CN114739983A - Method for determining high-content copper, lead and zinc in polymetallic ore and copper-lead-zinc alloy by utilizing ICP-AES (inductively coupled plasma-atomic emission Spectrometry) - Google Patents

Method for determining high-content copper, lead and zinc in polymetallic ore and copper-lead-zinc alloy by utilizing ICP-AES (inductively coupled plasma-atomic emission Spectrometry) Download PDF

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CN114739983A
CN114739983A CN202210384238.3A CN202210384238A CN114739983A CN 114739983 A CN114739983 A CN 114739983A CN 202210384238 A CN202210384238 A CN 202210384238A CN 114739983 A CN114739983 A CN 114739983A
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copper
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叶元顺
罗大芳
邓碧霞
钱玲瑶
车晓艳
余联凤
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Kunming Institute Of Geological Exploration General Administration Of Metallurgical Geology Of China
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Abstract

The invention relates to a method for determining high-content copper, lead and zinc in polymetallic ores and copper-lead-zinc alloys by utilizing ICP-AES (inductively coupled plasma-atomic emission Spectrometry), which belongs to the technical field of analysis and test of an ICP-AES method and comprises the following specific steps of: decomposing a polymetallic ore and a copper-lead-zinc alloy sample into a wet salt shape by using aqua regia; then adding a hydrochloric acid-ammonium acetate mixed extracting solution, and heating for micro-boiling for 10-15 min; the extracted sample is subjected to constant volume extraction by using deionized water in a 250mL volumetric flask; shaking up the sample after constant volume, standing and clarifying; dividing 5mL of the supernatant solution into 50mL of colorimetric tubes by using a 10mL high-volume pipette, adding 5mL of hydrochloric acid-ammonium acetate mixed extract, fixing the volume and shaking up; and carrying out ICP-AES test on the obtained sample, and determining the contents of copper, lead and zinc. The method avoids complex operation, solves the problem of serious low test result caused by mutual influence of lead, copper and zinc during testing, and can improve the test accuracy of high-content copper, lead and zinc in the polymetallic ore and the copper-lead-zinc alloy.

Description

Method for determining high-content copper, lead and zinc in polymetallic ore and copper-lead-zinc alloy by utilizing ICP-AES (inductively coupled plasma-atomic emission Spectrometry)
Technical Field
The invention relates to the technical field of analysis and test by an ICP-AES method, in particular to a method for determining high-content copper, lead and zinc in polymetallic ores and copper, lead and zinc alloys by utilizing the ICP-AES method.
Background
At present, high-content lead and zinc in polymetallic ores and copper-lead-zinc alloys adopt an EDTA volumetric method, and copper adopts an iodometric method; the determination principle in the lead determination process is that a sample is decomposed by hydrochloric acid and nitric acid, lead is generated into lead sulfate precipitate in the presence of sulfuric acid, the lead precipitate separated by filtration is dissolved by acetic acid-sodium acetate buffer solution, xylenol orange is used as an indicator, and EDTA standard solution is used for titration; the determination principle in the zinc determination process is that a sample is decomposed by hydrochloric acid and nitric acid, lead is generated into lead sulfate precipitate in the presence of sulfate radical, ammonia water is used for adjusting pH to form precipitate, zinc and ammonium ions are complexed, interference such as iron removal, chromium removal and the like is separated by filtration, the zinc and the ammonium ions are dissolved in acetic acid-sodium acetate buffer solution, xylenol orange is used as an indicator, and EDTA standard solution is used for titration, but copper ions cannot be separated in the process, a large amount of copper ions cannot be masked, and the determination of zinc is interfered; the determination principle of the copper determination process is that a sample is decomposed by hydrochloric acid and nitric acid, copper exists in the form of copper sulfate under the treatment of sulfuric acid smoking, divalent copper ions in a buffer solution after water extraction react with potassium iodide to generate an iodine simple substance, starch is used as an indicator, sodium thiosulfate standard solution is used for titration, and if a large amount of lead exists in the form of lead sulfate precipitation in the process, titration end point judgment is seriously influenced, and the copper content in polymetallic ore and copper-lead-zinc alloy cannot be accurately determined.
The traditional test method has the following defects: one is that the analysis period is long, and copper, lead and zinc in the polymetallic ore and the copper-lead-zinc alloy need to be respectively tested; secondly, when the copper, lead and zinc contents in the polymetallic ore and the copper-lead-zinc alloy are high, the copper affects the determination of the zinc, and the lead affects the determination of the copper, so that the copper, lead and zinc contents in the polymetallic ore and the copper-lead-zinc alloy can not be accurately obtained; thirdly, the influence factor is large, and as the analysis period is long, the steps are multiple, the analyst must have rich experience and sophisticated technology, the test result is distorted when careless mistakes occur in any link, and the result accuracy cannot be guaranteed.
Disclosure of Invention
In order to overcome the problems in the background art, the invention provides a method for determining high-content copper, lead and zinc in the polymetallic ore and the copper-lead-zinc alloy by utilizing ICP-AES, which avoids complicated operation, solves the problem that the test result is seriously low due to the mutual influence of lead, copper and zinc during the test, and can improve the test accuracy of the high-content copper, lead and zinc in the polymetallic ore and the copper-lead-zinc alloy.
In order to realize the purpose, the invention is realized by the following technical scheme:
the method for measuring high-content copper, lead and zinc in the polymetallic ore and the copper-lead-zinc alloy by utilizing the ICP-AES comprises the following specific steps:
1) decomposing a polymetallic ore and a copper-lead-zinc alloy sample into a wet salt shape by using aqua regia;
2) adding a hydrochloric acid-ammonium acetate mixed extracting solution into a wet salt sample subjected to aqua regia decomposition, and heating for micro-boiling for 10-15 min;
3) fixing the volume of the sample extracted in the step 2) in a 250mL volumetric flask by using deionized water;
4) shaking up the sample after constant volume, standing and clarifying;
5) dividing 5mL of the supernatant solution obtained in the step 4) into 50mL of colorimetric tubes by using a 10mL high-intensity pipette, adding 5mL of hydrochloric acid-ammonium acetate mixed extracting solution, metering the volume and shaking up;
6) and (3) carrying out ICP-AES (inductively coupled plasma-atomic emission Spectrometry) test on the sample obtained in the step 5) and determining the contents of copper, lead and zinc.
Preferably, in the step 1), the use ratio of the aqua regia is 0.05 g-0.5 g: 20 mL.
Preferably, in the step 2), the medium of the hydrochloric acid-ammonium acetate mixed extracting solution is 1+1 hydrochloric acid, the concentration of ammonium acetate is 200g/L, and the use ratio of the hydrochloric acid-ammonium acetate mixed extracting solution is 0.05 g-0.5 g: 50 mL.
Further, in step 6), the ICP-AES test conditions are: the power of the high-frequency generator is 1.15 KW; analyzing the pump speed at 50 rpm; the stabilization time is 15 s; the auxiliary gas flow is 0.5L/min; the vertical observation height is 12.0 mm; analytical line for copper 324.75 nm; analytical line for lead 220.35 nm; analytical line for zinc 213.86 nm.
Further, the ICP-AES test is used for drawing the preparation of an ICP-AES standard working curve: taking 0.00mL, 0.50mL, 5.00mL, 10.00mL, 20.00mL and 40.00mL of copper-lead-zinc mixed standard solution with the concentration of 1000 mu g/mL, respectively placing the mixed standard solution in a group of 100mL volumetric flasks, adding 10mL of hydrochloric acid-ammonium acetate mixed extracting solution, diluting to the scale with deionized water, and shaking up.
The invention has the beneficial effects that: when the polymetallic ore and the copper-lead-zinc alloy sample are treated, a certain amount of ammonium acetate is added for treatment, so that the problem that the test result is seriously low due to mutual influence when the contents of lead, copper and zinc ions are high can be solved, the test accuracy of high-content copper, lead and zinc in the polymetallic ore and the copper-lead-zinc alloy can be improved, and in addition, the contents of primary and secondary elements such as chromium, cadmium, nickel, cobalt, iron, manganese and the like in the polymetallic ore and the copper-lead-zinc alloy sample can be simultaneously analyzed.
Detailed Description
Example 1
Weighing 0.1000g of polymetallic ore samples (the contents of copper, lead and zinc are respectively 9.13%, 29.62% and 17.56%), placing the polymetallic ore samples in a 100mL beaker, adding a little water for wetting, and decomposing the polymetallic ore samples into wet salt by using aqua regia, wherein the use ratio of the polymetallic ore samples to the aqua regia is 0.1 g: 20 mL; adding hydrochloric acid-ammonium acetate mixed extract into a wet salt sample subjected to aqua regia decomposition, wherein the medium of the hydrochloric acid-ammonium acetate mixed extract is 1+1 hydrochloric acid, the concentration of ammonium acetate is 200g/L, and the use ratio is 0.05 g: heating for micro-boiling for 10-15 min at 50 mL; using deionized water to perform constant volume treatment on the polymetallic ore sample in a 250mL volumetric flask; shaking up the sample after constant volume, standing and clarifying; taking 5mL of the supernatant solution by using a 10mL heavy pipette, adding 5mL of hydrochloric acid-ammonium acetate mixed extracting solution into a 50mL colorimetric tube, fixing the volume and shaking up; and carrying out ICP-AES test on the obtained sample, and determining the contents of copper, lead and zinc.
And drawing an ICP-AES standard working curve for ICP-AES test for preparation: taking 0.00mL, 0.50mL, 5.00mL, 10.00mL, 20.00mL and 40.00mL of copper-lead-zinc mixed standard solution with the concentration of 1000 mu g/mL, respectively placing the mixed standard solution in a group of 100mL volumetric flasks, adding 10mL of hydrochloric acid-ammonium acetate mixed extracting solution, diluting to a scale with deionized water, shaking up and testing.
The ICP-AES test conditions are as follows: the power of the high-frequency generator is 1.15 KW; analyzing the pump speed at 50 rpm; the stabilization time is 15 s; the auxiliary gas flow is 1.2L/min; the flow rate of the atomizer is 0.5L/min; the vertical observation height is 12.0 mm; analytical line for copper 324.75 nm; analytical line for lead 220.35 nm; analytical line for zinc 213.86 nm.
Example 2
Weighing 0.0500g of a copper-lead-zinc alloy sample (the contents of copper, lead and zinc are respectively 15.32%, 24.37% and 39.22%), putting the copper-lead-zinc alloy sample into a 100mL beaker, adding a little water for wetting, and then decomposing the copper-lead-zinc alloy sample into a wet salt shape by using aqua regia, wherein the use ratio of the polymetallic ore sample to the aqua regia is 0.5 g: 20 mL; adding hydrochloric acid-ammonium acetate mixed extract into a wet salt sample subjected to aqua regia decomposition, wherein the medium of the hydrochloric acid-ammonium acetate mixed extract is 1+1 hydrochloric acid, the concentration of ammonium acetate is 200g/L, and the use ratio is 0.5 g: heating for micro-boiling for 10-15 min at 50 mL; using deionized water to perform constant volume treatment on the polymetallic ore sample in a 250mL volumetric flask; shaking up the sample after constant volume, standing and clarifying; dividing 5mL of the supernatant solution into 50mL of colorimetric tubes by using a 10mL high-volume pipette, adding 5mL of hydrochloric acid-ammonium acetate mixed extract, fixing the volume and shaking up; and carrying out ICP-AES test on the obtained sample, and determining the contents of copper, lead and zinc.
And drawing an ICP-AES standard working curve for ICP-AES test for preparation: taking 0.00mL, 0.50mL, 5.00mL, 10.00mL, 20.00mL and 40.00mL of copper-lead-zinc mixed standard solution with the concentration of 1000 mu g/mL, respectively placing the mixed standard solution in a group of 100mL volumetric flasks, adding 10mL of hydrochloric acid-ammonium acetate mixed extracting solution, diluting to a scale with deionized water, shaking up and testing.
The ICP-AES test conditions are as follows: the power of the high-frequency generator is 1.15 KW; analyzing the pump speed at 50 rpm; the stabilization time is 15 s; the auxiliary gas flow is 1.2L/min; the flow rate of the atomizer is 0.5L/min; the vertical observation height is 12.0 mm; analytical line for copper 324.75 nm; analytical line for lead 220.35 nm; analytical line for zinc 213.86 nm.
Comparative example 1
Weighing 0.1000g of polymetallic ore samples (the contents of copper, lead and zinc are respectively 9.13%, 29.62% and 17.56%), placing the polymetallic ore samples in a 100mL beaker, adding a little water for wetting, and then using aqua regia for decomposition, wherein the use ratio of the polymetallic ore samples to the aqua regia is 0.1 g: 20 mL; using deionized water to perform constant volume treatment on the polymetallic ore sample in a 250mL volumetric flask; shaking up the sample after constant volume, standing and clarifying; dividing 5mL of the supernatant solution into 50mL of colorimetric tubes by using a 10mL high-volume pipette, adding deionized water to a constant volume, and shaking up; and carrying out ICP-AES test on the obtained sample, and determining the contents of copper, lead and zinc.
And drawing an ICP-AES standard working curve for ICP-AES test for preparation: taking 0.00mL, 0.50mL, 5.00mL, 10.00mL, 20.00mL and 40.00mL of copper-lead-zinc mixed standard solution with the concentration of 1000 mu g/mL, respectively placing the mixed standard solution into a group of 100mL volumetric flasks, diluting the mixed standard solution to a scale with deionized water, shaking up and measuring.
The ICP-AES test conditions are as follows: the power of the high-frequency generator is 1.15 KW; analyzing the pump speed at 50 rpm; the stabilization time is 15 s; the auxiliary gas flow is 1.2L/min; the flow rate of the atomizer is 0.5L/min; the vertical observation height is 12.0 mm; analytical line for copper 324.75 nm; analytical line for lead 220.35 nm; analytical line for zinc 213.86 nm.
Comparative example 2
Weighing 0.0500g of a copper-lead-zinc alloy sample (the contents of copper, lead and zinc are respectively 15.32%, 24.37% and 39.22%), placing the sample in a 100mL beaker, adding a little water for wetting, and decomposing the sample into a wet salt shape by using aqua regia, wherein the using ratio of the polymetallic ore sample to the aqua regia is 0.5 g: 20 mL; fixing the volume of the treated sample in a 250mL volumetric flask by using deionized water; shaking up the sample after constant volume, standing and clarifying; dividing 5mL of the supernatant solution into 50mL of colorimetric tubes by using a 10mL high-volume pipette, adding deionized water to a constant volume, and shaking up; and carrying out ICP-AES test on the obtained sample, and determining the contents of copper, lead and zinc.
And drawing an ICP-AES standard working curve for ICP-AES test for preparation: taking 0.00mL, 0.50mL, 5.00mL, 10.00mL, 20.00mL and 40.00mL of copper-lead-zinc mixed standard solution with the concentration of 1000 mu g/mL, respectively placing the mixed standard solution into a group of 100mL volumetric flasks, diluting the mixed standard solution to a scale with deionized water, shaking up and measuring.
The ICP-AES test conditions are as follows: the power of the high-frequency generator is 1.15 KW; analyzing the pump speed at 50 rpm; the stabilization time is 15 s; the auxiliary gas flow is 1.2L/min; the flow rate of the atomizer is 0.5L/min; the vertical observation height is 12.0 mm; analytical line for copper 324.75 nm; analytical line for lead 220.35 nm; analytical line for zinc 213.86 nm.
The test results of the inventive examples and comparative examples are shown in Table 1:
TABLE 1 comparison of test results of examples and comparative examples
Figure BDA0003594141740000061
Note: statistics of test results for 6 parallel samples
As can be seen from table 1, the test results of the test samples of examples 1 and 2 are substantially the same as the reference values, the relative error is small, and the accuracy and precision are high; comparative examples 1 and 2 are the conventional ICP-AES test method, and the test results showed deviation from the reference value, and large precision and relative error, without using hydrochloric acid-ammonium acetate.
When the high-content copper-lead-zinc polymetallic ore and the copper-lead-zinc alloy sample are treated, a certain amount of ammonium acetate is added for treatment, so that the high-content lead and acetate can generate a stable complex, and the copper, zinc and ammonium ions generate a stable complex, so that the problem that the test result is seriously low due to mutual influence when the contents of the lead, copper and zinc ions are high is solved, the test accuracy of the high-content copper-lead-zinc in the polymetallic ore and the copper-lead-zinc alloy can be improved, and in addition, the contents of primary and secondary elements such as chromium, cadmium, nickel, cobalt, iron, manganese and the like in the polymetallic ore and the copper-lead-zinc alloy sample can be simultaneously analyzed.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.

Claims (5)

1. The method for measuring high-content copper, lead and zinc in the polymetallic ore and the copper-lead-zinc alloy by utilizing the ICP-AES is characterized by comprising the following specific steps of:
1) decomposing a polymetallic ore and a copper-lead-zinc alloy sample into a wet salt shape by using aqua regia;
2) adding a hydrochloric acid-ammonium acetate mixed extracting solution into a wet salt sample subjected to aqua regia decomposition, and heating for micro-boiling for 10-15 min;
3) fixing the volume of the sample extracted in the step 2) in a 250mL volumetric flask by using deionized water;
4) shaking up the sample after constant volume, standing and clarifying;
5) dividing 5mL of the supernatant solution obtained in the step 4) into 50mL of colorimetric tubes by using a 10mL high-intensity pipette, adding 5mL of hydrochloric acid-ammonium acetate mixed extracting solution, metering the volume and shaking up;
6) and (3) carrying out ICP-AES (inductively coupled plasma-atomic emission Spectrometry) test on the sample obtained in the step 5) and determining the contents of copper, lead and zinc.
2. The method for measuring high-content copper, lead and zinc in polymetallic ores and copper, lead and zinc alloys by utilizing ICP-AES as recited in claim 1, wherein the method comprises the following steps: in the step 1), the use ratio of the aqua regia is 0.05 g-0.5 g: 20 mL.
3. The method for determining high-content copper, lead and zinc in the polymetallic ore and the copper, lead and zinc alloy by utilizing ICP-AES as claimed in claim 1, wherein the method comprises the following steps: in the step 2), the medium of the hydrochloric acid-ammonium acetate mixed extracting solution is 1+1 hydrochloric acid, the concentration of ammonium acetate is 200g/L, and the use ratio of the hydrochloric acid-ammonium acetate mixed extracting solution is 0.05 g-0.5 g: 50 mL.
4. The method for determining high-content copper, lead and zinc in the polymetallic ore and the copper, lead and zinc alloy by utilizing ICP-AES as claimed in claim 1, wherein the method comprises the following steps: in the step 6), the ICP-AES test conditions are as follows: the power of the high-frequency generator is 1.15 KW; analyzing the pump speed at 50 rpm; the stabilization time is 15 s; the auxiliary gas flow is 0.5L/min; the vertical observation height is 12.0 mm; analytical line for copper 324.75 nm; analytical line for lead 220.35 nm; analytical line for zinc 213.86 nm.
5. The method for measuring high-content copper, lead and zinc in polymetallic ores and copper, lead and zinc alloys by utilizing ICP-AES as recited in claim 1, wherein the method comprises the following steps: preparing an ICP-AES standard working curve drawn by the ICP-AES test: taking 0.00mL, 0.50mL, 5.00mL, 10.00mL, 20.00mL and 40.00mL of copper-lead-zinc mixed standard solution with the concentration of 1000 mu g/mL, respectively placing the mixed standard solution in a group of 100mL volumetric flasks, adding 10mL of hydrochloric acid-ammonium acetate mixed extracting solution, diluting to the scale with deionized water, and shaking up.
CN202210384238.3A 2022-04-13 2022-04-13 Method for determining high-content copper, lead and zinc in polymetallic ore and copper-lead-zinc alloy by utilizing ICP-AES (inductively coupled plasma-atomic emission Spectrometry) Pending CN114739983A (en)

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