CN104777154A - Method for simultaneously determining mixed elements in industrially pure iron - Google Patents
Method for simultaneously determining mixed elements in industrially pure iron Download PDFInfo
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Abstract
The invention discloses a method for simultaneously determining mixed elements in industrially pure iron. The method comprises the following steps: processing all mixed elements to be determined, comprising Si, Mn, Cu, Cr, Ni and P to prepare standard solutions, scanning the signal intensities and analysis lines of the elements to be determined at the wavelengths of the analysis lines of co-existing elements to be determined through ICP-AES, selecting common carbon steel and highly pure iron as standard substances on the basis of determined absorption peak intensities, scanning under the ICP-AES, selecting above 6 different concentrations of mixed elements comprising Si, Mn, Cu, Cr, Ni and P to draw a standard curve, introducing an industrially pure iron sample solution and a blank sample solution into the ICP-AES, determining the signal intensities of ions to be determined, and solving the content of Si, Mn, Cu, Cr, Ni and P in the sample solution according to the calibration curve of standard solutions with known mass percentages of Si, Mn, Cu, Cr, Ni and P.
Description
Technical field
The present invention relates to technical field of ferrous metallurgical analysis, particularly relate to assorted element in a kind of Simultaneously test ingot iron, adopt hydrochloric acid, nitric acid nitration mixture to be decomposed by sample, utilize the method for the silicon of ICP-AES directly, side by side in working sample solution, manganese, copper, chromium, nickel, phosphorus.
Background technology
Ingot iron is the one of steel, its chemical composition mainly iron, and content is at 99.50%-99.90%, and carbon content is below 0.04%, and other constituent contents are fewer better.General industry pure iron quality is soft especially, and toughness is large especially, and electromagnetic performance is fine, iron fusing point is higher than iron, gets rusty in malaria than iron difficulty, so it is mainly as electromagnetic material, be widely used in electron and electrician, electric elements, magnetic material, noncrystal goods, relay, sensor, automotive brake, frame, the products such as ammeter solenoid valve.In ingot iron, the content of impurity directly affects the performance of product.
For the more existing researchs both at home and abroad of silicon, manganese, copper, chromium, nickel, phosphorus yield in ingot iron, but standard method there is no.Thank to new talent to discuss " inductively coupled plasma mass spectrometry measures assorted element in high purity iron ", although inductivity coupled plasma mass spectrometry detects dangerous low, iron-based bulk concentration is too high can produce serious matrix effect; After the phosphato-molybdic heteropolyacid that the method that Zhou Xilin, Yan Lidong etc. have studied " ICP-AES measures trace phosphorus in high purity iron " adopts methylisobutylketone extraction ammonium molybdate and phosphorus to generate, adopt ICP-AES to measure, the method adopt organic reagent methylisobutylketone toxicity large, operating personnel are endangered greatly, contaminated environment; In addition also have the bibliographical information of " in graphite furnace atomic absorption spectrometry high purity iron assorted element ", the method background interference is large, and precision is poor.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of highly sensitive, finding speed is fast, easy and simple to handle and little relative to additive method interference, there is good selectivity simultaneously, the analytical approach of the silicon in the ICP-AES mensuration ingot iron of accurate data, manganese, copper, chromium, nickel, phosphorus can be provided for smelting Composition Control process.
For reaching above-mentioned purpose, the method for assorted element in a kind of Simultaneously test ingot iron of the present invention, comprises the following steps:
Take ingot iron sample, be placed in acid and boil clean quartz beaker, add hydrochloric acid, nitric acid, high purity water successively; In low temp. electric hot plate heating for dissolving, and constantly add high purity water sample dissolution, after sample dissolution, be cooled to room temperature, move in color comparison tube, be diluted to scale, shake up, machine in wait, in company with making reagent blank;
Preparation Fe, Cu, Ni, Cr, P, Si standard solution ICP-AES scans signal intensity and the analytical line of element to be measured respectively at the ultimate analysis line wavelength place to be measured that coexists;
Be Fe, Cu, Cr, Ni solution of 500ug/mL respectively to mass concentration, mass concentration is that the P solution of 10ug/mL and blank reagent solution carry out spectrogram scanning in ICP-AES, sets up MSF model:
Select straight carbon steel and high purity iron standard substance, take the standard serial solution being mixed with calibration curve with ingot iron sample same method, in straight carbon steel or high purity iron standard substance, the content of each element covers the measurement range Si of each element, Mn, Cu, Cr, Ni is 0.003 ~ 0.400%, P is 0.001 ~ 0.050%, standard serial solution is introduced inductive coupling plasma emission spectrograph, measure the signal intensity treating measured ion, using reagent blank as the blank of curve, take mass percent as horizontal ordinate, the signal intensity of ion is that ordinate draws Si, Mn, Cu, Cr, Ni, P calibration curve, each element determination scope at least comprises minimum point content, peak content, the standard substance of more than 6 kinds different contents of intermediate point content,
Ingot iron specimen sample solution, blank sample solution are introduced inductive coupling plasma emission spectrograph, measure the signal intensity treating measured ion, according to Si, Mn, Cu, Cr, Ni, P standard solution calibration curve of known quality percentage, obtain the content of Si, Mn, Cu, Cr, Ni, P in sample solution;
In sample, the content of silicon, manganese, copper, chromium, nickel, phosphorus is calculated as follows:
W％＝Wi-W
0
In formula: the mass percent content of element in W-ingot iron;
W
0-element is at the mass percent of blank to be measured;
The mass percent of Wi-element in ingot iron to be measured.
The invention difference from existing technology is that the present invention achieves following technique effect:
1, of the present invention for the silicon in ingot iron, manganese, copper, chromium, nickel, phosphorus yield, by adopting silicon, manganese, copper, chromium, nickel, the phosphorus content in inductive coupling plasma emission spectrograph detection ingot iron, the present invention is by the repeatedly inspection to ingot iron sample, and effect is good;
2, the present invention adopts high purity iron and straight carbon steel standard substance to make working curve, overcomes Matrix effects; Adopt the multispectral matching of MSF to overcome Fe, Cu, Cr, Ni to disturb the mensuration of P, there is the range of linearity wide, highly sensitive, easy and simple to handle, accurate, the reliable feature of analysis result;
3, use this method to measure the silicon in ingot iron, manganese, copper, chromium, nickel, phosphorus, can complete by Simultaneously test in 2 hours, shorten sample processing time, it is 0.003at ~ 0.030at% that the scope of analytical approach can reach P; Si, Mn, Cu, Cr, Ni are 0.005at ~ 0.300at%;
4, the inventive method greatly reduces solvent use amount, is conducive to environmental protection.
Embodiment
Below in conjunction with embodiment, to above-mentioned being described in more detail with other technical characteristic and advantage of the present invention.
1., in the embodiment of the present invention, agents useful for same is preferred:
Nitric acid: top grade pure (16mol/L);
Hydrochloric acid: top grade pure (12mol/L);
Sulfuric acid: top grade pure (18mol/L);
Sodium carbonate: top grade is pure
Straight carbon steel, high purity iron standard substance: standard substance certificate provides exact level;
25mL color comparison tube; 300mL quartz beaker;
High purity iron, copper, nickel, potassium dichromate, potassium dihydrogen phosphate, silicon dioxide benchmark material;
Argon gas: purity of argon >=99.9%.
Pressurized air
Preferred inductive coupling plasma emission spectrograph model is PE company Optima 5300DV; ICP-AES Instrument working parameter is as follows:
2. sample analysis
2.1 sample preparation
Take 0.500g ingot iron sample, be placed in acid and boil clean 300mL quartz beaker, add 5mL hydrochloric acid, 5mL nitric acid, 15mL high purity water successively; In low temp. electric hot plate (300 DEG C ~ 400 DEG C), dissolve, and constantly add high purity water, keep liquor capacity at about 15 ~ 20mL, after sample dissolution, be cooled to room temperature, move in 25mL color comparison tube, be diluted to scale, shake up, machine in wait, in company with making reagent blank;
2.2 select spectral line: preparing standard solution carries out length scanning to each element, and sets up multispectral matching (MSF) model:
The Fe standard solution of 500ug/mL: take 0.5g high-purity iron powder in 300mL quartz beaker, adds 15mL hydrochloric acid, 15mL nitric acid, 25mL high purity water successively, after low temp. electric hot plate dissolves, moves in 1000mL volumetric flask, dilution scale;
The Cu standard solution of 500ug/mL: take the high-purity red copper of 0.5g in 300mL quartz beaker, add 3mL sulfuric acid, 15mL nitric acid, 25mL high purity water successively, after low temp. electric hot plate dissolves, sulfuric acid cigarette 1min is emitted in evaporation, cooling, with moving in 1000mL volumetric flask after high purity water dissolved salts, dilution scale, this solution is the Cu standard solution of 500ug/mL; The Cu standard solution 20mL pipetting 500ug/mL, in 100mL volumetric flask, adds 5mL nitric acid, dilutes scale with high purity water, and this solution is the Cu standard solution of 100ug/mL;
The Ni standard solution of 500ug/mL: take 0.5g high-purity metal nickel in 300mL quartz beaker, after adding 20mL high purity water, the dissolving of 10mL nitric acid low temp. electric hot plate, move in 1000mL volumetric flask, dilution scale, this solution is the Ni standard solution of 500ug/mL; The Ni standard solution 20mL pipetting 500ug/mL, in 100mL volumetric flask, adds 5mL nitric acid, dilutes scale with high purity water, and this solution is the Ni standard solution of 100ug/mL;
The Cr standard solution of 500ug/mL: take primary standard substance potassium dichromate (drying 1h through 150 DEG C) 1.415g, after water-soluble, constant volume is in 1000mL volumetric flask, and this solution is the Cr standard solution of 500ug/mL; The Cr standard solution 20mL pipetting 500ug/mL, in 100mL volumetric flask, dilutes scale with high purity water, and this solution is the Cr standard solution of 100ug/mL;
The P standard solution of 100ug/mL: take 0.440g potassium dihydrogen phosphate primary standard substance (drying 2h at 105 DEG C in advance) in 1000mL volumetric flask, dissolve with high purity water and add 10mL nitric acid, be diluted to scale with high purity water, this standard solution is 100ug/mL containing P.The P standard solution 10mL pipetting 100ug/mL, in 100mL volumetric flask, dilutes scale with high purity water, and this solution is the P standard solution of 10ug/mL;
The Si standard solution of 100ug/mL: take 0.214g silicon dioxide (in advance at 1000 DEG C of calcination 1h, room temperature is chilled in exsiccator) be placed in the platinum crucible adding 3g anhydrous Na2CO3, cover 1 ~ 2g anhydrous Na2CO3 more above, be placed in 950 DEG C of muffle furnace heating to melt, cooling, leaches frit to entirely molten with the plastic beaker filling cold water, moves in 1000mL volumetric flask, use high purity water constant volume, this solution is the Si standard solution of 100ug/mL;
Get the P that mass concentration is 100ug/mL, Cu, Cr, Ni, Si, Mn single element standard solution, scan the signal intensity of element to be measured respectively at the ultimate analysis line wavelength place to be measured that coexists with ICP-AES, highly sensitive spectral line is determined in the emissive porwer of each wavelength location and background signal: Si 251.611nm (Intensity:65119.0) according to each element, Mn 257.610nm (Intensity:295353.2), Cu 324.752nm (Intensity:36099.4), Cr 267.716nm (Intensity:125194.0), Ni 231.604nm (Intensity:27415.9), P 213.617nm (Intensity:1029.9) does analytical line.
Because Fe, Cu, Cr, Ni mensuration to P has interference, nitric acid with 1% is blank solution, be Fe, Cu, Cr, Ni solution of 500ug/mL respectively to mass concentration, mass concentration is that the P solution of 10ug/mL and blank reagent solution carry out spectrogram scanning in ICP-AES, sets up MSF model:
First, open the MSF page at instrumentation interface, setting spectral line region (213.47nm-213.77nm) makes multispectral fitting data simpler.Then by the nitric acid of 1%, mass concentration is Fe, Cu, Cr, Ni solution of 500ug/mL, and mass concentration is that the P solution of 10ug/mL is used as sample and is analyzed in ICP-AES;
Secondly, in the MSF page at instrumentation interface, the nitric acid of 1% is arranged blank solution, Fe, Cu, Cr, Ni solution is set to chaff interference, P solution is set to analyze thing, and store method is MSF method.
The peak computing method of deployment method file → peak process → Si, Mn, Cu, Cr, Ni are chosen as peak area, the peak computing method of P element selects MSF → spectral line correction → Si, the correction of Mn, Cu, Cr, Ni be chosen as completely without, the overlapping correction of P element selects MSF → Si, the background dot of Mn, Cu, Cr, Ni is 2 points, the MSF method that the background dot of P element selects MSF → selection to preserve.In assay surface, select new coefficient, again process data, again store method.
2.3 make calibration curve
In order to reduce matrix effect, selecting the standard substance such as straight carbon steel, high purity iron, processing by under above-mentioned sample analysis method and process sample the same terms, being mixed with the standard serial solution of calibration curve.In straight carbon steel, high purity iron standard substance, the content of each element will cover the measurement range Si of each element of the present invention, Mn, Cu, Cr, Ni be 0.003 ~ 0.400%, P be 0.001 ~ 0.050% (comprising the standard substance of at least 6 kinds of different contents such as each element determination scope minimum point content, peak content, intermediate point content).The standard serial solution of calibration curve is introduced inductive coupling plasma emission spectrograph, measure the signal intensity treating measured ion, using reagent blank as the blank of curve, take mass percent as horizontal ordinate, the signal intensity of ion is that ordinate draws Si, Mn, Cu, Cr, Ni, P calibration curve (often kind of element all needs the standard substance of 6 kinds of different contents).
Ingot iron specimen sample solution, blank sample solution are introduced inductive coupling plasma emission spectrograph, measure the signal intensity treating measured ion, according to Si, Mn, Cu, Cr, Ni, P standard solution calibration curve of known quality percentage, obtain the content of Si, Mn, Cu, Cr, Ni, P in sample solution;
2.4 results calculate
In sample, the content of silicon, manganese, copper, chromium, nickel, phosphorus is calculated as follows:
W％＝Wi-W
0
In formula: the mass percent content of element in W-ingot iron;
W
0-element is at the mass percent of blank to be measured;
The mass percent of Wi-element in ingot iron to be measured;
This method sensing range: P is 0.003at ~ 0.030at%; Si, Mn, Cu, Cr, Ni are 0.005at ~ 0.300at%.
Embodiment 1
Take carbon steel (YSBC11123-99), after ingot iron (GBW01407), (YSBC15002-93), (YSBC20112-95), (GBW01406), (BH0222), import standard specimen (1/1) dissolve as stated above, make working curve, curve correlation coefficient r is greater than 0.999, empirically method is prepared 11 parts of blank solutions and is divided and measure for 3 times, according to the detection limit formula C that IUPAC (IUPAC) defines
l=3S
b/ k (Sb is blank standard deviation, and k the is corresponding Slope of Calibration Curve) method of calculating detects and is limited to P 0.00026%; Si, Mn, Cu, Cr, Ni 0.00043%.
Embodiment 2
Take ingot iron (GBW01401a), (YSBC11011-99), (YSBC41014-99), (YSBC15001a-98) measure as stated above, the results are shown in Table 1.
Table 1 standard model measurement result
Implementation: all exceed measurement range of the present invention with the data of No. * in table can only be reference value.
Embodiment 3
Take ingot iron (GBW01404a), (BGY97-1), and ingot iron sample 1#, 2#, 3#, 4# measure as stated above, the results are shown in Table 2.
Table 2 standard model, sample specimens measurement result
Implementation: all exceed measurement range of the present invention with the data of No. * in table can only be reference value.
Therefore, by the checking of above-mentioned embodiment, can find out that ICP-AES of the present invention measures silicon, manganese, copper, chromium, nickel, phosphorus in ingot iron, P is 0.003at ~ 0.030at%; Si, Mn, Cu, Cr, Ni are 0.005at ~ 0.300at%.Analytical approach precision is high, accuracy is high.This method is quick, easy, promotes, uses in can producing.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (1)
1. the method for assorted element in Simultaneously test ingot iron, is characterized in that comprising the following steps:
Take ingot iron sample, be placed in acid and boil clean quartz beaker, add hydrochloric acid, nitric acid, high purity water successively; In low temp. electric hot plate heating for dissolving, and constantly add high purity water sample dissolution, after sample dissolution, be cooled to room temperature, move in color comparison tube, be diluted to scale, shake up, machine in wait, in company with making reagent blank;
Preparation Fe, Cu, Ni, Cr, P, Si standard solution ICP-AES scans signal intensity and the analytical line of element to be measured respectively at the ultimate analysis line wavelength place to be measured that coexists;
Be Fe, Cu, Cr, Ni solution of 500ug/mL respectively to mass concentration, mass concentration is that the P solution of 10ug/mL and blank reagent solution carry out spectrogram scanning in ICP-AES, sets up MSF model:
Select straight carbon steel and high purity iron standard substance, take the standard serial solution being mixed with calibration curve with ingot iron sample same method, in straight carbon steel or high purity iron standard substance, the content of each element covers the measurement range Si of each element, Mn, Cu, Cr, Ni is 0.003 ~ 0.400%, P is 0.001 ~ 0.050%, standard serial solution is introduced inductive coupling plasma emission spectrograph, measure the signal intensity treating measured ion, using reagent blank as the blank of curve, take mass percent as horizontal ordinate, the signal intensity of ion is that ordinate draws Si, Mn, Cu, Cr, Ni, P calibration curve, each element determination scope at least comprises minimum point content, peak content, the standard substance of more than 6 kinds different contents of intermediate point content,
Ingot iron specimen sample solution, blank sample solution are introduced inductive coupling plasma emission spectrograph, measure the signal intensity treating measured ion, according to Si, Mn, Cu, Cr, Ni, P standard solution calibration curve of known quality percentage, obtain the content of Si, Mn, Cu, Cr, Ni, P in sample solution;
In sample, the content of silicon, manganese, copper, chromium, nickel, phosphorus is calculated as follows:
W％＝Wi-W
0
In formula: the mass percent content of element in W-ingot iron;
W
0-element is at the mass percent of blank to be measured;
The mass percent of Wi-element in ingot iron to be measured.
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| CN107764802A (en) * | 2017-11-23 | 2018-03-06 | 中国航发北京航空材料研究院 | Trace Al in a kind of measure pure iron, chromium, copper, manganese, the method for nickel and element silicon |
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| CN107764802A (en) * | 2017-11-23 | 2018-03-06 | 中国航发北京航空材料研究院 | Trace Al in a kind of measure pure iron, chromium, copper, manganese, the method for nickel and element silicon |
| CN110927144A (en) * | 2019-12-10 | 2020-03-27 | 辽宁科技大学 | ICP-AES (inductively coupled plasma-atomic emission Spectrometry) measuring method for content of impurity phosphorus in steel |
| CN110907527A (en) * | 2019-12-16 | 2020-03-24 | 重庆市计量质量检测研究院 | Method for measuring content of impurity elements in high-purity gold jewelry |
| CN113063773A (en) * | 2021-03-12 | 2021-07-02 | 中航金属材料理化检测科技有限公司 | Method for measuring contents of chromium, tungsten and phosphorus in 1Cr11Ni2W2MoV |
| CN113418907A (en) * | 2021-07-26 | 2021-09-21 | 中车大连机车车辆有限公司 | Method for dissolving cast iron material and method for detecting element content in cast iron |
| CN113670895A (en) * | 2021-08-20 | 2021-11-19 | 江苏扬农化工集团有限公司 | Method for improving element determination accuracy in heteropoly acid catalyst |
| CN114324309A (en) * | 2022-01-04 | 2022-04-12 | 新余钢铁股份有限公司 | ICP (inductively coupled plasma) measuring method for synchronously testing total hardness, phosphate radical and iron in industrial water |
| CN116337805A (en) * | 2023-05-22 | 2023-06-27 | 成都博瑞科传科技有限公司 | Method and sensor for detecting total phosphorus in water based on array spectrum and ion selection method |
| CN116337805B (en) * | 2023-05-22 | 2023-07-21 | 成都博瑞科传科技有限公司 | Method and sensor for detecting total phosphorus in water based on array spectrum and ion selection method |
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Application publication date: 20150715 |