CN113466222A - Method for rapidly determining nickel content in nickel-containing pig iron - Google Patents
Method for rapidly determining nickel content in nickel-containing pig iron Download PDFInfo
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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Abstract
The invention belongs to the field of raw material detection in the steel industry, and particularly relates to a method for rapidly determining the nickel content in nickel-containing pig iron, which comprises the following steps: (1) preparing a nickel standard solution mother solution; (2) preparing a sample solution: adding hydrochloric acid and nitric acid into a nickel-containing pig iron sample, and heating for dissolving; adding perchloric acid after complete dissolution, heating until perchloric acid white smoke is emitted, and continuously heating until the solution becomes a flowable wet salt; adding distilled water to dissolve the salt; (3) respectively preparing a developing solution and a reference solution of a nickel standard solution and a sample solution; (4) drawing a standard curve by adopting a spectrophotometry; (5) and (5) measuring the absorbance of the sample solution, and calculating the content of the nickel element in the sample according to the standard curve. The method provided by the invention can improve the detection efficiency and detection precision of the nickel content, and simultaneously reduce the operation difficulty of sample preparation and sample detection.
Description
Technical Field
The invention belongs to the field of raw material detection in the steel industry, and particularly relates to a method for rapidly determining the nickel content in nickel-containing pig iron.
Background
Along with the continuous growth of the production scale of stainless steel and nickel-containing alloy steel at home and abroad, the price of nickel-containing pig iron is continuously changed, so that the method is one of ways for ensuring the high efficiency of steel-making production by accurately and quickly detecting the nickel content in the nickel-containing pig iron for steel-making in order to adapt to the rhythm of metallurgical production and reduce the occupation of ferronickel on capital.
The commonly used nickel content determination methods at present comprise a dimethylglyoxime gravimetric method, a dimethylglyoxime precipitation separation EDTA titration method, an extraction separation dimethylglyoxime photometric method, an atomic absorption spectrometry method and the like. The method is characterized in that a dimethylglyoxime gravimetric method and a dimethylglyoxime precipitation separation EDTA titration method are commonly adopted for high-content nickel-containing pig iron, the operation process is complicated, the detection period is long, and the method is not suitable for the requirement of mass detection in the modern metallurgical industry.
Disclosure of Invention
The invention aims to provide a method for rapidly determining the nickel content in nickel-containing pig iron, which can improve the detection efficiency and detection precision of the nickel content and simultaneously reduce the difficulty of sample preparation and sample detection operation.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a method for rapidly measuring the nickel content in nickel-containing pig iron adopts a dimethylglyoxime direct photometry method to measure, and the measuring process is as follows:
(1) preparing a nickel standard solution mother solution;
(2) preparing a sample solution: adding hydrochloric acid and nitric acid into a nickel-containing pig iron sample, and heating for dissolving; adding perchloric acid after complete dissolution, heating until perchloric acid white smoke is emitted, and continuously heating until the solution becomes a flowable wet salt; adding distilled water to dissolve the salt;
(3) respectively preparing a developing solution and a reference solution of a nickel standard solution and a sample solution;
(4) drawing a standard curve by adopting a spectrophotometry;
(5) and (5) measuring the absorbance of the sample solution, and calculating the content of the nickel element in the sample according to the standard curve.
The preparation process of the sample solution in the step (2) of the invention is as follows:
accurately weighing 0.1000g of nickel-containing pig iron sample, placing the sample in a conical flask, adding 15-30mL of hydrochloric acid and 5-10mL of nitric acid, and heating the sample on a 200-220 ℃ electric heating plate to dissolve the sample;
after the sample is completely dissolved, adding 5-10mL of perchloric acid, continuing to heat until perchloric acid white smoke is emitted, continuously shaking the conical flask until the solution becomes a flowable wet salt, taking down, continuing to smoke, slightly cooling, adding 3-5mL of distilled water to dissolve the salt, and fixing the volume to a 200mL volumetric flask to obtain the sample solution.
The preparation process of the color development liquid and the reference liquid in the step (3) of the invention is as follows:
color development liquid: transferring standard solution mother liquor with different volumes and sample solution with certain volume into different volumetric flasks of 100mL, then sequentially adding 10-20mL of potassium sodium tartrate solution, 8-18 mL of sodium hydroxide solution, 10-20mL of ammonium persulfate solution and 10-20mL of dimethylglyoxime solution, standing for 15-30min, and then fixing the volume to 100 mL;
reference solution: and transferring the standard solution mother liquor with different volumes and the sample solution with certain volume into different 100mL volumetric flasks, then sequentially adding 10-20mL of potassium sodium tartrate solution, 18-28 mL of sodium hydroxide solution and 10-20mL of ammonium persulfate solution, standing for 15-30min, and then fixing the volume to 100 mL.
The concentration of the potassium sodium tartrate solution is 20-30%, the concentration of the sodium hydroxide solution is 5-8%, the concentration of the ammonium persulfate solution is 4-6%, and the concentration of the dimethylglyoxime solution is 1-2%.
In the preparation process of the color developing solution and the reference solution, the color developing solution and the reference solution are required to be fully and uniformly mixed after a new solution is added each time.
The specific operation of drawing the standard curve in the step (4) of the invention is as follows: and (3) measuring the absorbance of the nickel standard solution with different concentrations at 530nm +/-5 nm by adopting a spectrophotometry, and drawing a standard curve by taking the nickel concentration as an abscissa and the absorbance as an ordinate.
In the step (5) of the present invention, the absorbance of the sample solution is measured at 530 nm. + -. 5 nm.
The measuring process of the nickel content in the nickel-containing pig iron provided by the invention is approximately as follows:
adding hydrochloric acid and nitric acid into nickel-containing pig iron to dissolve a sample, adopting perchloric acid to smoke to eliminate chromium interference, adopting sodium potassium tartrate to mask iron interference, enabling nickel and dimethylglyoxime to generate a stable complex under an alkaline condition, adopting a separation method to obtain a color developing solution, and measuring the nickel content in the nickel-containing pig iron at 530nm +/-5 nm. The result shows that the method is an effective method for measuring the nickel element in the nickel-containing pig iron, and the measurement error is within the allowable range of national standard of chemical analysis.
The invention has the beneficial effects that:
the inspection method provided by the invention overcomes the defects of long inspection period, complex operation, toxic and much reagent consumption, large labor intensity of personnel, low efficiency and the like of the traditional inspection method.
The invention adopts the direct spectrophotometry to detect the components of the sample, and has simple and convenient operation, high detection efficiency and good precision; the recovery rate of the nickel-containing manganese-nickel alloy reaches the requirement that the recovery rate of elements to be detected in the national standard GB/T31924-2015 'gravimetric method for determining nickel content in nickel-containing pig iron and dimethylglyoxime' should be controlled to be 80-120%.
Compared with the existing manual wet method, the technical scheme provided by the invention has the advantages that the analysis efficiency can be improved by 50%, the method is suitable for detecting samples with the nickel content of less than 12%, the analysis result is accurate, and the method has a good application prospect.
The method provided by the invention solves the problem of narrow measurement range of the existing photometric method, and the maximum value of the nickel content of the standard sample measured by the photometric method reaches about 12 percent, which is 12 times of the content of the prior detection method.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
The sample to be measured in this example is a standard sample of nickel-containing pig iron, GSB03-2681-2011, Middling group Gilin iron alloy Co., Ltd, and the measurement process is as follows:
(1) preparing a standard solution mother solution: accurately weighing 0.1000g of nickel-containing pig iron standard sample, placing the sample in a conical flask, adding 15mL of hydrochloric acid and 5mL of nitric acid, and heating the sample on a 200-220 ℃ electric hot plate to dissolve the sample;
after the sample is completely dissolved, adding 5mL of perchloric acid, continuing to heat until perchloric acid white smoke is emitted, continuously shaking the conical flask until the solution is in a flowable wet salt shape, taking down, continuing to smoke, slightly cooling, adding 3 mL of distilled water to dissolve salts, and fixing the volume to a 200mL volumetric flask to be used as standard solution mother liquor.
(2) Preparation of sample solution
Weighing 0.1000 +/-0.0005 g of the nickel-containing pig iron sample, placing the sample in a conical flask, adding 15mL of hydrochloric acid and 5mL of nitric acid, and heating the sample on a 200-220 ℃ electric heating plate to dissolve the sample;
after the sample is completely dissolved, adding 5mL of perchloric acid, continuing to heat until perchloric acid white smoke is emitted, continuously shaking the conical flask until the solution is in a flowable wet salt shape, taking down, continuing to smoke, slightly cooling, adding 3 mL of distilled water to dissolve the salt, and fixing the volume to a 200mL volumetric flask to be used as the sample solution.
(3) Preparation of color developing solution and reference solution
Respectively preparing a developing solution and a reference solution of a nickel standard solution and a sample solution, wherein the preparation process comprises the following steps:
color development liquid: respectively transferring 0mL of standard solution mother liquor, 2.50 mL of standard solution mother liquor, 5.00mL of standard solution mother liquor, 7.50 mL of standard solution mother liquor and 5.00mL of sample solution into 6 100mL volumetric flasks, sequentially adding 10mL of 30% potassium sodium tartrate solution, 8mL of 5% sodium hydroxide solution, 10mL of 4% ammonium persulfate solution and 10mL of 1% dimethylglyoxime solution, fully and uniformly mixing after adding a new solution each time, standing for 20min, and then fixing the volume to 100 mL;
reference solution: respectively transferring 0mL of standard solution mother liquor, 2.50 mL of standard solution mother liquor, 5.00mL of standard solution mother liquor, 7.50 mL of standard solution mother liquor and 5.00mL of sample solution into 6 100mL volumetric flasks, sequentially adding 10mL of 30% potassium sodium tartrate solution, 18mL of 5% sodium hydroxide solution and 10mL of 4% ammonium persulfate solution into the volumetric flasks, fully mixing the solutions after adding a new solution each time, standing for 20min, and then fixing the volume to 100 mL;
(4) drawing a standard curve
Measuring the absorbance of the nickel standard solution with different concentrations at 530nm by adopting a spectrophotometry, drawing a standard curve by taking the concentration of nickel element as an abscissa and the absorbance as an ordinate, and obtaining the result: y =55.858x +13.811, R2=0.9995；
(5) Determination of the Nickel content in the sample solution
Measuring the absorbance of the sample solution at 530nm +/-5 nm, and calculating the content of the nickel element in the sample according to a standard curve; the samples were run in parallel four times and the results are shown in table 1.
The same samples were measured by the dimethylglyoxime gravimetric method and the results are given in Table 1.
Example 2
The sample to be tested in this example is a standard sample of ferronickel, GBW (E) 010423, Steel research technologies, Inc., and the testing procedure is as follows:
(1) preparing a standard solution mother solution: accurately weighing 0.1000g of nickel-containing pig iron standard sample, placing the sample in a conical flask, adding 15mL of hydrochloric acid and 5mL of nitric acid, and heating the sample on a 200-220 ℃ electric hot plate to dissolve the sample;
after the sample is completely dissolved, adding 5mL of perchloric acid, continuing to heat until perchloric acid white smoke is emitted, continuously shaking the conical flask until the solution is in a flowable wet salt shape, taking down, continuing to smoke, slightly cooling, adding 3 mL of distilled water to dissolve salts, and fixing the volume to a 200mL volumetric flask to be used as standard solution mother liquor.
(2) Preparation of sample solution
Weighing 0.1000 +/-0.0005 g of the ferronickel standard sample, placing the ferronickel standard sample in a conical flask, adding 15mL of hydrochloric acid and 5mL of nitric acid, and heating on a 200-220 ℃ electric heating plate to dissolve the sample;
after the sample is completely dissolved, adding 5mL of perchloric acid, continuing to heat until perchloric acid white smoke is emitted, continuously shaking the conical flask until the solution is in a flowable wet salt shape, taking down, continuing to smoke, slightly cooling, adding 3 mL of distilled water to dissolve salts, and fixing the volume to a volumetric flask of 200mL to serve as a sample solution;
(3) preparation of color developing solution and reference solution
Respectively preparing color developing solution and reference solution of standard solution and sample solution, wherein the preparation process comprises the following steps:
color development liquid: respectively transferring 0mL of standard solution mother liquor, 2.50 mL of standard solution mother liquor, 5.00mL of standard solution mother liquor, 7.50 mL of standard solution mother liquor and 5.00mL of sample solution into 6 100mL volumetric flasks, then sequentially adding 10mL of 25% potassium sodium tartrate solution, 8mL of 8% sodium hydroxide solution, 10mL of 4% ammonium persulfate solution and 10mL of 1% dimethylglyoxime solution, fully and uniformly mixing after adding a new solution each time, standing for 20min, and then fixing the volume to 100 mL;
reference solution: respectively transferring 0mL of standard solution mother liquor, 2.50 mL of standard solution mother liquor, 5.00mL of standard solution mother liquor, 7.50 mL of standard solution mother liquor and 5.00mL of sample solution into 6 100mL volumetric flasks, then sequentially adding 10mL of 25% potassium sodium tartrate solution, 18mL of 8% sodium hydroxide solution and 10mL of 4% ammonium persulfate solution, fully and uniformly mixing after adding a new solution each time, standing for 20min, and then fixing the volume to 100 mL;
(4) drawing a standard curve
Measuring the absorbance of the nickel standard solution with different concentrations prepared in the step (1) at 530nm by adopting a spectrophotometry, drawing a standard curve by taking the concentration of the nickel element as an abscissa and the absorbance as an ordinate, and obtaining the result: y =55.698x +13.699, R2=0.9999；
(5) Determination of the Nickel content in the sample solution
Measuring the absorbance of the sample solution at 530nm, and calculating the content of the nickel element in the sample according to the standard curve; the samples were run in parallel four times and the results are shown in table 1.
The same samples were also measured by the dimethylglyoxime gravimetric method and the results are shown in Table 1.
Example 3
The sample to be tested in this example is a ferronickel standard sample, YSBC280382d-2008S, Shandong institute of metallurgy and science, and the testing process is as follows:
(1) preparing a standard solution mother solution: accurately weighing 0.1000g of nickel-containing pig iron standard sample, placing the sample in a conical flask, adding 15mL of hydrochloric acid and 5mL of nitric acid, and heating the sample on a 200-220 ℃ electric hot plate to dissolve the sample;
after the sample is completely dissolved, adding 5mL of perchloric acid, continuing to heat until perchloric acid white smoke is emitted, continuously shaking the conical flask until the solution is in a flowable wet salt shape, taking down, continuing to smoke, slightly cooling, adding 3 mL of distilled water to dissolve salts, and fixing the volume to a 200mL volumetric flask to be used as standard solution mother liquor.
(2) Preparation of sample solution
Weighing 0.2500 +/-0.0005 g of the ferronickel standard sample, placing the ferronickel standard sample in a conical flask, adding 15mL of hydrochloric acid and 10mL of nitric acid, and heating on a 200-220 ℃ electric heating plate to dissolve the sample;
after the sample is completely dissolved, adding 5mL of perchloric acid, continuing to heat until perchloric acid white smoke is emitted, continuously shaking the conical flask until the solution is in a flowable wet salt shape, taking down, continuing to smoke, slightly cooling, adding 3 mL of distilled water to dissolve salts, and fixing the volume to a volumetric flask of 200mL to serve as a sample solution;
(3) preparation of color developing solution and reference solution
Respectively preparing color developing solution and reference solution of standard solution and sample solution, wherein the preparation process comprises the following steps:
color development liquid: respectively transferring 0mL of standard solution mother liquor, 2.50 mL of standard solution mother liquor, 5.00mL of standard solution mother liquor, 7.50 mL of standard solution mother liquor and 5.00mL of sample solution into 6 100mL volumetric flasks, sequentially adding 10mL of 25% potassium sodium tartrate solution, 8mL of 6% sodium hydroxide solution, 10mL of 5% ammonium persulfate solution and 10mL of 1% dimethylglyoxime solution, fully and uniformly mixing after adding a new solution each time, standing for 20min, and then fixing the volume to 100 mL;
reference solution: respectively transferring 0mL of standard solution mother liquor, 2.50 mL of standard solution mother liquor, 5.00mL of standard solution mother liquor, 7.50 mL of standard solution mother liquor and 5.00mL of sample solution into 6 100mL volumetric flasks, then sequentially adding 10mL of 25% potassium sodium tartrate solution, 18mL of 6% sodium hydroxide solution and 10mL of 5% ammonium persulfate solution, fully and uniformly mixing after adding a new solution each time, standing for 20min, and then fixing the volume to 100 mL;
(4) drawing a standard curve
And (2) measuring the absorbance of the nickel standard solution with different concentrations prepared in the step (1) at 530nm by adopting a spectrophotometry, and drawing a standard curve by taking the concentration of the nickel element as an abscissa and the absorbance as an ordinate, wherein the result is as follows: y =55.655x +13.229, R2=0.9998；
(5) Determination of the Nickel content in the sample solution
Measuring the absorbance of the sample solution at 530nm, and calculating the content of the nickel element in the sample according to the standard curve; the samples were run in parallel four times and the results are shown in table 1.
The same samples were measured by the dimethylglyoxime gravimetric method and the results are given in Table 1.
Example 4
The sample to be tested in this example is a ferronickel standard sample, gbw (e)010421, analysis and test center of steel research institute, and the testing process is as follows:
(1) preparing a standard solution mother solution: accurately weighing 0.1000g of nickel-containing pig iron standard sample, placing the sample in a conical flask, adding 15mL of hydrochloric acid and 5mL of nitric acid, and heating the sample on a 200-220 ℃ electric hot plate to dissolve the sample;
after the sample is completely dissolved, adding 5mL of perchloric acid, continuing to heat until perchloric acid white smoke is emitted, continuously shaking the conical flask until the solution is in a flowable wet salt shape, taking down, continuing to smoke, slightly cooling, adding 3 mL of distilled water to dissolve salts, and fixing the volume to a 200mL volumetric flask to be used as standard solution mother liquor.
(2) Preparation of sample solution
Weighing 0.3500 +/-0.0005 g of the ferronickel standard sample, placing the ferronickel standard sample in a conical flask, adding 25mL of hydrochloric acid and 10mL of nitric acid, and heating the sample on a 200-220 ℃ electric heating plate to dissolve the sample;
after the sample is completely dissolved, adding 10mL of perchloric acid, continuing to heat until perchloric acid white smoke is emitted, continuously shaking the conical flask until the solution is in a flowable wet salt shape, taking down, continuing to smoke, slightly cooling, adding 5mL of distilled water to dissolve salts, and fixing the volume to a volumetric flask of 200mL to serve as a sample solution;
(3) preparation of color developing solution and reference solution
Respectively preparing color developing solution and reference solution of standard solution and sample solution, wherein the preparation process comprises the following steps:
color development liquid: respectively transferring 0mL of standard solution mother liquor, 2.50 mL of standard solution mother liquor, 5.00mL of standard solution mother liquor, 7.50 mL of standard solution mother liquor and 5.00mL of sample solution into 6 100mL volumetric flasks, sequentially adding 15mL of 20% potassium sodium tartrate solution, 15mL of 6% sodium hydroxide solution, 15mL of 6% ammonium persulfate solution and 15mL of 2% dimethylglyoxime solution, fully and uniformly mixing after adding a new solution each time, standing for 25min, and then fixing the volume to 100 mL;
reference solution: respectively transferring 0mL of standard solution mother liquor, 2.50 mL of standard solution mother liquor, 5.00mL of standard solution mother liquor, 7.50 mL of standard solution mother liquor and 5.00mL of sample solution into 6 100mL volumetric flasks, sequentially adding 15mL of 20% potassium sodium tartrate solution, 25mL of 6% sodium hydroxide solution and 15mL of 6% ammonium persulfate solution, fully and uniformly mixing after adding a new solution each time, standing for 25min, and then fixing the volume to 100 mL;
(4) drawing a standard curve
Measuring the absorbance of the nickel standard solution with different concentrations prepared in the step (1) at 530nm by adopting a spectrophotometry, taking the concentration of nickel element as an abscissa and the absorbance as an ordinate, and drawing a standard curve result to obtain the value of y =55.655x +13.229, wherein R is2=0.9998；
(5) Determination of the Nickel content in the sample solution
Measuring the absorbance of the sample solution at 530nm, and calculating the content of the nickel element in the sample according to the standard curve; the samples were run in parallel four times and the results are shown in table 1.
The same samples were measured by the dimethylglyoxime gravimetric method and the results are given in Table 1.
Example 5
The sample to be tested in this example is a ferronickel standard sample, gbw (e)010422, analysis and test center of steel research institute, and the testing process is as follows:
(1) preparing a standard solution mother solution: accurately weighing 0.1000g of nickel-containing pig iron standard sample, placing the sample in a conical flask, adding 15mL of hydrochloric acid and 5mL of nitric acid, and heating the sample on a 200-220 ℃ electric hot plate to dissolve the sample;
after the sample is completely dissolved, adding 5mL of perchloric acid, continuing to heat until perchloric acid white smoke is emitted, continuously shaking the conical flask until the solution is in a flowable wet salt shape, taking down, continuing to smoke, slightly cooling, adding 3 mL of distilled water to dissolve salts, and fixing the volume to a 200mL volumetric flask to be used as standard solution mother liquor.
(2) Preparation of sample solution
Weighing 0.5000 +/-0.0005 g of the ferronickel standard sample, placing the ferronickel standard sample in a conical flask, adding 30mL of hydrochloric acid and 10mL of nitric acid, and heating on a 200-220 ℃ electric heating plate to dissolve the sample;
after the sample is completely dissolved, adding 10mL of perchloric acid, continuing to heat until perchloric acid white smoke is emitted, continuously shaking the conical flask until the solution is in a flowable wet salt shape, taking down, continuing to smoke, slightly cooling, adding 5mL of distilled water to dissolve salts, and fixing the volume to a volumetric flask of 200mL to serve as a sample solution;
(3) preparation of color developing solution and reference solution
Respectively preparing color developing solution and reference solution of standard solution and sample solution, wherein the preparation process comprises the following steps:
color development liquid: respectively transferring 0mL, 2.50 mL, 5.00mL, 7.50 mL, 10.00mL of standard solution mother liquor and 5.00mL of sample solution into 6 100mL volumetric flasks, then sequentially adding 20mL of 30% potassium sodium tartrate solution, 18mL of 8% sodium hydroxide solution, 20mL of 6% ammonium persulfate solution and 20mL of 2% dimethylglyoxime solution, fully and uniformly mixing after adding a new solution each time, standing for 25min, and then fixing the volume to 100 mL;
reference solution: respectively transferring 0mL of standard solution mother liquor, 2.50 mL of standard solution mother liquor, 5.00mL of standard solution mother liquor, 7.50 mL of standard solution mother liquor and 5.00mL of sample solution into 6 100mL volumetric flasks, then sequentially adding 20mL of 30% potassium sodium tartrate solution, 28mL of 8% sodium hydroxide solution and 20mL of 6% ammonium persulfate solution, fully and uniformly mixing after adding a new solution each time, standing for 25min, and then fixing the volume to 100 mL;
(4) drawing a standard curve
And (2) measuring the absorbance of the nickel standard solution with different concentrations prepared in the step (1) at 530nm by adopting a spectrophotometry, and drawing a standard curve by taking the concentration of the nickel element as an abscissa and the absorbance as an ordinate, wherein the result is as follows: y =56.014x +12.228, R2=0.9999；
(5) Determination of the Nickel content in the sample solution
Measuring the absorbance of the sample solution at 530nm, and calculating the content of the nickel element in the sample according to the standard curve; the samples were run in parallel four times and the results are shown in table 1.
The same samples were measured by the dimethylglyoxime gravimetric method and the results are given in Table 1.
TABLE 1 results of measurement/The% of samples of the examples
By comparing the two methods, the result of the method provided by the invention is basically consistent with the result of the dimethylglyoxime gravimetric method, and the method has better accuracy within an allowable range.
Claims (7)
1. A method for rapidly measuring the nickel content in nickel-containing pig iron is characterized in that a dimethylglyoxime direct photometry method is adopted for measuring, and the measuring process is as follows:
(1) preparing a nickel standard solution mother solution;
(2) preparing a sample solution: adding hydrochloric acid and nitric acid into a nickel-containing pig iron sample, and heating for dissolving; adding perchloric acid after complete dissolution, heating until perchloric acid white smoke is emitted, continuously heating until the solution becomes a flowable wet salt shape, and adding distilled water to dissolve the salt;
(3) respectively preparing a developing solution and a reference solution of a nickel standard solution and a sample solution;
(4) drawing a standard curve by adopting a spectrophotometry;
(5) and (5) measuring the absorbance of the sample solution, and calculating the content of the nickel element in the sample according to the standard curve.
2. The method for rapidly determining the nickel content in nickel-containing pig iron according to claim 1, wherein the sample solution in step (2) is prepared by the following steps:
weighing 0.1000-0.5000g of nickel-containing pig iron sample, placing the sample in a conical flask, adding 15-30mL of hydrochloric acid and 5-10mL of nitric acid, and heating the sample on a 200-220 ℃ electric hot plate to dissolve the sample;
after the sample is completely dissolved, adding 5-10ml of perchloric acid, continuing heating until perchloric acid white smoke is emitted, and continuously shaking the conical flask until the solution is in a flowable wet salt shape; taking down, continuing fuming, slightly cooling, adding 3-5mL of distilled water to dissolve salts, and fixing the volume to a 200mL volumetric flask to obtain a sample solution.
3. The method for rapidly determining the nickel content in nickel-containing pig iron according to claim 1, wherein the color-developing solution and the reference solution in step (3) are prepared by the following steps:
color development liquid: transferring standard solution mother liquor with different volumes and sample solution with certain volume into different volumetric flasks of 100mL, then sequentially adding 10-20mL of potassium sodium tartrate solution, 8-18 mL of sodium hydroxide solution, 10-20mL of ammonium persulfate solution and 10-20mL of dimethylglyoxime solution, standing for 15-30min, and fixing the volume to 100 mL;
reference solution: and transferring the standard solution mother liquor with different volumes and the sample solution with a certain volume into different 100mL volumetric flasks, then sequentially adding 10-20mL of potassium sodium tartrate solution, 18-28 mL of sodium hydroxide solution and 10-20mL of ammonium persulfate solution, standing for 15-30min, and then fixing the volume to 100 mL.
4. The method for rapidly determining the nickel content in nickel-containing pig iron according to claim 5, wherein the concentration of the potassium sodium tartrate solution is 20% -30%, the concentration of the sodium hydroxide solution is 5% -8%, the concentration of the ammonium persulfate solution is 4% -6%, and the concentration of the dimethylglyoxime solution is 1% -2%.
5. The method as claimed in claim 5, wherein the developing solution and the reference solution are mixed thoroughly each time a new solution is added during the preparation process.
6. The method for rapidly determining the nickel content in the nickel-containing pig iron according to claim 1, wherein the step (4) of drawing a standard curve comprises the following specific operations: and (3) measuring the absorbance of the nickel standard solution with different concentrations at 530nm +/-5 nm by adopting a spectrophotometry, and drawing a standard curve by taking the nickel concentration as an abscissa and the absorbance as an ordinate.
7. The method as claimed in claim 1, wherein in step (5), the absorbance of the sample solution is measured at 530nm ± 5 nm.
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