CN103940650B - A kind of measure the method for ferrum nickel in high density tungsten basigamy pouring weight - Google Patents
A kind of measure the method for ferrum nickel in high density tungsten basigamy pouring weight Download PDFInfo
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Abstract
The invention belongs to alloy macroelement analytical technology, relate to a kind of measuring the analysis method of ferrum nickel in high density tungsten basigamy pouring weight.The present invention carries out complexation with phosphoric acid to the wolfram element that in course of dissolution, constantly hydrolysis separates out, and eliminates owing to the hydrolysis of tungsten separates out the impact on elemental iron nickel to be measured.By carrying out interference experiment, it is determined that optimized analysis spectral line, improve the accuracy of measurement；Method measurement range width, it is 0.10% that measurement is rolled off the production line, and measuring the upper limit is 10.0%；Using synchronization process sample and prepare high and low mark solution measurement ferrum nickel element, analytical error is minimum, and method is reproducible；The method using test solution to pipette, can preferably carry out high-load elementary analysis；Being reviewed by the analysis of standard sample, method and shown that made fixed analysis method accuracy is good with other unit analysis result comparison, method is stable, complies fully with the requirement of trace analysis.The inventive method is measured quickly, easy and simple to handle, has saved a large amount of man power and material.
Description
Technical field
The invention belongs to alloy macroelement analytical technology, relate to a kind of measuring ferrum nickel in high density tungsten basigamy pouring weight
Analysis method.
Background technology
High density tungsten basigamy pouring weight (W content 85%-99%) be tammite nickel alloy be a kind of with tungsten as matrix and add
The alloy of ferrum nickel element, this alloy has good plasticity and a machinability, good heat conductivity and electric conductivity, by
In its have excellence properties, be widely used in Aeronautics and Astronautics, military affairs, oil drilling, electrical instrumentation,
The stratospheres such as medical science.
Along with the development of national defense industry, new material is constantly released, the requirement to its composition of the various excellent performance materials
Further strict, in alloy, the content of various elements is most important on the impact of material property.At present, both at home and abroad to height
The analysis of density tungstenio balancing weight composition does not also have examination criteria method, and method of can seeing mostly is the emission spectrum of tungsten
Method, the chemical analysis i.e. ferrum-phenanthrolene spectrophotography of tungsten, nickel-molybdenum indigo plant spectrophotography and diacetyldioxime
Gravimetric methods etc., these method operating procedures are many, and labor intensity is big, takes tediously long, is unfavorable for quickly measuring；Meanwhile,
Alloying element is widely different, without reference to essential element in high density tungsten basigamy pouring weight material to be measured in method introduction
The interference problem of element, if using said method to need lot of experiments to verify, is not therefore suitable for from the perspective of two
In high density tungsten basigamy pouring weight material, the analysis of ferrum nickel element needs.
Inductively coupled plasma atomic emission spectrometer (ICP) is analyzed has accurate, quick, multielement simultaneously
The feature analyzed, is widely used in the necks such as geology, metallurgy, machine-building, environmental conservation, biomedicine, food
Territory, has good detection limit and analytical precision, and matrix interference is little, linear dynamic range width, analyzes worker
The advantages such as a series of standard, and sample pretreating easy (than chemical analysis) can be configured to primary standard substance.
The means that ferrum, nickel element are measured generally have colorimetry, ICP-AES method (inductively coupled plasma atomic emissions
Spectrographic method), atomic absorption method, volumetric method etc..Corresponding analysis method can be found for the different-alloy trade mark, close
The analysis of ferrum nickel in high density tungsten basigamy pouring weight, the most all without the method accurately analyzing this alloy, substantially
Being all to apply mechanically Ni-based, iron-base superalloy or other alloy approach, it is longer to there is the dissolved samples time in using method,
Dissolve not exclusively, uncertain etc. the shortcoming such as cause analytical cycle longer of the selection of analytical line.
Summary of the invention
It is an object of the invention to: propose that a kind of analytical element content is higher, wide ranges, can accurately carry out ferrum nickel and divide
The analysis method of ferrum nickel element in the mensuration high density tungsten basigamy pouring weight of analysis.
The technical scheme is that employing inductive coupling plasma emission spectrograph, the working condition of instrument and
Analytical line is as follows: higher frequency: 40.68MHz；Incident power: 0.95～1.1Kw；Reflection power: ＜ 15W；
Argon flow amount: wherein, cooling gas flow 12～20L/min, sheath throughput 0.1～0.6L/min；Sample carries
Rising amount: 1.0～1.5ml/min；The time of integration: 1～10s；Elementary analysis line: choose ferrum 239.562nm；
Nickel 231.604nm；
(1), the reagent used in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL；Top grade is pure；
(1.2), nitric acid, ρ 1.42g/mL；Top grade is pure；
(1.3), phosphoric acid, ρ 1.69g/mL；Top grade is pure；
(1.4), hydrochloric acid, 1+1；
(1.5) sodium hydroxide solution, 200g/L；
(1.6), ferrum standard solution: 1.00mg/mL；Weigh 1.0000g；＞ 99.99% pure iron, is placed in 300mL
In beaker, it is blown into secondary water 30mL, adds the hydrochloric acid 30mL described in step (1.1), be heated to ferrum the most molten
Solve, move in 1000mL volumetric flask after cooling, be diluted with water to scale, mixing；
(1.7), ferrum standard solution: 0.10mg/mL；Pipette the ferrum standard described in 20.00mL step (1.6) molten
Liquid, is placed in 200mL volumetric flask, adds the hydrochloric acid 5mL described in step (1.1), is diluted with water to scale,
Shake up；
(1.8), ferrum standard solution: 0.01mg/mL；Pipette the ferrum standard described in 20.00mL step (1.7) molten
Liquid, is placed in 200mL volumetric flask, adds the hydrochloric acid 5mL described in step (1.1), is diluted with water to scale,
Shake up；
(1.9), nickel standard solution 1.00mg/mL；Weigh 1.0000g；＞ 99.99% pure nickel, is placed in 300mL
In beaker, it is blown into secondary water 30mL, adds 30mL nitric acid, be heated to nickel and be completely dissolved, after cooling, move into 1000
In mL volumetric flask, it is diluted with water to scale, mixing；
(1.10), nickel standard solution: 0.10mg/mL；Pipette the nickel standard described in 20.00mL step (1.9)
Solution, is placed in 200mL volumetric flask, adds 5mL nitric acid, is diluted with water to scale, shakes up；
(1.11), nickel standard solution: 0.01mg/mL；Pipette the nickel mark described in 20.00mL step (1.10)
Quasi-solution, is placed in 200mL volumetric flask, adds the hydrochloric acid 5mL described in step (1.1), is diluted with water to carve
Degree, shakes up；
(1.12), copper standard solution: 0.10mg/mL；Weigh 0.1000g；＞ 99.99% fine copper, is placed in 250
In mL beaker, it is blown into bis-water of 10mL, adds 10mL nitric acid, be heated to copper and be completely dissolved, move into after cooling
In 1000mL volumetric flask, it is diluted with water to scale, mixing；
(1.13), cobalt standard solution: 0.10mg/mL；Weigh 0.1000g；The pure cobalt of ＞ 99.99%, is placed in 250
In mL beaker, it is blown into bis-water of 10mL, adds 10mL nitric acid, be heated to cobalt and be completely dissolved, move into after cooling
In 1000mL volumetric flask, it is diluted with water to scale, mixing；
(1.14), chromium standard solution: 0.10mg/mL；Weigh 0.1000g；The pure chromium of ＞ 99.98%, is placed in 250
In mL beaker, it is blown into bis-water of 10mL, adds the hydrochloric acid described in 10mL step (1.1), be heated to chromium complete
CL, drips 1.0mL nitric acid, moves in 1000mL volumetric flask, be diluted with water to scale after cooling, mixing；
(1.15), molybdenum standard solution: 0.10mg/mL；Weigh 0.1000g；The pure molybdenum of ＞ 99.98%, is placed in 250
In mL beaker, add the hydrochloric acid described in 20mL step (1.1), 5.0mL nitric acid, be heated to molybdenum and dissolve completely,
Move in 1000mL volumetric flask after cooling, be diluted with water to scale, mixing；
(1.16), tungsten basal body solution, 1.0mg/mL；Weigh specpure at 800 DEG C of calcination 30min in advance
Tungstic anhydride. 0.6305g, is placed in platinum ware, addition 10mL～15mL sodium hydroxide solution, heating for dissolving,
It is cooled to room temperature, moves in 500mL volumetric flask, be diluted with water to scale, shake up, then move into dry plastic bottle
Interior storage；
(1.17) Y Int Std solution, 0.2mg/mL；Weigh 0.1270g, ＞ 99.95% yittrium oxide, be placed in 250
In mL beaker, adding the hydrochloric acid described in 20mL step (1.4), low-temperature heat, to dissolving completely, moves after cooling
Enter in 500mL volumetric flask, add the hydrochloric acid described in 20mL step (1.4), be diluted with water to scale, shake up；
(2), sampling and sample preparation；The sample analyzed is sampled and sample preparation according to the requirement of HB/Z 205；
(3), element analysis spectrum line selects:
Prepare serial single solution, the tungsten basal body solution described in 5.0mL step (1.16), 8.5mL step (1.16)
Described in ferrum standard solution described in described tungsten basal body solution, 1.0mL step (1.8), 1.5mL step (1.6)
Described in nickel standard solution described in ferrum standard solution, 1.0mL step (1.11), 1.5mL step (1.9)
Described in copper standard solution described in nickel standard solution, 5.0mL step (1.12), 5.0mL step (1.13)
Described in chromium standard solution described in cobalt standard solution, 5.0mL step (1.14), 5.0mL step (1.15)
Hydrochloric acid described in molybdenum standard solution, 15mL step (1.1), the nitric acid described in 6mL step (1.2), 10mL
Phosphoric acid described in step (1.3) and the Y Int Std solution described in 2.00mL step (1.17) are respectively at 100mL
In volumetric flask, respectively by above-mentioned solution 5-6 bar ferrum, nickel analysis spectral line on carry out spectrogram scanning, superposition, from
The analytical line that middle Analysis on Selecting signal is strong, matrix in high density balancing weight, co-existing element interference are minimum is composed as separated time
Line；
(4), high density tungsten basigamy pouring weight sample dissolution test
Weigh three parts of 0.10g sample, be separately added into the hydrochloric acid described in 5mL step (1.1) and 2mL nitric acid,
Hydrochloric acid described in 10mL step (1.1) and the hydrochloric acid described in 4mL nitric acid, 15mL step (1.1) and 6mL
Nitric acid heats on electric furnace, and sample dissolution is incomplete, and solution is muddy；
Weigh three parts of 0.10g sample, be separately added into 1. hydrochloric acid described in 5mL step (1.1), 2mL nitric acid
And 10mL phosphoric acid；2. hydrochloric acid, 5mL nitric acid and the 20mL phosphoric acid described in 10mL step (1.1)；③20mL
Hydrochloric acid, 3mL nitric acid and 30mL phosphoric acid described in step (1.1), sample dissolution is complete, and solution is clarified；
(5), Y Int Std consumption test
Weigh 0.10g sample, be accurate to 0.0001g and be placed in 150mL beaker, add 20mL phosphoric acid, 20
Hydrochloric acid described in mL step (1.1), 5mL nitric acid, on electric hot plate, slight fever is completely dissolved to test portion；From electric heating
Taking off the coldest on plate, blow water walls of beaker, liquor capacity keeps about 50mL, boils dissolved salts；Cooling test solution is extremely
Room temperature；Move in 100mL volumetric flask, be diluted with water to scale, shake up；
20.00mL test solution is pipetted to five 100mL volumetric flasks, respectively at first to the 5th volumetric flask
Hydrochloric acid described in middle addition 10mL phosphoric acid and 10mL step (1.1), then in first to the 5th volumetric flask
The most accurately add 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL Y Int Std solution (1.17),
It is diluted with water to scale, shakes up；Research shows, adds 2.00mL Y Int Std solution measurement result relative standard inclined
Difference minimum, measures the most stable；
(6), analytical procedure is as follows:
(6.1), test portion: weigh 0.10g sample, be accurate to 0.0001g；
(6.2), blank assay solution: do blank assay in company with test portion；
(6.3) sample solution, is prepared: be placed in 150mL alkene beaker by the test portion of analytical procedure (6.1), add
Enter the hydrochloric acid described in 10mL～30mL phosphoric acid, 10mL～20mL step (1.1), 3mL～5mL nitric acid,
On electric hot plate, slight fever is completely dissolved to test portion；Taking off the coldest from electric hot plate, blow water walls of beaker, liquor capacity is protected
Hold about 50mL, boil dissolved salts；Cooling test solution is to room temperature；Move in 100mL volumetric flask, be diluted with water to
Scale, shakes up；
Pipette 10.00mL～20.00mL test solution in 100mL volumetric flask, add 5mL～10mL phosphoric acid,
Hydrochloric acid described in 10mL step (1.1), accurately adds the Y Int Std solution described in 2.00mL step (1.17),
Dilute to scale with water, shake up；
(6.4) preparation calibration solution；
(6.4.1), low mark solution is prepared；Low by main chemical compositions preparation in tested high density tungsten basigamy pouring weight
Mark solution is as follows；Pipette the blank assay solution of step described in 10.00mL～20.00mL (6.2) in 100mL
In volumetric flask, add the hydrochloric acid described in 5mL～10mL phosphoric acid, 10mL step (1.1), pipette and test portion master
Want the tungsten basal body solution of the described step (1.16) that composition W content is close, accurately add step described in 2.00mL
(1.17) Y Int Std solution, dilute to scale with water, shake up, as low mark solution；
(6.4.2) high standard solution, is prepared；Low by main chemical compositions preparation in tested high density tungsten basigamy pouring weight
Mark solution is as follows；Pipette the blank assay solution described in 10.00mL～20.00mL step (6.2) in 100mL
In volumetric flask, add the hydrochloric acid described in 5mL～10mL phosphoric acid, 10mL step (1.1), pipette and test portion master
Want the tungsten basal body solution of the described step (1.16) that composition W content is close, add described step (1.6) or (1.7)
Or the ferrum standard solution of (1.8), described step (1.9) or the nickel standard solution of (1.10) or (1.11),
Addition must cover ferrum, nickel element analyst coverage in high density tungsten basigamy pouring weight sample, accurately adds 2.00mL
Y Int Std solution (1.17), dilute to scale with water, shake up, as high standard solution；
(6.5), ferrum, the concentration of nickel in sample solution is measured；By inductively coupled plasma atomic emission spectrometer
Selected working condition and analysis spectral line, with yttrium as internal standard element, use low mark solution and high standard solution to instrument successively
Device is standardized, and then, measures ferrum, the concentration of nickel in sample solution, and must tap a blast furnace nickel percentage composition.
Use the standard sample that chemical composition is close, be configured to required after processing according to (6.1)～(6.3)
Low, high standard solution.
The method have the advantages that:
1) sample treatment technology is one of advantage of this invention, and the present invention uses addition 10mL～30mL phosphoric acid
(1.3), 10mL～20mL hydrochloric acid (1.1), 3mL～5mL nitric acid (1.2), heating, tungstenio sample is carried out
Dissolve.The present invention carries out complexation with phosphoric acid to the wolfram element that in course of dissolution, constantly hydrolysis separates out, and eliminates due to tungsten
Hydrolysis separates out the impact on elemental iron nickel to be measured.
2) by carrying out interference experiment, it is determined that optimized analysis spectral line, improve the accuracy of measurement；
3) method measurement range width, it is 0.10% that measurement is rolled off the production line, and measuring the upper limit is 10.0%；
4) using synchronization process sample and prepare high and low mark solution measurement ferrum nickel element, analytical error is minimum, side
Method is reproducible；
5) method using test solution to pipette, can preferably carry out high-load elementary analysis；
6) addition 2.0%-8.0%, response rate 97.0%-101.0%, relative standard deviation is less than 1.5%, reclaims
Rate, precision are preferable；
7) by the analysis of standard sample, method review and with other unit analysis result comparison show made fixed
Analysis method accuracy is good, and method is stable, complies fully with the requirement of trace analysis.
8) the application method is measured quickly, easy and simple to handle, has saved a large amount of man power and material.
Detailed description of the invention
Embodiment one
Measure ferrum nickel content in high density tungsten basigamy pouring weight, use inductively coupled plasma instrument, the work bar of instrument
Part and analytical line are as follows: higher frequency: 40.68MHz；Incident power: 1.05Kw；Reflection power: ＜ 15W；
Argon flow amount: cooling gas flow: 15L/min；Sheath throughput: 0.2L/min；Sample lifting capacity: 1.0ml/min；
The time of integration: 2s；Elementary analysis line:；
(1), the reagent used in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL；Top grade is pure；
(1.2), nitric acid, ρ 1.42g/mL；Top grade is pure；
(1.3), phosphoric acid, ρ 1.69g/mL；Top grade is pure；
(1.4), hydrochloric acid, 1+1；
(1.5) sodium hydroxide solution, 200g/L；
(1.6), ferrum standard solution: 1.00mg/mL；Weigh 1.0000g；＞ 99.99% pure iron, is placed in 300mL
In beaker, it is blown into secondary water 30mL, adds 30mL hydrochloric acid (1.1), be heated to ferrum and be completely dissolved, after cooling
Move in 1000mL volumetric flask, be diluted with water to scale, mixing.
(1.7), ferrum standard solution: 0.10mg/mL；Pipette 20.00mL ferrum standard solution (1.6), be placed in 200
In mL volumetric flask, add 5mL hydrochloric acid (1.1), be diluted with water to scale, shake up；
(1.8), ferrum standard solution: 0.01mg/mL；Pipette 20.00mL ferrum standard solution (1.7), be placed in 200
In mL volumetric flask, add 5mL hydrochloric acid (1.1), be diluted with water to scale, shake up；
(1.9), nickel standard solution 1.00mg/mL；Weigh 1.0000g；＞ 99.99% pure nickel, is placed in 300mL
In beaker, it is blown into secondary water 30mL, adds 30mL nitric acid (1.2), be heated to nickel and be completely dissolved, move after cooling
Enter in 1000mL volumetric flask, be diluted with water to scale, mixing；
(1.10), nickel standard solution: 0.10mg/mL；Pipette 20.00mL nickel standard solution (1.9), be placed in
In 200mL volumetric flask, add 5mL nitric acid (1.2), be diluted with water to scale, shake up；
(1.11), nickel standard solution: 0.01mg/mL；Pipette 20.00mL nickel standard solution (1.10), be placed in
In 200mL volumetric flask, add 5mL hydrochloric acid (1.1), be diluted with water to scale, shake up；
(1.12), copper standard solution: 0.10mg/mL；Weigh 0.1000g；＞ 99.99% fine copper, is placed in 250
In mL beaker, it is blown into bis-water of 10mL, adds 10mL nitric acid (1.2), be heated to copper and be completely dissolved, cooling
In rear immigration 1000mL volumetric flask, it is diluted with water to scale, mixing；
(1.13), cobalt standard solution: 0.10mg/mL；Weigh 0.1000g；The pure cobalt of ＞ 99.99%, is placed in 250
In mL beaker, it is blown into bis-water of 10mL, adds 10mL nitric acid (1.2), be heated to cobalt and be completely dissolved, cooling
In rear immigration 1000mL volumetric flask, it is diluted with water to scale, mixing；
(1.14), chromium standard solution: 0.10mg/mL；Weigh 0.1000g；The pure chromium of ＞ 99.98%, is placed in 250
In mL beaker, it is blown into bis-water of 10mL, adds 10mL hydrochloric acid (1.1), be heated to chromium and be completely dissolved, dropping
1.0mL nitric acid (1.2), moves in 1000mL volumetric flask after cooling, is diluted with water to scale, mixing；
(1.15), molybdenum standard solution: 0.10mg/mL；Weigh 0.1000g；The pure molybdenum of ＞ 99.98%, is placed in 250
In mL beaker, add 20mL hydrochloric acid (1.1), 5.0mL nitric acid (1.2), be heated to molybdenum and dissolve completely, cooling
In rear immigration 1000mL volumetric flask, it is diluted with water to scale, mixing；
(1.16), tungsten basal body solution, 1.0mg/mL；Weigh specpure at 800 DEG C of calcination 30min in advance
Tungstic anhydride. 0.6305g, is placed in platinum ware, adds 10mL～15mL sodium hydroxide solution (1.5), heating
Dissolve.It is cooled to room temperature, moves in 500mL volumetric flask, be diluted with water to scale, shake up, then move into and be dried
Storage in plastic bottle；
(1.17) Y Int Std solution, 0.2mg/mL；Weigh 0.1270g, ＞ 99.95% yittrium oxide, be placed in 250
In mL beaker, adding 20mL hydrochloric acid (1.4), low-temperature heat, to dissolving completely, moves into 500mL and holds after cooling
In measuring bottle, add 20mL hydrochloric acid (1.4), be diluted with water to scale, shake up；
(2), sampling and sample preparation；The sample analyzed is sampled and sample preparation according to the requirement of HB/Z 205；
(3), element analysis spectrum line selects:
Prepare serial single solution, 5.0mL tungsten basal body solution (1.12), 8.5mL tungsten basal body solution (1.12),
1.0mL ferrum standard solution (1.8), 1.5mL ferrum standard solution (1.6), 1.0mL nickel standard solution (1.11),
1.5mL nickel standard solution (1.9), 5.0mL copper standard solution (1.12), 5.0mL cobalt standard solution (1.13),
5.0mL chromium standard solution (1.14), 5.0mL molybdenum standard solution (1.15), 15mL hydrochloric acid (1.1), 6mL
Nitric acid (1.2), 10mL phosphoric acid (1.3) and 2.00mL Y Int Std solution (1.13) hold respectively at 100mL
In measuring bottle, respectively by above-mentioned solution 5-6 bar ferrum, nickel analysis spectral line on carry out spectrogram scanning, superposition, therefrom
Choose ferrum 239.562nm；Nickel 231.604nm；As analysis spectral line；
(4), high density tungsten basigamy pouring weight sample dissolution test
Weigh three parts of 0.10g sample, be separately added into 5mL hydrochloric acid and 2mL nitric acid, 10mL hydrochloric acid and 4mL
Nitric acid, 15mL hydrochloric acid and 6mL nitric acid heat on electric furnace, and sample dissolution is incomplete, and solution is muddy；
Weigh three parts of 0.10g sample, be separately added into 1. 5mL hydrochloric acid, 2mL nitric acid and phosphatase 11 0mL phosphoric acid；
2. 10mL hydrochloric acid, 5mL nitric acid and phosphoric acid 20mL phosphoric acid；3. 20mL hydrochloric acid, 3mL nitric acid and phosphoric acid 30mL
Phosphoric acid, sample dissolution is complete, and solution is clarified；
(5), Y Int Std consumption test
Weigh 0.10g sample, be accurate to 0.0001g and be placed in 150mL beaker, addition 20mL phosphoric acid (1.3),
20mL hydrochloric acid (1.1), 5mL nitric acid (1.2), on electric hot plate, slight fever is completely dissolved to test portion；From electric hot plate
Taking off the coldest, blow water walls of beaker, liquor capacity keeps about 50mL, boils dissolved salts；Cooling test solution is to room temperature；
Move in 100mL volumetric flask, be diluted with water to scale, shake up；
20.00mL test solution is pipetted to five 100mL volumetric flasks, respectively at first to the 5th volumetric flask
Middle addition 10mL phosphoric acid (1.3) and 10mL hydrochloric acid (1.1), then standard respectively in first to the 5th volumetric flask
Really add 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL Y Int Std solution (1.17), use
Water is diluted to scale, shakes up；Research shows, adds 2.00mL Y Int Std solution measurement result relative standard deviation
Minimum, measures the most stable；
(6), analytical procedure is as follows:
(6.1), test portion: weigh 0.10g sample, be accurate to 0.0001g；
(6.2), blank assay solution: do blank assay in company with test portion；
(6.3) sample solution, is prepared: be placed in 150mL alkene beaker by the test portion of analytical procedure (6.1), add
Entering 10mL phosphoric acid (1.3), 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), on electric hot plate, slight fever is to test portion
It is completely dissolved；Taking off the coldest from electric hot plate, blow water walls of beaker, liquor capacity keeps about 50mL, boils dissolving
Salt；Cooling test solution is to room temperature；Move in 100mL volumetric flask, be diluted with water to scale, shake up；
Pipette 20.00mL test solution in 100mL volumetric flask, add 5mL phosphoric acid (1.3), 10mL hydrochloric acid (1.1),
Accurately add 2.00mL Y Int Std solution (1.17), dilute to scale with water, shake up；
(6.4) preparation calibration solution；
(6.4.1), low mark solution is prepared；Low by main chemical compositions preparation in tested high density tungsten basigamy pouring weight
Mark solution is as follows；Pipette 20.00mL blank reagent solution (6.2) in 100mL volumetric flask, add 5mL phosphoric acid
(1.3), 10mL hydrochloric acid (1.1), pipette 19.0mL tungsten basal body solution (1.16), accurately add 2.00mL yttrium
Inner mark solution (1.17), dilute to scale with water, shake up, as low mark solution；
(6.4.2) high standard solution, is prepared；Low by main chemical compositions preparation in tested high density tungsten basigamy pouring weight
Mark solution is as follows；Pipette 20.00mL blank reagent solution (6.2) in 100mL volumetric flask, add 5mL phosphoric acid
(1.3), 10mL hydrochloric acid (1.1), pipette the tungsten basal body solution (1.16) close with test portion main component W content,
Add 10.00mL ferrum standard solution (1.8), 15.00mL nickel standard solution (1.11), accurately add 2.00
ML Y Int Std solution (1.17), dilute to scale with water, shake up, as high standard solution；
(6.5), ferrum, the concentration of nickel in sample solution is measured；By inductively coupled plasma atomic emission spectrometer
Selected working condition and analysis spectral line, with yttrium as internal standard element, use low mark solution and high standard solution to instrument successively
Device is standardized, and then, measures ferrum, the concentration of nickel in sample solution；
(7), the content of ferrum be 0.20%, the content 0.50% of nickel.
Embodiment two
Measure ferrum nickel content in high density tungsten basigamy pouring weight, use inductively coupled plasma instrument, the work bar of instrument
Part and analytical line are as follows: higher frequency: 40.68MHz；Incident power: 1.0Kw；Reflection power: ＜ 15W；
Argon flow amount: cooling gas flow: 14L/min；Sheath throughput: 0.5L/min；Sample lifting capacity: 1.5ml/min；
The time of integration: 5s；
(1), the reagent used in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL；Top grade is pure；
(1.2), nitric acid, ρ 1.42g/mL；Top grade is pure；
(1.3), phosphoric acid, ρ 1.69g/mL；Top grade is pure；
(1.4), hydrochloric acid, 1+1；
(1.5) sodium hydroxide solution, 200g/L；
(1.6), ferrum standard solution: 1.00mg/mL；Weigh 1.0000g；＞ 99.99% pure iron, is placed in 300mL
In beaker, it is blown into secondary water 30mL, adds 30mL hydrochloric acid (1.1), be heated to ferrum and be completely dissolved, after cooling
Move in 1000mL volumetric flask, be diluted with water to scale, mixing.
(1.7), ferrum standard solution: 0.10mg/mL；Pipette 20.00mL ferrum standard solution (1.6), be placed in 200
In mL volumetric flask, add 5mL hydrochloric acid (1.1), be diluted with water to scale, shake up；
(1.8), ferrum standard solution: 0.01mg/mL；Pipette 20.00mL ferrum standard solution (1.7), be placed in 200
In mL volumetric flask, add 5mL hydrochloric acid (1.1), be diluted with water to scale, shake up；
(1.9), nickel standard solution 1.00mg/mL；Weigh 1.0000g；＞ 99.99% pure nickel, is placed in 300mL
In beaker, it is blown into secondary water 30mL, adds 30mL nitric acid (1.2), be heated to nickel and be completely dissolved, move after cooling
Enter in 1000mL volumetric flask, be diluted with water to scale, mixing；
(1.10), nickel standard solution: 0.10mg/mL；Pipette 20.00mL nickel standard solution (1.9), be placed in
In 200mL volumetric flask, add 5mL nitric acid (1.2), be diluted with water to scale, shake up；
(1.11), nickel standard solution: 0.01mg/mL；Pipette 20.00mL nickel standard solution (1.10), be placed in
In 200mL volumetric flask, add 5mL hydrochloric acid (1.1), be diluted with water to scale, shake up；
(1.12), copper standard solution: 0.10mg/mL；Weigh 0.1000g；＞ 99.99% fine copper, is placed in 250
In mL beaker, it is blown into bis-water of 10mL, adds 10mL nitric acid (1.2), be heated to copper and be completely dissolved, cooling
In rear immigration 1000mL volumetric flask, it is diluted with water to scale, mixing；
(1.13), cobalt standard solution: 0.10mg/mL；Weigh 0.1000g；The pure cobalt of ＞ 99.99%, is placed in 250
In mL beaker, it is blown into bis-water of 10mL, adds 10mL nitric acid (1.2), be heated to cobalt and be completely dissolved, cooling
In rear immigration 1000mL volumetric flask, it is diluted with water to scale, mixing；
(1.14), chromium standard solution: 0.10mg/mL；Weigh 0.1000g；The pure chromium of ＞ 99.98%, is placed in 250
In mL beaker, it is blown into bis-water of 10mL, adds 10mL hydrochloric acid (1.1), be heated to chromium and be completely dissolved, dropping
1.0mL nitric acid (1.2), moves in 1000mL volumetric flask after cooling, is diluted with water to scale, mixing；
(1.15), molybdenum standard solution: 0.10mg/mL；Weigh 0.1000g；The pure molybdenum of ＞ 99.98%, is placed in 250
In mL beaker, add 20mL hydrochloric acid (1.1), 5.0mL nitric acid (1.2), be heated to molybdenum and dissolve completely, cooling
In rear immigration 1000mL volumetric flask, it is diluted with water to scale, mixing；
(1.16), tungsten basal body solution, 1.0mg/mL；Weigh specpure at 800 DEG C of calcination 30min in advance
Tungstic anhydride. 0.6305g, is placed in platinum ware, adds 10mL～15mL sodium hydroxide solution (1.5), heating
Dissolve.It is cooled to room temperature, moves in 500mL volumetric flask, be diluted with water to scale, shake up, then move into and be dried
Storage in plastic bottle；
(1.17) Y Int Std solution, 0.2mg/mL；Weigh 0.1270g, ＞ 99.95% yittrium oxide, be placed in 250
In mL beaker, adding 20mL hydrochloric acid (1.4), low-temperature heat, to dissolving completely, moves into 500mL and holds after cooling
In measuring bottle, add 20mL hydrochloric acid (1.4), be diluted with water to scale, shake up；
(2), sampling and sample preparation；The sample analyzed is sampled and sample preparation according to the requirement of HB/Z 205；
(3), element analysis spectrum line selects:
Prepare serial single solution, 5.0mL tungsten basal body solution (1.12), 8.5mL tungsten basal body solution (1.12),
1.0mL ferrum standard solution (1.8), 1.5mL ferrum standard solution (1.6), 1.0mL nickel standard solution (1.11),
1.5mL nickel standard solution (1.9), 5.0mL copper standard solution (1.12), 5.0mL cobalt standard solution (1.13),
5.0mL chromium standard solution (1.14), 5.0mL molybdenum standard solution (1.15), 15mL hydrochloric acid (1.1), 6mL
Nitric acid (1.2), 10mL phosphoric acid (1.3) and 2.00mL Y Int Std solution (1.13) hold respectively at 100mL
In measuring bottle, respectively by above-mentioned solution 5-6 bar ferrum, nickel analysis spectral line on carry out spectrogram scanning, superposition, therefrom
Choose ferrum 239.562nm；Nickel 231.604nm；As separated time spectral line；
(4), high density tungsten basigamy pouring weight sample dissolution test
Weigh three parts of 0.10g sample, be separately added into 5mL hydrochloric acid and 2mL nitric acid, 10mL hydrochloric acid and 4mL
Nitric acid, 15mL hydrochloric acid and 6mL nitric acid heat on electric furnace, and sample dissolution is incomplete, and solution is muddy；
Weigh three parts of 0.10g sample, be separately added into 1. 5mL hydrochloric acid, 2mL nitric acid and phosphatase 11 0mL phosphoric acid；
2. 10mL hydrochloric acid, 5mL nitric acid and phosphoric acid 20mL phosphoric acid；3. 20mL hydrochloric acid, 3mL nitric acid and phosphoric acid 30mL
Phosphoric acid, sample dissolution is complete, and solution is clarified；
(5), Y Int Std consumption test
Weigh 0.10g sample, be accurate to 0.0001g and be placed in 150mL beaker, addition 20mL phosphoric acid (1.3),
20mL hydrochloric acid (1.1), 5mL nitric acid (1.2), on electric hot plate, slight fever is completely dissolved to test portion；From electric hot plate
Taking off the coldest, blow water walls of beaker, liquor capacity keeps about 50mL, boils dissolved salts；Cooling test solution is to room temperature；
Move in 100mL volumetric flask, be diluted with water to scale, shake up；
20.00mL test solution is pipetted to five 100mL volumetric flasks, respectively at first to the 5th volumetric flask
Middle addition 10mL phosphoric acid (1.3), 10mL hydrochloric acid (1.1), then standard respectively in first to the 5th volumetric flask
Really add 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL Y Int Std solution (1.17), use
Water is diluted to scale, shakes up；Research shows, adds 2.00mL Y Int Std solution measurement result relative standard deviation
Minimum, measures the most stable；
(6), analytical procedure is as follows:
(6.1), test portion: weigh 0.10g sample, be accurate to 0.0001g；
(6.2), blank assay solution: do blank assay in company with test portion；
(6.3) sample solution, is prepared: be placed in 150mL alkene beaker by the test portion of analytical procedure (6.1), add
Entering 30mL phosphoric acid (1.3), 20mL hydrochloric acid (1.1), 3mL nitric acid (1.2), on electric hot plate, slight fever is to test portion
It is completely dissolved；Taking off the coldest from electric hot plate, blow water walls of beaker, liquor capacity keeps about 50mL, boils dissolving
Salt；Cooling test solution is to room temperature；Move in 100mL volumetric flask, be diluted with water to scale, shake up；
Pipette 10.00mL test solution in 100mL volumetric flask, add 5mL phosphoric acid (1.3), 10mL hydrochloric acid (1.1),
Accurately add 2.00mL Y Int Std solution (1.17), dilute to scale with water, shake up；
(6.4) preparation calibration solution；
(6.4.1), low mark solution is prepared；Low by main chemical compositions preparation in tested high density tungsten basigamy pouring weight
Mark solution is as follows；Pipette 10.00mL blank reagent solution (6.2) in 100mL volumetric flask, add 5mL phosphoric acid
(1.3), 10mL hydrochloric acid (1.1), pipette the tungsten basal body solution (1.16) close with test portion main component W content,
Accurately add 2.00mL Y Int Std solution (1.17), dilute to scale with water, shake up, as low mark solution；
(6.4.2) high standard solution, is prepared；Low mark is prepared by main chemical compositions in tested high density tungsten basigamy pouring weight
Solution is as follows；Pipette 10.00mL blank reagent solution (6.2) in 100mL volumetric flask, add 5mL phosphoric acid
(1.3), 10mL hydrochloric acid (1.1), pipette the tungsten basal body solution (1.16) close with test portion main component W content,
Add 5.0mL ferrum standard solution (1.7), 10.0mL nickel standard solution (1.10), accurately add 2.00mL
Y Int Std solution (1.17), dilute to scale with water, shake up, as high standard solution；
(6.5), ferrum, the concentration of nickel in sample solution is measured；By inductively coupled plasma atomic emission spectrometer
Selected working condition and analysis spectral line, with yttrium as internal standard element, use low mark solution and high standard solution to instrument successively
Device is standardized, and then, measures ferrum, the concentration of nickel in sample solution；
(7), the content of ferrum be 3.12%, the content 7.21% of nickel.
Embodiment three
Measure ferrum nickel content in high density tungsten basigamy pouring weight, use inductively coupled plasma instrument, the work bar of instrument
Part and analytical line are as follows: higher frequency: 40.68MHz；Incident power: 1.1Kw；Reflection power: ＜ 15W；
Argon flow amount: cooling gas flow: 16L/min；Sheath throughput: 0.3L/min；Sample lifting capacity: 1.0ml/min；
The time of integration: 10s；
(1), the reagent used in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL；Top grade is pure；
(1.2), nitric acid, ρ 1.42g/mL；Top grade is pure；
(1.3), phosphoric acid, ρ 1.69g/mL；Top grade is pure；
(1.4), hydrochloric acid, 1+1；
(1.5), sodium hydroxide solution, 200g/L；
(1.6), ferrum standard solution: 1.00mg/mL；Weigh 1.0000g；＞ 99.99% pure iron, is placed in 300mL
In beaker, it is blown into secondary water 30mL, adds 30mL hydrochloric acid (1.1), be heated to ferrum and be completely dissolved, after cooling
Move in 1000mL volumetric flask, be diluted with water to scale, mixing.
(1.7), ferrum standard solution: 0.10mg/mL；Pipette 20.00mL ferrum standard solution (1.6), be placed in 200
In mL volumetric flask, add 5mL hydrochloric acid (1.1), be diluted with water to scale, shake up；
(1.8), ferrum standard solution: 0.01mg/mL；Pipette 20.00mL ferrum standard solution (1.7), be placed in 200
In mL volumetric flask, add 5mL hydrochloric acid (1.1), be diluted with water to scale, shake up；
(1.9), nickel standard solution 1.00mg/mL；Weigh 1.0000g；＞ 99.99% pure nickel, is placed in 300mL
In beaker, it is blown into secondary water 30mL, adds 30mL nitric acid (1.2), be heated to nickel and be completely dissolved, move after cooling
Enter in 1000mL volumetric flask, be diluted with water to scale, mixing；
(1.10), nickel standard solution: 0.10mg/mL；Pipette 20.00mL nickel standard solution (1.9), be placed in
In 200mL volumetric flask, add 5mL nitric acid (1.2), be diluted with water to scale, shake up；
(1.11), nickel standard solution: 0.01mg/mL；Pipette 20.00mL nickel standard solution (1.10), be placed in
In 200mL volumetric flask, add 5mL hydrochloric acid (1.1), be diluted with water to scale, shake up；
(1.12), copper standard solution: 0.10mg/mL；Weigh 0.1000g；＞ 99.99% fine copper, is placed in 250
In mL beaker, it is blown into bis-water of 10mL, adds 10mL nitric acid (1.2), be heated to copper and be completely dissolved, cooling
In rear immigration 1000mL volumetric flask, it is diluted with water to scale, mixing；
(1.13), cobalt standard solution: 0.10mg/mL；Weigh 0.1000g；The pure cobalt of ＞ 99.99%, is placed in 250
In mL beaker, it is blown into bis-water of 10mL, adds 10mL nitric acid (1.2), be heated to cobalt and be completely dissolved, cooling
In rear immigration 1000mL volumetric flask, it is diluted with water to scale, mixing；
(1.14), chromium standard solution: 0.10mg/mL；Weigh 0.1000g；The pure chromium of ＞ 99.98%, is placed in 250
In mL beaker, it is blown into bis-water of 10mL, adds 10mL hydrochloric acid (1.1), be heated to chromium and be completely dissolved, dropping
1.0mL nitric acid (1.2), moves in 1000mL volumetric flask after cooling, is diluted with water to scale, mixing；
(1.15), molybdenum standard solution: 0.10mg/mL；Weigh 0.1000g；The pure molybdenum of ＞ 99.98%, is placed in 250
In mL beaker, add 20mL hydrochloric acid (1.1), 5.0mL nitric acid (1.2), be heated to molybdenum and dissolve completely, cooling
In rear immigration 1000mL volumetric flask, it is diluted with water to scale, mixing；
(1.16), tungsten basal body solution, 1.0mg/mL；Weigh specpure at 800 DEG C of calcination 30min in advance
Tungstic anhydride. 0.6305g, is placed in platinum ware, adds 10mL～15mL sodium hydroxide solution (1.5), heating
Dissolve.It is cooled to room temperature, moves in 500mL volumetric flask, be diluted with water to scale, shake up, then move into and be dried
Storage in plastic bottle；
(1.17) Y Int Std solution, 0.2mg/mL；Weigh 0.1270g, ＞ 99.95% yittrium oxide, be placed in 250
In mL beaker, adding 20mL hydrochloric acid (1.4), low-temperature heat, to dissolving completely, moves into 500mL and holds after cooling
In measuring bottle, add 20mL hydrochloric acid (1.4), be diluted with water to scale, shake up；
(2), sampling and sample preparation；The sample analyzed is sampled and sample preparation according to the requirement of HB/Z 205；
(3), element analysis spectrum line selects:
Prepare serial single solution, 5.0mL tungsten basal body solution (1.12), 8.5mL tungsten basal body solution (1.12),
1.0mL ferrum standard solution (1.8), 1.5mL ferrum standard solution (1.6), 1.0mL nickel standard solution (1.11),
1.5mL nickel standard solution (1.9), 5.0mL copper standard solution (1.12), 5.0mL cobalt standard solution (1.13),
5.0mL chromium standard solution (1.14), 5.0mL molybdenum standard solution (1.15), 15mL hydrochloric acid (1.1), 6mL
Nitric acid (1.2), 10mL phosphoric acid (1.3) and 2.00mL Y Int Std solution (1.13) hold respectively at 100mL
In measuring bottle, respectively by above-mentioned solution 5-6 bar ferrum, nickel analysis spectral line on carry out spectrogram scanning, superposition, therefrom
Choose ferrum 239.562nm；Nickel 231.604nm；As separated time spectral line；
(4), high density tungsten basigamy pouring weight sample dissolution test
Weigh three parts of 0.10g sample, be separately added into 5mL hydrochloric acid and 2mL nitric acid, 10mL hydrochloric acid and 4mL
Nitric acid, 15mL hydrochloric acid and 6mL nitric acid heat on electric furnace, and sample dissolution is incomplete, and solution is muddy；
Weigh three parts of 0.10g sample, be separately added into 1. 5mL hydrochloric acid, 2mL nitric acid and phosphatase 11 0mL phosphoric acid；
2. 10mL hydrochloric acid, 5mL nitric acid and phosphoric acid 20mL phosphoric acid；3. 20mL hydrochloric acid, 3mL nitric acid and phosphoric acid 30mL
Phosphoric acid, sample dissolution is complete, and solution is clarified；
(5), Y Int Std consumption test
Weigh 0.10g sample, be accurate to 0.0001g and be placed in 150mL beaker, addition 20mL phosphoric acid (1.3),
20mL hydrochloric acid (1.1), 5mL nitric acid (1.2), on electric hot plate, slight fever is completely dissolved to test portion；From electric hot plate
Taking off the coldest, blow water walls of beaker, liquor capacity keeps about 50mL, boils dissolved salts；Cooling test solution is to room temperature；
Move in 100mL volumetric flask, be diluted with water to scale, shake up；
20.00mL test solution is pipetted to five 100mL volumetric flasks, respectively at first to the 5th volumetric flask
Middle addition 10mL phosphoric acid (1.3), 10mL hydrochloric acid (1.1), then standard respectively in first to the 5th volumetric flask
Really add 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL Y Int Std solution (1.17), use
Water is diluted to scale, shakes up；Research shows, adds 2.00mL Y Int Std solution measurement result relative standard deviation
Minimum, measures the most stable；
(6), analytical procedure is as follows:
(6.1), test portion: weigh 0.10g sample, be accurate to 0.0001g；
(6.2), blank assay solution: do blank assay in company with test portion；
(6.3) sample solution, is prepared: be placed in 150mL alkene beaker by the test portion of analytical procedure (6.1), add
Entering 20mL phosphoric acid (1.3), 10mL hydrochloric acid (1.1), 4mL nitric acid (1.2), on electric hot plate, slight fever is to test portion
It is completely dissolved；Taking off the coldest from electric hot plate, blow water walls of beaker, liquor capacity keeps about 50mL, boils dissolving
Salt；Cooling test solution is to room temperature；Move in 100mL volumetric flask, be diluted with water to scale, shake up；
Pipette 10.00mL test solution in 100mL volumetric flask, add 10mL phosphoric acid (1.3), 10mL hydrochloric acid (1.1),
Accurately add 2.00mL Y Int Std solution (1.17), dilute to scale with water, shake up；
(6.4) preparation calibration solution；
(6.4.1), low mark solution is prepared；Low by main chemical compositions preparation in tested high density tungsten basigamy pouring weight
Mark solution is as follows；Pipette 10.00mL blank reagent solution (6.2) in 100mL volumetric flask, add 10mL
Phosphoric acid (1.3), 10mL hydrochloric acid (1.1), pipette the tungsten basal body solution (1.16) close with test portion main component W content,
Accurately add 2.00mL Y Int Std solution (1.17), dilute to scale with water, shake up, as low mark solution；
(6.4.2) high standard solution, is prepared；Low by main chemical compositions preparation in tested high density tungsten basigamy pouring weight
Mark solution is as follows；Pipette 10.00mL blank reagent solution (6.2) in 100mL volumetric flask, add 10mL
Phosphoric acid (1.3), 10mL hydrochloric acid (1.1), pipette the tungsten basal body solution (1.16) close with test portion main component W content,
Add 1.50mL ferrum standard solution (1.6), 1.00mL nickel standard solution (1.9), accurately add 2.00mL
Y Int Std solution (1.17), dilute to scale with water, shake up, as high standard solution；
(6.5), ferrum, the concentration of nickel in sample solution is measured；By inductively coupled plasma atomic emission spectrometer
Selected working condition and analysis spectral line, with yttrium as internal standard element, use low mark solution and high standard solution to instrument successively
Device is standardized, and then, measures ferrum, the concentration of nickel in sample solution；
(7), the content of ferrum be 10.24%, the content 9.89% of nickel.
Claims (2)
1. one kind measures the analysis method of ferrum nickel element in high density tungsten basigamy pouring weight, it is characterised in that: use electricity
Sense coupled plasma optical emission spectrogrph, working condition and the analytical line of instrument are as follows: higher frequency: 40.68MHz；
Incident power: 0.95～1.1Kw；Reflection power: ＜ 15W；Argon flow amount: wherein, cooling gas flow 12～
20L/min, sheath throughput 0.1～0.6L/min；Sample lifting capacity: 1.0～1.5ml/min；The time of integration:
1～10s；Elementary analysis line: choose ferrum 239.562nm；Nickel 231.604nm；
(1), the reagent used in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL；Top grade is pure；
(1.2), nitric acid, ρ 1.42g/mL；Top grade is pure；
(1.3), phosphoric acid, ρ 1.69g/mL；Top grade is pure；
(1.4), hydrochloric acid, 1+1；
(1.5) sodium hydroxide solution, 200g/L；
(1.6), ferrum standard solution: 1.00mg/mL；Weigh 1.0000g；＞ 99.99% pure iron, is placed in 300mL
In beaker, it is blown into secondary water 30mL, adds the hydrochloric acid 30mL described in step (1.1), be heated to ferrum the most molten
Solve, move in 1000mL volumetric flask after cooling, be diluted with water to scale, mixing；
(1.7), ferrum standard solution: 0.10mg/mL；Pipette the ferrum standard described in 20.00mL step (1.6) molten
Liquid, is placed in 200mL volumetric flask, adds the hydrochloric acid 5mL described in step (1.1), is diluted with water to scale,
Shake up；
(1.8), ferrum standard solution: 0.01mg/mL；Pipette the ferrum standard described in 20.00mL step (1.7) molten
Liquid, is placed in 200mL volumetric flask, adds the hydrochloric acid 5mL described in step (1.1), is diluted with water to scale,
Shake up；
(1.9), nickel standard solution 1.00mg/mL；Weigh 1.0000g；＞ 99.99% pure nickel, is placed in 300mL
In beaker, it is blown into secondary water 30mL, adds 30mL nitric acid, be heated to nickel and be completely dissolved, after cooling, move into 1000
In mL volumetric flask, it is diluted with water to scale, mixing；
(1.10), nickel standard solution: 0.10mg/mL；Pipette the nickel standard described in 20.00mL step (1.9)
Solution, is placed in 200mL volumetric flask, adds 5mL nitric acid, is diluted with water to scale, shakes up；
(1.11), nickel standard solution: 0.01mg/mL；Pipette the nickel mark described in 20.00mL step (1.10)
Quasi-solution, is placed in 200mL volumetric flask, adds the hydrochloric acid 5mL described in step (1.1), is diluted with water to carve
Degree, shakes up；
(1.12), copper standard solution: 0.10mg/mL；Weigh 0.1000g；＞ 99.99% fine copper, is placed in 250
In mL beaker, it is blown into bis-water of 10mL, adds 10mL nitric acid, be heated to copper and be completely dissolved, move into after cooling
In 1000mL volumetric flask, it is diluted with water to scale, mixing；
(1.13), cobalt standard solution: 0.10mg/mL；Weigh 0.1000g；The pure cobalt of ＞ 99.99%, is placed in 250
In mL beaker, it is blown into bis-water of 10mL, adds 10mL nitric acid, be heated to cobalt and be completely dissolved, move into after cooling
In 1000mL volumetric flask, it is diluted with water to scale, mixing；
(1.14), chromium standard solution: 0.10mg/mL；Weigh 0.1000g；The pure chromium of ＞ 99.98%, is placed in 250
In mL beaker, it is blown into bis-water of 10mL, adds the hydrochloric acid described in 10mL step (1.1), be heated to chromium complete
CL, drips 1.0mL nitric acid, moves in 1000mL volumetric flask, be diluted with water to scale after cooling, mixing；
(1.15), molybdenum standard solution: 0.10mg/mL；Weigh 0.1000g；The pure molybdenum of ＞ 99.98%, is placed in 250
In mL beaker, add the hydrochloric acid described in 20mL step (1.1), 5.0mL nitric acid, be heated to molybdenum and dissolve completely,
Move in 1000mL volumetric flask after cooling, be diluted with water to scale, mixing；
(1.16), tungsten basal body solution, 1.0mg/mL；Weigh specpure at 800 DEG C of calcination 30min in advance
Tungstic anhydride. 0.6305g, is placed in platinum ware, addition 10mL～15mL sodium hydroxide solution, heating for dissolving,
It is cooled to room temperature, moves in 500mL volumetric flask, be diluted with water to scale, shake up, then move into dry plastic bottle
Interior storage；
(1.17) Y Int Std solution, 0.2mg/mL；Weigh 0.1270g, ＞ 99.95% yittrium oxide, be placed in 250
In mL beaker, adding the hydrochloric acid described in 20mL step (1.4), low-temperature heat, to dissolving completely, moves after cooling
Enter in 500mL volumetric flask, add the hydrochloric acid described in 20mL step (1.4), be diluted with water to scale, shake up；
(2), sampling and sample preparation；The sample analyzed is sampled and sample preparation according to the requirement of HB/Z 205；
(3), element analysis spectrum line selects:
Prepare serial single solution, the tungsten basal body solution described in 5.0mL step (1.16), 8.5mL step (1.16)
Described in ferrum standard solution described in described tungsten basal body solution, 1.0mL step (1.8), 1.5mL step (1.6)
Described in nickel standard solution described in ferrum standard solution, 1.0mL step (1.11), 1.5mL step (1.9)
Described in copper standard solution described in nickel standard solution, 5.0mL step (1.12), 5.0mL step (1.13)
Described in chromium standard solution described in cobalt standard solution, 5.0mL step (1.14), 5.0mL step (1.15)
Hydrochloric acid described in molybdenum standard solution, 15mL step (1.1), the nitric acid described in 6mL step (1.2), 10mL
Phosphoric acid described in step (1.3) and the Y Int Std solution described in 2.00mL step (1.17) are respectively at 100mL
In volumetric flask, respectively by above-mentioned solution 5-6 bar ferrum, nickel analysis spectral line on carry out spectrogram scanning, superposition, from
The analytical line that middle Analysis on Selecting signal is strong, matrix in high density balancing weight, co-existing element interference are minimum is composed as separated time
Line；
(4), high density tungsten basigamy pouring weight sample dissolution test
Weigh three parts of 0.10g sample, be separately added into the hydrochloric acid described in 5mL step (1.1) and 2mL nitric acid,
Hydrochloric acid described in 10mL step (1.1) and the hydrochloric acid described in 4mL nitric acid, 15mL step (1.1) and 6mL
Nitric acid heats on electric furnace, and sample dissolution is incomplete, and solution is muddy；
Weigh three parts of 0.10g sample, be separately added into 1. hydrochloric acid described in 5mL step (1.1), 2mL nitric acid
And 10mL phosphoric acid；2. hydrochloric acid, 5mL nitric acid and the 20mL phosphoric acid described in 10mL step (1.1)；③20mL
Hydrochloric acid, 3mL nitric acid and 30mL phosphoric acid described in step (1.1), sample dissolution is complete, and solution is clarified；
(5), Y Int Std consumption test
Weigh 0.10g sample, be accurate to 0.0001g and be placed in 150mL beaker, add 20mL phosphoric acid, 20
Hydrochloric acid described in mL step (1.1), 5mL nitric acid, on electric hot plate, slight fever is completely dissolved to test portion；From electric heating
Taking off the coldest on plate, blow water walls of beaker, liquor capacity keeps about 50mL, boils dissolved salts；Cooling test solution is extremely
Room temperature；Move in 100mL volumetric flask, be diluted with water to scale, shake up；
20.00mL test solution is pipetted to five 100mL volumetric flasks, respectively at first to the 5th volumetric flask
Hydrochloric acid described in middle addition 10mL phosphoric acid and 10mL step (1.1), then in first to the 5th volumetric flask
The most accurately add 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL Y Int Std solution (1.17),
It is diluted with water to scale, shakes up；Research shows, adds 2.00mL Y Int Std solution measurement result relative standard inclined
Difference minimum, measures the most stable；
(6), analytical procedure is as follows:
(6.1), test portion: weigh 0.10g sample, be accurate to 0.0001g；
(6.2), blank assay solution: do blank assay in company with test portion；
(6.3) sample solution, is prepared: be placed in 150mL alkene beaker by the test portion of analytical procedure (6.1), add
Enter the hydrochloric acid described in 10mL～30mL phosphoric acid, 10mL～20mL step (1.1), 3mL～5mL nitric acid,
On electric hot plate, slight fever is completely dissolved to test portion；Taking off the coldest from electric hot plate, blow water walls of beaker, liquor capacity is protected
Hold about 50mL, boil dissolved salts；Cooling test solution is to room temperature；Move in 100mL volumetric flask, be diluted with water to
Scale, shakes up；
Pipette 10.00mL～20.00mL test solution in 100mL volumetric flask, add 5mL～10mL phosphoric acid,
Hydrochloric acid described in 10mL step (1.1), accurately adds the Y Int Std solution described in 2.00mL step (1.17),
Dilute to scale with water, shake up；
(6.4) preparation calibration solution；
(6.4.1), low mark solution is prepared；Low by main chemical compositions preparation in tested high density tungsten basigamy pouring weight
Mark solution is as follows；Pipette the blank assay solution of step described in 10.00mL～20.00mL (6.2) in 100mL
In volumetric flask, add the hydrochloric acid described in 5mL～10mL phosphoric acid, 10mL step (1.1), pipette and test portion master
Want the tungsten basal body solution of the described step (1.16) that composition W content is close, accurately add step described in 2.00mL
(1.17) Y Int Std solution, dilute to scale with water, shake up, as low mark solution；
(6.4.2) high standard solution, is prepared；Low by main chemical compositions preparation in tested high density tungsten basigamy pouring weight
Mark solution is as follows；Pipette the blank assay solution described in 10.00mL～20.00mL step (6.2) in 100mL
In volumetric flask, add the hydrochloric acid described in 5mL～10mL phosphoric acid, 10mL step (1.1), pipette and test portion master
Want the tungsten basal body solution of the described step (1.16) that composition W content is close, add described step (1.6) or (1.7)
Or the ferrum standard solution of (1.8), described step (1.9) or the nickel standard solution of (1.10) or (1.11),
Addition must cover ferrum, nickel element analyst coverage in high density tungsten basigamy pouring weight sample, accurately adds 2.00mL
Y Int Std solution (1.17), dilute to scale with water, shake up, as high standard solution；
(6.5), ferrum, the concentration of nickel in sample solution is measured；By inductively coupled plasma atomic emission spectrometer
Selected working condition and analysis spectral line, with yttrium as internal standard element, use low mark solution and high standard solution to instrument successively
Device is standardized, and then, measures ferrum, the concentration of nickel in sample solution, and must tap a blast furnace nickel percentage composition.
The most according to claim 1 a kind of measure the analysis side of ferrum nickel element in high density tungsten basigamy pouring weight
Method, is characterized in that, uses the standard sample that chemical composition is close, prepares after processing according to (6.1)～(6.3)
Low, high standard solution required for one-tenth.
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| CN112858261A (en) * | 2020-12-31 | 2021-05-28 | 江苏隆达超合金航材有限公司 | Real-time internal standard determination method for content of principal element in nickel-based superalloy |
| CN112834487A (en) * | 2020-12-31 | 2021-05-25 | 江苏隆达超合金航材有限公司 | Method for rapidly determining contents of chromium and iron in nickel-based superalloy by ICP-OES (inductively coupled plasma-optical emission spectrometry) |
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