CN110907593A - Chemical analysis method for determining nickel in nickel catalyst by changing complex anions - Google Patents
Chemical analysis method for determining nickel in nickel catalyst by changing complex anions Download PDFInfo
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Abstract
The invention provides a chemical analysis method for determining nickel in a nickel catalyst by changing complex anions, wherein the nickel dimethylglyoxime is precipitated by nitric-sulfuric mixed acid and is digested by filter paper, and after heavy smoke of sulfuric acid is exhausted, salts are subjected to two times of complex anion conversion treatment by using 10mL of concentrated hydrochloric acid; dissolving salt with distilled water, regulating pH with ammonia water, using ammonium uricate as indicator, and using EDTA to make titration. The invention has the advantages that: the color of the end point is obviously protruded, and the method has the advantages of simple operation, high speed, high accuracy and the like.
Description
Technical Field
The invention belongs to the field of chemical analysis, and relates to a method for determining nickel by using a nickel catalyst.
Background
Nickel is a silver white metal, has magnetism and good plasticity, and has good corrosion resistance. Nickel is a nearly silvery white, hard and ductile metallic element with ferromagnetic properties, which is highly polished and corrosion resistant. Mainly for alloys (such as nickel steel and nickel silver) and as catalysts (such as raney nickel, in particular as hydrogenation catalysts).
By looking up literature data, the analysis method of nickel in ore and mineral separation materials and metallurgical materials is more, and related national standards exist; there are few chemical analysis test methods for nickel in nickel catalysts; the existing analysis and test methods of nickel mainly comprise a titration method, a gravimetric method, an absorptiometry method and the like; the separation and enrichment method of nickel mainly uses the dimethylglyoxime method as a main method.
The nickel catalyst is mainly used in the hydrogenation process of chemical industry, and after the nickel catalyst is used for a period of time, the original catalytic activity is lost due to catalyst poisoning, and the nickel is eliminated, but the high-content nickel can be recovered as a secondary resource. The method for measuring the high-content nickel mainly comprises the steps of separating dimethylglyoxime and mainly adopting an EDTA titration method. The method adopts hydrochloric acid to dissolve the precipitate of the nickel dimethylglyoxime, and the chemical structure of the dimethylglyoxime in the solution is not destroyed, so that the titration end point is trailing in the subsequent EDTA titration process, and the end point phenomenon is not obvious, so that the error is larger, and a plurality of chemical analysis practitioners show that the method is not easy to master.
Disclosure of Invention
The invention provides a chemical analysis method for determining nickel in a nickel catalyst by changing complex anions.
The technical scheme is as follows: a chemical analysis method for nickel determination in a nickel catalyst by changing complex anions comprises the following specific steps:
(1) accurately weighing 0.2000 g-0.4000 g of nickel catalyst sample in a 30mL corundum crucible, respectively covering 2-3g of sodium peroxide on the upper and lower sides, putting the sample into a muffle furnace, heating the sample to 680 ℃ from low temperature, melting the sample for 20 minutes, taking out and cooling the molten sample.
(2) Placing the crucible cooled in the step (1) into a 1#300mL beaker, adding 100mL of distilled water, heating and leaching the melt, boiling for 5min after the melt is completely leached, decomposing peroxide, taking down and cooling, filtering by using medium-speed filter paper, washing the precipitate and the beaker by using 1% (mass fraction) of sodium hydroxide solution for 5 times respectively, and discarding the filtrate.
(3) Putting the precipitate filtered in the step (2) and filter paper into a No. 1 original beaker, adding 25mL of concentrated nitric acid (15 mol/L) and 15mL of 1:1 dilute sulfuric acid (1 volume of 18mol/L sulfuric acid is diluted by 1 volume of pure water) to nitrify the precipitate, steaming to a wet salt state, adding 5mL of concentrated hydrochloric acid (12 mol/L), washing to about 50mL by water, heating to dissolve the salt, cooling and fixing the volume to a 100mL volumetric flask.
(4) Transferring the solution with the constant volume in the step (3) to a beaker with the volume of 20.00-2 #300mL, adding 2g of ammonium citrate and 4g of ammonium chloride, boiling for 5min, adjusting the pH of the solution to 8-9 by using concentrated ammonia water (15 mol/L), adding 20mL of 1% (mass fraction) dimethylglyoxime solution, preserving the temperature at 75 ℃ for 40min, filtering by using medium-speed filter paper, washing the beaker by using ammonia-ammonium chloride solution and precipitating for 4 times respectively, and discarding the filtrate.
(5) Putting the precipitate filtered in the step (4) and filter paper into a No. 2 original beaker, adding 25mL of concentrated nitric acid (15 mol/L) and 15mL of 1:1 dilute sulfuric acid (1 volume of 18mol/L sulfuric acid is diluted by 1 volume of pure water) to nitrify the precipitate, adding 10mL of concentrated hydrochloric acid after the sulfuric acid smoke is exhausted, heating to dissolve salts, and evaporating at low temperature to be in a wet salt state, and repeating the steps twice.
(6) Adding 50mL of distilled water to the sample finally steamed to a wet salt state in (5), heating and boiling for 5min to dissolve the salt, cooling, adjusting the pH of the solution to =9 with ammonia water, adding an ammonium-uricase indicator, and titrating with EDTA.
The invention has the following advantages:
1. concentrated hydrochloric acid is repeatedly steamed to a wet salt state to convert complex anions in nitroso-nickel complex ions, so that ligands in newly generated nickel-chlorine complex ions are easily replaced by EDTA (ethylene diamine tetraacetic acid), the titration end point changes sharply, the abrupt change is obvious, and the titration result is stable, accurate and reliable.
2. The invention solves the problems that a practitioner is puzzled to trailing the titration end point for a long time in the process of titrating nickel by EDTA, the gradual change of the color has no obvious leap, and the stability and the accuracy of the titration result are poor. The method has the advantages of simple operation, high speed, high accuracy and the like.
Detailed Description
Working conditions of reagents and instruments:
the chemical reagents used in the test method adopted by the invention are all analytical pure reagents.
A 50mL burette, 20mL pipette (identified by the metering department and within the expiration date);
nitric acid (15 mol/L), hydrochloric acid (12 mol/L), sulfuric acid (18 mol/L) and ammonia water (15 mol/L).
The present invention is further illustrated by the following examples, which use standard recovery and standard sample analysis to verify the precision and recovery of the test results.
Examples 1
(1) Accurately weighing 0.4000g of nickel standard sample in a 30mL corundum crucible, respectively covering 3g of sodium peroxide (carbon needs to be burnt in advance) from top to bottom, putting the sample into a muffle furnace, heating the sample to 680 ℃ from low temperature, melting the sample for 20 minutes, and taking out the sample for cooling;
(2) placing the cooled crucible in (1) into a 1#300mL beaker, adding 100mL distilled water, heating and leaching the melt, boiling for 5min after the melt is completely leached, decomposing peroxide, taking down and cooling, filtering by using medium-speed filter paper, washing the precipitate and the beaker by using 1% sodium hydroxide solution for 5 times respectively, and discarding the filtrate.
(3) Putting the precipitate filtered in the step (2) and filter paper into a No. 1 original beaker, adding 25mL of concentrated nitric acid and 15mL of 1:1 dilute sulfuric acid to nitrify the precipitate, steaming to be in a wet salt state, adding 5mL of concentrated hydrochloric acid, flushing to 50mL, and heating to dissolve the salt.
(4) Adding 2g of ammonium citrate and 4g of ammonium chloride into the solution obtained in the step (3), boiling for 5min, adjusting the pH of the solution to 8-9 by using concentrated ammonia water, adding 20mL of 1% dimethylglyoxime solution, preserving the temperature at 75 ℃ for 40min, filtering by using medium-speed filter paper, washing a beaker by using ammonia-ammonium chloride solution, precipitating for 4 times respectively, and discarding the filtrate.
(5) Putting the precipitate filtered in the step (4) and filter paper into a No. 1 original beaker, adding 25mL of concentrated nitric acid and 15mL of 1:1 dilute sulfuric acid to nitrify the precipitate, adding 10mL of concentrated hydrochloric acid after the sulfuric acid smoke is exhausted, heating to dissolve salts, and steaming at low temperature to be in a wet salt state, and repeating the steps twice.
(6) Adding 50mL of distilled water to the sample steamed to the wet salt state in the step (5), heating and boiling for 5min to dissolve the salt, cooling, adjusting the pH of the solution to be about =9 with ammonia water, adding an ammonium-uricosuric indicator, and titrating with EDTA.
Table 1 example 1 analysis results and precision of standard samples
EXAMPLES example 2
(1) Accurately weighing 0.2000g of nickel catalyst sample in a 30mL corundum crucible, respectively covering 2g of sodium peroxide (carbon needs to be burnt in advance when carbon exists) from top to bottom, putting the sample into a muffle furnace, heating the sample to 680 ℃ from low temperature, melting the sample for 20 minutes, taking out and cooling the sample;
(2) placing the cooled crucible in (1) into a 1#300mL beaker, adding 100mL distilled water, heating and leaching the melt, boiling for 5min after the melt is completely leached, decomposing peroxide, taking down and cooling, filtering by using medium-speed filter paper, washing the precipitate and the beaker by using 1% sodium hydroxide solution for 5 times respectively, and discarding the filtrate.
(3) Putting the filtered precipitate in the step (2) and filter paper into a No. 1 original beaker, adding 25mL of concentrated nitric acid and 15mL of 1:1 dilute sulfuric acid to nitrify the precipitate, steaming to be in a wet salt state, adding 5mL of concentrated hydrochloric acid, flushing to 50mL, heating to dissolve salts, cooling and then fixing the volume to a 100mL volumetric flask.
(4) Transferring the solution with the constant volume in the step (3) to a beaker with the volume of 20.00-2 #300mL, adding 2g of ammonium citrate and 4g of ammonium chloride, boiling for 5min, adjusting the pH of the solution to 8-9 by using strong ammonia water, adding 20mL of 1% dimethylglyoxime solution, preserving the temperature at 75 ℃ for 40min, filtering by using medium-speed filter paper, washing the beaker by using ammonia-ammonium chloride solution and precipitating for 4 times respectively, and discarding the filtrate.
(5) And (3) putting the precipitate filtered in the step (4) and filter paper into a No. 2 original beaker, adding 25mL of concentrated nitric acid and 15mL of 1:1 dilute sulfuric acid to nitrify the precipitate, adding 10mL of concentrated hydrochloric acid after the sulfuric acid smoke is exhausted, heating to dissolve salts, and steaming at low temperature to form wet salts, and repeating the steps twice.
(6) Adding 50mL of distilled water to the sample steamed to the wet salt state in the step (5), heating and boiling for 5min to dissolve the salt, cooling, adjusting the pH of the solution to be about =9 with ammonia water, adding an ammonium-uricosuric indicator, and titrating with EDTA.
Table 2 example 2 sample analysis results and spiking recovery and precision
EXAMPLE 3
(1) Accurately transferring a proper amount (the transfer volume is shown in table 3) of nickel-copper-containing electrolyte into a 300mL beaker, flushing to about 100mL, adding 4g of ammonium citrate, boiling 4g of ammonium chloride for 5min, adjusting the pH of the solution to 8-9 by using strong ammonia water, adding 20mL of 1% dimethylglyoxime solution, preserving the temperature at 75 ℃ for 40min, filtering by using medium-speed filter paper, washing the beaker by using an ammonia-ammonium chloride solution and precipitating for 4 times respectively, and discarding the filtrate.
(2) Putting the precipitate filtered in the step (1) and filter paper into an original beaker, adding 25mL of concentrated nitric acid and 15mL of 1:1 dilute sulfuric acid to nitrify the precipitate, adding 10mL of concentrated hydrochloric acid to heat and dissolve salts after the smoke of sulfuric acid is exhausted, and steaming at low temperature to be in a wet salt state, and repeating the steps twice.
(3) Adding 50mL of distilled water to the sample steamed twice to form wet salt in the step (2), heating and boiling for 5min to dissolve the salt, cooling, adjusting the pH of the solution to be about =9 by using ammonia water, adding an ammonium uricate indicator, and titrating by using EDTA.
Table 3 example 3 sample analysis results and spiking recovery and precision
The invention solves the problems of trailing of the titration end point, no obvious sudden change of the color gradual change and poor stability and accuracy of the titration result, which bother practitioners for a long time in the process of EDTA titration of nickel. The innovation points of the invention are as follows: because a large amount of yellow nitrogen oxide gas (mainly nitrogen dioxide) is generated in the process of nitrating the dimethylglyoxime nickel by the nitric-sulfuric mixed acid and filtering filter paper, the gas is inversely dissolved in the solution to generate a large amount of nitrite, the nitrite is a strong complex anion and generates complex ions of nitrosonickel with the nickel in the solution, and because the complex stability constant of the nitrosonickel complex ions is greater than that of EDTA-nickel, EDTA is difficult to replace the position of nitrite in the nitrosonickel complex ions in the titration process, the titration end point is trailing, and no mutation exists. The invention adopts concentrated hydrochloric acid to carry out displacement complex anion treatment on nitroso-nickel, converts the ligand of nitrite into the chloride ion ligand, and then carries out titration, and the method has the advantages of sharp end point reaction, obvious mutation, easy visual observation and stable and reliable titration result.
Claims (1)
1. A chemical analysis method for nickel determination in a nickel catalyst by changing complex anions is characterized in that: the method comprises the following specific steps:
(1) accurately weighing 0.2000 g-0.4000 g of nickel catalyst sample in a 30mL corundum crucible, respectively covering 2-3g of sodium peroxide on the upper and lower sides, putting the sample into a muffle furnace, heating the sample to 680 ℃ from low temperature, melting the sample for 20 minutes, taking out and cooling the sample;
(2) putting the cooled crucible in the step (1) into a 1#300mL beaker, adding 100mL of distilled water, heating and leaching the melt, boiling for 5min after the melt is completely leached, decomposing peroxide, taking down and cooling, filtering by using medium-speed filter paper, washing the precipitate and the beaker by using a sodium hydroxide solution with the mass fraction of 1% for 5 times respectively, and discarding the filtrate;
(3) putting the filtered precipitate in the step (2) and filter paper into a No. 1 original beaker, adding 25mL of 15mol/L concentrated nitric acid and 15mL1:1 dilute sulfuric acid to nitrify the precipitate, steaming to a wet salt state, adding 5mL of 12mol/L concentrated hydrochloric acid, flushing with water to 50mL, heating to dissolve salts, cooling, and fixing the volume to a 100mL volumetric flask;
(4) transferring the solution with the constant volume in the step (3) to a beaker with the volume of 20.00-2 #300mL, adding 2g of ammonium citrate and 4g of ammonium chloride, boiling for 5min, adjusting the pH of the solution to 8-9 by using 15mol/L of strong ammonia water, adding 20mL of dimethylglyoxime solution with the mass fraction of 1%, preserving the temperature at 75 ℃ for 40min, filtering by using medium-speed filter paper, washing the beaker by using ammonia-ammonium chloride solution and precipitating for 4 times respectively, and discarding the filtrate;
(5) putting the filtered precipitate in the step (4) and filter paper into a No. 2 original beaker, adding 25mL of 15mol/L concentrated nitric acid and 15mL1:1 dilute sulfuric acid to nitrify the precipitate, adding 10mL of concentrated hydrochloric acid after the sulfuric acid smoke is exhausted, heating to dissolve salts, and steaming at low temperature to be in a wet salt state, and repeating the steps twice;
(6) adding 50mL of distilled water to the sample finally steamed to a wet salt state in (5), heating and boiling for 5min to dissolve the salt, cooling, adjusting the pH of the solution to =9 with ammonia water, adding an ammonium-uricase indicator, and titrating with EDTA.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112378900A (en) * | 2020-10-27 | 2021-02-19 | 西北矿冶研究院 | Method for determining tungsten in tungsten catalyst with activated carbon as carrier |
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Application publication date: 20200324 |