CN111537329A - Method for measuring nickel content in nickel-iron alloy and sample preparation process thereof - Google Patents
Method for measuring nickel content in nickel-iron alloy and sample preparation process thereof Download PDFInfo
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Abstract
The invention discloses a method for measuring nickel content in a nickel-iron alloy and a sample preparation process thereof, belonging to the technical field of analysis and detection. The invention provides a sample preparation process of a method for measuring the content of nickel in a nickel-iron alloy, which is used for overcoming the defects of the prior art and comprises the following steps: sodium peroxide is used as a fusing agent, and primary or secondary melting is carried out in a crucible at 700-850 ℃, so that the effect of complete melting of a sample is ensured, and meanwhile, the fusing agent and the sample slowly undergo a high-temperature double decomposition reaction, so that the nickel-iron alloy element is fully oxidized and combined with the fusing agent, the fused material is not easy to splash, no loss is caused, a large amount of acid reagents are avoided, and the method is more environment-friendly and green; the method has high efficiency, can melt samples in batches, has no loss of samples, can satisfactorily solve the difficult problem of refractory melting of the nickel-iron alloy, and has accurate detection result.
Description
Technical Field
The invention belongs to the technical field of analysis and detection, and particularly relates to a method for determining the content of nickel in a nickel-iron alloy and a sample preparation process thereof.
Background
The ferronickel is a ferronickel alloy containing nickel metal and iron, and is used as an alloy element additive in the steel-making industry, can improve the bending strength and hardness of steel, can make the structure of the cast iron uniform and improve the density of the cast iron, and can also be used as an additive for nickel-containing or nickel-chromium-containing cast iron rolls and other casting alloys. The nickel is divided into high nickel iron, medium nickel iron and low nickel iron according to the content of nickel metal.
The international standard for measuring the content of nickel in the nickel-iron is ISO 6352-1985-dimethylglyoxime gravimetric analysis method, and the national standards are GB/T30072-2013-EDTA titration method, GB/T21933.1-2008-dimethylglyoxime gravimetric method and GB/T24198-2009-wavelength dispersive X-ray fluorescence spectrometry, wherein GB/T21933.1-2008 is ISO 6352-1985-dimethylglyoxime gravimetric analysis method. According to the literature search, the most widely used method for measuring the nickel content is dimethylglyoxime gravimetric method and EDTA titration method when the nickel content is more than 2 percent. For example, GB/T223.25-1994 (weight method for measuring nickel content by dimethylglyoxime) of chemical analysis method for steel and alloy, YS/T928.2-2013 (chemical analysis method for three elements of nickel, cobalt and manganese) 2 part: determination of the amount of Nickel dimethylglyoxime gravimetric method, YS/T953.1-2014 chemical analysis of Nickel matrix materials by pyrometallurgy part 1: determination of nickel content dimethylglyoxime spectrophotometry and dimethylglyoxime weight method, YS/T1006.1-2014 part 1 of chemical analysis method of nickel cobalt lithium manganate: determination of the Total amount of Nickel, cobalt and manganese EDTA titration method.
In all the above analysis method standards, except that the X fluorescence method is used for polishing the surface of an alloy block and directly measuring, other wet analyses, no matter national standards or international standards, use a large amount of dangerous chemicals such as hydrochloric acid, nitric acid, hydrofluoric acid and perchloric acid, and generate a large amount of waste acid and waste gas, especially generate a large amount of perchloric acid white smoke when perchloric acid smokes and decomposes a sample; for example, the test sample was dissolved by heating with hydrochloric acid and nitric acid in CN 109060777A, the sample was digested with microwaves using mixed acids, i.e., nitric acid, hydrochloric acid, hydrofluoric acid, hydrogen peroxide, etc. in CN 1001294897A, and the sample was dissolved and fluorinated with ammonium fluoride and nitric acid in CN 102928422 a. At present, effective environmental protection measures for perchloric acid smoke recovery treatment are not available, so the acid decomposition method has serious environmental pollution.
Therefore, it is urgently needed to develop a method for measuring the nickel content in the nickel-iron alloy, which is environment-friendly.
Disclosure of Invention
In order to make up for the defects of the prior art, the invention firstly provides a sample preparation process of a method for measuring the content of nickel in a nickel-iron alloy, which comprises the following steps:
A. weighing a nickel-iron alloy sample;
B. putting the weighed sample into a crucible which is pre-added with sodium peroxide, then covering the sample with the sodium peroxide, melting the crucible at 700-850 ℃, and cooling to room temperature after the melting is finished;
C. placing the cooled crucible into a beaker filled with water in advance, and leaching until the melt is completely leached; washing the crucible with water, taking out the crucible, and dropwise adding hydrochloric acid into the test solution until the test solution is clear; if insoluble sample particles are found in the test solution, performing the step D; if no insoluble particles exist, directly transferring the test solution into a volumetric flask, and then carrying out the test according to the step E;
D. filtering the test solution, washing filter paper and sediment with water, collecting filtrate and washing solution in a volumetric flask, putting the washed sediment and filter paper back into a crucible, drying, heating and incinerating the filter paper, taking out the crucible after ashing is completed, adding sodium peroxide, melting at 700-850 ℃, cooling to room temperature after melting; placing the cooled crucible into a beaker filled with water in advance, covering a watch glass for leaching until the melt is completely leached, washing the crucible with water, taking out the crucible, and combining the filtrate in a volumetric flask;
E. diluting the test solution in the volumetric flask to a scale, fixing the volume and shaking up.
In the sample preparation process of the method for measuring the nickel content in the nickel-iron alloy, the nickel-iron alloy sample is granular, drilled or milled, and the granularity of the nickel-iron alloy sample is-0.180 mm.
In the sample preparation process of the method for measuring the nickel content in the nickel-iron alloy, the weighing amount of the nickel-iron alloy sample is 0.1-0.5 g, and the accuracy is 0.1 mg.
In the sample preparation process of the method for measuring the nickel content in the nickel-iron alloy, the using amount of sodium peroxide which is added in advance in the step B is recorded as m1, the using amount of sodium peroxide which covers the surface in the step B is recorded as m2, the using amount of sodium peroxide which is secondarily molten in the step D is recorded as m3, the total mass of sodium peroxide is recorded as m, and the ratio of the mass of the nickel-iron alloy sample to the total mass of sodium peroxide is controlled to be 1: 5-40 g, and the total mass of the sodium peroxide is not more than 7 g.
In the sample preparation process of the method for measuring the nickel content in the nickel-iron alloy, the purity of the sodium peroxide is not lower than analytical purity, and the content is more than or equal to 92.5%.
In the sample preparation process of the method for measuring the content of nickel in the nickel-iron alloy, in the step B, the melting time is 10-25 min.
In the sample preparation process of the method for measuring the nickel content in the nickel-iron alloy, in the step D, the melting time is 10-25 min.
In the sample preparation process of the method for measuring the content of nickel in the nickel-iron alloy, the crucible is an iron crucible, a high-purity arc high-aluminum crucible or a corundum crucible, and the volume of the crucible is not less than 30 mL.
In the sample preparation process of the method for measuring the nickel content in the nickel-iron alloy, the purity of the used water is not lower than that of the third-level water.
In the sample preparation process of the method for measuring the nickel content in the nickel-iron alloy, the purity of the hydrochloric acid is not lower than that of analytical grade.
On the basis of the sample preparation process, the invention further provides a method for measuring the content of nickel in the nickel-iron alloy, which further comprises the following steps:
F. and (4) measuring and calculating the nickel content in the sample according to the conventional nickel content measuring method after the volume is fixed. In step F, the existing methods conforming to wet measurement can be applied, such as dimethylglyoxime gravimetric method, dimethylglyoxime spectrophotometric method or EDTA titration method.
The invention has the beneficial effects that:
the method selects the sodium peroxide with strong oxidizing property and strong corrosivity as the fusing agent, melts the sample at high temperature, oxidizes elements in the sample into a high-valence state, can perform secondary high-temperature melting of non-melting residues when primary melting cannot be completely melted, ensures the effect of completely melting the sample, and does not cause interference to measurement and introduce impurities by sodium ions.
By scientifically controlling the reasonable dilution ratio and melting temperature of the flux sodium peroxide and the sample, the flux and the sample slowly undergo high-temperature double decomposition reaction, so that the nickel-iron alloy element is fully oxidized and combined with the flux, and the flux is not easy to splash and lose.
An iron crucible, a high-aluminum crucible or a corundum crucible is selected as a melting crucible material, so that the crucible material does not interfere with measurement and does not introduce elements to be measured; the sodium peroxide is adopted for high-temperature melting decomposition, so that a large amount of acid reagents, especially perchloric acid which is strong corrosive and irritant and has danger of combustion and explosion are avoided, the pollution of a large amount of perchloric acid mist to air is avoided, and the environment is protected and green.
The method has the advantages of high melting mode, high efficiency, batch sample melting, no sample loss and capability of satisfactorily solving the difficult problem of refractory melting of the nickel-iron alloy.
Detailed Description
Specifically, the sample preparation process of the method for measuring the nickel content in the nickel-iron alloy comprises the following steps:
A. weighing a nickel-iron alloy sample;
B. putting the weighed sample into a crucible which is added with sodium peroxide in advance (in a flat spreading mode), then covering the sample with the sodium peroxide, melting the crucible at 700-850 ℃, and cooling to room temperature after the melting is finished;
C. placing the cooled crucible into a beaker filled with water in advance, and leaching until the melt is completely leached; washing the crucible with water, taking out the crucible, and dropwise adding hydrochloric acid into the test solution until the test solution is clear; if insoluble sample particles are found in the test solution, performing the step D; if no insoluble particles exist, directly transferring the test solution into a volumetric flask, and then carrying out the test according to the step E;
D. filtering the test solution, washing filter paper and sediment with water, collecting filtrate and washing solution in a volumetric flask, putting the washed sediment and filter paper back into a crucible, drying, heating and incinerating the filter paper, taking out the crucible after ashing is completed, adding sodium peroxide, melting at 700-850 ℃, cooling to room temperature after melting; placing the cooled crucible into a beaker filled with water in advance, covering a watch glass for leaching until the melt is completely leached, washing the crucible with water, taking out the crucible, and combining the filtrate in a volumetric flask;
E. diluting the test solution in the volumetric flask to a scale, fixing the volume and shaking up.
The ferronickel sample is usually granular, drilled or milled, the finer the granularity of the sample is, the better the sample is melted, but the ferronickel has high hardness, is difficult to drill and mill, and can achieve good effect by melting twice as long as the granularity is controlled at-0.180 mm. In the existing detection method, the weighing amount of a nickel-iron alloy sample is generally 0.1-0.5 g, and is accurate to 0.1 mg.
The analysis flux used in the invention is sodium peroxide, and the analysis flux is analytically pure and more than the analysis flux, has molecular weight of 77.97 and main content of more than 92.5 percent by weight, and has the following functions in the invention: by utilizing the good strong oxidizing property of molten sodium peroxide, Fe, Ni, Cr, Mn, C, S, P, Si and other elements in the nickel-iron are oxidized into high-valence state and acid radical and other forms at 700-850 ℃, so that the nickel-iron alloy is decomposed by eutectic melting.
The larger the sample dilution ratio is during melting, the better the melting effect is, but easily causes the flux to be wasted, and increases the corrosivity to the crucible, reduces crucible life, causes the analysis cost to increase, so, need during the analysis according to the size of ferronickel alloy granularity, the height of nickel content, will dilute the ratio control at reasonable scope. Through tests, the using amount of sodium peroxide added in advance in the step B is recorded as m1, the using amount of sodium peroxide covering the surface in the step B is recorded as m2, the using amount of sodium peroxide subjected to secondary melting in the step D is recorded as m3, and the total mass of sodium peroxide is recorded as m, so that the ratio of the mass of the nickel-iron alloy sample to the total mass of sodium peroxide is controlled to be 1: 5-40 g, and the total mass of the sodium peroxide is not more than 7 g.
In the invention, the selection of the melting temperature is a key control element, and the flux and the sample can slowly generate high-temperature double decomposition reaction at the melting temperature of 700-850 ℃ by scientifically controlling the granularity of the sample, the reasonable dilution ratio of the flux sodium peroxide and the sample and the adding mode of the sodium peroxide and the sample, so that the nickel-iron alloy element is fully oxidized and combined with the flux, and the melt is not easy to splash and has no loss. When a small amount of insoluble sample particles still remain after the primary melting and leaching, the sample can be completely melted through secondary melting, and the sample loss is avoided.
When the crucible is melted, the melt cannot be popped and splashed, so that whether the crucible is covered by a cover or not has no influence on the result; the melting equipment can adopt a high-temperature furnace with the common temperature reaching the requirement, such as a high-temperature muffle furnace.
When the melt is leached, the water consumption can be properly adjusted according to the sample weighing and the specification of a volumetric flask, and is generally 30-50 mL/0.1-0.5 g of a nickel-iron alloy sample; meanwhile, in order to avoid sample loss, the watch glass can be covered when in leaching.
According to the invention, an iron crucible, a high-alumina crucible or a corundum crucible is selected as a melting crucible material, the content of aluminum oxide is not less than 95%, the volume of the crucible is not less than 30mL, and the crucible material does not interfere with the measurement.
In order to ensure the accuracy of the detection result, the purity of the water used in the method is not lower than that of the tertiary water, and the purity of the hydrochloric acid used in the method is not lower than that of the analytically pure water.
On the basis of the sample preparation process, the invention further provides a method for measuring the content of nickel in the nickel-iron alloy, which further comprises the following steps:
F. and (4) measuring and calculating the nickel content in the sample according to the conventional nickel content measuring method after the volume is fixed. The existing methods conforming to the wet method can be applied to the dimethylglyoxime gravimetric method, the dimethylglyoxime spectrophotometry method or the EDTA titration method, etc.
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1: method for measuring nickel content in nickel-iron alloy by iron crucible one-time melting method
1. Sample melting was accomplished by the following steps:
A. accurately weighing 0.400g (accurate to 0.1mg) of ferronickel standard sample (granularity is less than or equal to 0.125mm) in a 50mL iron crucible which is pre-added with about 2g of sodium peroxide, and then adding about 2g of sodium peroxide to cover the surface of the sample.
B. And (3) moving the crucible into a high-temperature furnace at 600 ℃, heating to be molten, then heating to 700 ℃, melting for 10min at the temperature, taking out and cooling the crucible to room temperature.
2. The determination of the nickel content is carried out by the following steps
C. Putting the crucible into a beaker filled with a proper amount of water in advance, covering a watch glass and leaching until the melt is completely leached; the crucible was washed with water, removed, and hydrochloric acid was slowly added dropwise to the sample solution until the sample solution was clear (pH about 2.5), and the sample solution was transferred to a 200mL volumetric flask and diluted to the scale.
D. 50.0mL of test solution is respectively put into a 600mL beaker, water is added to about 300mL, and the determination and calculation are carried out according to GB/T21933.1-2008 'weight method for determining nickel-iron content' 7.5.2-8.
3. Measurement of samples
3 ferronickel standard samples are selected to verify the accuracy of the method, as shown in table 1, the comparison between the measured value and the standard value shows that the difference between the measured result and the standard value is within the error range allowed by the national standard.
TABLE 1 accuracy verification
| Numbering | Measured value | Recommended value | Tolerance difference |
| GBW(E)010422 | 16.55 | 16.45 | 0.24 |
| IARM24B | 35.74 | 35.86 | 0.35 |
| JIS760-3 | 19.43 | 19.56 | 0.24 |
As can be seen from Table 1, when the method is used for analyzing the standard sample of the nickel-iron alloy, the measurement result is accurate and reliable, and the extreme difference between the measured value and the recommended value meets the requirement of allowable difference.
Example 2: method for determining nickel content in nickel-iron alloy by corundum crucible secondary melting method
1. Sample melting was accomplished by the following procedure
A. Accurately weighing 0.300g (accurate to 0.1mg) of nickel-iron sample (the granularity is less than or equal to 0.0.180mm, namely the sample completely passes through a sieve with 80 meshes) into a 30mL corundum crucible which is pre-added with about 2g of sodium peroxide, and then adding about 2g of sodium peroxide to cover the surface of the sample.
B. And (3) moving the crucible into a 680 ℃ high-temperature furnace, melting the sodium peroxide at the temperature, heating to 800 ℃ for melting for 20min, taking out and cooling the crucible to room temperature.
C. Putting the crucible into a beaker filled with 50mL of water in advance, covering a watch glass and leaching until the melt is completely leached; the crucible was washed with water, taken out, and hydrochloric acid was slowly dropped into the sample solution until the sample solution was clear (pH was about 2.5).
D. Filtering the test solution by using common quick filter paper, collecting the filtrate in a 500mL volumetric flask, washing the filter paper and the precipitate for 5-6 times by using water (collecting the washing solution in the volumetric flask), putting the precipitate and the filter paper back into the original crucible, drying, heating and ashing the filter paper, taking out the crucible after ashing is completed, adding 2g of sodium peroxide, melting at 850 ℃ for 10min, taking out and cooling the crucible to room temperature; putting the crucible into a beaker filled with 50mL of water in advance, covering a watch glass and leaching until the melt is completely leached; the crucible was washed with water, taken out, and the filtrate was combined in a 500mL volumetric flask.
2. The determination of the nickel content is carried out by the following steps
E. Diluting the test solution to a scale, fixing the volume and shaking up.
F. 50.0mL of test solution is respectively put into a 600mL beaker, water is added to about 300mL, and the determination and calculation are carried out according to GB/T21933.1-2008 'weight method for determining nickel-iron content' 7.5.2-8.
3. Measurement of samples
2 ferronickel samples are selected to verify the precision of the method, and GB/T21933.1-2008 'weight method for measuring nickel-nickel content dimethylglyoxime' is applied to measure the 2 samples and compare the results with the method in the text, and the results are shown in Table 2.
TABLE 2 precision and method comparison
As can be seen from Table 2, because the nickel content of the two samples is high, residues exist in the first melting, and after the residues are melted for the second time, the method has good precision and is consistent with the measurement result of the national standard GB/T21933.1-2008, and the method is proved to be accurate and reliable.
Example 3: method for measuring nickel content in nickel-iron alloy by high-aluminum crucible one-time melting method
A. Accurately weighing 0.200g (accurate to 0.1mg) of nickel-iron sample (the granularity is less than or equal to 0.0.180mm, namely the sample completely passes through a sieve with 80 meshes) in a 30mL high-alumina crucible which is pre-added with about 2g of sodium peroxide, and then adding about 3g of sodium peroxide to cover the surface of the sample.
B. And (3) moving the crucible into a 680 ℃ high-temperature furnace, melting the sodium peroxide at the temperature, heating to 820 ℃ again, melting for 25min, taking out and cooling the crucible to room temperature.
C. The crucible was placed in a beaker containing 50mL of water in advance, and the beaker was covered and leached until the melt was completely leached. The crucible was washed with water, taken out, hydrochloric acid was slowly dropped into the sample solution until the sample solution was clear (pH was about 2.5), and the sample solution was transferred to a 100mL volumetric flask and diluted to the scale.
D. 25.0mL of test solution is dispensed into a 600mL beaker, water is added to the beaker to reach about 300mL, and the determination and calculation are carried out according to GB/T21933.1-2008 'weight method for determining nickel-iron content' 7.5.2-8.
3 ferronickel samples are selected to verify the accuracy of the method, and meanwhile, the 3 samples are compared with the method in the text when GB/T21933.1-2008 'weight method for measuring nickel-nickel content of dimethylglyoxime' is applied, and the results are shown in Table 3.
TABLE 3 alignment of methods
Claims (10)
1. The sample preparation process of the method for measuring the nickel content in the nickel-iron alloy is characterized by comprising the following steps of: the method comprises the following steps:
A. weighing a nickel-iron alloy sample;
B. putting the weighed sample into a crucible which is pre-added with sodium peroxide, then covering the sample with the sodium peroxide, melting the crucible at 700-850 ℃, and cooling to room temperature after the melting is finished;
C. placing the cooled crucible into a beaker filled with water in advance, and leaching until the melt is completely leached; washing the crucible with water, taking out the crucible, and dropwise adding hydrochloric acid into the test solution until the test solution is clear; if insoluble sample particles are found in the test solution, performing the step D; if no insoluble particles exist, directly transferring the test solution into a volumetric flask, and then carrying out the test according to the step E;
D. filtering the test solution, washing filter paper and sediment with water, collecting filtrate and washing solution in a volumetric flask, putting the washed sediment and filter paper back into a crucible, drying, heating and incinerating the filter paper, taking out the crucible after ashing is completed, adding sodium peroxide, melting at 700-850 ℃, cooling to room temperature after melting; placing the cooled crucible into a beaker filled with water in advance, covering a watch glass for leaching until the melt is completely leached, washing the crucible with water, taking out the crucible, and combining the filtrate in a volumetric flask;
E. diluting the test solution in the volumetric flask to a scale, fixing the volume and shaking up.
2. The sample preparation process of the method for determining the content of nickel in a nickel-iron alloy according to claim 1, characterized in that: the nickel-iron alloy sample is granular, drilled or milled scraps, and the granularity of the nickel-iron alloy sample is-0.180 mm.
3. The sample preparation process of the method for determining the content of nickel in a nickel-iron alloy according to claim 2, characterized in that: the weighing amount of the nickel-iron alloy sample is 0.1-0.5 g, and the accuracy is 0.1 mg.
4. The sample preparation process of the method for determining the content of nickel in a nickel-iron alloy according to any one of claims 1 to 3, characterized in that: the using amount of sodium peroxide added in advance in the step B is recorded as m1, the using amount of the sodium peroxide covered on the surface in the step B is recorded as m2, the using amount of the sodium peroxide subjected to secondary melting in the step D is recorded as m3, the total mass of the sodium peroxide is recorded as m, and the ratio of the mass of the nickel-iron alloy sample to the total mass of the sodium peroxide is controlled to be 1: 5-40 g, and the total mass of the sodium peroxide is not more than 7 g.
5. The sample preparation process of the method for determining the content of nickel in a nickel-iron alloy according to claim 4, characterized in that: the purity of the sodium peroxide is not lower than analytical purity, and the content is more than or equal to 92.5 percent.
6. The sample preparation process of the method for determining the content of nickel in a nickel-iron alloy according to claim 1, characterized in that: in the step B, the melting time is 10-25 min; in the step D, the melting time is 10 min-25 min.
7. The sample preparation process of the method for determining the content of nickel in a nickel-iron alloy according to claim 1, characterized in that: the crucible is an iron crucible, a high-purity arc high-aluminum crucible or a corundum crucible, and the volume of the crucible is not less than 30 mL.
8. The sample preparation process of the method for determining the content of nickel in a nickel-iron alloy according to claim 1, characterized in that: the purity of the water used is not lower than that of the tertiary water.
9. The sample preparation process of the method for determining the content of nickel in a nickel-iron alloy according to claim 1, characterized in that: the purity of the hydrochloric acid used is not lower than that of analytical grade.
10. The method for measuring the nickel content in the nickel-iron alloy is characterized by comprising the following steps: the method is as claimed in any one of claims 1 to 9, and comprises the following steps:
F. and (4) measuring and calculating the nickel content in the sample according to the conventional nickel content measuring method after the volume is fixed.
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Cited By (2)
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|---|---|---|---|---|
| CN112461878A (en) * | 2020-11-19 | 2021-03-09 | 金川集团股份有限公司 | Method for determining content of ferronickel in carbonyl ferronickel alloy powder |
| CN113504254A (en) * | 2021-07-02 | 2021-10-15 | 金川集团股份有限公司 | Combined measurement method for nickel, copper, iron and cobalt elements in solid material in nickel pyrometallurgical process |
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