CN111077091B - Method for detecting hexavalent chromium in soil - Google Patents
Method for detecting hexavalent chromium in soil Download PDFInfo
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- CN111077091B CN111077091B CN201911292178.7A CN201911292178A CN111077091B CN 111077091 B CN111077091 B CN 111077091B CN 201911292178 A CN201911292178 A CN 201911292178A CN 111077091 B CN111077091 B CN 111077091B
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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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
Abstract
The invention belongs to the technical field of hexavalent chromium detection methods, and particularly relates to a method for detecting the content of hexavalent chromium in soil. The method can be used for detecting hexavalent chromium in soil samples containing a large amount of reducing agents after pretreatment such as ventilation, heating and the like, does not oxidize trivalent chromium by using reducing agents based on an iron oxide system and a sulfur system, and can keep an oxidation environment to inhibit reduction reaction under a certain air flow; therefore, the interference of the reducing agent on the alkali digestion result is reduced, the dissolved hexavalent chromium is protected to the maximum extent, and the concentration of the hexavalent chromium in the solution is rapidly and accurately measured. The invention provides Cr6+The detection method has the advantages of simple and convenient operation, rapid detection and low cost, is suitable for the restoration acceptance detection of the chromium-polluted site, and has wide application value.
Description
Technical Field
The invention belongs to the technical field of hexavalent chromium detection methods, and particularly relates to a method for detecting the content of hexavalent chromium in soil.
Background
The heavy metal pollution sources of soil pollution are wide, unreasonable discharge of three wastes in the industries of mineral processing and smelting, electroplating, batteries, chemical engineering, dyes and the like, and heavy metal pollution of soil can be caused by sewage irrigation, sludge fertilization, automobile exhaust emission in urban transportation, improper electronic waste treatment and the like. Soil heavy metal pollution has the characteristics of poor mobility, long detention time, irreversible capacity and the like of pollutants in soil, causes soil fertility reduction, reduces crop yield and quality, and pollutes underground water and surface water through runoff and leaching effects.
Among the chemical contaminants, chromium is one of the most common and most hazardous contaminants. With the rapid development of industries such as metal processing, leather, electroplating, ferrochromium smelting, refractory materials, chemical engineering and the like and the continuous application of chromium chemical substances, a large amount of chromium slag is generated in each link of mining, using, processing, abandoning and the like. Most of the chromium slag is piled in the open and is soaked by rain and snow, and the chromium is dissolved in water and then permeates into soil and underground water, thereby causing the problems of soil chromium pollution and the like all over the world. The chromium in the soil exists in two valence states of Cr (III) and Cr (VI), the trivalent chromium has low toxicity, the hexavalent chromium has extremely strong toxicity, is easy to migrate and is easy to dissolve in water, the trivalent chromium is one of recognized carcinogens, the harm to the health of human is great, the adsorption capacity of the soil to the hexavalent chromium is only 8.5-36.2%, and therefore, the hexavalent chromium is mainly considered to be repaired in the chromium-polluted soil repairing treatment. At present, the chromium-polluted soil remediation approaches mainly comprise two approaches: the chromium is thoroughly removed from the soil, and the hexavalent chromium is reduced to trivalent chromium, so that the toxicity and the migration capability in the environment are reduced. The main repairing technology comprises a leaching method, a soil changing method, a biological repairing method, a chemical reduction method, a stabilization solidification method, an electric repairing method and the like.
At present, risk management and control or repair treatment projects are already completed or are being developed in partial plots, and the most adopted technical route is 'soil excavation-reduction stabilization treatment-in-situ blocking landfill or off-site construction landfill site landfill'. In order to ensure that the restoration effect reaches the standard, an excessive reducing agent is usually added into the chromium-polluted soil for restoration treatment. However, the excessive reducing agent will react with hexavalent chromium released from the soil lattice in the alkali digestion procedure of soil pretreatment, resulting in inaccurate detection results of subsequent analysis. The current various detection methods are difficult to be applied to such samples, and the engineering acceptance accuracy related to such fields is also interfered.
Therefore, the method for quickly, timely and simply eliminating the interference of the excessive reducing agent has important application value in the field of acceptance of soil remediation engineering.
Disclosure of Invention
In order to overcome the technical problems, the invention provides a hexavalent chromium detection method, which can eliminate the interference of excessive reducing agents, and has short determination time and high accuracy.
In order to achieve the above purpose, the technical scheme provided by the invention is as follows:
a detection method of hexavalent chromium ions comprises the following steps:
(1) taking a soil sample, and placing the soil sample in a container;
(2) placing the sample in a heating device, and introducing air;
(3) heating and maintaining the temperature to obtain pretreated soil;
(4) adding MgCl into the pretreated soil2Adding alkali solution into potassium dihydrogen phosphate buffer solution,carrying out alkali digestion and dissolution, heating and solid-liquid separation;
(5) measuring Cr in liquid phase obtained by solid-liquid separation according to diphenylcarbodihydrazide spectrophotometry6+Calculating the total Cr in the soil sample6+Mass m of (2).
Preferably, in the step (1), the soil is flattened, thin and uniform; preferably, the soil in step (1) is soil containing a reducing agent, wherein the reducing agent comprises at least one of sodium sulfite, ferrous sulfate, sodium sulfide and calcium polysulfide;
preferably, in the step (2), the flow rate of the air is 3-8L/min, preferably 6L/min;
preferably, in the step (3), the heating temperature is 80-120 ℃, preferably 100 ℃;
preferably, in the step (3), the heating rate is 8-12 ℃/min, preferably 10 ℃/min.
Preferably, in the step (3), the heat preservation time is 36-72 h;
preferably, in step (4), the MgCl is used2The adding amount of (A) is 0.1-0.3 times, preferably 0.16 times of the soil mass;
preferably, in the step (4), the addition amount of the potassium dihydrogen phosphate buffer solution is 0.2-1ml/g soil, and preferably 0.2ml/g soil;
preferably, in the step (4), the alkali solution is a mixed solution of sodium hydroxide and sodium carbonate, and the pH value of the mixed solution is 12-13;
preferably, the addition amount of the alkali solution is 15-30ml/g soil, preferably 20ml/g soil;
preferably, in the step (4), the heating temperature is 90-95 ℃, and the heating time is 40-60 min; preferably, the specific operation process of step (5) is as follows: adding a sulfuric acid solution after the liquid phase obtained by solid-liquid separation is subjected to constant volume, adjusting the pH value, adding an acetone solution of diphenylcarbonyldihydrazide, developing, performing constant volume, and measuring the absorbance value; with Cr2O7 2-Drawing a standard curve for the standard substance, substituting the absorbance value to obtain the total Cr in the sample6+Mass m of (a);
preferably, in step (5), the pH is 1.5-2.5.
Compared with the prior art, the invention has the technical advantages that:
(1) the invention provides a method for detecting hexavalent chromium in a soil sample containing a large amount of reducing agents, which uses reducing agents based on ferric oxide and sulfur, does not oxidize trivalent chromium, can maintain an oxidation environment under a certain air flow and inhibit the occurrence of reduction reaction; therefore, the interference of the reducing agent on the alkali digestion result is reduced, the dissolved hexavalent chromium is protected to the maximum extent, the concentration of the hexavalent chromium in the solution can be rapidly and accurately measured through a dibenzoyl dihydrazide spectrophotometry, and the accurate concentration of the hexavalent chromium in the soil sample is obtained.
(2) The invention provides Cr6+The detection method has the advantages of simple and convenient operation, rapid detection and low cost, is suitable for the restoration acceptance detection of the chromium-polluted site, and has wide application value.
Detailed Description
The present invention is described in further detail below with reference to examples, which are intended to facilitate the understanding of the present invention without limiting it in any way.
Example 1
A detection method of hexavalent chromium ions comprises the following steps:
(1) taking 2.5g of a soil sample reduced by ferrous sulfate, placing the soil sample in a 4cm by 6cm porcelain boat, and uniformly paving the soil;
(2) placing the sample in a tube furnace, and introducing air at the flow rate of 6L/min;
(3) heating to 100 ℃ at the heating rate of 10 ℃/min, and preserving heat for 72 hours to obtain the pretreated soil;
(4) 0.4g of MgCl was added to the pretreated soil20.5ml of potassium dihydrogen phosphate buffer solution, 50ml of NaOH and Na having a pH of 12 were added2CO3Carrying out alkali digestion and dissolution on the formed mixed alkali solution, heating to 95 ℃ for 60min, and carrying out solid-liquid separation;
(5) adding sulfuric acid solution after the liquid phase obtained by solid-liquid separation is subjected to constant volume, adjusting the pH value to 2,adding acetone solution of diphenyl carbodihydrazide, developing, fixing volume, and measuring absorbance value; with Cr2O7 2-Drawing a standard curve for the standard substance, substituting the absorbance value to obtain the total Cr in the sample6+m。
Example 2
A detection method of hexavalent chromium ions comprises the following steps:
(1) taking 2.5g of a soil sample reduced by calcium polysulfide, placing the soil sample in a 4cm by 6cm porcelain boat, and uniformly paving the soil;
(2) placing the sample in a tube furnace, and introducing air at the flow rate of 6L/min;
(3) heating to 100 ℃ at the heating rate of 10 ℃/min, and preserving heat for 72 hours to obtain the pretreated soil;
(4) the pretreated soil was placed in 200ml and 0.4g of MgCl was added20.5ml of potassium dihydrogen phosphate buffer solution, 50ml of NaOH and Na having a pH of 12 were added2CO3Carrying out alkali digestion and dissolution on the formed mixed alkali solution, heating to 90 ℃ for 60min, and carrying out solid-liquid separation;
(5) adding a sulfuric acid solution after the liquid phase obtained by solid-liquid separation is subjected to constant volume, adjusting the pH value to 2, adding an acetone solution of diphenylcarbodihydrazide, developing, performing constant volume, and measuring the absorbance value; with Cr2O7 2-Drawing a standard curve for the standard substance, substituting the absorbance value to obtain the total Cr in the sample6+m。
Example 3
A detection method of hexavalent chromium ions comprises the following steps:
(1) taking 2.5g of a soil sample reduced by sodium sulfide, placing the soil sample in a 4cm by 6cm porcelain boat, and uniformly paving the soil;
(2) placing the sample in a tube furnace, and introducing air at the flow rate of 6L/min;
(3) heating to 100 ℃ at the heating rate of 10 ℃/min, and preserving heat for 72 hours to obtain the pretreated soil;
(4) the pretreated soil was placed in 200ml and 0.4g of MgCl was added20.5ml of potassium dihydrogen phosphate buffer solution, 50ml of pH 12 composed of NaOH and Na2CO3Carrying out alkali digestion and dissolution on the formed mixed alkali solution, heating to 90 ℃ for 60min, and carrying out solid-liquid separation;
(5) adding a sulfuric acid solution after the liquid phase obtained by solid-liquid separation is subjected to constant volume, adjusting the pH value to 2, adding an acetone solution of diphenylcarbodihydrazide, developing, performing constant volume, and measuring the absorbance value; with Cr2O7 2-Drawing a standard curve for the standard substance, substituting the absorbance value to obtain the total Cr in the sample6+m。
Example 4
A detection method of hexavalent chromium ions comprises the following steps:
(1) taking 2.5g of a soil sample reduced by sodium sulfite, placing the soil sample in a 4cm by 6cm porcelain boat, and uniformly paving the soil;
(2) placing the sample in a tube furnace, and introducing air at the flow rate of 6L/min;
(3) heating to 100 ℃ at the heating rate of 10 ℃/min, and preserving heat for 72 hours to obtain the pretreated soil;
(4) the pretreated soil was placed in 200ml and 0.4g of MgCl was added20.5ml of potassium dihydrogen phosphate buffer solution, 50ml of NaOH and Na having a pH of 12 were added2CO3Carrying out alkali digestion and dissolution on the formed mixed alkali solution, heating to 90 ℃ for 60min, and carrying out solid-liquid separation;
(5) adding a sulfuric acid solution after the liquid phase obtained by solid-liquid separation is subjected to constant volume, adjusting the pH value to 2, adding an acetone solution of diphenylcarbodihydrazide, developing, performing constant volume, and measuring the absorbance value; with Cr2O7 2-Drawing a standard curve for the standard substance, substituting the absorbance value to obtain the total Cr in the sample6+m。
Example 5
A detection method of hexavalent chromium ions comprises the following steps:
(1) taking 2.5g of a soil sample reduced by ferrous sulfate, placing the soil sample in a 4cm by 6cm porcelain boat, and uniformly paving the soil;
(2) placing the sample in a tube furnace, and introducing air at the flow rate of 3L/min;
(3) heating to 80 ℃ at the heating rate of 8 ℃/min, and preserving heat for 36 hours to obtain the pretreated soil;
(4) 0.25g of MgCl was added to the pretreated soil20.5ml of potassium dihydrogen phosphate buffer solution, 37.5ml of a pH 12 solution of NaOH and Na2CO3Carrying out alkali digestion and dissolution on the formed mixed alkali solution, heating to 95 ℃ for 40min, and carrying out solid-liquid separation;
(5) adding a sulfuric acid solution after the liquid phase obtained by solid-liquid separation is subjected to constant volume, adjusting the pH value to 1.5, adding an acetone solution of diphenylcarbodihydrazide, developing, performing constant volume, and measuring the absorbance value; with Cr2O7 2-Drawing a standard curve for the standard substance, substituting the absorbance value to obtain the total Cr in the sample6+m。
Example 6
A detection method of hexavalent chromium ions comprises the following steps:
(1) taking 2.5g of a soil sample reduced by calcium polysulfide, placing the soil sample in a 4cm by 6cm porcelain boat, and uniformly paving the soil;
(2) placing the sample in a tube furnace, and introducing air at the flow rate of 8L/min;
(3) heating to 120 ℃ at the heating rate of 12 ℃/min, and preserving heat for 72 hours to obtain the pretreated soil;
(4) the pretreated soil was placed in 200ml and 0.75g of MgCl was added22.5ml of potassium dihydrogen phosphate buffer solution, 75ml of NaOH and Na having a pH of 13 were added2CO3Carrying out alkali digestion and dissolution on the formed mixed alkali solution, heating to 90 ℃ for 50min, and carrying out solid-liquid separation;
(5) adding a sulfuric acid solution after the liquid phase obtained by solid-liquid separation is subjected to constant volume, adjusting the pH value to 2.5, adding an acetone solution of diphenylcarbodihydrazide, developing, performing constant volume, and measuring the absorbance value; with Cr2O7 2-Drawing a standard curve for the standard substance, substituting the absorbance value to obtain the total Cr in the sample6+m。
Comparative example 1
The air flow rate was different compared to example 1.
A detection method of hexavalent chromium ions comprises the following steps:
(1) taking 2.5g of a soil sample reduced by ferrous sulfate, placing the soil sample in a 4cm by 6cm porcelain boat, and uniformly paving the soil;
(2) placing the sample in a tube furnace, and introducing air at the flow rate of 12L/min;
(3) - (5) same as in example 1.
Comparative example 2
The temperature rise rate was different from that of example 1.
A detection method of hexavalent chromium ions comprises the following steps:
(1) taking 2.5g of a soil sample reduced by ferrous sulfate, placing the soil sample in a 4cm by 6cm porcelain boat, and uniformly paving the soil;
(2) placing the sample in a tube furnace, and introducing air at the flow rate of 6L/min;
(3) heating to 100 ℃ at a heating rate of 15 ℃/min, and preserving heat for 72 hours to obtain the pretreated soil;
(4) - (5) same as in example 1.
Comparative example 3
The heating temperature in step (3) was different from that in example 1.
A detection method of hexavalent chromium ions comprises the following steps:
(1) taking 2.5g of a soil sample reduced by ferrous sulfate, placing the soil sample in a 4cm by 6cm porcelain boat, and uniformly paving the soil;
(2) placing the sample in a tube furnace, and introducing air at the flow rate of 6L/min;
(3) heating to 150 ℃ at the heating rate of 10 ℃/min, and preserving heat for 72h to obtain the pretreated soil;
(4) - (5) same as in example 1.
Comparative example 4
The method for detecting hexavalent chromium in soil in the prior art comprises the steps of not carrying out heating pretreatment, collecting a soil sample, directly carrying out alkali digestion by referring to HJ687-2014 alkali digestion/flame atomic absorption spectrophotometry for determining hexavalent chromium in solid wastes (embodiment 1), filtering to obtain filtrate, and referring to dibenzoyl dihydrazide spectrophotometry for determining hexavalent chromium in water quality (GB 7467-8)7) Measurement of Cr in the filtrate6+Finally calculating Cr in soil6+Content (c);
the method comprises the following specific steps:
(1) 0.4g of MgCl was added to the soil20.5ml of potassium dihydrogen phosphate buffer solution, 50ml of NaOH and Na having a pH of 12 were added2CO3Carrying out alkali digestion and dissolution on the formed mixed alkali solution, heating to 95 ℃ for 60min, and carrying out solid-liquid separation;
(2) adding a sulfuric acid solution after the liquid phase obtained by solid-liquid separation is subjected to constant volume, adjusting the pH value to 2, adding an acetone solution of diphenylcarbodihydrazide, developing, performing constant volume, and measuring the absorbance value; with Cr2O7 2-Drawing a standard curve for the standard substance, substituting the absorbance value to obtain the total Cr in the sample6+m。
Examples of effects
Examples 1-6 and comparative examples 1-4 were tested for accuracy. Hexavalent chromium in soil is actually treated with chemical (K)2Cr2O7) The actual content of hexavalent chromium in the soil can be determined by the amount of the added chemical agent. The accuracy test results are shown in table 1. accuracy-Cr measured by the present invention6+Total amount of (1)/actual Cr in soil6+The total amount is × 100%.
TABLE 1 examples 1-6 and comparative examples 1-4 accuracy tests
Thus, the method provided by the invention can be used for measuring Cr in a soil sample containing a large amount of reducing agent6+Content, and has high accuracy.
The above detailed description is specific to one possible embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, and all equivalent implementations or modifications without departing from the scope of the present invention should be included in the technical scope of the present invention.
Claims (13)
1. A detection method of hexavalent chromium ions is characterized by comprising the following steps: the method comprises the following steps:
(1) taking a soil sample;
(2) placing the sample in a heating device, and introducing air;
(3) heating and maintaining the temperature to obtain pretreated soil;
(4) adding MgCl into the pretreated soil2Adding an alkali solution into a monopotassium phosphate buffer solution for alkali digestion and dissolution, heating and carrying out solid-liquid separation;
(5) measuring Cr in liquid phase obtained by solid-liquid separation according to diphenylcarbodihydrazide spectrophotometry6+Calculating the total Cr in the soil sample6+Mass m of (a);
in the step (2), the flow rate of the air is 3-8L/min;
in the step (3), the heating temperature is 80-120 ℃;
in the step (3), the heating rate is 8-12 ℃/min;
the soil in the step (1) is soil containing a large amount of reducing agents, and the reducing agents comprise at least one of sodium sulfite, ferrous sulfate, sodium sulfide and calcium polysulfide.
2. The method for detecting hexavalent chromium ions according to claim 1, wherein: in the step (2), the flow rate of the air is 6L/min.
3. The method for detecting hexavalent chromium ions according to claim 1, wherein: in the step (3), the heating temperature is 100 ℃.
4. The method of detecting hexavalent chromium ions of claim 3, wherein: in the step (3), the heating rate is 10 ℃/min; the heat preservation time is 36-72 h.
5. As claimed in claim1 the method for detecting hexavalent chromium ions, which is characterized by comprising the following steps: in the step (4), the MgCl2The addition amount of the fertilizer is 0.1 to 0.3 time of the mass of the soil; the adding amount of the potassium dihydrogen phosphate buffer solution is 0.2-1ml/g soil.
6. The method of detecting hexavalent chromium ions of claim 5, wherein: in the step (4), the MgCl2The addition amount of (A) is 0.16 times of the soil mass.
7. The method of detecting hexavalent chromium ions of claim 5, wherein: the addition amount of the potassium dihydrogen phosphate buffer solution is 0.2ml/g soil.
8. The method for detecting hexavalent chromium ions according to claim 1, wherein: in the step (4), the alkali solution is a mixed solution of sodium hydroxide and sodium carbonate, and the pH value of the mixed solution is 12-13.
9. The method of detecting hexavalent chromium ions of claim 8, wherein: the addition amount of the alkali solution is 15-30ml/g soil.
10. The method of detecting hexavalent chromium ions of claim 9, wherein: the addition amount of the alkali solution is 20ml/g soil.
11. The method for detecting hexavalent chromium ions according to claim 1, wherein: in the step (4), the heating temperature is 90-95 ℃, and the heating time is 40-60 min.
12. The method for detecting hexavalent chromium ions according to claim 1, wherein: the specific operation process of the step (5) is as follows: adding a sulfuric acid solution after the liquid phase obtained by solid-liquid separation is subjected to constant volume, adjusting the pH value, adding an acetone solution of diphenylcarbonyldihydrazide, developing, performing constant volume, and measuring the absorbance value; with Cr2O7 2-Drawing for standard substancePreparing a standard curve, substituting the absorbance value to obtain the total Cr in the sample6+Mass m of (2).
13. The method of detecting hexavalent chromium ions of claim 12, wherein: in the step (5), the pH value is 1.5-2.5.
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