Method for detecting content of indium in tin smoke dust

Abstract

The invention discloses a method for detecting the content of indium in tin smoke dust, which belongs to the technical field of analysis and detection, and specifically comprises the following steps: (1) adding hydrochloric acid and first nitric acid into the tin smoke dust, heating and steaming until the tin smoke dust is nearly dry, then adding second nitric acid for dissolving, fixing the volume, and filtering to obtain filtrate and filter residues; and (2) carbonizing the filter residue, melting the carbonized filter residue with sodium peroxide, sequentially leaching with water, adjusting the pH value, acidizing and fixing the volume after melting, and finally measuring to obtain the content of indium in the filter residue, and (3) measuring the filtrate to obtain the indium content of the filtrate, wherein the sum of the indium content of the filter residue and the indium content of the filter residue is the indium content in the tin smoke. The detection method provided by the invention can reduce the error rate of indium determination in the tin smoke dust, thereby accurately providing the content of indium in the tin smoke dust.

Description

Technical Field

[0001] The invention belongs to the technical field of analysis and detection, and in particular relates to a method for detecting the indium content in tin smoke. Background Art

[0002] Tin smoke is a mixture of fine particles and smoke produced during the smelting, processing and related industrial production of tin. It usually contains tin compounds, other metal impurities, oxides and smoke produced by combustion. It is an important secondary resource of tin. With the introduction of the concept of green development, the recycling of secondary resources has begun to take shape. Indium is one of the valuable metals in tin smoke. If indium can be effectively recovered and purified, it can not only reduce pollution to the environment, but also generate significant economic benefits. Therefore, in order to meet the needs of market development, it is particularly important to accurately detect indium in tin smoke.

[0003] At present, the main methods for detecting indium are EDTA titration and flame atomic absorption spectrometry, which are mainly used for zinc raw materials and zinc concentrate materials. Acid-dissolved samples are used in the analysis methods, but there is no corresponding detection method for tin fume. At the same time, it is found in the analysis work that when tin fume is dissolved by acid, there will be a wrapping phenomenon, and the sample cannot be completely dissolved, resulting in a low result and unable to meet the analysis requirements.

[0004] Therefore, being able to provide a method for accurately detecting the indium content in tin fume is an urgent problem to be solved by those skilled in the art. Summary of the invention

[0005] In view of this, the present invention provides a method for detecting the indium content in tin fume. The detection method of the present invention can reduce the error rate of measuring indium in tin fume, thereby accurately providing the indium content in tin fume.

[0006] In order to achieve the above object, the present invention adopts the following technical solution:

[0007] A method for detecting the indium content in tin smoke specifically comprises the following steps:

[0008] (1) adding hydrochloric acid and a first nitric acid to tin smoke, heating and evaporating the mixture until the mixture is nearly dry, then adding a second nitric acid to dissolve the mixture, fixing the volume, and filtering the mixture to obtain a filtrate and a filter residue;

[0009] (2) carbonizing the filter residue and then melting it with sodium peroxide, and then leaching with water, adjusting the pH value, acidifying and fixing the volume in sequence, and finally measuring the indium content of the filter residue;

[0010] (3) The indium content of the filtrate is measured, and the sum of the indium content of the filter residue and the indium content of the filtrate is the indium content in the tin fume.

[0011] Preferably, in step (1), the mass ratio of the tin fume, the hydrochloric acid and the first nitric acid is 1:5:15-1:15:5;

[0012] The volume ratio of the second nitric acid to the constant volume is 5:100-10:100.

[0013] Preferably, the heating temperature in step (1) is 200-220° C. and the heating time is 10-15 min;

[0014] The hydrochloric acid concentration is 1.10-1.19 g / mL, and the first nitric acid concentration is 1.30-1.42 g / mL;

[0015] The concentration of the second nitric acid is 1.30-1.42 g / mL.

[0016] Preferably, the filter paper in step (1) is medium-speed quantitative filter paper, and the constant volume is a volumetric flask.

[0017] Preferably, the mass ratio of the sodium peroxide and the carbonized filter residue in step (2) is 10-15:1.

[0018] Preferably, the carbonization temperature in step (2) is 600-750° C. and the time is 20 min-30 min.

[0019] Preferably, the temperature of the leaching water in step (2) is 50-80° C., the leaching time is 5-10 min, and the mass ratio of the water used to the filter residue after carbonization is 15-50:1.

[0020] Preferably, the pH value in step (2) is adjusted using nitric acid to a value of 6.5-7.5;

[0021] The acidification adopts hydrochloric acid and nitric acid, and the volume ratio of the hydrochloric acid, the nitric acid and the constant volume is 2:4-8:100.

[0022] Preferably, the concentration of nitric acid is 1.30-1.42 g / mL, and the concentration of hydrochloric acid is 1.10-1.19 g / mL.

[0023] Preferably, the measurements in steps (3) and (4) are performed using inductively coupled plasma.

[0024] Preferably, the inductively coupled plasma uses an atomizing gas, and the atomizing chamber is a corrosion-resistant system;

[0025] The spectrum line is 325.609nm;

[0026] The calculation formula of the analysis results is:

[0027]

[0028] Where:

[0029] ρ x -The mass concentration of the element to be measured in the test sample obtained from the working curve, in micrograms per milliliter (μg / mL);

[0030] ρ0-mass concentration of the element to be measured in the blank test solution found on the working curve, in micrograms per milliliter (μg / mL);

[0031] V0-test solution volume, in milliliters (mL);

[0032] m-mass of the sample, in grams (g).

[0033] It can be seen from the above technical solution that compared with the prior art, the beneficial effects of the present invention are as follows:

[0034] In the detection method provided by the present invention, hydrochloric acid and nitric acid are first used to pretreat the sample, and the sample is filtered after being fixed in volume, and the filtrate is measured on an inductively coupled plasma emission spectrometer. After the filter paper and the residue are carbonized, they are treated with sodium peroxide, and after the treatment, they are measured on an inductively coupled plasma emission spectrometer, so as to accurately measure the content of indium. The method is simple to operate, has accurate results, and can accurately determine the content of indium in tin smoke. DETAILED DESCRIPTION

[0035] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0036] Example 1

[0037] The present invention provides a method for detecting the indium content in tin smoke, and the specific steps are as follows:

[0038] (1) Weigh 0.2000-0.5000 g of tin fume sample into a 250 mL beaker, add water to wet the sample, add 15 mL of hydrochloric acid and 5 mL of nitric acid in sequence, heat at 200° C. for 15 min, evaporate to near dryness, and cool; wherein the concentration of hydrochloric acid is 1.19 g / mL, and the concentration of nitric acid is 1.42 g / mL; after the sample is cooled, add 25 mL of nitric acid (1.42 g / mL), place on an electric furnace to heat and dissolve the salts, cool after dissolution, and then dilute to 100-500 mL with water, filter into a beaker with medium-speed quantitative filter paper, and obtain a filtrate, filter paper, and residue;

[0039] (2) The filter paper and the residue were dried in an oven at 105°C, and then carbonized in a muffle furnace at 600°C for 30 minutes. After carbonization, 1.5 g of sodium peroxide was used to melt the mixture, and then 20 mL of hot water at 50°C was used to soak the mixture for 5 minutes. Then, nitric acid was added to adjust the pH value to about 7, and then the mixture was acidified with hydrochloric acid and nitric acid. The concentration of hydrochloric acid was 1.19 g / mL, and the concentration of nitric acid was 1.42 g / mL. The amount of hydrochloric acid used was 2 mL, and the amount of nitric acid used was 5 mL. The mixture was then diluted with water and measured by inductively coupled plasma to obtain the indium content of the filter residue.

[0040] (3) After the filtrate is fixed to volume, it is measured using inductively coupled plasma to obtain the indium content of the filtrate; the indium result is the sum of the measurement results of the indium content of the filter residue and the indium content of the filtrate;

[0041] As a preparation method, the preparation process of the indium standard storage solution used is as follows: weigh 0.5000g of metallic indium (99.99%) in a 300mL beaker, add 15mL of aqua regia, cover with a watch glass, heat at low temperature to dissolve and evaporate to near dryness, add 25mL of nitric acid, the concentration of nitric acid is 1.42g / mL, blow a small amount of water along the wall of the cup, boil to dissolve the salt, transfer to a 500mL volumetric flask after cooling, dilute to the scale with water, and shake well;

[0042] Indium standard solution: Accurately transfer 10.00 mL of indium standard stock solution into a 100 mL volumetric flask, add 10 mL of nitric acid (the concentration of nitric acid is 1.42 g / mL), dilute to the mark with water, and shake well;

[0043] Preparation of working curve: Pipette 0.00mL, 1.00mL, 5.00mL, 10.00mL, 15.00mL, and 20.00mL of indium standard solution into a set of 100mL volumetric flasks, add 5mL of nitric acid with a nitric acid concentration of 1.42g / mL, dilute to the scale with water, mix well, and prepare the working curve;

[0044] The tin fume was tested by the method of Example 1, and the test was repeated 6 times. The test results are shown in Table 1.

[0045] Table 1 Indium analysis and test results record

[0046]

[0047]

[0048] Example 2

[0049] The present invention provides a method for detecting the indium content in tin smoke, and the specific steps are as follows:

[0050] (1) Weigh 0.2000-0.5000 g of tin fume sample into a 250 mL beaker, add water to wet the sample, add 20 mL of hydrochloric acid and 10 mL of nitric acid in sequence, heat at 220° C. for 13 min, evaporate to near dryness, and cool; wherein the concentration of hydrochloric acid is 1.17 g / mL, and the concentration of nitric acid is 1.37 g / mL; after the sample is cooled, add 15 mL of nitric acid (1.37 g / mL), place on an electric furnace to heat and dissolve the salts, cool after dissolution, and then dilute to 100-500 mL with water, filter into a beaker with medium-speed quantitative filter paper, and obtain a filtrate, filter paper, and residue;

[0051] (2) The filter paper and the residue were dried in an oven at 105°C, and then carbonized in a muffle furnace at 650°C for 27 minutes. After carbonization, 1.3 g of sodium peroxide was used for melting, and after melting, 25 mL of hot water at 60°C was used for leaching for 7 minutes. Then, nitric acid was added to adjust the pH value to about 6.5, and then hydrochloric acid and nitric acid were used for acidification. The concentration of hydrochloric acid was 1.17 g / mL, the concentration of nitric acid was 1.37 g / mL, the amount of hydrochloric acid was 1.5 mL, and the amount of nitric acid was 4.5 mL. Then, the volume was fixed with water, and the inductively coupled plasma was used for measurement to obtain the indium content of the filter residue.

[0052] (3) After the filtrate is fixed to volume, it is measured using inductively coupled plasma to obtain the indium content of the filtrate; the indium result is the sum of the measurement results of the indium content of the filter residue and the indium content of the filtrate;

[0053] The tin fume was tested by the method of Example 2, and the test was repeated 6 times. The test results are shown in Table 2.

[0054] Table 2 Indium analysis and test results record

[0055]

[0056]

[0057] Example 3

[0058] The present invention provides a method for detecting the indium content in tin smoke, and the specific steps are as follows:

[0059] (1) Weigh 0.2000-0.5000 g of tin fume sample into a 250 mL beaker, add water to the beaker to wet the sample, add 5 mL of hydrochloric acid and 15 mL of nitric acid in sequence, heat at 210° C. for 15 min, evaporate until nearly dry, and cool; wherein the concentration of hydrochloric acid is 1.15 g / mL and the concentration of nitric acid is 1.33 g / mL; after the sample is cooled, add 8 mL of nitric acid (1.33 g / mL), place on an electric furnace to heat and dissolve the salts, cool after dissolution, and then dilute to 100-500 mL with water, filter into a beaker with medium-speed quantitative filter paper, and obtain a filtrate, filter paper, and residue;

[0060] (2) The filter paper and the residue were dried in an oven at 105°C, and then carbonized in a muffle furnace at 700°C for 25 min. After carbonization, 1.0 g of sodium peroxide was used to melt the mixture, and then 30 mL of hot water at 70°C was used to soak the mixture for 9 min. Then nitric acid was added to adjust the pH value to about 7.5, and then the mixture was acidified with hydrochloric acid and nitric acid. The concentration of hydrochloric acid was 1.15 g / mL, the concentration of nitric acid was 1.33 g / mL, the amount of hydrochloric acid was 2 mL, and the amount of nitric acid was 8 mL. The mixture was then diluted with water and measured by inductively coupled plasma to obtain the indium content of the filter residue.

[0061] (3) After the filtrate is fixed to volume, it is measured using inductively coupled plasma to obtain the indium content of the filtrate; the indium result is the sum of the measurement results of the indium content of the filter residue and the indium content of the filtrate;

[0062] The tin fume was tested by the method of Example 3, and the test was repeated 6 times. The test results are shown in Table 3.

[0063] Table 3 Indium analysis test results record

[0064]

[0065] Example 4

[0066] The present invention provides a method for detecting the indium content in tin smoke, and the specific steps are as follows:

[0067] (1) Weigh 0.2000-0.5000 g of tin fume sample into a 250 mL beaker, add water to wet the sample, add 10 mL of hydrochloric acid and 10 mL of nitric acid in sequence, heat at 200° C. for 15 min, evaporate until nearly dry, and cool; wherein the concentration of hydrochloric acid is 1.10 g / mL and the concentration of nitric acid is 1.30 g / mL; after the sample is cooled, add 6 mL of nitric acid (1.30 g / mL), place on an electric furnace to heat and dissolve the salts, cool after dissolution, and then dilute to 100-500 mL with water, filter into a beaker with medium-speed quantitative filter paper, and obtain a filtrate, filter paper, and residue;

[0068] (2) The filter paper and the residue are dried in an oven at 105°C, and then carbonized in a muffle furnace at 750°C for 20 minutes. After carbonization, 0.8 g of sodium peroxide is used for melting, and after melting, 30 mL of hot water at 80°C is used for leaching for 10 minutes. Then, nitric acid is added to adjust the pH value to about 6.7, and then hydrochloric acid and nitric acid are used for acidification. The concentration of hydrochloric acid is 1.10 g / mL, the concentration of nitric acid is 1.30 g / mL, the amount of hydrochloric acid used is 1.5 mL, and the amount of nitric acid used is 6 mL. Then, the volume is fixed with water, and the inductively coupled plasma is used for measurement to obtain the indium content of the filter residue;

[0069] (3) After the filtrate is fixed to volume, it is measured using inductively coupled plasma to obtain the indium content of the filtrate; the indium result is the sum of the measurement results of the indium content of the filter residue and the indium content of the filtrate;

[0070] The tin fume was tested by the method of Example 4, and the test was repeated 6 times. The test results are shown in Table 4.

[0071] Table 4 Indium analysis test results record

[0072]

[0073] It can be seen from the results of the examples that the method provided by the present invention is used to determine the indium in tin fume with good precision.

[0074] The results of the method of the present invention were verified to be accurate by spike recovery. The relevant results are shown in Table 5.

[0075] Table 5 Recovery analysis test results record

[0076]

[0077] It can be seen from the above table that the spiked recovery rate is between 98.57% and 102.30%, indicating that the analysis method of the present invention is feasible, the result is accurate and reliable, and the error rate of indium analysis in tin fume can be reduced.

[0078] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A method for detecting the indium content in tin smoke, characterized in that: The specific steps include: (1) adding hydrochloric acid and a first nitric acid to tin smoke, heating and evaporating the mixture until the mixture is nearly dry, then adding a second nitric acid to dissolve the mixture, fixing the volume, and filtering the mixture to obtain a filtrate and a filter residue; (2) carbonizing the filter residue and then melting it with sodium peroxide, and then leaching with water, adjusting the pH value, acidifying and fixing the volume in sequence, and finally measuring the indium content of the filter residue; (3) The indium content of the filtrate is measured, and the sum of the indium content of the filter residue and the indium content of the filtrate is the indium content in the tin fume.

2. The method for detecting the indium content in tin fume according to claim 1, characterized in that: The mass ratio of the tin fume, the hydrochloric acid and the first nitric acid in step (1) is 1:5:15-1:15:5; The volume ratio of the second nitric acid to the constant volume is 5:100-10:

100.

3. The method for detecting the indium content in tin fume according to claim 1, characterized in that: The heating temperature in step (1) is 200-220° C. and the heating time is 10-15 min; The hydrochloric acid concentration is 1.10-1.19 g / mL, and the first nitric acid concentration is 1.30-1.42 g / mL; The concentration of the second nitric acid is 1.30-1.42 g / mL.

4. The method for detecting the indium content in tin fume according to claim 1, characterized in that: The filter paper in step (1) is medium-speed quantitative filter paper, and the constant volume is a volumetric flask.

5. The method for detecting the indium content in tin fume according to claim 1, characterized in that: The mass ratio of the sodium peroxide to the carbonized filter residue in step (2) is 10-15:

1.

6. The method for detecting the indium content in tin fume according to claim 1, characterized in that: The carbonization temperature in step (2) is 600-750°C and the time is 20min-30min.

7. The method for detecting the indium content in tin fume according to claim 1, characterized in that: The temperature of the leaching water in step (2) is 50-80° C., the leaching time is 5-10 min, and the mass ratio of the water used to the filter residue after carbonization is 15-50:

1.

8. The method for detecting the indium content in tin fume according to claim 1, characterized in that: In step (2), the pH value is adjusted to 6.5-7.5 using nitric acid; The acidification adopts hydrochloric acid and nitric acid, and the volume ratio of the hydrochloric acid, the nitric acid and the constant volume is 2:4-8:

100.

9. The method for detecting the indium content in tin fume according to claim 8, characterized in that: The concentration of the nitric acid is 1.30-1.42 g / mL, and the concentration of the hydrochloric acid is 1.10-1.19 g / mL.

10. The method for detecting the indium content in tin fume according to claim 1, characterized in that: The measurements in steps (3) and (4) are performed using inductively coupled plasma.

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