CN102735584A - Liquid buoyancy weighing method for determination of aluminum and iron content in steel grit aluminum - Google Patents
Liquid buoyancy weighing method for determination of aluminum and iron content in steel grit aluminum Download PDFInfo
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- CN102735584A CN102735584A CN2012101861738A CN201210186173A CN102735584A CN 102735584 A CN102735584 A CN 102735584A CN 2012101861738 A CN2012101861738 A CN 2012101861738A CN 201210186173 A CN201210186173 A CN 201210186173A CN 102735584 A CN102735584 A CN 102735584A
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Abstract
The invention discloses a liquid buoyancy weighing method for determination of aluminum and iron content in steel grit aluminum. The method comprises the following steps: (1) preparing a steel grit aluminum sample, then fully drying and accurately weighing a weight m1 of the sample; (2) placing the weighed sample in an immersion liquid groove, then placing the immersion liquid groove in a vacuumizing device; vacuumizing till an internal pressure in the vacuumizing device no more than 2500Pa and maintaining for 5-10min; (3) slowly injecting water into the immersion liquid groove until the immersion liquid covering the sample, and maintaining pressure in the vacuumizing no more than 2500Pa for 5-10min; (4) removing the immersion liquid groove from the vacuumizing device, standing the immersion liquid groove in the air to completely infiltrate and saturate the sample; and then weighing a suspended weight of the sample; (5) calculating density of the sample; and (6) calculating aluminum content and iron content in the sample. The method for the determination of aluminum and iron content in the steel grit aluminum can effectively avoid influences from the structure and shape of the steel grit aluminum, so as to significantly improve accuracy and reliability of analysis data, and realize good reproducibility.
Description
Technical field
The present invention relates to a kind of assay method of alloy content, especially a kind of liquid buoyancy weighing method is measured the method for ferro-aluminum content in the steel sand aluminium.
Background technology
For satisfying steel and iron industry and auto manufacturing, need in steelmaking process, add steel sand aluminum element and carry out the microalloying processing, to improve the mechanics and the physical property of steel crystal structure, raising material to the steel performance requirement.Thereby steel production enterprise still instructs the process for making operating aspect no matter aspect aluminium alloy buying quality control, all need carry out assay to steel sand aluminum alloy chemically composition.Aluminum in Alloy, iron contain constituent content in the employing conventional wet chemical analysis mensuration steel sand aluminium alloy; Complicated operation is loaded down with trivial details, step is tediously long, take time and effort, efficient is low; And analysis result accuracy and stability often are affected because of operating personnel's experience and level; Need unite strong acid such as using nitric acid, hydrochloric acid, NaOH in addition in the analytic process, alkali and other chemical reagent cause personal injury or environmental pollution easily.
Many apertures and slit are arranged in the middle of the steel sand aluminum alloy organization complex structure, sample.It is representative to materials in order to satisfy, and can fully represent the component characteristic of this kind alloy.The preparation of sample requires sample size much bigger than traditional chemical test method and instrument analytical method.Cause huge difficulty therefore just for traditional chemical experiment method.Simultaneously for this kind sample; If adopt traditional chemical analysis method, representative for experimental data, must adopt complete bulk sample directly to dissolve appearance; Because being mingled with steel sand by the aluminum matrix, sample forms; The hardness of iron makes the steel sand composition slide to the edge that drill bit drills through the zone when bit drills is materialsed far above aluminium base, makes sample not drill through with drill bit; While is owing to identical reason and the sample stem tuber is bigger and irregular this alloy kind that makes also is not suitable for getting with the lathe car, more can not the crushing grinding sample preparation.The structure of sample is formed inhomogeneous, and many pores are arranged in the institutional framework in addition, and this has just determined sample can not adopt light source activation kind equipment such as spark direct-reading spectrometer to excite analysis.Simultaneously because the complicacy of structure and the analysis that unevenness also is not suitable for the X XRF.If adopt the wet chemical analysis sample, in order to satisfy the representativeness of sample, sample size is very big so, needs a few hectogram samples, such concentrated acid dissolved samples that just needs several liters.Not only wasted a large amount of material resources, manpower, dissolving the appearance time simultaneously also can be very very long.Cause huge pollution to environment simultaneously, the sample of saying nothing of after the test is applied to produce again.
Though the domestic related substance Determination of true density method that also occurred; But do not see the report that is applied to analyze the ferroalloy chemical constitution with the hydrostatic weighing method at present; For the mensuration of steel sand aluminum chemistry composition because ferroalloy smelting technology and use the difference of raw material; Make the alloy substrate of same kind and form structure to exist, and receive that the influence of tight ness rating causes and can't sample between steel sand granularity and steel sand and the aluminum substrate, produce suitable traditional chemical analytic sample than big-difference.Its result makes traditional chemical analysis data stability and poor accuracy, can not reflect the quality situation of sample fully really.And then cause adopting the application of conventional wet chemistry and spectroscopic methodology to be restricted.The hydrostatic weighing method is measured the method for alloy compositions, and analysis result is stable, and accuracy reliably satisfies the production needs fully.But like the real density of the condition determination of the weight of sample own, weight suspension and volume of sample and the sample that calculates thus, and the computing method of sample fraction content become and implement the hydrostatic weighing method and measure the bottleneck that aluminium in the steel sand aluminium, iron content method are used in the alloy measuring process.
Summary of the invention
The technical matters that the present invention will solve provides the method that a kind of simple to operate, precision, accuracy better fluid buoyancy weighing method are measured ferro-aluminum content in the steel sand aluminium.
For solving the problems of the technologies described above, step of the present invention is: the sample of steel sand aluminium is produced in (1), and is fully dry then, accurately weighing sample mass m
1
(2) sample after the weighing places in the immersion liquid groove, then the immersion liquid groove is placed vacuum extractor; Be evacuated to vacuum plant internal pressure≤2500Pa, keep 5～10min;
(3) in the immersion liquid groove, slowly inject water, cover sample until immersion liquid; Vacuum plant internal pressure≤2500Pa keeps 5～10min;
(4) from vacuum plant, take out the immersion liquid groove, leave standstill in air that sample is fully soaked into is saturated; Take by weighing the weight suspension m of sample then
2
The density p of sample is calculated in
(5) according to formula ()
(1)
In the formula (): ρ
WaterFor measuring the density of water under the temperature;
(6) calculate the quality percentage composition Al% of aluminium in the sample and the quality percentage composition Fe% of iron according to formula (two) and (three),
(two)
(3)
Among formula (two) and (three):
ρ
IronBe the density of iron,
ρ
AluminiumDensity for aluminium.
The specification of sample is the mm of Φ (25-45) mm * (25-70) in the step according to the invention (1).
The present invention adopts following step to samples dried, weighing: the outer list processing (LISP) of sample is weighed after clean, place oven dry in the drying box then; Sample takes out the back and in exsiccator, naturally cools to room temperature in drying box, weigh once more; Repeat dry, weighing process, of poor qualityly be no more than 0.1% until weighing for last twice, the weight of then weighing for the last time is the quality m of sample
1Said bake out temperature is 100～115 ℃ of oven dry, drying time>=15min.
In the step according to the invention (3), in 3min, in the immersion liquid groove, slowly inject water, cover sample 20mm until immersion liquid.
In the step according to the invention (4), the immersion liquid groove leaves standstill 30min in air.
Take following method to take by weighing the weight suspension of sample in the step according to the invention (4): will fully soak in the immersion liquid groove that saturated sample moves to the carry potential overflow pipe rapidly, and after sample floods fully, sample is hung on the hook that hangs formula weighing balance from above take by weighing.
Adopt the beneficial effect that technique scheme produced to be: to the present invention is directed to the difficult problem that the liquid buoyancy weighing method is measured aluminium, iron in the steel sand aluminium; Through repetition test research; Look for another way, dry in strict accordance with operation steps and assurance, vacuumize; The control of infiltrating time and the control of vacuum tightness accurately weigh the test physical quantity of asking.Ask the real density of calculating sample further to calculate the aluminium in the steel sand aluminium, iron content through mathematical computations.Show that through repetition test and mass data the inventive method is measured aluminium in the steel sand aluminium, iron content can be avoided the influence of aspects such as institutional framework and the specimen shape of steel sand aluminium effectively, and accuracy, the reliability of analyzing data are significantly improved, and repeatability is good.
The inventive method is with the direct weighing of steel sand aluminium sample; Vacuumize; Soak into then to measure and soak into the suffered buoyancy of saturated sample, go up physical quantity according to this aluminium, the iron content of sample are asked calculation, can effectively avoid to satisfy in the sample sampling process problem of typical sample; Simultaneously be able to thorough solution for carrying out consuming in the chemical dissolution process super amount solubilising reagent and these reagent severe contamination problem to environment; Sample after the test does not influence the use of steelmaking process at all; Make the liquid buoyancy weighing method measure aluminium in the steel sand aluminium, the method for iron content is achieved.
Embodiment
Below in conjunction with specific embodiment the present invention is done further detailed explanation.
The method that this liquid buoyancy weighing method is measured ferro-aluminum content in the steel sand aluminium adopts following processing step:
(1) it is suitable to prepare test specimen by the mm of Φ (25-45) mm * (25-70), and this method is applicable to abrasive grit purity >=99.00%; Steel sand granularity Φ (1-3mm); Aluminium base purity >=99.5%.
(2) be weighing method owing to what adopt; So at first will accurately measure the quality of dried and clean sample; Because sample might be contaminated in transportation and transporting procedures or be made moist; Therefore select 3～6 parts on representational sample the outer list processing (LISP) of sample is weighed respectively after clean and place can the drying box of accurate temperature controlling in, sample is put into drying box, dry to constant weight at 105～110 ℃; Be dried to promptly that last twice weighing is of poor quality to be no more than till 0.1%, could guarantee the accuracy of samples dried quality like this.Through experiment, confirm that drying time is can reach the constant weight requirement behind the 15min, therefore confirm dry sample drying time >=15min.105 ℃～110 ℃ of drying box design temperatures, accuracy of temperature control ± 5 ℃; Weighing requires sensibility reciprocal d≤0.01g and range>=200g with balance.In exsiccator, naturally cool to room temperature after sample takes out and weigh in drying box, finally recording sample mass is m
1
(3) owing to steel sand aluminium is that abrasive grit even distribution in high temperature aluminum liquid forms, so there is certain pore to exist in the sample; In order accurately to record the true volume of steel sand aluminium; Need in vacuum plant, sample be extracted to vacuum state; The sample internal voids is filled by water; Measure its volume with the hydrostatic weighing method again, the situation and the retention time that therefore vacuumize back pressure guarantee that the vacuum state time is important step and the prerequisite that guarantees precision of analysis.The back sample of weighing places in the immersion liquid groove, places vacuum extractor to the immersion liquid groove that fills sample, and vacuum plant requires with the water injection valve and the air release that connect water injection pipe.The open vacuum pump is evacuated to surplus pressure≤2500Pa and keeps 5～10min.
(4) open the water injection valve of vacuum plant; In 3min, slowly inject pure water then; The pressure in the water filling final vacuum device covers the about 20mm of sample until immersion liquid, keeps the about 5min of this surplus pressure≤2500pa, if then need be evacuated to pressure less than 2500Pa once more greater than 2500Pa.Open the air release of vacuum plant, take out the immersion liquid groove, in air, leave standstill 30min, it is saturated that sample is fully soaked into.
(5) will fully soak in the immersion liquid groove that saturated sample moves to the carry potential overflow pipe rapidly, after sample floods fully, sample will be hung on the hook that hangs formula weighing balance from above, take by weighing saturated sample weight suspension m
2
(6) for calculating required mathematics value because the restriction of specimen shape makes the commonsense method of calculating through geometric formula not solve in the mensuration process of the steel sand aluminium of iron aluminium mixed attitude.Therefore only look for another way and adopt the method for measuring sample suffered buoyancy in water.Known f
Floating=(m
1-m
2)G=ρ
WaterVg; Can derive V=(m
1-m
2)/ρ
Waterm
1, m
2Be measured value, simultaneously known under experimental temperature the proportion of water.Thus can be through calculating the volume of sample.Real density for sample can pass through formula ρ=m
1/ V draws.Comprehensive following formula can get
.
(7) sample is made up of iron, two kinds of materials of aluminium.Be sample mass m
1=m
Iron+ m
Aluminium=ρ
IronV
Iron+ ρ
AluminiumV
AluminiumKnow volume of sample V=V again
Iron+ V
Aluminium
ρ in the formula
Iron, ρ
AluminiumBe known quantity, ρ is for measuring calculated value.
Embodiment: the technology that this liquid buoyancy weighing method is measured the method for ferro-aluminum content in the steel sand aluminium is described below.
(1) by Φ (25-45) mm * (25-70) mm prepares the sample of steel sand aluminium.
(2) select 4 parts on representational sample with the outer list processing (LISP) of sample clean after, carry out label (1# with marking pen; 2#; 3#; 4#).Weigh respectively and place can accurate temperature controlling air dry oven in; Sample is put into drying box; Dry to constant weight at 105～110 ℃, take out to be placed in the drying box behind the oven dry 15min and naturally cool to room temperature in the exsiccator, weigh with sensibility reciprocal d≤0.01g and range>=200g balance; Repeat the oven dry step of weighing, be no more than 0.1% until last twice weighing is of poor quality.The sample measured value is m
1(1#:135.204g; 2#:134.205g; 3#:137.229g; 4#:129.172g).
(3) place sample in the immersion liquid groove of vacuum plant, place vacuum plant.The open vacuum pump is evacuated to surplus pressure≤2500Pa and keeps 5min.
(4) open water injection valve, inject distilled water to liquid level submergence sample and exceed sample 2cm; Guarantee pressure≤2500Pa,, need vacuumize again until meeting above-mentioned condition, and keep five minutes if pressure can not guarantee above-mentioned condition.Open air release, treat that tensimeter pressure reaches to take out the immersion liquid groove behind the atmospheric pressure and place atmosphere, leave standstill 30min.
(5) will fully soak in the immersion liquid groove that saturated sample moves to the carry potential overflow pipe rapidly, after sample floods fully, sample taken by weighing saturated sample weight suspension m with hanging formula weighing balance from above
2(1#:92.574g; 2#:93.765g; 3#:96.128g; 4#:90.196g).
(6) must bring above measured value into formula
Obtain ρ value (1#:3.172g/cm
32#:4.080g/cm
33#:3.339g/cm
34#:3.314g/cm
3).
(7) calculate aluminium, iron content according to following formula:
The weight content of aluminium is in the sample of steel sand aluminium: 1#:77.23%; 2#:71.45%; 3#:70.70%; 4#:71.62%, the weight content of iron is: 1#:22.77%; 2#:28.55%; 3#:29.30%; 4#:28.38%.
Test Example: adopt following this liquid buoyancy of method validation weighing method to measure precision, repeatability and the accuracy of the method for ferro-aluminum content in the steel sand aluminium.
1, precision test: same sample is done the precision test as stated above, is example with the content of aluminium, and it is as shown in table 1 to measure the result.
Table 1: Precision test result (8# sample)
Can be found out by table 1: the real density error meets the precision requirement of GB, is no more than 0.02 g/cm
3, show that this method precision is good, can satisfy the mensuration demand of process for making to aluminium in the steel sand aluminium.
2, repeatability test: because steel sand aluminium is a kind of new sections aluminium potpourri; Do not have standard model at present, its sample is the solid column structure, can not measure its recovery with standard addition method; Therefore; Selecting different personnel that same sample measured by above-mentioned experimental technique, is example with the mensuration result of aluminium, and it is as shown in table 2 to measure the result.
Table 2: repeatability test findings (3# sample)
Can be found out by table 2: the real density error meets the accuracy requirement of GB, is no more than 0.04g/cm
3, showing that the analysis repeatability is good, accuracy is high, can satisfy the analysis requirement.
3, accuracy test: select four parts of samples to measure the steel with manufacturer utilization, mensuration result's (recommendation) that aluminium separates test of comparing, the result is as shown in table 3 for mensuration.
This method is carried out accuracy validation with sample (1#, 2#, 3#, 4#), and data result shows in the table 3, and measured value and recommendation meet better.
Claims (7)
1. a liquid buoyancy weighing method is measured the method for ferro-aluminum content in the steel sand aluminium, and it is characterized in that this method step is: the sample of steel sand aluminium is produced in (1), and is fully dry then, accurately weighing sample mass m
1
(2) sample after the weighing places in the immersion liquid groove, then the immersion liquid groove is placed vacuum extractor; Be evacuated to vacuum plant internal pressure≤2500Pa, keep 5～10min;
(3) in the immersion liquid groove, slowly inject water, cover sample until immersion liquid; Vacuum plant internal pressure≤2500Pa keeps 5～10min;
(4) from vacuum plant, take out the immersion liquid groove, leave standstill in air that sample is fully soaked into is saturated; Take by weighing the weight suspension m of sample then
2
The density p of sample is calculated in
(5) according to formula ()
(1)
In the formula (): ρ
WaterFor measuring the density of water under the temperature;
(6) calculate the quality percentage composition Al% of aluminium in the sample and the quality percentage composition Fe% of iron according to formula (two) and (three),
(3)
Among formula (two) and (three):
ρ
IronBe the density of iron,
ρ
AluminiumDensity for aluminium.
2. liquid buoyancy weighing method according to claim 1 is measured the method for ferro-aluminum content in the steel sand aluminium, it is characterized in that: the specification of sample is the mm of Φ (25-45) mm * (25-70) in the said step (1).
3. liquid buoyancy weighing method according to claim 1 is measured the method for ferro-aluminum content in the steel sand aluminium; It is characterized in that; Adopt in the said step (1) following step to samples dried, weighing: the outer list processing (LISP) of sample to be weighed after clean, place oven dry in the drying box then; Sample takes out the back and in exsiccator, naturally cools to room temperature in drying box, weigh once more; Repeat dry, weighing process, of poor qualityly be no more than 0.1% until weighing for last twice, the weight of then weighing for the last time is the quality m of sample
1
4. liquid buoyancy weighing method according to claim 3 is measured the method for ferro-aluminum content in the steel sand aluminium, and it is characterized in that: said bake out temperature is 100～115 ℃ of oven dry, drying time >=15min.
5. liquid buoyancy weighing method according to claim 1 is measured the method for ferro-aluminum content in the steel sand aluminium, it is characterized in that: in the said step (3), in 3min, in the immersion liquid groove, slowly inject water, cover sample 20mm until immersion liquid.
6. liquid buoyancy weighing method according to claim 1 is measured the method for ferro-aluminum content in the steel sand aluminium, and it is characterized in that: in the said step (4), the immersion liquid groove leaves standstill 30min in air.
7. measure the method for ferro-aluminum content in the steel sand aluminium according to described any one liquid buoyancy weighing method of claim 1-6; It is characterized in that; Take following method to take by weighing the weight suspension of sample in the said step (4): will fully soak in the immersion liquid groove that saturated sample moves to the carry potential overflow pipe rapidly; After sample floods fully, sample is hung on the hook that hangs formula weighing balance from above takes by weighing.
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| CN103293077A (en) * | 2013-05-29 | 2013-09-11 | 广西壮族自治区农业科学院经济作物研究所 | Simple detection method for contents of starch and dry matters in cassava |
| CN105372154A (en) * | 2015-11-24 | 2016-03-02 | 中冶节能环保有限责任公司 | Method for measuring metallic iron content in steel slag |
| CN105445136A (en) * | 2015-11-20 | 2016-03-30 | 成都发动机（集团）有限公司 | Film weight measurement method for manganese phosphate film on stainless steel material surface |
| CN107525737A (en) * | 2017-08-29 | 2017-12-29 | 中核四0四有限公司 | MOX pellet density measuring methods |
| CN108956374A (en) * | 2018-04-25 | 2018-12-07 | 山西建龙实业有限公司 | The measuring method of aluminium and iron content in a kind of steel shot aluminum |
| CN111044409A (en) * | 2019-12-02 | 2020-04-21 | 无锡英特派金属制品有限公司 | Method for testing mass fraction of rhodium in platinum-rhodium alloy |
| CN112924258A (en) * | 2021-03-24 | 2021-06-08 | 中铁八局集团第七工程有限公司 | Method for indirectly reflecting pore structure of mortar |
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| CN103293077A (en) * | 2013-05-29 | 2013-09-11 | 广西壮族自治区农业科学院经济作物研究所 | Simple detection method for contents of starch and dry matters in cassava |
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| CN105445136A (en) * | 2015-11-20 | 2016-03-30 | 成都发动机（集团）有限公司 | Film weight measurement method for manganese phosphate film on stainless steel material surface |
| CN105372154A (en) * | 2015-11-24 | 2016-03-02 | 中冶节能环保有限责任公司 | Method for measuring metallic iron content in steel slag |
| CN107525737A (en) * | 2017-08-29 | 2017-12-29 | 中核四0四有限公司 | MOX pellet density measuring methods |
| CN108956374A (en) * | 2018-04-25 | 2018-12-07 | 山西建龙实业有限公司 | The measuring method of aluminium and iron content in a kind of steel shot aluminum |
| CN111044409A (en) * | 2019-12-02 | 2020-04-21 | 无锡英特派金属制品有限公司 | Method for testing mass fraction of rhodium in platinum-rhodium alloy |
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Application publication date: 20121017 |