CN108318476A - The ICP-AES measurement methods of micro- antimony content in a kind of ferro-molybdenum - Google Patents
The ICP-AES measurement methods of micro- antimony content in a kind of ferro-molybdenum Download PDFInfo
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- CN108318476A CN108318476A CN201810439680.5A CN201810439680A CN108318476A CN 108318476 A CN108318476 A CN 108318476A CN 201810439680 A CN201810439680 A CN 201810439680A CN 108318476 A CN108318476 A CN 108318476A
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
The measurement method of micro- antimony content in a kind of ferro-molybdenum, this method measures the content of antimony in ferro-molybdenum sample using ICP AES methods, this method is first dissolved to containing antimony sample, it is added after a certain amount of potassium permanganate, salpeter solution and the heating of the solution such as n-butanol chloroform is added is cleared up, effectively antimony can be dissolved.Then the content of antimony is measured using ICP AES spectroscopic methodologies, it is small using this method detection Matrix effects, it disclosure satisfy that the needs of production.
Description
Technical field
The present invention relates to the measurements of element, in particular to using ICP-AES coupled plasma atomic emission spectrums
Method measures the micro- antimony in ferro-molybdenum.
Background technology
Ferro-molybdenum 55%-75% containing molybdenum, iron 25%-45%, remaining is low content impurity.Molybdenum-iron is widely used in metallurgy
Structural steel, heat resisting steel, acidproof rigid and tool steel smelting.In tool steel and military project steel smelting, these low content impurities are easily right
The metallurgical performance of finished steel affects, and especially antimony must be strictly controlled within 2ppm, therefore how to find one
The method that kind quickly and effectively measures antimony content in ferro-molybdenum is particularly important.However, the measurement side used at present
Method such as spectrophotometry measures complexity, and it is inconvenient that solution is prepared, and measurement result is inaccurate, and repeatability is low, has limited life
The needs of production.Inductively coupled plasma atomic emission spectrometry (ICP-AES) is using inductively coupled plasma square as exciting light
The spectroscopic analysis methods in source, with accuracy height and precision are high, detection limit is low, measurement is quick, the range of linearity is wide, can survey simultaneously
The advantages that determining multiple element, foreign countries are widely used in the survey of tens of kinds of elements in the samples such as environmental sample and rock, mineral, metal
It is fixed.This method is applied to the detection of trace impurity in ferro-molybdenum, accuracy is high, can meet the needs of production.
Invention content
The measurement method of micro- antimony, this method include in a kind of ferro-molybdenum：
(1) it weighs sample 50mg to be placed in the conical flask of 100mL, 60% potassium permanganate 5mL, nitric acid (1 is added:1) 5mL,
Heating continues to be evaporated to and closely do, be subsequently cooled to outdoor after sample all dissolving；(1 is added again:1) 10mL, then by this
Solution is poured into 60mL separatory funnels, and n-butanol-chloroform 20mL, ammonium molybdate solution 10mL are then added in funnel, and capping is shaken
It swings 60 seconds, after stratification, is heated to 100-125 degrees Celsius, then cools to room temperature, stand and wait for that layering discards organic phase；
Again plus ethyl acetate 15mL, oscillation 90 seconds, then chlorination imitate 15mL, vibrate 30 seconds, ultra-pure water is used after organic phase is discarded after being layered
It is for use to be settled to 100mL；Or continue to stand and organic phase is placed in another 60mL separatory funnels after being layered, stannous chloride is added
20mL vibrates 30 seconds, discards after organic phase that be settled to 100mL with ultra-pure water for use after being layered；
(2) inductively coupled plasma atomic emission spectrometer is used according to the Specimen eliminating solution that step (1) obtains, i.e.,
Contained Sb elements spectral intensity at 193.696nm, measures Sb intensity values in ICP-AES Instrument measuring Specimen eliminating solution；
(3) configuration standard working solution：Weigh Sb Standard Stock solutions 0mL, 10mL of a concentration of 1.0 μ g/mL, 20mL,
40mL, 60mL, 80mL, 100mL are respectively placed in 100mL volumetric flasks, and constant volume is carried out with ultra-pure water；The standard working solution of acquisition
The content of middle Sb elements correspond to respectively 0 μ g/mL, 100 μ g/mL, 200 μ g/mL, 400 μ g/mL, 600 μ g/mL, 800 μ g/mL,
1000μg/mL；
(4) inductively coupled plasma atomic emission spectrometer will be imported according to the standard working solution that step (3) obtain,
That is ICP-AES instruments mix before entering atomizer, and the best isotope of Sb elements is selected to be measured；First metric works
Solution, further according to the known content of Sb elements in standard working solution and ICP-AES Instrument measurings to Sb element-intensities values paint
The standard working curve of Sb elements processed；Then the response of determination sample solution is obtained in conjunction with step (2) Specimen eliminating solution
The concentration value of Specimen eliminating solution S b elements is calculated according to standard working curve for the intensity value of Sb elements, to according to this
The existing formula method in field calculates the concentration value of trace element Sb in ferro-molybdenum；
Inductively coupled plasma atomic emission spectrometer in the step, running parameter are：
Radio-frequency power 1000W；
Plasma gas flow rate 20.0L/min；
Time of integration 20s；
Nebulizer flow 0.3L/min；
Secondary air amount 1.80L/min.
Heating stepses are introduced by the solution processes of the method especially antimony of above-mentioned record, can be very good to prepare abundant
The antimony solution of dissolving is to facilitate test.It can be very good to solve Matrix effects using ICP-AES methods, accuracy is high.
Specific implementation mode
Technical scheme of the present invention is described in further detail with reference to embodiment, but the present invention is not limited to following implementations
Example.Experimental method in following embodiments is unless otherwise specified conventional method.
Embodiment 1：
The measurement method of micro- antimony, this method include in a kind of ferro-molybdenum：
(1) it weighs sample 50mg to be placed in the conical flask of 100mL, 60% potassium permanganate 5mL, nitric acid (1 is added:1) 5mL,
Heating continues to be evaporated to and closely do, be subsequently cooled to outdoor after sample all dissolving；(1 is added again:1) 10mL, then by this
Solution is poured into 60mL separatory funnels, and n-butanol-chloroform 20mL, ammonium molybdate solution 10mL are then added in funnel, and capping is shaken
It swings 60 seconds, after stratification, is heated to 100 degrees Celsius, then cools to room temperature, stand and wait for that layering discards organic phase；Again plus
Ethyl acetate 15mL vibrates 90 seconds, then chlorination imitates 15mL, vibrates 30 seconds, and ultra-pure water constant volume is used after organic phase is discarded after being layered
It is for use to 100mL；Or continue to stand and organic phase is placed in another 60mL separatory funnels after being layered, stannous chloride is added
20mL vibrates 30 seconds, discards after organic phase that be settled to 100mL with ultra-pure water for use after being layered；
(2) inductively coupled plasma atomic emission spectrometer is used according to the Specimen eliminating solution that step (1) obtains, i.e.,
Contained Sb elements spectral intensity at 193.696nm, measures Sb intensity values in ICP-AES Instrument measuring Specimen eliminating solution；
(3) configuration standard working solution：Weigh Sb Standard Stock solutions 0mL, 10mL of a concentration of 1.0 μ g/mL, 20mL,
40mL, 60mL, 80mL, 100mL are respectively placed in 100mL volumetric flasks, and constant volume is carried out with ultra-pure water；The standard working solution of acquisition
The content of middle Sb elements correspond to respectively 0 μ g/mL, 100 μ g/mL, 200 μ g/mL, 400 μ g/mL, 600 μ g/mL, 800 μ g/mL,
1000μg/mL；
(4) inductively coupled plasma atomic emission spectrometer will be imported according to the standard working solution that step (3) obtain,
That is ICP-AES instruments mix before entering atomizer, and the best isotope of Sb elements is selected to be measured；First metric works
Solution, further according to the known content of Sb elements in standard working solution and ICP-AES Instrument measurings to Sb element-intensities values paint
The standard working curve of Sb elements processed；Then the response of determination sample solution is obtained in conjunction with step (2) Specimen eliminating solution
The concentration value of Specimen eliminating solution S b elements is calculated according to standard working curve for the intensity value of Sb elements, to according to this
The existing formula method in field calculates the concentration value of trace element Sb in ferro-molybdenum；
Inductively coupled plasma atomic emission spectrometer in the step, running parameter are：
Radio-frequency power 1000W；
Plasma gas flow rate 20.0L/min；
Time of integration 20s；
Nebulizer flow 0.3L/min；
Secondary air amount 1.80L/min.
Embodiment 2：
The measurement method of micro- antimony, this method include in a kind of ferro-molybdenum：
(1) it weighs sample 50mg to be placed in the conical flask of 100mL, 60% potassium permanganate 5mL, nitric acid (1 is added:1) 5mL,
Heating continues to be evaporated to and closely do, be subsequently cooled to outdoor after sample all dissolving；(1 is added again:1) 10mL, then by this
Solution is poured into 60mL separatory funnels, and n-butanol-chloroform 20mL, ammonium molybdate solution 10mL are then added in funnel, and capping is shaken
It swings 60 seconds, after stratification, is heated to 125 degrees Celsius, then cools to room temperature, stand and wait for that layering discards organic phase；Again plus
Ethyl acetate 15mL vibrates 90 seconds, then chlorination imitates 15mL, vibrates 30 seconds, and ultra-pure water constant volume is used after organic phase is discarded after being layered
It is for use to 100mL；Or continue to stand and organic phase is placed in another 60mL separatory funnels after being layered, stannous chloride is added
20mL vibrates 30 seconds, discards after organic phase that be settled to 100mL with ultra-pure water for use after being layered；
(2) inductively coupled plasma atomic emission spectrometer is used according to the Specimen eliminating solution that step (1) obtains, i.e.,
Contained Sb elements spectral intensity at 193.696nm, measures Sb intensity values in ICP-AES Instrument measuring Specimen eliminating solution；
(3) configuration standard working solution：Weigh Sb Standard Stock solutions 0mL, 10mL of a concentration of 1.0 μ g/mL, 20mL,
40mL, 60mL, 80mL, 100mL are respectively placed in 100mL volumetric flasks, and constant volume is carried out with ultra-pure water；The standard working solution of acquisition
The content of middle Sb elements correspond to respectively 0 μ g/mL, 100 μ g/mL, 200 μ g/mL, 400 μ g/mL, 600 μ g/mL, 800 μ g/mL,
1000μg/mL；
(4) inductively coupled plasma atomic emission spectrometer will be imported according to the standard working solution that step (3) obtain,
That is ICP-AES instruments mix before entering atomizer, and the best isotope of Sb elements is selected to be measured；First metric works
Solution, further according to the known content of Sb elements in standard working solution and ICP-AES Instrument measurings to Sb element-intensities values paint
The standard working curve of Sb elements processed；Then the response of determination sample solution is obtained in conjunction with step (2) Specimen eliminating solution
The concentration value of Specimen eliminating solution S b elements is calculated according to standard working curve for the intensity value of Sb elements, to according to this
The existing formula method in field calculates the concentration value of trace element Sb in ferro-molybdenum；
Inductively coupled plasma atomic emission spectrometer in the step, running parameter are：
Radio-frequency power 1000W；
Plasma gas flow rate 20.0L/min；
Time of integration 20s；
Nebulizer flow 0.3L/min；
Secondary air amount 1.80L/min.
The method that the present invention uses to ferro-molybdenum sample carry out pre-treatment, by ICP-AES methods measure 193.696nm into
Row measure, solve resolution not exclusively and cause instrument loss and pollution or because Matrix effects are larger cause result error compared with
Big problem.Sb elements are determined using ICP-AES standard measures, for the detection limit of method between 1.5-3.0 μ g/kg, matrix is dry
It disturbs small, disclosure satisfy that the needs of production and living.
Above example is only several embodiments of the present invention, but the present invention is not limited to this.Based in the present invention
Embodiment, those of ordinary skill in the art's obtained every other reality under the premise of not making any creative work
Mode is applied, the range that the present invention is protected is belonged to.
Claims (3)
1. the measurement method of micro- antimony, this method include in a kind of ferro-molybdenum：
(1) it weighs sample 50mg to be placed in the conical flask of 100mL, is added 60% potassium permanganate 5mL, 1:1 nitric acid 5mL, heating wait for
Sample all after dissolving, continues to be evaporated to and closely do, be subsequently cooled to outdoor；1 is added again:1 nitric acid 10mL, capping oscillation 60
Second, after stratification, it is heated to 100-125 degrees Celsius, is then cooled to room temperature, stands and waits for that layering discards organic phase；Again plus
Ethyl acetate 15mL vibrates 90 seconds, then chlorination imitates 15mL, vibrates 30 seconds；Ultra-pure water constant volume is used after discarding organic phase after being layered
It is for use to 100mL；
(2) inductively coupled plasma atomic emission spectrometer, i.e. ICP- are used according to the Specimen eliminating solution that step (1) obtains
Contained Sb elements spectral intensity at 193.696nm, measures Sb intensity values in AES Instrument measuring Specimen eliminating solution；
(3) configuration standard working solution：Weigh Sb Standard Stock solutions 0mL, 10mL of a concentration of 1.0 μ g/mL, 20mL, 40mL,
60mL, 80mL, 100mL are respectively placed in 100mL volumetric flasks, and constant volume is carried out with ultra-pure water；Sb in the standard working solution of acquisition
The content of element corresponds to 0 μ g/mL, 100 μ g/mL, 200 μ g/mL, 400 μ g/mL, 600 μ g/mL, 800 μ g/mL, 1000 μ respectively
g/mL；
(4) inductively coupled plasma atomic emission spectrometer will be imported according to the standard working solution that step (3) obtain, i.e.,
ICP-AES instruments mix before entering atomizer, and the best isotope of Sb elements is selected to be measured；According to standard working solution
The Sb element-intensities values that the known content and ICP-AES Instrument measurings of middle Sb elements arrive draw the standard working curve of Sb elements；
In conjunction with the intensity value for the Sb elements that step (2) Specimen eliminating solution obtains, Specimen eliminating is calculated according to standard working curve
The concentration value of solution S b elements, to calculate the dense of trace element Sb in ferro-molybdenum according to the existing formula method of this field
Angle value；
Inductively coupled plasma atomic emission spectrometer in the step, running parameter are：
Radio-frequency power 1000W；
Plasma gas flow rate 20.0L/min；
Time of integration 20s；
Nebulizer flow 0.3L/min；
Secondary air amount 1.80L/min.
2. measurement method according to claim 1, described to be heated to 100 to 125 degrees Celsius by being heated to 100 degrees Celsius of generations
It replaces.
3. measurement method according to claim 1, described to be heated to 100 to 125 degrees Celsius by being heated to 125 degrees Celsius of generations
It replaces.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101609047A (en) * | 2009-06-24 | 2009-12-23 | 谱尼测试科技（北京）有限公司 | The assay method of antimony in a kind of electric equipment products |
| CN103293144A (en) * | 2013-06-26 | 2013-09-11 | 天津虹炎科技有限公司 | ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) measurement of content of impurity phosphorus in steel |
| CN103344628A (en) * | 2013-06-26 | 2013-10-09 | 天津虹炎科技有限公司 | ICP-AES (inductively coupled plasma-atomic emission spectrometer) measurement method for content of arsenic in steel |
| CN104237209A (en) * | 2014-10-16 | 2014-12-24 | 云南驰宏锌锗股份有限公司 | Method for synchronously detecting copper, bismuth, iron, lead, tellurium, selenium, antimony and palladium in electrolytic silver through ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) |
| CN105259159A (en) * | 2015-10-20 | 2016-01-20 | 武汉钢铁(集团)公司 | Analysis method for measuring content of phosphorus in ferro-molybdenum |
-
2018
- 2018-05-09 CN CN201810439680.5A patent/CN108318476A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101609047A (en) * | 2009-06-24 | 2009-12-23 | 谱尼测试科技（北京）有限公司 | The assay method of antimony in a kind of electric equipment products |
| CN103293144A (en) * | 2013-06-26 | 2013-09-11 | 天津虹炎科技有限公司 | ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) measurement of content of impurity phosphorus in steel |
| CN103344628A (en) * | 2013-06-26 | 2013-10-09 | 天津虹炎科技有限公司 | ICP-AES (inductively coupled plasma-atomic emission spectrometer) measurement method for content of arsenic in steel |
| CN104237209A (en) * | 2014-10-16 | 2014-12-24 | 云南驰宏锌锗股份有限公司 | Method for synchronously detecting copper, bismuth, iron, lead, tellurium, selenium, antimony and palladium in electrolytic silver through ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) |
| CN105259159A (en) * | 2015-10-20 | 2016-01-20 | 武汉钢铁(集团)公司 | Analysis method for measuring content of phosphorus in ferro-molybdenum |
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