CN114113041A - Method for testing gold and palladium by gold and palladium-containing material - Google Patents
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Abstract
The invention relates to the technical field of analytical chemistry, and relates to a method for testing gold and palladium by using gold and palladium-containing materials. The invention adopts the steps of carrying out primary crushing and grinding treatment on gold-containing and palladium-containing solids, adding hydrochloric acid for dissolving to obtain hydrochloric acid treatment solution, completely dissolving nickel, iron, tin and other base metals in gold-containing and palladium-containing materials, extracting gold and palladium elements with high selectivity, ensuring the product purity of the gold-containing and palladium-containing liquids, preparing for subsequent assay of the contents of gold and palladium, filtering filter residues in the hydrochloric acid treatment solution, adding aqua regia for dissolving to obtain gold-containing and palladium-containing liquids, carrying out filtration and washing to obtain a constant volume, analyzing the concentrations of gold and palladium in the gold-containing and palladium-containing liquids by adopting ICP (inductively coupled plasma), and calculating the contents of gold and palladium according to the volumes and the weighed weights of the gold-containing and palladium-containing liquids.
Description
Technical Field
The invention relates to the technical field of analytical chemistry, and relates to a method for testing gold and palladium by using gold and palladium-containing materials.
Background
The gold and palladium-containing materials generally refer to industrial waste products such as waste catalysts, anode mud and the like, are secondary resources with high added values and contain a large amount of valuable metal elements, are important resources for extracting valuable precious metals such as gold, silver, palladium, platinum and the like, and must be fully utilized to change waste into valuable. The existing gold and palladium-containing materials generally have a large amount of copper, tin and other base metals, which can influence the assay results of gold and palladium. If the base metal is not properly treated, the adsorption or the wrapping of metal compound precipitates can be caused, the detection flow of gold and palladium is interfered, and the detection results of gold and palladium are lower.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for testing gold and palladium by using gold and palladium-containing materials, which has the advantages of good process controllability, shortened detection time and accurate detection result of the content of gold and palladium.
In order to solve the technical problems, the technical scheme adopted by the invention for solving the technical problems is as follows:
a method for testing gold and palladium by using gold and palladium-containing materials comprises the following steps:
a. primarily crushing the gold-and palladium-containing solid, and then grinding the crushed gold-and palladium-containing solid to obtain gold-and palladium-containing materials;
b. adding gold-containing and palladium-containing materials into a hydrochloric acid solution, adding the materials while stirring until all the gold-containing and palladium-containing materials are added into the hydrochloric acid solution to form a hydrochloric acid treatment solution, heating the hydrochloric acid treatment solution, keeping slight boiling for a period of time, stopping heating, and cooling the hydrochloric acid treatment solution to room temperature;
c. filtering and washing the cooled hydrochloric acid cooling liquid to obtain filter residue;
d. dissolving the filter residue by aqua regia, heating the aqua regia in the dissolving process, keeping the aqua regia in a slightly boiling state for a period of time, and then stopping heating, and cooling the aqua regia to room temperature;
e. filtering and washing the dissolved aqua regia, performing constant volume on the filtrate, analyzing the concentrations of the gold and the palladium in the constant volume filtrate by adopting ICP (inductively coupled plasma), and calculating the contents of the gold and the palladium in gold and palladium-containing solids according to the volume of the constant volume filtrate and the weighed weight of gold and palladium-containing materials.
Further, in the step a, the crushed gold and palladium-containing solid is ground by a 100-mesh grinder, and a certain weight of gold and palladium-containing materials are weighed by an analytical balance.
Further, in the step b, the mass ratio of the gold-containing and palladium-containing materials to the hydrochloric acid solution is 1: 3-5.
Further, in the step b, when the hydrochloric acid treatment solution is placed on an electric furnace for heating, the power of the electric furnace is set to be 1KW, and the slightly boiling state is kept for dissolving treatment for 8-14 min.
Further, in step c, the hydrochloric acid cooling liquid is filtered and washed until the pH value of the filtrate is 6.8-7.2.
Further, in the step d, the filter residue is placed in a beaker, the aqua regia is slowly added into the beaker, the filter residue is stirred while the aqua regia is added, and when the aqua regia is heated, a glass surface dish is covered on the beaker to keep the aqua regia in a slightly boiling state.
Further, the aqua regia is prepared from nitric acid with the mass concentration of 60-65% and hydrochloric acid with the mass concentration of 30-35% according to the weight ratio of 3: 1, and mixing the components according to the volume ratio.
Further, in step d, putting the aqua regia solution on an electric furnace, heating, setting the power of the electric furnace to be 1KW, and keeping the aqua regia solution in a slightly boiling state for dissolving treatment for 12-20 min.
Further, in step e, the filtrate was put into a volumetric flask for constant volume, and the concentrations of gold and palladium in the filtrate in the volumetric flask were analyzed by ICP.
Further, the adding speed of the aqua regia is 20-40ml/min, and the aqua regia is added while stirring; the adding speed of the gold-containing and palladium-containing materials to the hydrochloric acid solution is 10-30 g/min.
The invention has the beneficial effects that:
the invention adopts the steps of carrying out primary crushing and grinding treatment on gold-containing and palladium-containing solids, adding hydrochloric acid for dissolving to obtain hydrochloric acid treatment solution, completely dissolving nickel, iron, tin and other base metals in gold-containing and palladium-containing materials, extracting gold and palladium elements with high selectivity, ensuring the product purity of the gold-containing and palladium-containing liquids, preparing for subsequent assay of the contents of gold and palladium, filtering filter residues in the hydrochloric acid treatment solution, adding aqua regia for dissolving to obtain gold-containing and palladium-containing liquids, carrying out filtration and washing to obtain a constant volume, analyzing the concentrations of gold and palladium in the gold-containing and palladium-containing liquids by adopting ICP (inductively coupled plasma), and calculating the contents of gold and palladium according to the volumes and the weighed weights of the gold-containing and palladium-containing liquids.
Detailed Description
The present invention is further described below in conjunction with specific examples to enable those skilled in the art to better understand the present invention and to practice it, but the examples are not intended to limit the present invention.
Example 1
A method for testing gold and palladium by using gold and palladium-containing materials comprises the following steps:
a. primarily crushing a gold-containing solid and a palladium-containing solid, grinding the crushed gold-containing solid and palladium-containing solid by a 100-mesh grinder, and weighing a gold-containing material and a palladium-containing material by a certain weight by using an analytical balance;
b. adding gold-containing and palladium-containing materials into a hydrochloric acid solution, wherein the mass ratio of the gold-containing and palladium-containing materials to the hydrochloric acid solution is 1: 3, adding the gold-containing and palladium-containing materials while stirring until the adding speed of the hydrochloric acid solution is 10g/min, adding all the gold-containing and palladium-containing materials into the hydrochloric acid solution to form hydrochloric acid treatment liquid, heating the hydrochloric acid treatment liquid on an electric furnace, setting the power of the electric furnace to be 1KW, keeping the micro-boiling state for dissolving treatment for 14min, stopping heating, and cooling the hydrochloric acid treatment liquid to room temperature;
c. filtering and washing the cooled hydrochloric acid cooling liquid to obtain filter residues, wherein the pH value of the filtered liquid is 7.2 after filtering and washing;
d. placing filter residues in a beaker, slowly adding aqua regia into the beaker at the speed of 20ml/min, and adding the aqua regia while stirring, wherein the aqua regia is prepared by mixing nitric acid with the mass concentration of 60% and hydrochloric acid with the mass concentration of 35% according to the ratio of 3: 1, adding the filter residue while stirring for dissolving, setting the power of an electric furnace to be 1KW when putting the aqua regia on the electric furnace for heating in the dissolving process, covering a glass watch glass on a beaker, keeping the micro-boiling state for dissolving treatment for 20min, stopping heating, and cooling the aqua regia to room temperature;
e. and filtering and washing the dissolved aqua regia, putting the filtrate into a volumetric flask for constant volume, analyzing the concentrations of the gold and the palladium in the filtrate in the volumetric flask by adopting ICP (inductively coupled plasma), and calculating the contents of the gold and the palladium in gold and palladium-containing solids according to the volume of the filtrate after constant volume and the weighed weight of the gold and palladium-containing materials.
The invention adopts the steps of carrying out primary crushing and grinding treatment on gold-containing and palladium-containing solids, adding hydrochloric acid for dissolving to obtain hydrochloric acid treatment solution, completely dissolving nickel, iron, tin and other base metals in gold-containing and palladium-containing materials, extracting gold and palladium elements with high selectivity, ensuring the product purity of the gold-containing and palladium-containing liquids, preparing for subsequent assay of the contents of gold and palladium, filtering filter residues in the hydrochloric acid treatment solution, adding aqua regia for dissolving to obtain gold-containing and palladium-containing liquids, carrying out filtration and washing to obtain a constant volume, analyzing the concentrations of gold and palladium in the gold-containing and palladium-containing liquids by adopting ICP (inductively coupled plasma), and calculating the contents of gold and palladium according to the volumes and the weighed weights of the gold-containing and palladium-containing liquids.
b. Adding gold-containing and palladium-containing materials into a hydrochloric acid solution, wherein the mass ratio of the gold-containing and palladium-containing materials to the hydrochloric acid solution is 1: 3, adding the gold-containing and palladium-containing materials while stirring until the adding speed of the hydrochloric acid solution is 10g/min, adding all the gold-containing and palladium-containing materials into the hydrochloric acid solution to form hydrochloric acid treatment liquid, heating the hydrochloric acid treatment liquid on an electric furnace, setting the power of the electric furnace to be 1KW, keeping the micro-boiling state for dissolving treatment for 14min, stopping heating, and cooling the hydrochloric acid treatment liquid to room temperature;
in the invention, in the step b, after the gold and palladium-containing materials are completely added into the hydrochloric acid solution, 0.4-0.8L of hydrochloric acid solution is added, the mixture is stirred for 1-10min, then the mixture is kept standing for 2-5min, the heating process is continued, and the hydrochloric acid solution is added to ensure that the nickel, iron, tin and other base metals are completely dissolved, so that the purity of filter residues is improved, and the accuracy of the test result is improved.
Example 2
A method for testing gold and palladium by using gold and palladium-containing materials comprises the following steps:
a. primarily crushing a gold-containing solid and a palladium-containing solid, grinding the crushed gold-containing solid and palladium-containing solid by a 100-mesh grinder, and weighing a gold-containing material and a palladium-containing material by a certain weight by using an analytical balance;
b. adding gold-containing and palladium-containing materials into a hydrochloric acid solution, wherein the mass ratio of the gold-containing and palladium-containing materials to the hydrochloric acid solution is 1: 4, adding the gold-containing and palladium-containing materials while stirring until the adding speed of the hydrochloric acid solution is 15g/min, adding all the gold-containing and palladium-containing materials into the hydrochloric acid solution to form hydrochloric acid treatment liquid, heating the hydrochloric acid treatment liquid on an electric furnace, setting the power of the electric furnace to be 1KW, keeping the micro-boiling state for dissolving treatment for 12min, stopping heating, and cooling the hydrochloric acid treatment liquid to room temperature;
c. filtering and washing the cooled hydrochloric acid cooling liquid to obtain filter residues, wherein the pH value of the filtered liquid is 7.1 after filtering and washing;
d. placing filter residues in a beaker, slowly adding aqua regia into the beaker at the speed of 25ml/min, and adding the aqua regia while stirring, wherein the aqua regia is prepared by mixing nitric acid with the mass concentration of 65% and hydrochloric acid with the mass concentration of 30% according to the ratio of 3: 1, adding the filter residue while stirring for dissolving, setting the power of an electric furnace to be 1KW when putting the aqua regia on the electric furnace for heating in the dissolving process, covering a glass watch glass on a beaker, keeping the micro-boiling state for dissolving treatment for 18min, stopping heating, and cooling the aqua regia to room temperature;
e. and filtering and washing the dissolved aqua regia, putting the filtrate into a volumetric flask for constant volume, analyzing the concentrations of the gold and the palladium in the filtrate in the volumetric flask by adopting ICP (inductively coupled plasma), and calculating the contents of the gold and the palladium in gold and palladium-containing solids according to the volume of the filtrate after constant volume and the weighed weight of the gold and palladium-containing materials.
Example 3
A method for testing gold and palladium by using gold and palladium-containing materials comprises the following steps:
a. primarily crushing a gold-containing solid and a palladium-containing solid, grinding the crushed gold-containing solid and palladium-containing solid by a 100-mesh grinder, and weighing a gold-containing material and a palladium-containing material by a certain weight by using an analytical balance;
b. adding gold-containing and palladium-containing materials into a hydrochloric acid solution, wherein the mass ratio of the gold-containing and palladium-containing materials to the hydrochloric acid solution is 1: 3, adding the gold-containing and palladium-containing materials while stirring until the adding speed of the hydrochloric acid solution is 20g/min, adding all the gold-containing and palladium-containing materials into the hydrochloric acid solution to form hydrochloric acid treatment liquid, heating the hydrochloric acid treatment liquid on an electric furnace, setting the power of the electric furnace to be 1KW, keeping the micro-boiling state for dissolving treatment for 10min, stopping heating, and cooling the hydrochloric acid treatment liquid to room temperature;
c. filtering and washing the cooled hydrochloric acid cooling liquid to obtain filter residues, wherein the pH value of the filtered liquid is 7 after filtering and washing;
d. placing filter residues in a beaker, slowly adding aqua regia into the beaker at the speed of 30ml/min, and adding the aqua regia while stirring, wherein the aqua regia is prepared by mixing nitric acid with the mass concentration of 65% and hydrochloric acid with the mass concentration of 31% according to the ratio of 3: 1, adding the filter residue while stirring for dissolving, setting the power of an electric furnace to be 1KW when putting the aqua regia on the electric furnace for heating in the dissolving process, covering a glass watch glass on a beaker, keeping the micro-boiling state for dissolving treatment for 15min, stopping heating, and cooling the aqua regia to room temperature;
e. and filtering and washing the dissolved aqua regia, putting the filtrate into a volumetric flask for constant volume, analyzing the concentrations of the gold and the palladium in the filtrate in the volumetric flask by adopting ICP (inductively coupled plasma), and calculating the contents of the gold and the palladium in gold and palladium-containing solids according to the volume of the filtrate after constant volume and the weighed weight of the gold and palladium-containing materials.
Example 4
A method for testing gold and palladium by using gold and palladium-containing materials comprises the following steps:
a. primarily crushing a gold-containing solid and a palladium-containing solid, grinding the crushed gold-containing solid and palladium-containing solid by a 100-mesh grinder, and weighing a gold-containing material and a palladium-containing material by a certain weight by using an analytical balance;
b. adding gold-containing and palladium-containing materials into a hydrochloric acid solution, wherein the mass ratio of the gold-containing and palladium-containing materials to the hydrochloric acid solution is 1: 3, adding the gold-containing and palladium-containing materials while stirring until the adding speed of the hydrochloric acid solution is 25g/min, adding all the gold-containing and palladium-containing materials into the hydrochloric acid solution to form hydrochloric acid treatment liquid, heating the hydrochloric acid treatment liquid on an electric furnace, setting the power of the electric furnace to be 1KW, keeping the micro-boiling state for dissolving treatment for 9min, stopping heating, and cooling the hydrochloric acid treatment liquid to room temperature;
c. filtering and washing the cooled hydrochloric acid cooling liquid to obtain filter residues, wherein the pH value of the filtered liquid is 7 after filtering and washing;
d. placing filter residues in a beaker, slowly adding aqua regia into the beaker at the speed of 35ml/min, and adding the aqua regia while stirring, wherein the aqua regia is prepared by mixing nitric acid with the mass concentration of 63% and hydrochloric acid with the mass concentration of 32% according to the ratio of 3: 1, adding the filter residue while stirring for dissolving, setting the power of an electric furnace to be 1KW when putting the aqua regia on the electric furnace for heating in the dissolving process, covering a glass watch glass on a beaker, keeping the glass watch glass in a slightly boiling state for dissolving treatment for 14min, stopping heating, and cooling the aqua regia to room temperature;
e. and filtering and washing the dissolved aqua regia, putting the filtrate into a volumetric flask for constant volume, analyzing the concentrations of the gold and the palladium in the filtrate in the volumetric flask by adopting ICP (inductively coupled plasma), and calculating the contents of the gold and the palladium in gold and palladium-containing solids according to the volume of the filtrate after constant volume and the weighed weight of the gold and palladium-containing materials.
Example 5
A method for testing gold and palladium by using gold and palladium-containing materials comprises the following steps:
a. primarily crushing a gold-containing solid and a palladium-containing solid, grinding the crushed gold-containing solid and palladium-containing solid by a 100-mesh grinder, and weighing a gold-containing material and a palladium-containing material by a certain weight by using an analytical balance;
b. adding gold-containing and palladium-containing materials into a hydrochloric acid solution, wherein the mass ratio of the gold-containing and palladium-containing materials to the hydrochloric acid solution is 1: 5, adding the gold-containing and palladium-containing materials while stirring until the adding speed of the hydrochloric acid solution is 30g/min, adding all the gold-containing and palladium-containing materials into the hydrochloric acid solution to form hydrochloric acid treatment liquid, heating the hydrochloric acid treatment liquid on an electric furnace, setting the power of the electric furnace to be 1KW, keeping the micro-boiling state for dissolving treatment for 8min, stopping heating, and cooling the hydrochloric acid treatment liquid to room temperature;
c. filtering and washing the cooled hydrochloric acid cooling liquid to obtain filter residues, wherein the pH value of the filtered liquid is 6.8 after filtering and washing;
d. placing filter residues in a beaker, slowly adding aqua regia into the beaker at the speed of 40ml/min, and adding the aqua regia while stirring, wherein the aqua regia is prepared by mixing nitric acid with the mass concentration of 64% and hydrochloric acid with the mass concentration of 31% according to the ratio of 3: 1, adding the filter residue while stirring for dissolving, setting the power of an electric furnace to be 1KW when putting the aqua regia on the electric furnace for heating in the dissolving process, covering a glass watch glass on a beaker, keeping the micro-boiling state for dissolving treatment for 12min, stopping heating, and cooling the aqua regia to room temperature;
e. and filtering and washing the dissolved aqua regia, putting the filtrate into a volumetric flask for constant volume, analyzing the concentrations of the gold and the palladium in the filtrate in the volumetric flask by adopting ICP (inductively coupled plasma), and calculating the contents of the gold and the palladium in gold and palladium-containing solids according to the volume of the filtrate after constant volume and the weighed weight of the gold and palladium-containing materials.
Example 6
A method for testing gold and palladium by using gold and palladium-containing materials comprises the following steps:
a. primarily crushing a gold-containing solid and a palladium-containing solid, grinding the crushed gold-containing solid and palladium-containing solid by a 100-mesh grinder, and weighing a gold-containing material and a palladium-containing material by a certain weight by using an analytical balance;
b. adding gold-containing and palladium-containing materials into a hydrochloric acid solution, wherein the mass ratio of the gold-containing and palladium-containing materials to the hydrochloric acid solution is 1: 3, adding the gold-containing and palladium-containing materials while stirring until the adding speed of the hydrochloric acid solution is 18g/min, adding all the gold-containing and palladium-containing materials into the hydrochloric acid solution to form hydrochloric acid treatment liquid, heating the hydrochloric acid treatment liquid on an electric furnace, setting the power of the electric furnace to be 1KW, keeping the micro-boiling state for dissolving treatment for 11min, stopping heating, and cooling the hydrochloric acid treatment liquid to room temperature;
c. filtering and washing the cooled hydrochloric acid cooling liquid to obtain filter residues, wherein the pH value of the filtered liquid is 7 after filtering and washing;
d. placing filter residues in a beaker, slowly adding aqua regia into the beaker at the speed of 32ml/min, and adding the aqua regia while stirring, wherein the aqua regia is prepared by mixing nitric acid with the mass concentration of 65% and hydrochloric acid with the mass concentration of 31% according to the ratio of 3: 1, adding the filter residue while stirring for dissolving, setting the power of an electric furnace to be 1KW when putting the aqua regia on the electric furnace for heating in the dissolving process, covering a glass watch glass on a beaker, keeping the micro-boiling state for dissolving treatment for 16min, stopping heating, and cooling the aqua regia to room temperature;
e. and filtering and washing the dissolved aqua regia, putting the filtrate into a volumetric flask for constant volume, analyzing the concentrations of the gold and the palladium in the filtrate in the volumetric flask by adopting ICP (inductively coupled plasma), and calculating the contents of the gold and the palladium in gold and palladium-containing solids according to the volume of the filtrate after constant volume and the weighed weight of the gold and palladium-containing materials.
In conclusion, the method for testing gold and palladium by using the gold and palladium-containing materials can accurately test the contents of gold and palladium elements, simplifies the gold and palladium testing process, reduces the use cost, and can effectively reduce the impurity residual rate and improve the precision of the testing result.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (10)
1. A method for testing gold and palladium by using gold and palladium-containing materials is characterized by comprising the following steps:
a. primarily crushing the gold-and palladium-containing solid, and then grinding the crushed gold-and palladium-containing solid to obtain gold-and palladium-containing materials;
b. adding gold-containing and palladium-containing materials into a hydrochloric acid solution, adding the materials while stirring until all the gold-containing and palladium-containing materials are added into the hydrochloric acid solution to form a hydrochloric acid treatment solution, heating the hydrochloric acid treatment solution, keeping slight boiling for a period of time, stopping heating, and cooling the hydrochloric acid treatment solution to room temperature;
c. filtering and washing the cooled hydrochloric acid cooling liquid to obtain filter residue;
d. dissolving the filter residue by aqua regia, heating the aqua regia in the dissolving process, keeping the aqua regia in a slightly boiling state for a period of time, and then stopping heating, and cooling the aqua regia to room temperature;
e. filtering and washing the dissolved aqua regia, performing constant volume on the filtrate, analyzing the concentrations of the gold and the palladium in the constant volume filtrate by adopting ICP (inductively coupled plasma), and calculating the contents of the gold and the palladium in gold and palladium-containing solids according to the volume of the constant volume filtrate and the weighed weight of gold and palladium-containing materials.
2. The method for assaying gold and palladium according to claim 1, wherein in step a, the crushed gold and palladium-containing solid is ground by a 100-mesh grinder, and a certain weight of gold and palladium-containing material is weighed by an analytical balance.
3. The method for assaying gold and palladium according to claim 1, wherein in step b, the mass ratio of the gold and palladium containing material to the hydrochloric acid solution is 1: 3-5.
4. The method for assaying gold and palladium according to claim 1, wherein in step b, the hydrochloric acid treatment solution is heated in an electric furnace with a power of 1KW for dissolution treatment for 8-14min while maintaining a slightly boiling state.
5. The method for assaying gold and palladium according to claim 1, wherein the hydrochloric acid cooling liquid is filtered and washed until the pH value of the filtrate is 6.8-7.2 in step c.
6. The method according to claim 1, wherein in step d, the filter residue is placed in a beaker, aqua regia is slowly added into the beaker, the filter residue is stirred while the aqua regia is added, and a glass watch glass is covered on the beaker to keep the aqua regia in a slightly boiling state while the aqua regia is heated.
7. The method for assaying gold and palladium according to claim 1, wherein the aqua regia is prepared by mixing nitric acid with a mass concentration of 60-65% and hydrochloric acid with a mass concentration of 30-35% according to a ratio of 3: 1, and mixing the components according to the volume ratio.
8. The method for assaying gold and palladium according to claim 1, wherein in step d, the aqua regia solution is placed on an electric furnace and heated, the power of the electric furnace is set to 1KW, and the dissolution treatment is maintained in a micro-boiling state for 12-20 min.
9. The method for testing gold and palladium according to the gold and palladium-containing material of claim 1, wherein in the step e, the filtrate is put into a volumetric flask for constant volume, and the ICP is adopted to analyze the concentrations of gold and palladium in the filtrate in the volumetric flask.
10. The method for assaying gold and palladium according to a gold and palladium-containing material of claim 1, wherein the aqua regia is added at a rate of 20-40ml/min and stirred; the adding speed of the gold-containing and palladium-containing materials to the hydrochloric acid solution is 10-30 g/min.
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