CN102879384A - Method for detecting zirconium content in tantalum-cobalt-base alloy in microwave solution sample dissolving manner - Google Patents
Method for detecting zirconium content in tantalum-cobalt-base alloy in microwave solution sample dissolving manner Download PDFInfo
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Abstract
The invention provides a method for detecting the zirconium content in tantalum-cobalt-base alloy in a microwave solution sample dissolving manner. The method comprises the analyzing steps of: weighing a sample; preparing a sample solution; preparing a calibration solution; drawing a working curve; measuring the concentration of zirconium in the sample solution; and calculating a measurement result, so as to obtain the zirconium content. The problems that the sample is difficult to dissolve, a measurement spectral line is interfered seriously and the like can be overcome, so that the sample dissolving speed is greatly accelerated; the spectral interference of a base body on measurement elements can be avoided by base body matching; and the accuracy of the measurement is improved. The method has the advantages of rapid sample solution and measurement, simplicity and convenience in operation, and good labor and material saving performance.
Description
Technical field
The present invention is
Belong to the alloying element analytical technology, relate to a kind of Microwave samples digestion method and measure the method that contains zirconium content in the tantalum cobalt-base alloys.
Background technology
Containing tantalum cobalt base superalloy K6509 is Co-Cr-Ni based precipitation hardening type equiax crystal cast superalloy, and serviceability temperature is below 1000 ℃.Cr content accounts for 23% in the alloy, add simultaneously tantalum, tungsten, titaniums etc. form the element of carbonide, so alloy has excellent anti-oxidant and decay resistance, and higher elevated temperature strength, 900 ℃ of creep rupture strengths of alloy exceed 40MPa～50MPa than similar X40 alloy, hold warm ability and improve 40 ℃～50 ℃, major product is guide vane, alloy has been used for being produced on the hot-end components such as gas-turbine unit guide vane of working below 1000 ℃, exemplary application pushes away in height and compares aeromotor, advanced carrier-borne aeromotor, and the abominable engine of service condition.Adjusting alloy composition is the important means of improving alloy property, the content of impurity element zirconium can improve cast superalloy room temperature tensile and lasting intensity and the plasticity of middle temperature, along with the widespread use that contains the tantalum cobalt base superalloy, the Accurate Determining of element zirconium chemical constitution seems more and more urgent.Zirconium assay method in the high temperature alloy has " the direct Their Determination by Spectrophotometry zirconium of azo arsenic III content " to measure zr element content, but the running time is long, complex steps.
Icp analysis has accurately, fast, the characteristics analyzed simultaneously of multielement; be widely used in the fields such as geology, metallurgy, machine-building, environmental protection, biomedicine, food; have good detection limit and analytical precision; matrix disturbs little; linear dynamic range is wide; analytical work person can be mixed with a series of standard with primary standard substance, and the advantage such as sample pretreating easy (than chemical analysis).Microwave digestion technology is that a kind of method of high temperature, high-pressure closed vessel of using of development in recent years is for a kind of efficient sample-dissolving technology of insoluble metal.
But at present domestic now still not for the analytical approach that contains the tantalum cobalt base superalloy, common cobalt base superalloy adopts hydrochloric acid, nitric acid dissolve, the sampler-dissolving method that uses sulphur phosphoric acid to smolder in the process, just can dissolve, contain the tantalum cobalt base superalloy then because the existence of high tantalum, be difficult to dissolving, if and zr element has the phosphoric acid existence can be easy to form sediment in the system when dissolving, because it is larger that the existence of high tantalum causes that spectrum disturbs, therefore be necessary the problems such as the molten sample that contains the tantalum cobalt-base alloys and spectrum interference are studied.Gao Song etc. applied for a patent " method of aluminium, titanium, manganese, nickel, tungsten, iron content in a kind of CoCrMo of mensuration cobalt-base alloys " in 2009, although solved molten sample and the mensuration problem of common cobalt-base alloys, the method is for the dissolving that adds the cobalt-base alloys behind the high-melting-point element tantalum and measure inapplicable.
Therefore, foundation contains zr element analytical approach in the tantalum cobalt base superalloy, the blank that can replenish spectroscopic analysis methods, shorten analysis time, improve the accuracy of analyzing, be the research and production service, to promote simultaneously and the exchanging of the unit of colleague to have widely promotion and application and be worth.
Summary of the invention
The present invention designs for the situation of above-mentioned prior art just a kind of method that adopts the Microwave samples digestion method to measure zirconium content in the tantalum cobalt-base alloys is provided, its objective is propose that a kind of molten sample speed is fast, analysis precision is high, easy and simple to handle, method that mensuration that efficient is high contains zirconium content in the tantalum cobalt-base alloys.
The objective of the invention is to be achieved through the following technical solutions:
This kind adopts the Microwave samples digestion method to measure the method for zirconium content in the tantalum cobalt-base alloys, it is characterized in that:
⑴ the reagent that the method is used in the mensuration process has:
1.1 hydrochloric acid, ρ 1.19g/mL, the pure or MOS level of top grade;
1.2 nitric acid, ρ 1.42g/mL; , the pure or MOS level of top grade
1.3 hydrofluorite, ρ 1.15g/mL, top grade is pure;
1.4 sulfuric acid, ρ 1.84g/mL, top grade is pure;
1.5 the zirconium standard solution, 0.10mg/mL, the preparation method takes by weighing the 0.1351g zirconium dioxide, place platinum crucible, hydrofluorite 10mL in the adding above-mentioned steps 1.3 and the nitric acid 6mL in the above-mentioned steps 1.2 after the low-temperature heat dissolving, add the sulfuric acid 10mL in the above-mentioned steps 1.4, heating evaporation is to emitting the sulfuric acid cigarette, add entry with the careful mixing of solution, after the cooling solution is moved in the 1000mL volumetric flask, add the hydrochloric acid 100mL in the above-mentioned steps 1.1, be diluted with water to scale, mixing;
1.6 cobalt standard solution, 10.0mg/mL.The preparation method takes by weighing the 5.000g metallic cobalt, and the massfraction of metallic cobalt is not less than 99.98%, places the 150mL beaker, low-temperature heat dissolving behind the hydrochloric acid in the adding above-mentioned steps 1.1, and cooling moves in the 500mL volumetric flask, is diluted with water to scale, mixing;
1.7 the yttrium inner mark solution, 0.2mg/mL takes by weighing the 0.127g yttria, places the 150mL beaker, add the hydrochloric acid 20mL in the above-mentioned steps 1.1, after the low-temperature heat dissolving, cooling moves in the 500mL volumetric flask, add the hydrochloric acid 15mL in the above-mentioned steps 1.1, be diluted with water to scale, mixing;
⑵ the step that the method is measured process is:
2.1 sampling and sample preparation
Sample is taken a sample and sample preparation according to the requirement of HB/Z205, takes by weighing the 0.10g sample, is accurate to 0.0001g;
2.2 preparation sample solution
Test portion is placed the 40mL micro-wave diminishing pot, add hydrochloric acid 3mL, the nitric acid 1mL in the above-mentioned steps 1.2, the hydrofluorite 1mL in the above-mentioned steps 1.3 in 5mL water, the above-mentioned steps 1.1, under the normal temperature gas behind the acid reaction is discharged, with microwave digestion device test portion is cleared up, after the cooling, taken out the micro-wave diminishing pot venting, test solution is moved in the 100mL plastics volumetric flask, add the yttrium inner mark solution 2.00mL in the above-mentioned steps 1.3, be diluted with water to scale, mixing;
The running parameter of microwave digestion device is: RF power: 1600W; Heating-up time: 25min; Pressure: 800psi; Keep temperature: 200 ℃; Temperature retention time: 20min;
2.3 preparation work curve solution
In 5～8 100mL beakers, do not add sample, process synchronously blank solution by step 2.2, move in several corresponding 100mL volumetric flasks, cobalt standard solution 6.00mL in yttrium inner mark solution 2mL in each volumetric flask in the adding above-mentioned steps 1.7 and the above-mentioned steps 1.6, again according to the content range of zirconium in the sample of learning in advance, in each volumetric flask, add the different volumes number, zirconium standard solution in the above-mentioned steps 1.5, the content that makes the zirconium in each volumetric flask be in the sample of learning zirconium content 0%～200%, then be diluted with water to scale, mixing is as working curve solution;
2.4 drawing curve
Adopt the intensity of inductively coupled plasma atomic emission spectrometer zirconium and yttrium in spectral line zirconium 339.198nm and yttrium 371.029nm successively surveying work curve solution, take the intensity rate of zirconium and yttrium as ordinate, with the mass concentration of zirconium as horizontal ordinate, the drawing curve;
2.5 the mass concentration of element zirconium in the measurement sample solution
Adopt inductively coupled plasma atomic emission spectrometer to measure the intensity of zirconium and yttrium in the sample solution at spectral line zirconium 339.198nm and yttrium 371.029nm, find the mass concentration of respective element zirconium with the intensity rate of zirconium and yttrium at corresponding working curve;
2.7 the computation and measurement result obtains the content of zirconium;
Be calculated as follows the mass percent w of element zirconium in the sample, numerical value represents with %:
In the formula:
ρ---the mass concentration of element zirconium in the sample solution, unit: μ g/mL;
V---sample solution volume, unit: mL;
M---test portion quality, unit: g;
Low-temperature heat described in the said method refers to that heated perimeter is at 50～200 ℃.
The running parameter of inductively coupled plasma atomic emission spectrometer is as follows: high frequency frequency: 40.68MHz; Entrance slit: 20 μ m; Exit slit: 80 μ m; 15 μ m; Incident power: 1.0Kw; Reflective power:＜15W; Sample lifting capacity: 1.2L/min; Cooling gas flow: 15L/min; Integral time: 2s; Sheath airshed: 0.2L/min.
Advantage of the present invention is:
One, use microwave digestion technology greatly to accelerate molten sample speed, the molten sample time shortens to one hour from about couple of days;
Two, overcome cobalt-based body and other elements etc. the interference of multiple spectrum, improved the accuracy of measuring;
Three, measure fast, easy and simple to handle, saved a large amount of man power and materials.
Embodiment
Embodiment
Measure the content of zirconium among the tantalum cobalt base superalloy K6509, it is characterized in that: the step of this assay method is:
⑴ the reagent that the method is used in the mensuration process has:
1.1 hydrochloric acid, ρ 1.19g/mL, the pure or MOS level of top grade;
1.2 nitric acid, ρ 1.42g/mL; , the pure or MOS level of top grade
1.3 hydrofluorite, ρ 1.15g/mL, top grade is pure;
1.4 sulfuric acid, ρ 1.84g/mL, top grade is pure;
1.5 the zirconium standard solution, 0.10mg/mL, the preparation method takes by weighing the 0.1351g zirconium dioxide, place platinum crucible, hydrofluorite 10mL in the adding above-mentioned steps 1.3 and the nitric acid 6mL in the above-mentioned steps 1.2 after the low-temperature heat dissolving, add the sulfuric acid 10mL in the above-mentioned steps 1.4, heating evaporation is to emitting the sulfuric acid cigarette, add entry with the careful mixing of solution, after the cooling solution is moved in the 1000mL volumetric flask, add the hydrochloric acid 100mL in the above-mentioned steps 1.1, be diluted with water to scale, mixing;
1.6 cobalt standard solution, 10.0mg/mL.The preparation method takes by weighing the 5.000g metallic cobalt, and the massfraction of metallic cobalt is not less than 99.98%, places the 150mL beaker, low-temperature heat dissolving behind the hydrochloric acid in the adding above-mentioned steps 1.1, and cooling moves in the 500mL volumetric flask, is diluted with water to scale, mixing;
1.7 the yttrium inner mark solution, 0.2mg/mL takes by weighing the 0.127g yttria, places the 150mL beaker, add the hydrochloric acid 20mL in the above-mentioned steps 1.1, after the low-temperature heat dissolving, cooling moves in the 500mL volumetric flask, add the hydrochloric acid 15mL in the above-mentioned steps 1.1, be diluted with water to scale, mixing;
⑵ the step that the method is measured process is:
2.1 sampling and sample preparation
Sample is taken a sample and sample preparation according to the requirement of HB/Z205, takes by weighing the 0.10g sample, is accurate to 0.0001g;
2.2 preparation sample solution
Test portion is placed the 40mL micro-wave diminishing pot, add hydrochloric acid 3mL, the nitric acid 1mL in the above-mentioned steps 1.2, the hydrofluorite 1mL in the above-mentioned steps 1.3 in 5mL water, the above-mentioned steps 1.1, under the normal temperature gas behind the acid reaction is discharged, with microwave digestion device test portion is cleared up, after the cooling, taken out the micro-wave diminishing pot venting, test solution is moved in the 100mL plastics volumetric flask, add the yttrium inner mark solution 2.00mL in the above-mentioned steps 1.3, be diluted with water to scale, mixing;
The running parameter of microwave digestion device is: RF power: 1600W; Heating-up time: 25min; Pressure: 800psi; Keep temperature: 200 ℃; Temperature retention time: 20min;
2.3 preparation work curve solution
In 5～8 100mL beakers, do not add sample, process synchronously blank solution by step 2.2, move in several corresponding 100mL volumetric flasks, cobalt standard solution 6.00mL in yttrium inner mark solution 2mL in each volumetric flask in the adding above-mentioned steps 1.7 and the above-mentioned steps 1.6, again according to the content range of zirconium in the sample of learning in advance, in each volumetric flask, add the different volumes number, zirconium standard solution in the above-mentioned steps 1.5, the content that makes the zirconium in each volumetric flask be in the sample of learning zirconium content 0%～200%, then be diluted with water to scale, mixing is as working curve solution;
2.4 drawing curve
Adopt the intensity of inductively coupled plasma atomic emission spectrometer zirconium and yttrium in spectral line zirconium 339.198nm and yttrium 371.029nm successively surveying work curve solution, take the intensity rate of zirconium and yttrium as ordinate, with the mass concentration of zirconium as horizontal ordinate, the drawing curve;
2.5 the mass concentration of element zirconium in the measurement sample solution
Adopt inductively coupled plasma atomic emission spectrometer to measure the intensity of zirconium and yttrium in the sample solution at spectral line zirconium 339.198nm and yttrium 371.029nm, find the mass concentration of respective element zirconium with the intensity rate of zirconium and yttrium at corresponding working curve;
2.7 the computation and measurement result obtains the content of zirconium;
Be calculated as follows the mass percent w of element zirconium in the sample, numerical value represents with %:
In the formula:
ρ---the mass concentration of element zirconium in the sample solution, unit: μ g/mL;
V---sample solution volume, unit: mL;
M---test portion quality, unit: g;
Low-temperature heat described in the said method refers to that heated perimeter is at 50～200 ℃.
The running parameter of inductively coupled plasma atomic emission spectrometer is as follows: high frequency frequency: 40.68MHz; Entrance slit: 20 μ m; Exit slit: 80 μ m; 15 μ m; Incident power: 1.0Kw; Reflective power:＜15W; Sample lifting capacity: 1.2L/min; Cooling gas flow: 15L/min; Integral time: 2s; Sheath airshed: 0.2L/min.
Press the selected condition of work of inductively coupled plasma atomic emission spectrometer, take yttrium as internal standard element, the drawing curve is measured sample solution, obtains the mass concentration of element zirconium in the sample solution, the computation and measurement result, and the content that obtains zirconium is 0.41%.
Compared with prior art, technical solution of the present invention has solved the mensuration requirement that contains zr element in the tantalum cobalt base superalloy, and has highly sensitively, and selectivity is good, detects the advantages such as lower limit is low.
Claims (2)
1. method that adopts the Microwave samples digestion method to measure zirconium content in the tantalum cobalt-base alloys is characterized in that:
⑴ the reagent that the method is used in the mensuration process has:
1.1 hydrochloric acid, ρ 1.19g/mL, the pure or MOS level of top grade;
1.2 nitric acid, ρ 1.42g/mL; , the pure or MOS level of top grade
1.3 hydrofluorite, ρ 1.15g/mL, top grade is pure;
1.4 sulfuric acid, ρ 1.84g/mL, top grade is pure;
1.5 the zirconium standard solution, 0.10mg/mL, the preparation method takes by weighing the 0.1351g zirconium dioxide, place platinum crucible, hydrofluorite 10mL in the adding above-mentioned steps 1.3 and the nitric acid 6mL in the above-mentioned steps 1.2 after the low-temperature heat dissolving, add the sulfuric acid 10mL in the above-mentioned steps 1.4, heating evaporation is to emitting the sulfuric acid cigarette, add entry with the careful mixing of solution, after the cooling solution is moved in the 1000mL volumetric flask, add the hydrochloric acid 100mL in the above-mentioned steps 1.1, be diluted with water to scale, mixing;
1.6 cobalt standard solution, 10.0mg/mL.The preparation method takes by weighing the 5.000g metallic cobalt, and the massfraction of metallic cobalt is not less than 99.98%, places the 150mL beaker, low-temperature heat dissolving behind the hydrochloric acid in the adding above-mentioned steps 1.1, and cooling moves in the 500mL volumetric flask, is diluted with water to scale, mixing;
1.7 the yttrium inner mark solution, 0.2mg/mL takes by weighing the 0.127g yttria, places the 150mL beaker, add the hydrochloric acid 20mL in the above-mentioned steps 1.1, after the low-temperature heat dissolving, cooling moves in the 500mL volumetric flask, add the hydrochloric acid 15mL in the above-mentioned steps 1.1, be diluted with water to scale, mixing;
⑵ the step that the method is measured process is:
2.1 sampling and sample preparation
Sample is taken a sample and sample preparation according to the requirement of HB/Z205, takes by weighing the 0.10g sample, is accurate to 0.0001g;
2.2 preparation sample solution
Test portion is placed the 40mL micro-wave diminishing pot, add hydrochloric acid 3mL, the nitric acid 1mL in the above-mentioned steps 1.2, the hydrofluorite 1mL in the above-mentioned steps 1.3 in 5mL water, the above-mentioned steps 1.1, under the normal temperature gas behind the acid reaction is discharged, with microwave digestion device test portion is cleared up, after the cooling, taken out the micro-wave diminishing pot venting, test solution is moved in the 100mL plastics volumetric flask, add the yttrium inner mark solution 2.00mL in the above-mentioned steps 1.7, be diluted with water to scale, mixing;
The running parameter of microwave digestion device is: RF power: 1600W; Heating-up time: 25min; Pressure: 800psi; Keep temperature: 200 ℃; Temperature retention time: 20min;
2.3 preparation work curve solution
In 5～8 100mL beakers, do not add sample, process synchronously blank solution by step 2.2, move in several corresponding 100mL volumetric flasks, cobalt standard solution 6.00mL in yttrium inner mark solution 2mL in each volumetric flask in the adding above-mentioned steps 1.7 and the above-mentioned steps 1.6, again according to the content range of zirconium in the sample of learning in advance, in each volumetric flask, add the different volumes number, zirconium standard solution in the above-mentioned steps 1.5, the content that makes the zirconium in each volumetric flask be in the sample of learning zirconium content 0%～200%, then be diluted with water to scale, mixing is as working curve solution;
2.4 drawing curve
Adopt the intensity of inductively coupled plasma atomic emission spectrometer zirconium and yttrium in spectral line zirconium 339.198nm and yttrium 371.029nm successively surveying work curve solution, take the intensity rate of zirconium and yttrium as ordinate, with the mass concentration of zirconium as horizontal ordinate, the drawing curve;
2.5 the mass concentration of element zirconium in the measurement sample solution
Adopt inductively coupled plasma atomic emission spectrometer to measure the intensity of zirconium and yttrium in the sample solution at spectral line zirconium 339.198nm and yttrium 371.029nm, find the mass concentration of respective element zirconium with the intensity rate of zirconium and yttrium at corresponding working curve;
2.6 the computation and measurement result obtains the content of zirconium;
The mass percent w numerical value that is calculated as follows element zirconium in the sample represents with %:
In the formula:
ρ---the mass concentration of element zirconium in the sample solution, unit: μ g/mL;
V---sample solution volume, unit: mL;
M---test portion quality, unit: g;
Low-temperature heat described in the said method or heating refer to that heated perimeter is at 50～200 ℃.
2. employing Microwave samples digestion method according to claim 1 is measured the method for zirconium content in the tantalum cobalt-base alloys, and it is characterized in that: the running parameter of inductively coupled plasma atomic emission spectrometer is as follows: high frequency frequency: 40.68MHz; Entrance slit: 20 μ m; Exit slit: 80 μ m; 15 μ m; Incident power: 1.0Kw; Reflective power:＜15W; Sample lifting capacity: 1.2L/min; Cooling gas flow: 15L/min; Integral time: 2s; Sheath airshed: 0.2L/min.
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