CN102393427A - Analyzing method of Ni content in melted steel ingot - Google Patents
Analyzing method of Ni content in melted steel ingot Download PDFInfo
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- CN102393427A CN102393427A CN201110341433XA CN201110341433A CN102393427A CN 102393427 A CN102393427 A CN 102393427A CN 201110341433X A CN201110341433X A CN 201110341433XA CN 201110341433 A CN201110341433 A CN 201110341433A CN 102393427 A CN102393427 A CN 102393427A
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Abstract
An analyzing method of Ni content in a melted steel ingot belongs to the test method of laboratories in metallurgy industries, and comprises the following operation links: weighing samples, dissolving samples, filtering, cleaning, ashing, melting and cooling filter matters, combining filtrate, adjusting the degree of acidity of the solution, settling, aging, filtering, drying and calculating. The analyzing method effectively overcomes the defects that undissolved substances often can not be resolved thoroughly in the analyzing process of melting the steel ingot by stainless steel slag or dust removing ash, so that the sample can be resolved thoroughly, and further the effects of accurate and reliable test result can be achieved.
Description
Technical field:
The invention belongs to smelter laboratory assay method, be specifically related to the chemico-analytic method of Ni content in a kind of fusing steel ingot.
Background technology
The fusing steel ingot that stainless steel slag or dedusting ash remelting form is a kind of slag regenerant between the pig iron and stainless steel, as steel scrap supply steel mill, needs to analyze C, S, P, Cr, Ni, TFe content.The processing factory laboratory is to use iron and steel methods analyst Ni content wherein at present, and there is following defective in this method: have the part insolubles in the sample dissolution process and occur, sample is difficult to dissolve fully, will have a strong impact on precision of analysis.
Summary of the invention:
The present invention proposes Ni analysis on Content method in a kind of fusing steel ingot, its objective is the defective in overcoming above-mentioned Ni ultimate analysis process, and a kind of thoroughly method of dissolved samples is provided, thereby makes analysis result accurately, reliably.
Technical scheme of the present invention comprises and takes by weighing sample---dissolved samples---filter, clean---filtrate ashing, fusion, cooling---filtrating merges---adjustment solution acidity---deposition, ageing---filter, the oven dry---operation link of calculating, concrete steps are:
(1), claims the beaker that kind 0.500g places 600ml with stainless steel;
(2), in beaker, add chloroazotic acid 20ml, beaker cap surface ware is placed on the electric hot plate, heats with the low temperature shelves of electric hot plate; Produce a large amount of minute bubbles, disappear, in beaker, drip hydrofluorite 3-4 again and drip until minute bubbles; Add perchloric acid 5ml then, make that solution is syrupy shape in the beaker;
(3), adding hydrochloric acid 10ml makes the solubility salt dissolving in the beaker in beaker, adds water then the total solution in the beaker is controlled in the 100ml, uses fast quantification filter paper that the solution in the beaker is filtered into former filtrating;
(4), filter paper and the particle that is adsorbed on the filter paper are placed platinum crucible; Particle charing on platinum crucible places and makes filter paper on the electric furnace and be adsorbed on filter paper becomes carbide; The platinum crucible that carbide will be housed is again put into calcination on the muffle furnace; Calcination temperature is 1000 ℃, and calcination 20 minutes becomes calcination with the carbide ashing;
(5), platinum crucible taken out naturally cool to room temperature, in platinum crucible, drip the wetting calcination of 2ml distilled water then successively and---drip two 1+1 sulfuric acid solutions---and add the hydrofluorite of 5ml; Platinum crucible is placed electric hot plate, and electric plate temperature is 70-100 ℃, evaporates the liquid in the platinum crucible, and the sulfuric acid cigarette to platinum crucible emits to the greatest extent; And then platinum crucible put into the muffle furnace calcination 10-15 minute, calcination temperature is 1000 ℃; Take out platinum crucible and make platinum crucible naturally cool to room temperature; In platinum crucible, add potassium pyrosulfate 4 grams, with platinum crucible
PutIn muffle furnace, muffle furnace is set at 700-800 ℃, and platinum crucible melts to aglow bright;
(6), take off and generate the potassium pyrosulfate frit behind the platinum crucible natural cooling; Place former filtrating to make the molten dissolving fully of potassium pyrosulfate the potassium pyrosulfate frit, clean platinum crucible with distilled water, total solution is controlled between 350-400ml in the former filtrating beaker;
(7), in former filtrating beaker, add hydrochloric acid 10ml successively---citric acid 10ml; Add ammoniacal liquor then while stirring and transfer the solution pH value, making the solution pH value is 8-9, checks with the PH test paper;
(8), in former filtrating beaker, add boiling water; Making the volume in the former filtrating beaker is 480ml, and solution temperature is controlled at more than 75 ℃ in the former filtrating beaker, in solution, slowly adds dimethylglyoxime solution 50ml; Stir while adding, generate red dimethylglyoxime nickel deposition;
(9), former filtrating beaker is placed ageing on the electric hot plate, be incubated 45 minutes, temperature is controlled at 70 ℃;
(10), use sintered filter funnel to filter dimethylglyoxime nickel deposition, the weak aqua ammonia washing dimethylglyoxime nickel deposition with 2% 5-8 time is washed 3-5 time with distilling again, gets rid of the water column of funnel bottom;
(11), dimethylglyoxime nickel deposition is put into baking oven together with funnel, oven temperature is set at 135 ℃, dry 2 hours, takes out the exsiccator of putting into of funnel and deposition after drying, naturally cools to room temperature, the weight of steelyard slepsydra bucket and deposition.
(12), calculate Ni content in the fusing steel ingot
In the formula: the sedimentary quality of G_____ is the Mass Calculation that is deducted the sky funnel by the quality that has sedimentary funnel, and unit is g;
0.2032_____ the conversion coefficient of dimethylglyoxime nickel and nickel;
0.5000_____ the sample weighting amount of analytical sample, unit are g.
Note:
(1) sintered filter funnel: should clean up before 1. using, put into baking oven, oven temperature is set at about 135 ℃, dries 1 hour, takes out and places exsiccator, is cooled to room temperature, and the back of weighing is subsequent use.Do water column when 2. using and be convenient to quick filtration.3. use back flushing in clear water to put into beaker, add 2% watery hydrochloric acid and place on the electric furnace bubble to wash, to be cleanedly clean subsequent use with distilled water again after clean.
(2) empty funnel is placed in the exsiccator with sedimentary funnel oven dry is arranged, and the type of cooling should be consistent with cool time.
(3) described solubility salt produces in step 2, is after " solution is syrupy shape in the beaker ", separates out because the minimizing of solution amount has some solubility salts.
The present invention has effectively overcome the defective that the frequent insolubles that occurs can not thoroughly decompose in stainless steel slag or the dedusting ash fusing steel ingot analytic process, and sample can thoroughly be dissolved, thereby reaches accurate, the reliable effect of result of laboratory test.
Embodiment:
Embodiment:Present embodiment is the chemical examination instance of in May, 2007 processing factory of Taiyuan Iron and Steel Co. stainless steel incorporated company in Shanxi.
Practice shows that result of use of the present invention is good, for operating personnel grasp, has realized that sample thoroughly decomposes, and has guaranteed precision of analysis easily.
Embodiment:
Dedusting ash fusing ingot pattern sample weighting amount is 0.500g, and sample places the beaker in 600ml.
In beaker, add chloroazotic acid 20ml, beaker cap surface ware is placed on the electric hot plate, and the low temperature shelves heating with electric hot plate produces a large amount of minute bubbles, disappears until minute bubbles, carries out sample dissolution; In beaker, drip hydrofluorite 3-4 and drip, continue the low temperature shelves with electric hot plate, stop until reaction, add perchloric acid 5ml, continuation is syrupy shape with the liquid that the low temperature shelves of electric hot plate are heated in the beaker.
In beaker, add hydrochloric acid 10ml, the solubility salt in the beaker is dissolved fully; Add water then, the solution in the beaker is controlled in the 100ml; Use fast quantification filter paper that the solution in the beaker is filtered; After 70-80 ℃ distilled water flushing beaker 7-8 time, the WS that cleaned and filtered fluid combine and are referred to as former filtrating, and the beaker that holds former filtrating is referred to as former filtrating beaker.
Filter paper and the particle that is adsorbed on the filter paper are placed platinum crucible, place charing on the electric furnace, put into muffle furnace again 1000 ℃ of temperature are set, calcination 20 minutes with filter paper be adsorbed on the particle ashing on the filter paper.
After the ashing platinum crucible taken out and naturally cools to room temperature, in platinum crucible, add successively two drip, drip two 1+1 sulfuric acid solutions, 5ml hydrofluorite; Platinum crucible is placed on the electric hot plate,, treat to emit in the platinum crucible sulfuric acid cigarette until the sulfuric acid cigarette being emitted to the greatest extent with the solution in the electric hot plate low temperature retaining evaporation platinum crucible; And then platinum crucible put into muffle furnace, muffle furnace is provided with 1000 ℃ of temperature, calcination 10-15 minute.
Take out platinum crucible and naturally cool to room temperature, in platinum crucible, add potassium pyrosulfate 4 grams, it is aglow bright to place muffle furnace to melt to platinum crucible again, and muffle furnace is set between 700-800 ℃.
After taking off the platinum crucible natural cooling, the potassium pyrosulfate frit is placed former filtrating beaker, potassium pyrosulfate is melted be dissolved in fully in the former filtrating; Use distilled water that platinum crucible is cleaned, the water of washing platinum crucible adds in the former filtrating beaker, and solution is controlled between 350-400ml in the former filtrating beaker.
In former filtrating beaker, add hydrochloric acid 10ml, again adding citric acid 10ml; Add ammoniacal liquor then while stirring and transfer the solution pH value, making the solution pH value is 8-9 (can not greater than 10), checks with the PH test paper;
In former filtrating beaker, add boiling water and make the volume of solution in the filtrating beaker reach 480ml, solution temperature is controlled at more than 75 ℃ in the former filtrating beaker;
In solution, slowly add dimethylglyoxime solution 50ml, stir while adding, generating red complex is dimethylglyoxime nickel deposition.
Former filtrating beaker is placed ageing on the electric hot plate, be incubated 45 minutes, temperature is controlled at 70 ℃.
Use sintered filter funnel to filter dimethylglyoxime nickel deposition, the weak aqua ammonia washing dimethylglyoxime nickel deposition with 2% 5-8 time with distillation washing 3-5 time, is got rid of the water column of funnel bottom again.
Dimethylglyoxime nickel deposition is put into baking oven together with funnel, and oven temperature is set at about 135 ℃, dry 2 hours, takes out the exsiccator of putting into of funnel and deposition after drying, naturally cools to room temperature, the weight of steelyard slepsydra bucket and deposition.
Calculate nickel content according to computing formula.
Computing formula:
In the formula: the sedimentary quality of G_____ is the Mass Calculation that is deducted the sky funnel by the quality that has sedimentary funnel, and unit is g.
0.2032_____ the conversion coefficient of dimethylglyoxime nickel and nickel.
0.5000_____ the sample weighting amount of analytical sample, unit are g.
G1=34.0351?g?-33.9234?g?=0.1117?g
G2=35.7775?g?-35.6646?g?=0.1129?g
Data are following:
Described ashing is about to the process that the charcoal in the filter paper burnouts.
Described ageing impels dimethylglyoxime and nickel element to form stable bulky grain deposition and the more pure process of deposition promptly through solution is incubated, leaves standstill.
Claims (1)
1. one kind melts Ni analysis on Content method in the steel ingot
,It is characterized in that comprising following step successively:
(1), claims the beaker that kind 0.500g places 600ml with stainless steel;
(2), in beaker, add chloroazotic acid 20ml, beaker cap surface ware is placed on the electric hot plate, heats with the low temperature shelves of electric hot plate; Produce a large amount of minute bubbles, disappear, in beaker, drip hydrofluorite 3-4 again and drip until minute bubbles; Add perchloric acid 5ml then, make that solution is syrupy shape in the beaker;
(3), adding hydrochloric acid 10ml makes the solubility salt dissolving in the beaker in beaker, adds water then the total solution in the beaker is controlled in the 100ml, uses fast quantification filter paper that the solution in the beaker is filtered into former filtrating;
(4), filter paper and the particle that is adsorbed on the filter paper are placed platinum crucible; Particle charing on platinum crucible places and makes filter paper on the electric furnace and be adsorbed on filter paper becomes carbide; The platinum crucible that carbide will be housed is again put into calcination on the muffle furnace; Calcination temperature is 1000 ℃, and calcination 20 minutes becomes calcination with the carbide ashing;
(5), platinum crucible taken out naturally cool to room temperature, in platinum crucible, drip the wetting calcination of 2ml distilled water then successively and---drip two 1+1 sulfuric acid solutions---and add the hydrofluorite of 5ml; Platinum crucible is placed electric hot plate, and electric plate temperature is 70-100 ℃, evaporates the liquid in the platinum crucible, and the sulfuric acid cigarette to platinum crucible emits to the greatest extent; And then platinum crucible put into the muffle furnace calcination 10-15 minute, calcination temperature is 1000 ℃; Take out platinum crucible and make platinum crucible naturally cool to room temperature; In platinum crucible, add potassium pyrosulfate 4 grams, with platinum crucible
PutIn muffle furnace, muffle furnace is set at 700-800 ℃, and platinum crucible melts to aglow bright;
(6), take off and generate the potassium pyrosulfate frit behind the platinum crucible natural cooling; Place former filtrating to make the molten dissolving fully of potassium pyrosulfate the potassium pyrosulfate frit, clean platinum crucible with distilled water, total solution is controlled between 350-400ml in the former filtrating beaker;
(7), in former filtrating beaker, add hydrochloric acid 10ml successively---citric acid 10ml; Add ammoniacal liquor then while stirring and transfer the solution pH value, making the solution pH value is 8-9, checks with the PH test paper;
(8), in former filtrating beaker, add boiling water; Making the volume in the former filtrating beaker is 480ml, and solution temperature is controlled at more than 75 ℃ in the former filtrating beaker, in solution, slowly adds dimethylglyoxime solution 50ml; Stir while adding, generate red dimethylglyoxime nickel deposition;
(9), former filtrating beaker is placed ageing on the electric hot plate, be incubated 45 minutes, temperature is controlled at 70 ℃;
(10), use sintered filter funnel to filter dimethylglyoxime nickel deposition, the weak aqua ammonia washing dimethylglyoxime nickel deposition with 2% 5-8 time is washed 3-5 time with distilling again, gets rid of the water column of funnel bottom;
(11), dimethylglyoxime nickel deposition is put into baking oven together with funnel, oven temperature is set at 135 ℃, dry 2 hours, takes out the exsiccator of putting into of funnel and deposition after drying, naturally cools to room temperature, the weight of steelyard slepsydra bucket and deposition;
(12), calculate Ni content in the fusing steel ingot
In the formula: the sedimentary quality of G_____ is the Mass Calculation that is deducted the sky funnel by the quality that has sedimentary funnel, and unit is g;
0.2032_____ the conversion coefficient of dimethylglyoxime nickel and nickel;
0.5000_____ the sample weighting amount of analytical sample, unit are g.
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Cited By (4)
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| CN106840956A (en) * | 2017-03-31 | 2017-06-13 | 周学成 | Cold and hot two-chamber evaporation residue analyzer |
| CN109211812A (en) * | 2018-10-21 | 2019-01-15 | 福建通海镍业科技有限公司 | The analysis method of nickel, phosphorus content in a kind of simultaneous determination nickel-base alloy |
| CN109283023A (en) * | 2018-11-06 | 2019-01-29 | 华北电力大学（保定） | The experimental provision and application method that simulated flue gas content influences sulfur trioxide concentration |
| CN114112837A (en) * | 2021-11-12 | 2022-03-01 | 中航光电科技股份有限公司 | Method for detecting porosity of plating layer |
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| CN1945283A (en) * | 2006-10-19 | 2007-04-11 | 大连华锐股份有限公司 | Method for detecting nickel, molybdemum and chromium content range in stainless steel |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106840956A (en) * | 2017-03-31 | 2017-06-13 | 周学成 | Cold and hot two-chamber evaporation residue analyzer |
| CN109211812A (en) * | 2018-10-21 | 2019-01-15 | 福建通海镍业科技有限公司 | The analysis method of nickel, phosphorus content in a kind of simultaneous determination nickel-base alloy |
| CN109283023A (en) * | 2018-11-06 | 2019-01-29 | 华北电力大学（保定） | The experimental provision and application method that simulated flue gas content influences sulfur trioxide concentration |
| CN109283023B (en) * | 2018-11-06 | 2024-04-16 | 华北电力大学（保定） | Experimental device for simulating influence of smoke content on sulfur trioxide concentration and application method |
| CN114112837A (en) * | 2021-11-12 | 2022-03-01 | 中航光电科技股份有限公司 | Method for detecting porosity of plating layer |
| CN114112837B (en) * | 2021-11-12 | 2023-12-19 | 中航光电科技股份有限公司 | Method for detecting porosity of coating |
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