CN108152270A - A kind of method of ruthenium element content in Digestion high temperature alloy - Google Patents
A kind of method of ruthenium element content in Digestion high temperature alloy Download PDFInfo
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- CN108152270A CN108152270A CN201711188877.8A CN201711188877A CN108152270A CN 108152270 A CN108152270 A CN 108152270A CN 201711188877 A CN201711188877 A CN 201711188877A CN 108152270 A CN108152270 A CN 108152270A
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- 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
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- G01N1/00—Sampling; Preparing specimens for investigation
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- G—PHYSICS
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- 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
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Abstract
The present invention is a kind of method of ruthenium element content in Digestion high temperature alloy, this method is to claim sample to resolution inner canister, after adding in digestion solution resolution completely, it is placed on electronic balance, solution net weight is diluted with water in resolution inner canister to 100.0g, Matrix Match working curve is prepared, the content of ruthenium element in high temperature alloy is measured on inductively coupled plasma atomic emission spectrometer.The present invention eliminates transfer process in sample course of dissolution, avoids loss caused by transfer not exclusively, and easy to operate, analysis result is accurate, reliable.
Description
Technical field
The present invention is a kind of method of ruthenium element content in Digestion high temperature alloy, belongs to Analysis of Metallic Materials
Technical field.
Background technology
At present, in terms of high temperature alloy element means are detected, inductively coupled plasma (ICP) emission spectrometer is from 1975
Since year comes out, just because of it, detection limit is low, precision is high, the measure range of linearity of concentration is wide, interfering with each other between sample composition
The advantages that small, becomes a kind of incomparable analysis means of other analytical technologies in terms of constituent content mensure.
Under normal circumstances, the dissolving method of high temperature alloy sample is：It is molten using hydrochloric acid, nitric acid, hydrofluoric acid, sulfuric acid, phosphoric acid
Sample is solved, volumetric flask is transferred to after dissolving completely, is then measured in analytical instrument.It is but special for infusibility high temperature alloy
It is not when measuring ruthenium element in high temperature alloy, common sample dissolving method is difficult to be completely dissolved ruthenium element, is disappeared using microwave
Solution mode well solves the problems of dissolution of high-content ruthenium element in infusibility high temperature alloy, but has dissolved sample with micro-wave digestion mode
It after product, needs sample solution being transferred into volumetric flask from resolution inner canister, since resolution inner canister is unlike beaker has sharp mouth, will
It when sample solution in inner canister is transferred in volumetric flask, be easy to cause liquid and spills, make sample loss, obtain the analysis knot of mistake
Fruit.
Invention content
The present invention be exactly for the above-mentioned prior art situation and design and provide a kind of Digestion high temperature alloy
The method of middle ruthenium element content, the purpose is to the high-content ruthenium element in easy, quick, effective dissolving infusibility high temperature alloy, and
And it is accurately measured.
In order to achieve the above object, the technical solution used is as follows：
It is as follows the step of the method for ruthenium element content in this kind of Digestion high temperature alloy：
1) the resolution inner canister of microwave dissolver is cleaned, dried, numbered, each resolution inner canister is weighed on electronic balance
The quality of slack tank, and record；
2) 0.1~0.2 gram of high temperature alloy sample is accurately weighed in clearing up in inner canister, adds in digestion solution, and digestion solution includes dense
Resolution inner canister capping is tightened and is put into counteracting tank housing, put by 4~6mL of hydrochloric acid, 1~2mL of concentrated nitric acid, 0.5~2mL of hydrofluoric acid
It puts in microwave dissolver, is cleared up, resolution terminates postcooling, takes out resolution inner canister, with 2~3 flushing resolutions of distilled water
The inner wall of lid adds in the 2.00mL Y Int Std solution that quality-volumetric concentration is 0.1~0.5mg/mL, dries to clearing up in inner canister
Resolution inner canister is placed on electronic balance by tank wall in resolution, dilute with water according to the number of resolution inner canister and the quality of slack tank
Solution in resolution inner canister is released, to net weight 100.0g, to shake up, obtain sample solution；
3) 2~7 working curve solution vessel are cleaned, dried, numbered, each vessel are weighed on electronic balance
Blank quality, and record；
4) according to the content range of coexistence elements in superalloy coupons, alloy member of the degree more than 5% is chosen
Element, adds in the standard solution of the alloying element in step 3) treated 2~7 working curve solution vessel, addition with
The content of this in sample kind alloying element is basically identical；
According to the content range of ruthenium element in superalloy coupons, ruthenium member is added in 2~7 working curve solution vessel
Plain standard solution, it is 0~20mg to make the ruthenium element content in 2~7 working curve solution vessel in working curve solution, is added in
With the 2.00mL Y Int Std solution of step 2) phase homogenous quantities-volumetric concentration, 2~7 working curve solution vessel are placed on electricity
On sub- balance, according to the number of each vessel and blank quality, solution net weight is diluted with water in working curve solution vessel extremely
100.0g shakes up, and obtains 2~7 working curve solution；
5) working curve solution is introduced into inductive coupling plasma emission spectrograph, measures ruthenium element and Y Int Std member
The intensity of element, using internal standard method drawing curve；Sample solution is introduced into inductive coupling plasma emission spectrograph, is surveyed
Determine the intensity of ruthenium element and Y Int Std element, the content of ruthenium element in sample solution is determined according to working curve；
Resolution parameter is power 1600W, temperature program is to keep the temperature 10~20 minutes after being warming up to 200 DEG C within 10 minutes, then
With same power, 5~10 minutes are kept the temperature after being warming up to 150 DEG C within 5 minutes, completes micro-wave digestion program.
It is that will weigh stent to be placed on electricity that solution to the step of net weight 100.0g in resolution inner canister is diluted with water in step 2)
On sub- balance, resolution inner canister is placed on and weighs in stent, is placed on electronic balance by balance zero setting, adds in water dilution.It weighs
Stent is made of bracket base (1) and stand tube (2), and bracket base (1) is less than the round tablet of balance on goods and services, stent for diameter
It manages (2) and is less than bracket base (1) diameter and slightly larger than the open-end tube of resolution inner canister diameter for diameter, stand tube (2) is welded on
On bracket base (1).
The analysis spectral line of ruthenium element is 240.272nm, 372.803nm or 379.940nm, and the spectral line of Y Int Std element is
371.03nm or 360.07nm.
The invention difference from existing technology is that the present invention achieves following technique effect：
1st, in Digestion high temperature alloy of the present invention the method for ruthenium element content by using inductive coupling
Ruthenium element content in plasma emission spectrometer detection high temperature alloy, the present invention pass through the multiple inspection to high temperature alloy sample
It tests, application effect is good；
2nd, the present invention synthesizes Matrix Match working curve using standard solution, overcomes Matrix effects, has the range of linearity
The characteristics of width, high sensitivity is easy to operate, and analysis result is accurate, reliable；
3rd, the present invention eliminates transfer process in sample course of dissolution, simplifies sample course of dissolution, avoids shifting endless
Loss caused by complete；
4th, inconvenience caused by the weighing stent used avoids round bottom resolution inner canister shakiness, makes constant volume process simpler,
It is easy to operate.
5th, the assay method molten sample speed of the invention taken is fast, analysis precision is high, easy to operate, efficient, disappears in microwave
In solution high temperature alloy, measure high temperature alloy good effect is achieved in terms of ruthenium element content.
6th, the method for the present invention greatly reduces solvent usage amount, is conducive to environmental protection.
7th, the method for the present invention measures quick, easy to operate, has saved a large amount of man power and materials.
Description of the drawings
Fig. 1 is the structure diagram of weighing stent used in technical solution of the present invention
Specific embodiment：
With reference to embodiments, the forgoing and additional technical features and advantages are described in more detail.
The method of ruthenium element content uses HJY ULTIMA IIC type inductance in this kind of Digestion high temperature alloy
Coupled plasma optical emission spectrometer, the operating condition of instrument are as follows：Incident power 1050W；Reflection power<10W；Cooling air-flow
Measure 15L/min；Sample lifting capacity 1.5mL/min；Time of integration 5s；Elemental analysis line：Ru 240.272nm or 372.803nm or
379.940nm, the spectral line of Y Int Std element is 371.03nm or 360.07nm.
The reagent that the method for ruthenium element content uses in this kind of Digestion high temperature alloy is as follows：
Hydrochloric acid I, density 1.19g/mL, more than top pure grade；
Hydrochloric acid II, 1+1, hydrochloric acid I and water by volume 1：1 mixes；
Nitric acid, density 1.42g/mL, more than top pure grade；
Hydrofluoric acid, density 1.15g/mL, more than top pure grade；
The single-elements standard solution such as chromium, cobalt, molybdenum, tungsten, tantalum, quality-volumetric concentration are 1.00mg/mL, are purchased.
Nickel bottom liquid, quality-volumetric concentration are 10.0mg/mL, and preparation method is to weigh 10.0g pure nickels (mass fraction is not small
40mL water, 20mL nitric acid in 400mL beakers, are added in 99.95%), low-temperature heat is complete to dissolving, and is moved into after cooling
In 1000mL volumetric flasks, 40mL nitric acid is added, is diluted with water to scale, is shaken up.
Ruthenium element standard solution, quality-volumetric concentration are 1.00mg/mL, are purchased.
Y Int Std solution, quality-volumetric concentration are 0.2mg/mL, and preparation method is to weigh 0.2540g yttrium oxides in 250mL
In beaker, the mass fraction of yttrium oxide adds in 20~60mL hydrochloric acid II, low-temperature heat is complete to dissolving, cold not less than 99.95%
But it moves into 1000mL volumetric flasks afterwards, adds 20~80mL hydrochloric acid II, be diluted with water to scale, shake up；
Sampling and sample preparation：The sample of analysis is sampled according to the requirement of GB/T 20066 and sample preparation；
It is as follows the step of the method for ruthenium element content in this kind of Digestion high temperature alloy：
1) the resolution inner canister of microwave dissolver is cleaned, dried, numbered, each resolution inner canister is weighed on electronic balance
The quality of slack tank, and record；
2) 0.1 gram of high temperature alloy sample accurately is weighed in clearing up in inner canister, be accurate to 0.0001 gram；
Digestion solution is added in, digestion solution includes hydrochloric acid I 6mL, nitric acid 2mL, hydrofluoric acid 1.0mL, and resolution inner canister capping is tightened
It is put into counteracting tank housing, is placed in microwave dissolver, cleared up, resolution parameter is power 1600W, temperature program 10
Minute keeps the temperature 15 minutes after being warming up to 200 DEG C, and then with same power, 5~10 minutes are kept the temperature after being warming up to 150 DEG C within 5 minutes,
Resolution terminates postcooling, takes out resolution inner canister, with 2~3 inner walls for rinsing resolution lid of distilled water to clearing up in inner canister, adds in matter
Amount-volumetric concentration is the 2.00mL Y Int Std solution of 0.1~0.5mg/mL, dries tank wall in resolution, and resolution inner canister is placed
On electronic balance, according to the number of resolution inner canister and the quality of slack tank, solution is diluted with water in resolution inner canister to net weight
100.0g shakes up, and obtains sample solution；
Be diluted with water resolution inner canister in solution to the step of net weight 100.0g be：Stent will be weighed and be placed on electronic balance
On, resolution inner canister is placed on and weighs in stent, is placed on electronic balance by balance zero setting, adds in water dilution.
It weighs stent to be made of bracket base 1 and stand tube 2, bracket base 1 is less than the circular flat of balance on goods and services for diameter
Plate, stand tube 2 are less than 1 diameter of bracket base and slightly larger than the open-end tube of resolution inner canister diameter for diameter, and stand tube 2 is welded on
On bracket base 1.
3) 3 working curve solution vessel are cleaned, dried, numbered, the sky of each vessel is weighed on electronic balance
White matter amount, and record；
4) according to the content range of coexistence elements in superalloy coupons, alloy member of the degree more than 5% is chosen
Element adds in the standard solution of the alloying element, respectively 4mL nickel in step 3) treated 3 working curve solution vessel
Bottom liquid, 10mL chromium standard solutions, 10mL cobalt standard solutions, 5mL molybdenums standard solution, 5mL tungsten standard solution, 5mL tantalum standard solution,
Addition and the content of this in sample kind alloying element are basically identical；
According to the content range of ruthenium element in superalloy coupons, ruthenium element is added in 3 working curve solution vessel
Standard solution, respectively 0mL, 2.00mL, 5.00mL ruthenium element standard solution add in and step 2) phase homogenous quantities-volumetric concentration
2.00mL Y Int Std solution, 3 working curve solution vessel are individually positioned on electronic balance, according to the volume of each vessel
Number and blank quality, solution net weight in working curve solution vessel is diluted with water and, to 100.0g, shakes up, obtains 3 working curves
Solution；
5) working curve solution is introduced into inductive coupling plasma emission spectrograph, measures ruthenium element and Y Int Std member
The intensity of element, using internal standard method drawing curve, working curve abscissa is bent in work with ruthenium element in working curve solution
Mass fraction in line solution, the ratio drawing of the intensity of working curve ordinate ruthenium element and the intensity of yttrium are bent
Then line, sample solution is introduced into inductive coupling plasma emission spectrograph, measure the strong of ruthenium element and Y Int Std element
Degree finds the corresponding ruthenium element quality in sample solution point with ruthenium element to the ratio of the intensity of yttrium on working curve
Number determines the content of ruthenium element in sample solution according to working curve；Measurement result obtains on HJY ULTIMAIIC instruments
The content of ruthenium is 3.62%.
Claims (5)
1. a kind of method of ruthenium element content in Digestion high temperature alloy, it is characterised in that：The step of this method, is such as
Under：
1) the resolution inner canister of microwave dissolver is cleaned, dried, numbered, each resolution inner canister slack tank is weighed on electronic balance
Quality, and record；
2) 0.1~0.2 gram of high temperature alloy sample is weighed in clearing up in inner canister, adds in digestion solution, digestion solution includes 4~6mL of hydrochloric acid,
Resolution inner canister capping is tightened and is put into counteracting tank housing, is placed on microwave dissolver by 1~2mL of nitric acid, 0.5~2mL of hydrofluoric acid
In, it is cleared up, resolution terminates postcooling, takes out and clears up inner canister, with 2~3 inner walls for rinsing resolution lid of distilled water to resolution
In inner canister, the 2.00mL Y Int Std solution that quality-volumetric concentration is 0.1~0.5mg/mL is added in, dries tank wall in resolution, it will
Resolution inner canister is placed on electronic balance, according to the number of resolution inner canister and the quality of slack tank, is diluted with water molten in resolution inner canister
Liquid shakes up to net weight 100.0g, obtains sample solution；
3) 2~7 working curve solution vessel are cleaned, dried, numbered, the blank of each vessel is weighed on electronic balance
Quality, and record；
4) according to the content range of coexistence elements in superalloy coupons, the alloying element that degree is more than 5% is chosen,
Add in the standard solution of the alloying element in step 3) treated 2~7 working curve solution vessel, addition in sample
The content of this kind of alloying element is basically identical；
According to the content range of ruthenium element in superalloy coupons, ruthenium element mark is added in 2~7 working curve solution vessel
Quasi- solution, it is 0~20mg to make the ruthenium element content in 2~7 working curve solution vessel in working curve solution, adds in and walks
2~7 working curve solution vessel are placed on electronics day by the 2.00mL Y Int Std solution of rapid 2) phase homogenous quantities-volumetric concentration
On flat, according to the number of each vessel and blank quality, solution net weight is diluted with water in working curve solution vessel to 100.0g,
It shakes up, obtains 2~7 working curve solution；
5) working curve solution is introduced into inductive coupling plasma emission spectrograph, measures ruthenium element and Y Int Std element
Intensity, using internal standard method drawing curve；Sample solution is introduced into inductive coupling plasma emission spectrograph, measures ruthenium
The intensity of element and Y Int Std element determines the content of ruthenium element in sample solution according to working curve.
2. the method for ruthenium element content in Digestion high temperature alloy according to claim 1, it is characterised in that：
Resolution parameter is power 1600W, temperature program is to keep the temperature 10~20 minutes after being warming up to 200 DEG C within 10 minutes, then with same
Power keeps the temperature 5~10 minutes after being warming up to 150 DEG C within 5 minutes, completes micro-wave digestion program.
3. the method for ruthenium element content in Digestion high temperature alloy according to claim 1, it is characterised in that：
It is that will weigh stent to be placed on electronic balance that solution to the step of net weight 100.0g in resolution inner canister is diluted with water in step 2)
On, resolution inner canister is placed on and weighs in stent, is placed on electronic balance by balance zero setting, adds in water dilution.
4. the method for ruthenium element content in Digestion high temperature alloy according to claim 3, it is characterised in that：
Stent is weighed to be made of bracket base (1) and stand tube (2), bracket base (1) is less than the round tablet of balance on goods and services for diameter,
Stand tube (2) is less than bracket base (1) diameter and slightly larger than the open-end tube of resolution inner canister diameter, stand tube (2) weldering for diameter
It is connected on bracket base (1).
5. the method for ruthenium element content in Digestion high temperature alloy according to claim 1, it is characterised in that：
The analysis spectral line of ruthenium element is 240.272nm, 372.803nm or 379.940nm, the spectral line of Y Int Std element for 371.03nm or
360.07nm。
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| CN112362447A (en) * | 2020-12-15 | 2021-02-12 | 天津海关化矿金属材料检测中心 | Method for digesting high-temperature alloy by using low-temperature digestion method |
| CN112557324A (en) * | 2020-12-07 | 2021-03-26 | 攀钢集团江油长城特殊钢有限公司 | Method for measuring titanium mass content in steel |
| CN113063743A (en) * | 2021-03-03 | 2021-07-02 | 中航金属材料理化检测科技有限公司 | Method for measuring trace magnesium content in tungsten-containing high-temperature alloy material |
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| CN113063743A (en) * | 2021-03-03 | 2021-07-02 | 中航金属材料理化检测科技有限公司 | Method for measuring trace magnesium content in tungsten-containing high-temperature alloy material |
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