Rapid determination method for nickel content in nickel-containing pig iron

A rapid measurement, nickel pig iron technology, applied in measuring devices, analysis by chemical reaction of materials, material analysis by observing the influence of chemical indicators, etc., can solve the problems of long detection cycle and cumbersome operation process, etc. Achieve the effect of high labor intensity, accurate analysis results, and simple and convenient operation

Pending Publication Date: 2021-10-01

石钢京诚装备技术有限公司

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Problems solved by technology

For nickel-containing pig iron with high content, diacetyl oxime gravimetric method and diacetyl oxime precipitation separation EDTA titration method are commonly used. The op...

Abstract

The invention belongs to the field of raw material detection in the iron and steel industry, and particularly relates to a rapid determination method of nickel content in nickel-containing pig iron, the determination method is as follows: (1) preparing a nickel standard solution mother solution; (2) preparing a sample solution: adding hydrochloric acid and nitric acid into the nickel-containing pig iron sample, and heating for dissolving; adding perchloric acid after the solution is completely dissolved, heating until perchloric acid white smoke is emitted, and continuously heating until the solution is in a flowable wet salt shape; and adding distilled water to dissolve the salt; (3) respectively preparing a developing solution and a reference solution of the nickel standard solution and the sample solution; (4) drawing a standard curve by adopting a spectrophotometric method; and (5) determining 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 not only can improve the detection efficiency and detection precision of the nickel content, but also reduces the operation difficulty of sample preparation and sample detection.

Application Domain

Material analysis by observing effect on chemical indicator

Technology Topic

Standard curveNickel content +9

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Experimental program(5)

Example Embodiment

[0030] Example 1

[0031] The sample to be measured in this embodiment is a nickel-containing pig iron standard sample, GSB03-2681-2011, Sinosteel Jilin Ferroalloy Co., Ltd., and the measurement process is as follows:

[0032] (1) Prepare standard solution mother liquor: Accurately weigh 0.1000g of nickel-containing pig iron standard sample, place it in a conical flask, add 15 mL of hydrochloric acid and 5 mL of nitric acid, heat on a 200-220°C electric heating plate to dissolve the sample;

[0033] After the sample is completely dissolved, add 5 ml of perchloric acid, continue to heat until white smoke of perchloric acid is emitted, shake the conical flask continuously until the solution becomes a flowable wet salt, remove it, continue to smoke, cool slightly, add 3 Dissolve salts in mL of distilled water, and dilute to a 200mL volumetric flask as the mother solution of the standard solution.

[0034] (2) Preparation of sample solution

[0035] Weigh 0.1000±0.0005g of the above nickel-containing pig iron sample, place it in a conical flask, add 15 mL of hydrochloric acid and 5 mL of nitric acid, and heat on a 200-220°C electric heating plate to dissolve the sample;

[0036] After the sample is completely dissolved, add 5 ml of perchloric acid, continue to heat until white smoke of perchloric acid is emitted, shake the conical flask continuously until the solution becomes a flowable wet salt, remove it, continue to smoke, cool slightly, add 3 Dissolve salts in mL of distilled water, and dilute to a 200mL volumetric flask as the sample solution.

[0037] (3) Preparation of chromogenic solution and reference solution

[0038] Prepare the chromogenic solution and reference solution of nickel standard solution and sample solution respectively, and the preparation process is as follows:

[0039] Chromogenic solution: Pipette 0, 2.50, 5.00, 7.50, 10.00ml of standard solution mother solution and 5.00ml of sample solution into six 100ml volumetric flasks, and then add 10mL of 30% potassium sodium tartrate solution, 8mL of 5% sodium hydroxide solution, 10 mL of 4% ammonium persulfate solution, and 10 mL of 1% dimethylglyoxime solution. Each time a new solution is added, it needs to be fully mixed, let it stand for 20 minutes, and then set aside. Capacity to 100mL;

[0040] Reference solution: Pipette 0, 2.50, 5.00, 7.50, 10.00ml of standard solution mother solution and 5.00ml of sample solution into six 100ml volumetric flasks, and then add 10 mL of 30% potassium sodium tartrate solution, 18mL of 5% sodium hydroxide solution and 10mL of 4% ammonium persulfate solution, each time after adding a new solution, fully mix, let stand for 20min, and then dilute to 100mL;

[0041] (4) Draw a standard curve

[0042] Using spectrophotometry, measure the absorbance of different concentrations of nickel standard solutions at 530nm, take the concentration of nickel element as the abscissa, and the absorbance as the ordinate, draw a standard curve, the result is: y=55.858x+13.811, R 2 =0.9995;

[0043] (5) Determination of nickel content in the sample solution

[0044] The absorbance of the sample solution was measured at 530nm±5nm, and the content of nickel element in the sample was calculated according to the standard curve; the samples were measured in parallel four times, and the results are shown in Table 1.

[0045] The same sample was measured by diacetyl oxime gravimetric method, and the results are shown in Table 1.

Example Embodiment

[0046] Example 2

[0047] The sample to be measured in this embodiment is the nickel-iron standard sample, GBW (E) 010423, from Steel Research Nanoco Testing Technology Co., Ltd. The measurement process is as follows:

[0048] (1) Prepare standard solution mother liquor: Accurately weigh 0.1000g of nickel-containing pig iron standard sample, place it in a conical flask, add 15 mL of hydrochloric acid and 5 mL of nitric acid, heat on a 200-220°C electric heating plate to dissolve the sample;

[0049] After the sample is completely dissolved, add 5 ml of perchloric acid, continue to heat until white smoke of perchloric acid is emitted, shake the conical flask continuously until the solution becomes a flowable wet salt, remove it, continue to smoke, cool slightly, add 3 Dissolve salts in mL of distilled water, and dilute to a 200mL volumetric flask as the mother solution of the standard solution.

[0050] (2) Preparation of sample solution

[0051] Weigh 0.1000±0.0005g of the above nickel-iron standard sample, place it in a conical flask, add 15mL hydrochloric acid and 5mL nitric acid, heat on a 200-220°C electric heating plate to dissolve the sample;

[0052]After the sample is completely dissolved, add 5 ml of perchloric acid, continue to heat until white smoke of perchloric acid is emitted, shake the conical flask continuously until the solution becomes a flowable wet salt, remove it, continue to smoke, cool slightly, add 3 Dissolve salts in mL distilled water, and dilute to 200mL volumetric flask as sample solution;

[0053] (3) Preparation of chromogenic solution and reference solution

[0054] Make the chromogenic solution and reference solution of standard solution and sample solution respectively, and the preparation process is as follows:

[0055] Chromogenic solution: Pipette 0, 2.50, 5.00, 7.50, 10.00ml standard solution mother solution and 5.00ml sample solution into six 100ml volumetric flasks, then add 10mL potassium sodium tartrate solution with a concentration of 25%, and 8mL with a concentration of 8 % sodium hydroxide solution, 10 mL of 4% ammonium persulfate solution, and 10 mL of 1% dimethylglyoxime solution, each time a new solution is added, it needs to be fully mixed, let it stand for 20 minutes, and then dilute to 100mL;

[0056] Reference solution: pipette 0, 2.50, 5.00, 7.50, 10.00ml of standard solution mother solution and 5.00ml of sample solution into six 100ml volumetric flasks, then add 10mL of 25% sodium potassium tartrate solution, 18mL of It is 8% sodium hydroxide solution and 10 mL of 4% ammonium persulfate solution. After each addition of new solution, it needs to be fully mixed, let it stand for 20 minutes, and then set the volume to 100 mL;

[0057] (4) Draw a standard curve

[0058] Using spectrophotometry, measure the absorbance of nickel standard solutions with different concentrations in step (1) at 530nm, take the concentration of nickel element as the abscissa, absorbance as the ordinate, draw the standard curve, the result is: y=55.698x+13.699 , R 2 =0.9999;

[0059] (5) Determination of nickel content in the sample solution

[0060] The absorbance of the sample solution was measured at 530 nm, and the content of nickel element in the sample was calculated according to the standard curve; the samples were measured in parallel four times, and the results are shown in Table 1.

[0061] Simultaneously, the same sample was measured by the gravimetric method of dimethylglyoxime, and the results are shown in Table 1.

Example Embodiment

[0062] Example 3

[0063] The sample to be measured in this embodiment is a nickel-iron standard sample, YSBC280382d-2008S, Shandong Academy of Metallurgical Sciences, and the measurement process is as follows:

[0064] (1) Prepare standard solution mother liquor: Accurately weigh 0.1000g of nickel-containing pig iron standard sample, place it in a conical flask, add 15 mL of hydrochloric acid and 5 mL of nitric acid, heat on a 200-220°C electric heating plate to dissolve the sample;

[0065] After the sample is completely dissolved, add 5 ml of perchloric acid, continue to heat until white smoke of perchloric acid is emitted, shake the conical flask continuously until the solution becomes a flowable wet salt, remove it, continue to smoke, cool slightly, add 3 Dissolve salts in mL of distilled water, and dilute to a 200mL volumetric flask as the mother solution of the standard solution.

[0066] (2) Preparation of sample solution

[0067] Weigh 0.2500±0.0005g of the above nickel-iron standard sample, place it in a conical flask, add 15mL hydrochloric acid and 10mL nitric acid, heat on a 200-220°C electric heating plate to dissolve the sample;

[0068] After the sample is completely dissolved, add 5 ml of perchloric acid, continue to heat until white smoke of perchloric acid is emitted, shake the conical flask continuously until the solution becomes a flowable wet salt, remove it, continue to smoke, cool slightly, add 3 Dissolve salts in mL distilled water, and dilute to 200mL volumetric flask as sample solution;

[0069] (3) Preparation of chromogenic solution and reference solution

[0070] Make the chromogenic solution and reference solution of standard solution and sample solution respectively, and the preparation process is as follows:

[0071] Chromogenic solution: pipette 0, 2.50, 5.00, 7.50, 10.00ml standard solution mother solution and 5.00ml sample solution into six 100ml volumetric flasks, then add 10mL potassium sodium tartrate solution with a concentration of 25% and 8mL with a concentration of 6 % sodium hydroxide solution, 10 mL of 5% ammonium persulfate solution, and 10 mL of 1% dimethylglyoxime solution, each time a new solution is added, it needs to be fully mixed, let it stand for 20 minutes, and then dilute to 100mL;

[0072] Reference solution: pipette 0, 2.50, 5.00, 7.50, 10.00ml of standard solution mother solution and 5.00ml of sample solution into six 100ml volumetric flasks, then add 10mL of 25% sodium potassium tartrate solution, 18mL of It is 6% sodium hydroxide solution and 10 mL of 5% ammonium persulfate solution. Each time a new solution is added, it needs to be fully mixed, let it stand for 20 minutes, and then set the volume to 100 mL;

[0073] (4) Draw a standard curve

[0074] Using spectrophotometry, measure the absorbance of different concentrations of nickel standard solutions prepared in step (1) at 530nm, take the concentration of nickel element as the abscissa, and the absorbance as the ordinate, and the result of drawing the standard curve is: y=55.655x+13.229, R 2 =0.9998;

[0075] (5) Determination of nickel content in the sample solution

[0076] The absorbance of the sample solution was measured at 530 nm, and the content of nickel element in the sample was calculated according to the standard curve; the samples were measured in parallel four times, and the results are shown in Table 1.

[0077] The same sample was measured by diacetyl oxime gravimetric method, and the results are shown in Table 1.

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InactiveCN104673816AHigh gene knockout efficiencyeasy to operate

Owner:GUANGDONG MEDICAL UNIV

Classification and recommendation of technical efficacy words

easy to operate
Manual labor intensity is high

Rapid determination method for nickel content in nickel-containing pig iron

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Example Embodiment

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Example Embodiment

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Description & Claims & Application Information

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