waste according to claim 2, wherein the alkaline extraction solution of the first step is prepared by: 20g of sodium hydroxide and 30g of sodium carbonate are weighed and dissolved in water, and water is added for dilution to reach the constant volume of 1L, and the solution is stored in a polyethylene bottle.
4. The method for measuring hexavalent chromium in the solid waste according to claim 3, wherein the dipotassium hydrogen phosphate-potassium dihydrogen phosphate buffer solution in the second step is prepared by: 87.1g of dipotassium hydrogen phosphate and 68.0g of monopotassium phosphate are weighed and dissolved in water, and water is added for dilution to reach the volume of 1L.
5. The method for determining hexavalent chromium in the solid waste according to claim 4, wherein said step five comprises preparing a chromium standard stock solution: 0.2829 +/-0.0001 g of potassium dichromate dried for 2 hours at 110 ℃ is weighed, dissolved by water, transferred into a volumetric flask of 1000ml, diluted by water to a marked line and shaken up, and the solution contains 0.1mg of hexavalent chromium;
the preparation method of the chromium standard use solution comprises the following steps: sucking 5.00ml of chromium standard stock solution, placing the stock solution in a 500ml volumetric flask, diluting the stock solution with water to a marked line, shaking up, and preparing the stock solution when the stock solution is used, wherein 1ug of hexavalent chromium is contained in 1ml of chromium standard use solution;
the color developing agent is prepared by the following steps: 0.2g of diphenylcarbodihydrazide is weighed, dissolved in 50m of 1 acetone, diluted to l00ml by adding water, shaken up and stored in a brown bottle to be prepared as required.
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