CN108572235B - Method for detecting chromium content in chromium passivation waste liquid - Google Patents
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Abstract
The invention discloses a method for detecting chromium content in chromium passivation waste liquid, which mainly solves the technical problem that the chromium content in the chromium passivation waste liquid in the prior art cannot be detected. The technical scheme of the invention is as follows: a method for detecting chromium content in chromium passivation waste liquid comprises the following steps: preparing a solution to be detected; sequentially adding a phosphoric acid solution, a silver nitrate solution and an ammonium persulfate solution into the solution to be detected; then adding a hydrochloric acid solution into the mixed solution containing the solution to be detected; adding a phenylated anthranilic acid solution into the mixed solution containing the solution to be tested, titrating the mixed solution containing the solution to be tested by using an ammonium ferrous sulfate standard solution until the solution is completely bright green, stopping titration and reading the titration volume; and calculating the chromium content in the chromium passivation waste liquid to be detected. The method can accurately measure the chromium content in the chromium passivation waste liquid, effectively avoids the interference of a large amount of organic resin, has accurate and reliable detection data, and provides scientific basis for harmless treatment and effective utilization of the chromium passivation waste liquid.
Description
Technical Field
The invention belongs to the technical field of chemical analysis, relates to a method for detecting chromium content in chromium passivation waste liquid, and particularly relates to a method for detecting chromium content in chromium passivation waste liquid generated in the production process of cold-rolled hot-dip (aluminum) zinc products.
Background
In the production process of the cold-rolled hot-dipped (aluminum) zinc plate, in order to improve the corrosion resistance of the cold-rolled hot-dipped (aluminum) zinc plate, the surface of the cold-rolled hot-dipped (aluminum) zinc plate is generally required to be passivated, and the chromium passivation solution has the advantages of simple operation, low cost, simple and convenient control, bright color of the formed passivation film, outstanding weather resistance and wear resistance and self-repairing function, so the chromium passivation solution is widely used. However, a large amount of chromium passivation waste liquid is inevitably generated in the using process, and if the waste liquid is not properly treated, the environment is greatly damaged, so that the generated chromium passivation waste liquid must be reasonably, effectively and harmlessly treated, and the detection of the chromium content in the chromium passivation waste liquid has important significance for the treatment of the waste liquid.
In the prior art, no corresponding Chinese national standard method exists for a chromium passivation waste liquid detection method at present, but in the prior art, a small amount of reports about a chromium content detection method exist, and Chinese patent application with application publication No. CN102279162A discloses a method for detecting chromium content in organic chromium, which mainly comprises the steps of decomposing a sample by acid, oxidizing chromium to hexavalent, adding a dibenzoyl dihydrazide color developing agent to generate a mauve complex, carrying out color comparison, and calculating the content of the sample; however, the method cannot be applied to the determination of the chromium content in the chromium passivation waste liquid mainly because the chromium passivation waste liquid contains a large amount of organic resin, and when acid treatment is adopted, the organic resin generates an aggregation phenomenon and cannot be damaged, so that the subsequent chromium oxidation and color development are directly influenced. The Chinese patent application with application publication No. CN104007078A discloses a method for rapidly detecting total chromium in water and a detection kit, wherein after pH is adjusted by mainly adopting phosphoric acid, the chromium in water and a diphenylcarbonyldihydrazide color developing agent generate a mauve complex for color comparison, and then the mauve complex is compared with a standard curve to calculate the chromium in water; the method is only suitable for measuring the content of chromium in water, but for waste liquid containing a large amount of organic chromium passivation, chromium cannot generate a mauve complex with a dibenzoyl dihydrazide color developing agent, and simultaneously, a large amount of emulsion organic resin influences the transmittance and generates wrong absorbance to obtain a wrong detection result. The Chinese patent application with application publication number CN104330361A discloses a chromium rapid detection agent, which is mainly characterized in that low-valent chromium in a solution to be detected is oxidized to hexavalent chromium by a manganese oxidizing agent, then diphenylcarbonyldihydrazide mixed reagent developing powder is added, the color is developed by complexing with chromium in the solution, and the chromium content in the solution is calculated; the method is only suitable for detecting the chromium content in clear water or a water-soluble solid sample, is not suitable for detecting the chromium content in milky and opaque chromium passivation waste liquid, and mainly has two problems: (1) chromium in the chromium passivation waste liquid is combined with organic resin in a complex form and cannot be oxidized to be hexavalent by manganese oxide powder. (2) The chromium in the solution can not be directly developed with the diphenyl carbodihydrazide mixed reagent color development powder.
The method for detecting the chromium content in the prior art cannot meet the requirement of accurately detecting the chromium content in the chromium passivation waste liquid.
Disclosure of Invention
The invention aims to provide a method for detecting chromium content in chromium passivation waste liquid, mainly solves the technical problem that the chromium content in the chromium passivation waste liquid in the prior art cannot be detected, and provides scientific basis for harmless disposal and effective utilization of the chromium passivation waste liquid generated in the production process of cold-rolled and hot-dipped (aluminum) zinc products.
The invention adopts the technical scheme that the method for detecting the chromium content in the chromium passivation waste liquid comprises the following steps:
1) preparing a solution to be detected, weighing a quantitative sample, placing the quantitative sample in a platinum crucible, removing water and organic resin in the sample, specifically, heating the sample from 15-25 ℃ to 105-115 ℃ at a heating rate of 3-5 ℃/min, and keeping the temperature for 150-200 min; then heating the sample from 105-115 ℃ to 250-300 ℃ at a heating rate of 7-9 ℃/min, and preserving heat for 10-20 min; heating the sample from 250-300 ℃ to 500-550 ℃ at a heating rate of 8-10 ℃/min, and preserving heat for 20-40 min; heating the sample from 500-550 ℃ to 815-850 ℃ at a heating rate of 9-12 ℃/min, and keeping the temperature for 100-150 min;
and then adding 2-4 g of the mixture into a platinum crucible according to the mass ratio of 2: 1 mixed reagent of sodium carbonate and boric acid; placing the platinum crucible in a high-temperature furnace, melting at the high temperature of 950-1050 ℃ for 15-20 min, taking out the platinum crucible from the high-temperature furnace, adding 150-200 ml of dilute sulfuric acid solution with the volume concentration of 10% into the platinum crucible when the platinum crucible is cooled to 200-300 ℃ to heat and dissolve the melt in the platinum crucible, and transferring the solution in the platinum crucible into a conical flask to prepare a solution to be detected;
2) sequentially adding 10-15 ml of phosphoric acid solution with volume concentration of 50%, 5-8 ml of silver nitrate solution with mass concentration of 1% and 10-20 ml of ammonium persulfate solution with mass concentration of 20% into the solution to be detected; heating the mixed solution containing the solution to be detected to 105-115 ℃, preserving heat for 3-5 min, and then adding 5-8 ml of hydrochloric acid solution with the volume concentration of 20% into the mixed solution containing the solution to be detected; heating the mixed solution containing the solution to be detected to 95-100 ℃ and preserving heat for 2-3 min; when the mixed solution containing the solution to be detected is cooled to 15-25 ℃, adding 0.5-1.0 ml of 0.02% by mass of a phenylanthranilic acid solution into the mixed solution containing the solution to be detected; then titrating the mixed solution containing the solution to be measured by using an ammonium ferrous sulfate standard solution, stopping titration when the mixed solution containing the solution to be measured is completely changed into bright green, and reading the titration volume of the ammonium ferrous sulfate standard solution;
3) calculating the chromium content in the chromium passivation waste liquid to be detected, wherein the chromium content in the chromium passivation waste liquid is calculated according to the following formula, and W ═ MCr×C×V)/(3×mTest for) X 100%, wherein W is the mass percent of chromium in the sample and has the unit of percent; m isTest forWeighing the sample in g; mCrIs the molar mass of chromium, and the unit is g/mol; c is the concentration of the ammonium ferrous sulfate standard solution, and the unit is mol/L; v is the titration volume of the standard solution of ferrous ammonium sulfate, and the unit is L.
Further, in the step 1), removing water and organic resin in the sample, specifically, heating the sample from 15-25 ℃ to 105-110 ℃ at a heating rate of 3-4 ℃/min, and keeping the temperature for 180-200 min; then heating the sample from 105-110 ℃ to 250-280 ℃ at a heating rate of 8-9 ℃/min, and preserving heat for 15-20 min; heating the sample from 250-280 ℃ to 500-520 ℃ at a heating rate of 8-9 ℃/min, and preserving heat for 20-30 min; heating the sample from 500-520 ℃ to 815-820 ℃ at a heating rate of 9-10 ℃/min, and keeping the temperature for 100-150 min; the effect is good.
Under the specified conditions of temperature rise and heat preservation, the method ensures that the moisture and the organic resin in the chromium passivation waste liquid are stably removed, the chromium contained in the sample is kept in the crucible, and then sodium carbonate and boric acid are added to convert the chromium into soluble salt substances; dissolving soluble salt with dilute sulfuric acid, and preparing the product according to the chemical ion equation I, 3S2O8 2-+2Cr3+＝2Cr6++6SO4 2-Oxidizing all chromium in the solution to hexavalent chromium by ammonium persulfate, and then performing 3Fe according to a chemical ion equation II2++Cr6+＝3Fe3++Cr3+And titrating with an ammonium ferrous sulfate standard solution until the solution becomes bright green, stopping titrating, reading the titration volume, and calculating the chromium content in the chromium passivation waste liquid.
The technology of the invention effectively solves the problem that chromium in the chromium passivation waste liquid generated in the production of the cold-rolled galvanized (aluminum) plate can not be detected, and provides data support for reasonable, effective and harmless treatment in the chromium passivation waste liquid.
Compared with the prior art, the invention has the following positive effects: 1. the method realizes accurate determination of chromium content in the chromium passivation waste liquid, is simple and convenient to operate and strong in operability, and avoids effectively solving the problem that a large amount of emulsion resin interferes chromium detection. 2. The method is not only suitable for detecting the chromium content in the chromium passivation waste liquid, but also suitable for detecting the chromium content in complex organic solutions such as chromium passivation solution, chromium in organic solution and the like.
Detailed Description
A method for detecting chromium content in chromium passivation waste liquid comprises the following steps:
1) preparing a solution to be detected, weighing 10.0053g of chromium passivation waste liquid, placing the chromium passivation waste liquid in a platinum crucible, removing water and organic resin in a sample, specifically, heating the sample from 20 ℃ to 105 ℃ at a heating rate of 4 ℃/min, and keeping the temperature for 180 min; then heating the sample from 105 ℃ to 250 ℃ at the heating rate of 8 ℃/min, and preserving the heat for 15 min; heating the sample from 250 ℃ to 500 ℃ at the heating rate of 8 ℃/min, and preserving the temperature for 30 min; then heating the sample from 500 ℃ to 815 ℃ at the heating rate of 10 ℃/min, and preserving the temperature for 120 min;
then adding 3g of the mixture with the mass ratio of 2: 1 mixed reagent of sodium carbonate and boric acid; placing the platinum crucible in a high-temperature furnace, melting at the high temperature of 1000 ℃ for 15min, taking out the platinum crucible from the high-temperature furnace, adding 150ml of 10% dilute sulfuric acid solution into the platinum crucible when the platinum crucible is cooled to 200-300 ℃ to heat and dissolve the melt in the platinum crucible, and transferring the solution in the platinum crucible to a conical flask to prepare a solution to be detected;
2) sequentially adding 10ml of phosphoric acid solution with the volume concentration of 50%, 5ml of silver nitrate solution with the mass concentration of 1% and 20ml of ammonium persulfate solution with the mass concentration of 20% into the solution to be detected; heating the mixed solution containing the solution to be detected to 105 ℃, preserving the heat for 5min, and then adding 5ml of hydrochloric acid solution with the volume concentration of 20% into the mixed solution containing the solution to be detected; heating the mixed solution containing the solution to be detected to 100 ℃ and preserving the heat for 3 min; when the mixed solution containing the solution to be detected is cooled to 15-25 ℃, adding 0.5ml of 0.02 mass percent phenylanthranilic acid solution into the mixed solution containing the solution to be detected; then titrating the mixed solution containing the solution to be measured by using an ammonium ferrous sulfate standard solution, stopping titration when the mixed solution containing the solution to be measured is completely changed into bright green, and reading the titration volume of the ammonium ferrous sulfate standard solution;
3) calculating the chromium content in the chromium passivation waste liquid to be detected, wherein the chromium content in the chromium passivation waste liquid is calculated according to the following formula, and W ═ MCr×C×V)/(3×mTest for) X 100%, wherein W is the mass percent of chromium in the sample and has the unit of percent; m isTest forWeighing the sample in g; mCrIs the molar mass of chromium, and the unit is g/mol; c is the concentration of the ammonium ferrous sulfate standard solution, and the unit is mol/L; v is the titration volume of the standard solution of ferrous ammonium sulfate, and the unit is L.
The precision and accuracy of the method are confirmed by the standard addition recovery experiment and the precision experiment of the sample.
And (3) a recovery experiment, namely after a certain amount of chromium is added into a chromium passivation waste liquid sample, detecting the standard addition recovery rate of the sample according to the method, wherein the test result is shown in table 1.
TABLE 1 sample recovery test with addition of standard
| Adding chromium in an amount of per mg | Recovery/mg | Percent recovery% |
| 2.0 | 1.98 | 99.0 |
| 4.0 | 4.03 | 100.8 |
| 6.0 | 6.02 | 100.3 |
| 8.0 | 7.98 | 99.8 |
| 10.0 | 10.06 | 100.6 |
Precision experiment, 11 times of precision experiments are carried out on the chromium content in the 2 groups of chromium passivation waste liquid, and the analysis results are shown in table 2.
TABLE 2 sample precision test%
The experimental result shows that the recovery rate of the chromium content in the chromium passivation waste liquid is 99.0-100.8%, the recovery rate is high, the detection data statistics RSD is less than 3%, the detection data precision is good, the method is accurate and reliable, and the requirement of effective and reasonable treatment, detection and analysis of the chromium passivation waste liquid is completely met.
Claims (2)
1. A method for detecting chromium content in chromium passivation waste liquid is characterized by comprising the following steps:
1) preparing a solution to be detected, weighing a quantitative sample, placing the quantitative sample in a platinum crucible, removing water and organic resin in the sample, specifically, heating the sample from 15-25 ℃ to 105-115 ℃ at a heating rate of 3-5 ℃/min, and keeping the temperature for 150-200 min; then heating the sample from 105-115 ℃ to 250-300 ℃ at a heating rate of 7-9 ℃/min, and preserving heat for 10-20 min; heating the sample from 250-300 ℃ to 500-550 ℃ at a heating rate of 8-10 ℃/min, and preserving heat for 20-40 min; heating the sample from 500-550 ℃ to 815-850 ℃ at a heating rate of 9-12 ℃/min, and keeping the temperature for 100-150 min;
and then adding 2-4 g of the mixture into a platinum crucible according to the mass ratio of 2: 1 mixed reagent of sodium carbonate and boric acid; placing the platinum crucible in a high-temperature furnace, melting at the high temperature of 950-1050 ℃ for 15-20 min, taking out the platinum crucible from the high-temperature furnace, adding 150-200 ml of dilute sulfuric acid solution with the volume concentration of 10% into the platinum crucible when the platinum crucible is cooled to 200-300 ℃ to heat and dissolve the melt in the platinum crucible, and transferring the solution in the platinum crucible into a conical flask to prepare a solution to be detected;
2) sequentially adding 10-15 ml of phosphoric acid solution with volume concentration of 50%, 5-8 ml of silver nitrate solution with mass concentration of 1% and 10-20 ml of ammonium persulfate solution with mass concentration of 20% into the solution to be detected; heating the mixed solution containing the solution to be detected to 105-115 ℃, preserving heat for 3-5 min, and then adding 5-8 ml of hydrochloric acid solution with the volume concentration of 20% into the mixed solution containing the solution to be detected; heating the mixed solution containing the solution to be detected to 95-100 ℃ and preserving heat for 2-3 min; when the mixed solution containing the solution to be detected is cooled to 15-25 ℃, adding 0.5-1.0 ml of 0.02% by mass of a phenylanthranilic acid solution into the mixed solution containing the solution to be detected; then titrating the mixed solution containing the solution to be measured by using an ammonium ferrous sulfate standard solution, stopping titration when the mixed solution containing the solution to be measured is completely changed into bright green, and reading the titration volume of the ammonium ferrous sulfate standard solution;
3) calculating the chromium content in the chromium passivation waste liquid to be detected, wherein the chromium content in the chromium passivation waste liquid is calculated according to the following formula, and W ═ MCr×C×V)/(3×mTest for) X 100%, wherein W is the mass percent of chromium in the sample and has the unit of percent; m isTest forWeighing the sample in g; mCrIs the molar mass of chromium, and the unit is g/mol; c is the concentration of the ammonium ferrous sulfate standard solution, and the unit is mol/L; v is the titration volume of the standard solution of ferrous ammonium sulfate, and the unit is L.
2. The method for detecting the chromium content in the chromium passivation waste liquid as claimed in claim 1, wherein in the step 1), the water and the organic resin in the sample are removed, specifically, the sample is heated from 15-25 ℃ to 105-110 ℃ at a heating rate of 3-4 ℃/min, and the temperature is kept for 180-200 min; then heating the sample from 105-110 ℃ to 250-280 ℃ at a heating rate of 8-9 ℃/min, and preserving heat for 15-20 min; heating the sample from 250-280 ℃ to 500-520 ℃ at a heating rate of 8-9 ℃/min, and preserving heat for 20-30 min; then heating the sample from 500-520 ℃ to 815-820 ℃ at a heating rate of 9-10 ℃/min, and preserving the temperature for 100-150 min.
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| CN110954383B (en) * | 2019-12-16 | 2022-03-22 | 湖南众鑫新材料科技股份有限公司 | Method for measuring chromium content in vanadium-aluminum alloy |
| CN112326875A (en) * | 2021-01-06 | 2021-02-05 | 中海储能科技(北京)有限公司 | Detection method of iron-chromium redox flow battery electrolyte |
| CN113834899B (en) * | 2021-09-15 | 2024-04-12 | 大连科技学院 | Digital twinning-based aluminum chromium-free passivation process free acid content monitoring method |
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