CN103543136A - Atomic fluorescence method for measuring selenium and tellurium in high-temperature alloy FGH96 - Google Patents
Atomic fluorescence method for measuring selenium and tellurium in high-temperature alloy FGH96 Download PDFInfo
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Abstract
The invention belongs to an alloy trace element analysis technology and relates to a method for measuring selenium and tellurium in a high-temperature alloy FGH96. The method comprises the analysis steps of weighing a test material; preparing a test sample solution; preparing a calibration solution; preparing a low-standard solution; preparing a high-standard solution; measuring the concentration of selenium and the concentration of tellurium in the test sample solution; and calculating according to measured results to obtain the content of selenium and the content of tellurium. The hydride generation atomic fluorescence method provided by the invention is used for measuring the selenium content and the tellurium content in the high-temperature alloy and is high in analysis sensitivity, easy to operate, short in analysis period and high in efficiency. The atomic fluorescence method has wide application prospect and can meet the trend that along with the engineering application of the alloy FGH96, a requirement on the impurity element content is more and more strict, and particularly, the impurities such as selenium and tellurium are controlled strictly. The method can meet requirements of scientific research and production on the quality control of raw materials, reduce the rejection rate of products, and save the development and production costs.
Description
Technical field
The invention belongs to alloy trace element analysis technology, relate to a kind of method of measuring selenium in high temperature alloy FGH96, tellurium content.
Background technology
Demand for engine to high thrust-weight ratio, powder metallurgy superalloy FGH96 is for the crucial hot-end component of engine.In order to improve the degree of purity level of diskware alloy, need strict impurity content, the especially content of low melting point element selenium, tellurium of controlling alloy, improve engine safety in operation and reliability..
Through literature survey, atomic fluorescence technology is analytical technology with Chinese characteristics, in ASTM and foreign literature without correlation analysis content.In high temperature alloy, method for analyzing very small amount of element mainly contains the method that national military standard GJB5404 provides, mainly wherein classical chemical method and part instrumental method, we can use for reference employing instrument analytical method, but must set up the detection method that is applicable to oneself according to the feature for FGH96 alloy material, FGH96 belongs to novel powder alloy, Nb constituent content is higher, if simply apply mechanically the deviation that national military standard GJB5404 may bring testing result.Therefore must determine the impact of above special composition on trace element testing result through experiment, set up the technology of selenium, tellurium content detection in a kind of high temperature alloy FGH96.
According to wanting analytical element kind, content difference, the instrument of conventional trace analysis mainly contains following several: Inductively coupled plasma mass spectrometry (ICP – MS), atomic absorption spectrography (AAS) (AAS.But exist when the low melting point element selenium in ICP-MS analysis FGH96, tellurium, cost is high, the problem of serious interference; While analyzing low melting point element selenium in FGH96, tellurium, there is serious interference, problem that analysis precision is low in AAS.
Summary of the invention
The object of the invention is: propose a kind of hydride-generation atomic fluorescence method of analyzing selenium, tellurium content in sensitive height, the mensuration high temperature alloy FGH96 that easy and simple to handle, analytical cycle is short, efficiency is high.
Technical scheme of the present invention is: a kind of method of measuring selenium in high temperature alloy FGH96, tellurium content, is characterized in that: adopt atomic fluorescence spectrometer, the condition of work of elemental selenium instrument is as follows: photomultiplier negative high voltage: 360V; Atomizer height: 8mm; Lamp current: 80mA; Carrier gas flux: 400ml/mim; Shield gas flow amount: 900ml/mim.Elemental selenium measuring condition is as follows: the reading duration: 10s; Metering system: calibration curve method; Time delay: 1s; Reading mode: peak area integration; Multiplicity: 1 time.The condition of work of elemental tellurium instrument is as follows: photomultiplier negative high voltage: 300V; Atomizer height: 8mm; Lamp current: 80mA; Carrier gas flux: 400ml/mim; Shield gas flow amount: 900ml/mim.Elemental tellurium measuring condition is as follows: the reading duration: 10s; Metering system: calibration curve method; Time delay: 1s; Reading mode: peak area integration; Multiplicity: 1 time.
(1) reagent using in measuring process is as follows:
(1.1) hydrochloric acid, ρ 1.19g/mL; Pure or the MOS level of top grade;
(1.2) nitric acid, ρ 1.42g/mL; Pure or the MOS level of top grade;
(1.3) sulfuric acid, ρ 1.84g/mL; Pure or the MOS level of top grade;
(1.4) hydrofluorite, ρ 1.15g/mL; Pure or the MOS level of top grade;
(1.5) citric acid solution, 400g/L;
(1.6) NaOH, solid, top grade is pure;
(1.7) sodium hydroxide solution, 100g/L(is stored in plastic bottle);
Take 100g NaOH (1.6) and be placed in 500mL beaker, add after dissolve complete, move in 1000mL volumetric flask, be diluted with water to scale, mix.
(1.8) potassium borohydride, solid, top grade is pure;
(1.9) solution of potassium borohydride; 12g/L;
Take 5g NaOH (1.6) and be placed in 200mL beaker, after dissolve complete, add 12g potassium borohydride (1.8), add after dissolve complete, move in 100mL volumetric flask, be diluted with water to scale, mix, the used time now joins.
(1.10) nitric acid, (1+1);
(1.11) chloroazotic acid, (1+3);
(1.12) selenium standard solution A:0.10mg/mL;
Take 0.1000g pure selenium (massfraction is not less than 99.99%) in 100mL beaker, add 10mL hydrochloric acid (1.1), in water-bath, heating for dissolving is complete, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes.
(1.13) selenium standard solution B:0.01mg/mL;
Pipette 25.00mL selenium standard solution A(1.12) in 250mL volumetric flask, add 10mL hydrochloric acid (1.1), be diluted with water to scale, mix;
(1.14) selenium standard solution C:0.001mg/mL;
Pipette 25.00mL selenium standard solution B(1.13) in 250mL volumetric flask, add 10mL hydrochloric acid (1.1), be diluted with water to scale, mix;
(1.15) tellurium standard solution A:0.10mg/mL.
Take 0.1000 gram of the pure tellurium of metal (massfraction is not less than 99.99%), be placed in 150ml beaker, add 20mL nitric acid (1.2), low-temperature heat adds 10mL sulfuric acid (1.3) after dissolving, and is evaporated to and smolders, slightly cold, with a small amount of water, rinse wall of cup, cooling after, add 20～30mL Water dissolve salt class, be cooled to room temperature, move in 1000ml volumetric flask, be diluted with water to scale, mix.
(1.16) tellurium standard solution B:0.01mg/mL;
Pipette 25.00mL tellurium standard solution A(1.15) in 250mL volumetric flask, add 10mL chloroazotic acid (1.10), be diluted with water to scale, mix;
(1.17) tellurium standard solution C:0.001mg/mL;
Pipette 25.00mL tellurium standard solution B(1.16) in 250mL volumetric flask, add 10mL chloroazotic acid, be diluted with water to scale, mix;
(1.18) nickel standard solution solution: 10mg/mL;
Take 1.0000 grams of metallic nickels (massfraction is not less than 99.99%), be placed in 150ml beaker, add nitric acid (1.10), after heating for dissolving, cooling, move in 100ml volumetric flask, be diluted with water to scale, mix.
(2) sampling and sample preparation; The sample of analyzing use samples and sample preparation according to the requirement of HB/Z205;
(3) analytical procedure is as follows:
(3.1) test portion: take 0.10g test portion, be accurate to 0.0001g;
(3.2) prepare sample solution:
(3.2.1) prepare sample solution: the test portion of analytical procedure (3.1) is placed in to 100mL beaker, adds 20mL hydrochloric acid (1.1), 5mL nitric acid (1.2) to heat, and drip 1～1.5mL hydrofluorite (1.4), heating for dissolving on low-temperature furnace.Add 5mL citric acid solution (1.6), heating is boiled, slightly cold, adds 10mL hydrochloric acid (1.1), low-grade fever, cooling after, test solution is moved in 50mL volumetric flask, be diluted with water to scale, mix.
(3.2.2) blank test: do blank test with same analytical procedure and identical reagent are parallel with test portion.
(3.3) preparation standard solution and carrier fluid:
(3.3.1) preparation of working curve solution
In several 100mL beakers, all add 9mL nickel standard solution solution (1.18) to synchronize and process with sample, then add respectively 0,0.50,1.00,2.00,5.00 selenium C(1.14), tellurium C(1.17) standard solution.
(3.3.2) preparation of carrier fluid
In 500mL beaker, add 240mL water, then add 160mL hydrochloric acid, mix, be cooled to room temperature.
(3.4) measure
Press condition of work selected in 1 and set atomic fluorescence spectrometer, measure successively blank test (3.2.2), standard serial solution (3.3.1) and sample solution, take solution concentration as horizontal ordinate, take fluorescence intensity as ordinate, drawing curve is also printed.
(3.5) by instrument, directly provide analysis result
Described preparation calibration curve solution is mixed with needed calibration curve solution to substitute (3.3.1) calibration curve solution after using the approaching standard model of chemical composition to process according to (3.1)～(3.2).
Advantage of the present invention is:
1) elemental selenium, tellurium measurement are highly sensitive, and selectivity is good, detection limit selenium 0.000003, tellurium 0.000005%; .This detection limit, greatly owing to using other equipment in the past, has met the high performance requirements of FGH96 alloy;
2) method measurement range is wide, under selenium measurement, is limited to 0.00003%, is limited to 0.002% in measurement; Under tellurium measurement, be limited to 0.00005%, in measurement, be limited to 0.002%; This measurement range can the several orders of magnitude of one-shot measurement content, having reduced some method needs bigness scale, then again prepares the troublesome operation of curve.
3) instrument that this method adopts is that domestic equipment price is low, only have the prices such as equipment I CP of other test trace elements or GDMS tens of/mono-; Low to environmental requirement, do not need to set up ultrapure test bay; Laboratory maintenance cost is low, does not need constant temperature and humidity, only needs common laboratory to safeguard just passable;
4) the method is measured fast, easy and simple to handle, from processing sample to measurement, can test tens bag Duplicate Samples, save a large amount of man power and materials for one batch.
Embodiment
Embodiment mono-
1, the atomic fluorescence technology of measuring selenium, tellurium in high temperature alloy FGH96, is characterized in that: adopt atomic fluorescence spectrometer, the condition of work of elemental selenium instrument is as follows: photomultiplier negative high voltage: 360V; Atomizer height: 8mm; Lamp current: 80mA; Carrier gas flux: 400ml/mim; Shield gas flow amount: 900ml/mim.Elemental selenium measuring condition is as follows: the reading duration: 10s; Metering system: calibration curve method; Time delay: 1s; Reading mode: peak area integration; Multiplicity: 1 time.The condition of work of elemental tellurium instrument is as follows: photomultiplier negative high voltage: 300V; Atomizer height: 8mm; Lamp current: 80mA; Carrier gas flux: 400ml/mim; Shield gas flow amount: 900ml/mim.Elemental tellurium measuring condition is as follows: the reading duration: 10s; Metering system: calibration curve method; Time delay: 1s; Reading mode: peak area integration; Multiplicity: 1 time.
(1) reagent using in mensuration process is as follows:
(1.1) hydrochloric acid, ρ 1.19g/mL; Pure or the MOS level of top grade;
(1.2) nitric acid, ρ 1.42g/mL; Pure or the MOS level of top grade;
(1.3) sulfuric acid, ρ 1.84g/mL; Pure or the MOS level of top grade;
(1.4) hydrofluorite, ρ 1.15g/mL; Pure or the MOS level of top grade;
(1.5) citric acid solution, 400g/L;
(1.6) NaOH, solid, top grade is pure;
(1.7) sodium hydroxide solution, 100g/L(is stored in plastic bottle);
Take 100g NaOH (1.6) and be placed in 500mL beaker, add after dissolve complete, move in 1000mL volumetric flask, be diluted with water to scale, mix.
(1.8) potassium borohydride, solid, top grade is pure;
(1.9) solution of potassium borohydride; 12g/L;
Take 5g NaOH (1.6) and be placed in 200mL beaker, after dissolve complete, add 12g potassium borohydride (1.8), add after dissolve complete, move in 100mL volumetric flask, be diluted with water to scale, mix, the used time now joins.
(1.10) nitric acid, (1+1);
(1.11) chloroazotic acid, (1+3);
(1.12) selenium standard solution A:0.10mg/mL;
Take 0.1000g pure selenium (massfraction is not less than 99.99%) in 100mL beaker, add 10mL hydrochloric acid (1.1), in water-bath, heating for dissolving is complete, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes.
(1.13) selenium standard solution B:0.01mg/mL;
Pipette 25.00mL selenium standard solution A(1.12) in 250mL volumetric flask, add 10mL hydrochloric acid (1.1), be diluted with water to scale, mix;
(1.14) selenium standard solution C:0.001mg/mL;
Pipette 25.00mL selenium standard solution B(1.13) in 250mL volumetric flask, add 10mL hydrochloric acid (1.1), be diluted with water to scale, mix;
(1.15) tellurium standard solution A:0.10mg/mL.
Take 0.1000 gram of the pure tellurium of metal (massfraction is not less than 99.99%), be placed in 150ml beaker, add 20mL nitric acid (1.2), low-temperature heat adds 10mL sulfuric acid (1.3) after dissolving, and is evaporated to and smolders, slightly cold, with a small amount of water, rinse wall of cup, cooling after, add 20～30mL Water dissolve salt class, be cooled to room temperature, move in 1000ml volumetric flask, be diluted with water to scale, mix.
(1.16) tellurium standard solution B:0.01mg/mL;
Pipette 25.00mL tellurium standard solution A(1.15) in 250mL volumetric flask, add 10mL chloroazotic acid (1.10), be diluted with water to scale, mix;
(1.17) tellurium standard solution C:0.001mg/mL;
Pipette 25.00mL tellurium standard solution B(1.16) in 250mL volumetric flask, add 10mL chloroazotic acid, be diluted with water to scale, mix;
(1.18) nickel standard solution solution: 10mg/mL;
Take 1.0000 grams of metallic nickels (massfraction is not less than 99.99%), be placed in 150ml beaker, add nitric acid (1.10), after heating for dissolving, cooling, move in 100ml volumetric flask, be diluted with water to scale, mix.
(2) sampling and sample preparation; The sample of analyzing use samples and sample preparation according to the requirement of HB/Z205;
(3) analytical procedure is as follows:
(3.1) test portion: take 0.10g test portion, be accurate to 0.0001g;
(3.2) prepare sample solution:
(3.2.1) prepare sample solution: the test portion of analytical procedure (3.1) is placed in to 100mL beaker, adds 20mL hydrochloric acid (1.1), 5mL nitric acid (1.2) to heat, and drip 1～1.5mL hydrofluorite (1.4), heating for dissolving on low-temperature furnace.Add 5mL citric acid solution (1.6), heating is boiled, slightly cold, adds 10mL hydrochloric acid (1.1), low-grade fever, cooling after, test solution is moved in 50mL volumetric flask, be diluted with water to scale, mix.
(3.3) preparation calibration solution and carrier fluid:
(3.3.1) preparation of calibration curve solution
In several 100mL beakers, all add 9mL nickel standard solution solution (1.17) to synchronize and process with sample, then add respectively 0,0.50,1.00,2.00,5.00 selenium C(1.14), tellurium C(1.17) standard solution.
(3.3.2) preparation of carrier fluid
In 500mL beaker, add 240mL water, then add 160mL hydrochloric acid, mix, be cooled to room temperature.
(3.4) measure
Press condition of work selected in 1 and set atomic fluorescence spectrometer, Measurement and calibration series solution (3.3.1) and sample solution, take solution concentration as horizontal ordinate successively, take fluorescence intensity as ordinate, and drawing curve is also printed.Computation and measurement result, obtains selenium, tellurium content; The content of selenium, tellurium is respectively 0.00008 and 0.00006, add the recovery be respectively 114% and 85%, RSD be respectively 4.7 and 8.3, result meets the demands.
Claims (2)
1. an atomic fluorescence method of measuring selenium, tellurium in high temperature alloy FGH96, is characterized in that: adopt atomic fluorescence spectrometer, the condition of work of measuring elemental selenium instrument is as follows: photomultiplier negative high voltage: 360V; Atomizer height: 8mm; Lamp current: 80mA; Carrier gas flux: 400ml/mim; Shield gas flow amount: 900ml/mim; Elemental selenium measuring condition is as follows: the reading duration: 10s; Metering system: calibration curve method; Time delay: 1s; Reading mode: peak area integration; Multiplicity: 1 time.The condition of work of measuring elemental tellurium instrument is as follows: photomultiplier negative high voltage: 300V; Atomizer height: 8mm; Lamp current: 80mA; Carrier gas flux: 400ml/mim; Shield gas flow amount: 900ml/mim.Measure elemental tellurium measuring condition as follows: the reading duration: 10s; Metering system: calibration curve method; Time delay: 1s; Reading mode: peak area integration; Multiplicity: 1 time;
(1) reagent using in measuring process is as follows:
(1.1) hydrochloric acid, ρ 1.19g/mL; Pure or the MOS level of top grade;
(1.2) nitric acid, ρ 1.42g/mL; Pure or the MOS level of top grade;
(1.3) sulfuric acid, ρ 1.84g/mL; Pure or the MOS level of top grade;
(1.4) hydrofluorite, ρ 1.15g/mL; Pure or the MOS level of top grade;
(1.5) citric acid solution, 400g/L;
(1.6) NaOH, solid, top grade is pure;
(1.7) sodium hydroxide solution, 100g/L;
Take 100g NaOH and be placed in 500mL beaker, add after dissolve complete, move in 1000mL volumetric flask, be diluted with water to scale, mix;
(1.8) potassium borohydride, solid, top grade is pure;
(1.9) solution of potassium borohydride; 12g/L;
Take 5g NaOH and be placed in 200mL beaker, after dissolve complete, add 12g potassium borohydride, add after dissolve complete, move in 100mL volumetric flask, be diluted with water to scale, mix, the used time now joins.
(1.10) nitric acid, (1+1);
(1.11) chloroazotic acid, (1+3);
(1.12) selenium standard solution A:0.10mg/mL;
Take massfraction and be not less than 99.99% 0.1000g pure selenium in 100mL beaker, add 10mL hydrochloric acid (1.1), in water-bath, heating for dissolving is complete, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.13) selenium standard solution B:0.01mg/mL;
Pipette 25.00mL selenium standard solution A(1.12) in 250mL volumetric flask, add 10mL hydrochloric acid (1.1), be diluted with water to scale, mix;
(1.14) selenium standard solution C:0.001mg/mL;
Pipette 25.00mL selenium standard solution B(1.13) in 250mL volumetric flask, add 10mL hydrochloric acid (1.1), be diluted with water to scale, mix;
(1.15) tellurium standard solution A:0.10mg/mL;
Take massfraction and be not less than 0.1000 gram of 99.99% the pure tellurium of metal, be placed in 150ml beaker, add 20mL nitric acid (1.2), low-temperature heat adds 10mL sulfuric acid (1.3) after dissolving, and is evaporated to and smolders, slightly cold, with a small amount of water, rinse wall of cup, cooling after, add 20～30mL Water dissolve salt class, be cooled to room temperature, move in 1000ml volumetric flask, be diluted with water to scale, mix.
(1.16) tellurium standard solution B:0.01mg/mL;
Pipette 25.00mL tellurium standard solution A(1.15) in 250mL volumetric flask, add 10mL chloroazotic acid (1.10), be diluted with water to scale, mix;
(1.17) tellurium standard solution C:0.001mg/mL;
Pipette 25.00mL tellurium standard solution B(1.16) in 250mL volumetric flask, add 10mL chloroazotic acid, be diluted with water to scale, mix;
(1.18) nickel standard solution solution: 10mg/mL;
Take massfraction and be not less than 1.0000 grams of 99.99% metallic nickels, be placed in 150ml beaker, add nitric acid (1.10), after heating for dissolving, cooling, move in 100ml volumetric flask, be diluted with water to scale, mix;
(2) sampling and sample preparation; The sample of analyzing use samples and sample preparation according to the requirement of HB/Z205;
(3) analytical procedure is as follows:
(3.1) test portion: take 0.10g test portion, be accurate to 0.0001g;
(3.2) prepare sample solution:
(3.2.1) prepare sample solution: the test portion of analytical procedure (3.1) is placed in to 100mL beaker, adds 20mL hydrochloric acid (1.1), 5mL nitric acid (1.2) to heat, and drip 1～1.5mL hydrofluorite (1.4), heating for dissolving on low-temperature furnace.Add 5mL citric acid solution (1.6), heating is boiled, slightly cold, adds 10mL hydrochloric acid (1.1), low-grade fever, cooling after, test solution is moved in 50mL volumetric flask, be diluted with water to scale, mix;
(3.2.2) blank test: do blank test with same analytical procedure and identical reagent are parallel with test portion;
(3.3) preparation standard solution and carrier fluid:
(3.3.1) preparation of working curve solution
In several 100mL beakers, all add 9mL nickel standard solution solution (1.18) to synchronize and process with sample, then add respectively 0,0.50,1.00,2.00,5.00 selenium C(1.14), tellurium C(1.17) standard solution;
(3.3.2) preparation of carrier fluid
In 500mL beaker, add 240mL water, then add 160mL hydrochloric acid, mix, be cooled to room temperature;
(3.4) measure
Press condition of work selected in 1 and set atomic fluorescence spectrometer, measure successively blank test (3.2.2), standard serial solution (3.3.1) and sample solution, take solution concentration as horizontal ordinate, take fluorescence intensity as ordinate, drawing curve is also printed;
(3.5) by instrument, directly provide analysis result.
2. a kind of atomic fluorescence technology of measuring selenium, tellurium in high temperature alloy FGH96 according to claim 1, its feature is being to prepare after low high standard solution also can be used the approaching standard model of chemical composition to process according to (3.1)～(3.2) and be mixed with needed low high standard solution.
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| CN108680561A (en) * | 2018-04-26 | 2018-10-19 | 长春黄金研究院有限公司 | A kind of method that efficiently and accurately measures selen-tellurjum content in ore |
| CN108844928A (en) * | 2018-04-27 | 2018-11-20 | 长春黄金研究院有限公司 | A kind of method of tellurium content in rapid and accurate determination geology sample |
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Application publication date: 20140129 |