CN103411937B - A kind of AFS DETERMINATION is containing the analytical approach of tellurium in tantalum high temperature alloy - Google Patents
A kind of AFS DETERMINATION is containing the analytical approach of tellurium in tantalum high temperature alloy Download PDFInfo
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Abstract
The invention belongs to alloy trace element analysis technology, relate to the analytical approach of AFS DETERMINATION containing tellurium in tantalum high temperature alloy.The present invention adopts standard addition method namely to take to add hydrochloric acid, nitric acid containing the some parts of tantalum high temperature alloy test portion, and on electric hot plate, low-grade fever is dissolved completely to test portion; Add citric acid solution, heating is boiled; Solution is moved in 50mL volumetric flask, add tellurium standard solution successively, be diluted to scale with water, shake up.The present invention's Standard entertion and add the method for citric acid solution, eliminates matrix element nickel and coexistence elements tantalum, cobalt to the interference of tellurium.By carrying out interference experiment, have found interference element, eliminating the interference of each element to tellurium measurement, improve the accuracy of measurement; Method measurement range is wide, and it is 0.00005% that measurement is rolled off the production line, and measuring the upper limit is 0.0005%, and adopt synchronous process sample and Standard entertion working curve measurement tellurium, analytical error is minimum, and method is reproducible; Utilize this law directly to measure, need not be separated.
Description
Technical field
The invention belongs to alloy trace element analysis technology, relate to the analytical approach of AFS DETERMINATION containing tellurium in tantalum high temperature alloy.
Background technology
High temperature alloy has higher elevated temperature strength due to it, good anti-oxidant and hot corrosion resistance, the combination properties such as good fatigue behaviour, fracture toughness, plasticity, are mainly used in aeromotor, rocket engine and gas turbine high temperature hot-end component material.
In view of the importance of high temperature alloy purposes, tight to high temperature alloy quality control, be that other metal materials are unexistent more than test item.The chemical element of high temperature alloy, except Main elements, has certain requirement to the content of gas oxygen, nitrogen, hydrogen and trace, Determination of Trace Selenium, tellurium, arsenic, bismuth, lead and other elements.In alloy, the element such as oxygen, nitrogen, hydrogen, bismuth, tellurium, selenium, lead, thallium is low melting point objectionable impurities, and the existence of element can have a strong impact on the performance of alloy, will have an immense impact on once exceed allowed band in alloy to material property.Therefore the content of analytical approach to these elements accurately and reliably must be adopted to measure, guarantee quality of materials.
Tellurium element studies its analytical approach as a kind of objectionable impurities becomes a job highly significant.The analyzing detecting method of Determination of Trace Te mainly contains: Extraction and back extraction separation and concentration one By Hg-afs, extracts a graphite oven atomic absorption, extracts a polarography, extraction spectrophotometric method, extraction flame atomic absorption method etc.Find out from said method, most of method for first to extract, then adopts flame atomic absorption method, graphite oven atomic absorption, By Hg-afs and photometry to measure.As everyone knows, extraction means complex operation, the test period is long, and it is large that the analysis for trace element exists the possibility polluted.Hydride-generation atomic fluorescence method has higher sensitivity for the measurement of tellurium, the interference of the element such as matrix nickel and the tantalum that coexists, cobalt, chromium can be eliminated by standard addition method, substantially realize the noiseless AFS DETERMINATION of tellurium, method is highly sensitive, and accuracy is good.
The object of the invention is: propose that a kind of analytical element content is low, wide ranges, accurately can carry out containing trace tellurium element in tantalum high temperature alloy analytical approach.
Technical scheme of the present invention is: adopt atomic fluorescence emission spectrometer, the measuring condition of instrument is as follows: atomic fluorescence emission spectrometer measuring condition, photomultiplier negative high voltage 340V ~ 380V; Atomization temperature 800 DEG C ~ 840 DEG C; Stove height 6.0mm ~ 10.0mm; Flow rate of carrier gas 500mL/min ~ 700mL/min; Shield gas flow speed 800mL/min ~ 1000mL/min; Lamp current 50mA ~ 80mA; Be equipped with the special hollow cathode lamp of tellurium, analytical line is 214.3nm;
(1) 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), perchloric acid, ρ 1.67g/mL; Top grade is pure;
(1.4), nitric acid, 1+1; Top grade is pure;
(1.5), citric acid solution, 400g/L;
Take 200g citric acid to be dissolved in 200mL water, being diluted with water to volume is 500mL;
(1.6), solution of potassium borohydride: 16g/L; In the sodium hydroxide solution of 4g/L, matching while using;
Take 2g NaOH to be dissolved in 500mL water, then add 8.0g potassium borohydride, shake is dissolved, if there is muddiness, filters rear use;
(1.7), tellurium standard solution A:0.100mg/mL; Take 0.1000g; > 99.995% tellurium powder, is placed in 100mL beaker, slowly adds 10mL nitric acid (1.4), heating for dissolving, after entirely molten, slightly cold, add 2mL perchloric acid (1.3), continue to be heated to emit white cigarette, take off slightly cold, add about 10mL water, heating for dissolving salt, take off after all dissolving, be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, shake up;
(1.8), tellurium standard solution B, 10.0 μ g/mL; Pipette 20.00mL tellurium standard solution A (1.7) in 200mL volumetric flask, add 10mL nitric acid (1.4), be diluted with water to scale, shake up;
(1.9), tellurium standard solution C, 1.0 μ g/mL; Pipette 20.00mL tellurium standard solution B (1.8) in 200mL volumetric flask, add 10mL nitric acid (1.4), be diluted with water to scale, shake up;
(1.10), tellurium standard solution D, 0.1 μ g/mL, matching while using; Pipette 20.00mL tellurium standard solution C (1.9) in 200mL volumetric flask, add 10mL nitric acid (1.4), be diluted with water to scale, shake up;
(1.11), nickel solution, 20mg/mL; Take 10.00g; > 99.99% metallic nickel, adds 65mL nitric acid (1.4), heating for dissolving, boils expeling nitrogen oxide, cooling, moves in 500mL volumetric flask, is diluted with water to scale, shakes up;
(1.12), cobalt liquor: 5mg/mL; Take 2.50g; > 99.98% metallic cobalt, adds 20mL nitric acid (1.4), and low-temperature heat is dissolved, and cooling moves in 500mL volumetric flask, is diluted with water to scale, shakes up;
(1.13), carrier fluid; In the port grinding bottle of 500mL, add 240mL water, then add 160mL hydrochloric acid (1.1), shake up, be cooled to room temperature, for subsequent use;
(2), sampling and sample preparation; The sample analyzed carries out sampling and sample preparation according to the requirement of HB/Z205;
(3) prepare before, analyzing
Co-existing element interference, 65 milligrams-85 milligrams, nickel, chromium 5 milligrams-30 milligrams, molybdenum are less than 20 milligrams, titanium is less than 15 milligrams, tantalum is less than 10 milligrams, hafnium is less than 10 milligrams, tantalum is less than 10 milligrams, tungsten is less than 15 milligrams, manganese tantalum is less than 7 milligrams;
Solution of potassium borohydride, matching while using;
(4), analytical procedure is as follows:
(4.1), test portion: take 0.10g sample, be accurate to 0.0001g;
(4.2), blank test solution: do blank test in company with test portion;
(4.3), prepare sample solution: the test portion of analytical procedure (4.1) is placed in 100mL beaker, add 15mL ~ 25mL hydrochloric acid (1.1), 1mL ~ 1.5mL nitric acid (1.2), on electric hot plate, low-grade fever is dissolved completely to test portion; Take off slightly cold from electric hot plate, add 5mL citric acid solution (1.5), electric furnace voltage is adjusted to 200V, and heating is boiled; Solution, to room temperature, moves in 50mL volumetric flask, is diluted with water to scale, shake up by cooling test solution;
(4.4), preparation standard adds working curve solution
(4.4.1) test portion Standard entertion working curve solution, is prepared; Take containing tantalum high temperature alloy test portion in 100 mL beakers, add 15mL ~ 25mL hydrochloric acid (1.1), 1mL ~ 1.5mL nitric acid (1.2), on electric hot plate, low-grade fever is dissolved completely to test portion; Take off slightly cold from electric hot plate, add 5mL citric acid solution (1.5), electric furnace voltage is adjusted to 200V, and heating is boiled; Solution, to room temperature, moves in 50mL volumetric flask, adds 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL tellurium standard solution (1.10) successively, be diluted to scale, shake up with water by cooling test solution;
(4.4.2) reagent blank Standard entertion working curve solution, is prepared; Prepare reagent blank with sample operation repetitive, add 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL tellurium standard solution (1.10) successively, be diluted to scale with water, shake up, the Standard entertion serial solution of preparation reagent blank;
(4.5) concentration of tellurium in test solution, is measured, by condition of work, pump line parameter and injection procedure that atomic fluorescence emission spectrometer, Generation-Atomic Fluorescence Spectrometry hydride generator are selected, pump line parameter, passage A sample or carrier fluid solution, bore 2mm, channel B reductant solution, bore 1mm, channel C waste liquid, bore 2mm, on atomic fluorescence emission spectrometer, with special tellurium hollow cathode lamp, at Te214.3nm wavelength place, injection procedure setting steps one: sample feeding pipe inserts sample solution, stops 6 ~ 10 seconds through passage A, revolution speed 90rpm ~ 110rpm, meanwhile, reductive agent solution of potassium borohydride, stops 6 ~ 10 seconds through channel B, revolution speed 90rpm ~ 110rpm, now sample solution and reductive agent just enter the endless tube end of sample storage tube, step 2, pump stall 6 seconds, step 3, sample feeding pipe is transferred in current-carrying solution, stop 12 ~ 16 seconds through passage A, revolution speed 100rpm ~ 120rpm, import solution of potassium borohydride (1.6), carrier fluid (1.13) and solution (4.2) (4.3) (4.4), atomic fluorescence spectrometry is adopted to measure the atomic fluorescence intensity of tellurium in reagent blank Standard entertion working curve solution and test portion Standard entertion working curve solution, draw reagent blank Standard entertion working curve and test portion Standard entertion working curve respectively, reagent blank Standard entertion working curve checks in the Te quality of reagent blank, test portion Standard entertion working curve checks in the Te quality of test portion, deduct the Te quality of reagent blank by the Te quality of the test portion checked in, converting with following formula obtains Te content in the test portion recorded as atomic fluorescence spectrometry,
In formula:
M
1---the quality of the tellurium element checked on working curve, unit is microgram;
The quality of m---test portion, unit is gram.
Use the standard solution of same single treatment to measure the same trade mark test solution that front and back process for twice respectively, control final sample solution volume and unanimously namely control solution acidity unanimously, reduce analytical error.
Advantage of the present invention is:
1) the present invention adopts standard addition method namely to take to add hydrochloric acid, nitric acid containing the some parts of tantalum high temperature alloy test portion, and on electric hot plate, low-grade fever is dissolved completely to test portion; Add citric acid solution, heating is boiled; Solution is moved in 50mL volumetric flask, add tellurium standard solution successively, be diluted to scale with water, shake up.The present invention's Standard entertion and add the method for citric acid solution, eliminates matrix element nickel and coexistence elements tantalum, cobalt to the interference of tellurium.
2) by carrying out interference experiment, have found interference element, eliminating the interference of each element to tellurium measurement, improve the accuracy of measurement;
3) method measurement range is wide, and it is 0.00005% that measurement is rolled off the production line, and measuring the upper limit is 0.0005%, differs an order of magnitude;
4) adopt synchronous process sample and Standard entertion working curve to measure tellurium, analytical error is minimum, and method is reproducible;
5) hydride-generation atomic fluorescence method has higher sensitivity and is applicable to trace tellurium de-termination;
6) utilize this law directly to measure, need not be separated;
7) addition 0.00005%-0.0005%, the recovery 85%, relative standard deviation is less than 15%, and the recovery, precision are better;
8) reviewed by the analysis of standard model, method and shown that made fixed analytical approach accuracy is good with the comparison of other unit analysis result, method is stablized, and meets the requirement of trace analysis completely.
9) the application's method is measured fast, easy and simple to handle, has saved a large amount of man power and material.
Embodiment
Embodiment one
Measure tellurium content in DZ125 high temperature alloy, adopt atomic fluorescence emission spectrometer, the measuring condition of instrument is as follows: atomic fluorescence emission spectrometer measuring condition, photomultiplier negative high voltage 340V ~ 380V; Atomization temperature 800 DEG C ~ 840 DEG C; Stove height 6.0mm ~ 10.0mm; Flow rate of carrier gas 500mL/min ~ 700mL/min; Shield gas flow speed 800mL/min ~ 1000mL/min; Lamp current 50mA ~ 80mA; Be equipped with the special hollow cathode lamp of tellurium, analytical line is 214.3nm;
(1) 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), perchloric acid, ρ 1.67g/mL; Top grade is pure;
(1.4), nitric acid, 1+1; Top grade is pure;
(1.5), citric acid solution, 400g/L;
Take 200g citric acid to be dissolved in 200mL water, being diluted with water to volume is 500mL;
(1.6), solution of potassium borohydride: 16g/L; In the sodium hydroxide solution of 4g/L, matching while using;
Take 2g NaOH to be dissolved in 500mL water, then add 8.0g potassium borohydride, shake is dissolved, if there is muddiness, filters rear use;
(1.7), tellurium standard solution A:0.100mg/mL; Take 0.1000g; > 99.995% tellurium powder, is placed in 100mL beaker, slowly adds 10mL nitric acid (1.4), heating for dissolving, after entirely molten, slightly cold, add 2mL perchloric acid (1.3), continue to be heated to emit white cigarette, take off slightly cold, add about 10mL water, heating for dissolving salt, take off after all dissolving, be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, shake up;
(1.8), tellurium standard solution B, 10.0 μ g/mL; Pipette 20.00mL tellurium standard solution A (1.7) in 200mL volumetric flask, add 10mL nitric acid (1.4), be diluted with water to scale, shake up;
(1.9), tellurium standard solution C, 1.0 μ g/mL; Pipette 20.00mL tellurium standard solution B (1.8) in 200mL volumetric flask, add 10mL nitric acid (1.4), be diluted with water to scale, shake up;
(1.10), tellurium standard solution D, 0.1 μ g/mL, matching while using; Pipette 20.00mL tellurium standard solution C (1.9) in 200mL volumetric flask, add 10mL nitric acid (1.4), be diluted with water to scale, shake up;
(1.11), nickel solution, 20mg/mL; Take 10.00g; > 99.99% metallic nickel, adds 65mL nitric acid (1.4), heating for dissolving, boils expeling nitrogen oxide, cooling, moves in 500mL volumetric flask, is diluted with water to scale, shakes up;
(1.12), cobalt liquor: 5mg/mL; Take 2.50g; > 99.98% metallic cobalt, adds 20mL nitric acid (1.4), and low-temperature heat is dissolved, and cooling moves in 500mL volumetric flask, is diluted with water to scale, shakes up;
(1.13), carrier fluid; In the port grinding bottle of 500mL, add 240mL water, then add 160mL hydrochloric acid (1.1), shake up, be cooled to room temperature, for subsequent use;
(2), sampling and sample preparation; The sample analyzed carries out sampling and sample preparation according to the requirement of HB/Z205;
(3) prepare before, analyzing
Co-existing element interference, 65 milligrams-85 milligrams, nickel, chromium 5 milligrams-30 milligrams, molybdenum are less than 20 milligrams, titanium is less than 15 milligrams, tantalum is less than 10 milligrams, hafnium is less than 10 milligrams, tantalum is less than 10 milligrams, tungsten is less than 15 milligrams, manganese tantalum is less than 7 milligrams;
Solution of potassium borohydride, matching while using;
(4), analytical procedure is as follows:
(4.1), test portion: take 0.10g sample, be accurate to 0.0001g;
(4.2), blank test solution: do blank test in company with test portion;
(4.3), prepare sample solution: the test portion of analytical procedure (4.1) is placed in 100mL beaker, add 15mL ~ 25mL hydrochloric acid (1.1), 1mL ~ 1.5mL nitric acid (1.2), on electric hot plate, low-grade fever is dissolved completely to test portion; Take off slightly cold from electric hot plate, add 5mL citric acid solution (1.5), electric furnace voltage is adjusted to 200V, and heating is boiled; Solution, to room temperature, moves in 50mL volumetric flask, is diluted with water to scale, shake up by cooling test solution;
(4.4), preparation standard adds working curve solution
(4.4.1) test portion Standard entertion working curve solution, is prepared; Take containing tantalum high temperature alloy test portion in 100mL beaker, add 15mL ~ 25mL hydrochloric acid (1.1), 1mL ~ 1.5mL nitric acid (1.2), on electric hot plate, low-grade fever is dissolved completely to test portion; Take off slightly cold from electric hot plate, add 5mL citric acid solution (1.5), electric furnace voltage is adjusted to 200V, and heating is boiled; Solution, to room temperature, moves in 50mL volumetric flask, adds 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL tellurium standard solution (1.10) successively, be diluted to scale, shake up with water by cooling test solution;
(4.4.2) reagent blank Standard entertion working curve solution, is prepared; Prepare reagent blank with sample operation repetitive, add 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL tellurium standard solution (1.10) successively, be diluted to scale with water, shake up, the Standard entertion serial solution of preparation reagent blank;
(4.5) concentration of tellurium in test solution, is measured, by condition of work, pump line parameter and injection procedure that atomic fluorescence emission spectrometer, Generation-Atomic Fluorescence Spectrometry hydride generator are selected, pump line parameter, passage A sample or carrier fluid solution, bore 2mm, channel B reductant solution, bore 1mm, channel C waste liquid, bore 2mm, on atomic fluorescence emission spectrometer, with special tellurium hollow cathode lamp, at Te214.3nm wavelength place, injection procedure setting steps one: sample feeding pipe inserts sample solution, stops 6 ~ 10 seconds through passage A, revolution speed 90rpm ~ 110rpm, meanwhile, reductive agent solution of potassium borohydride, stops 6 ~ 10 seconds through channel B, revolution speed 90rpm ~ 110rpm, now sample solution and reductive agent just enter the endless tube end of sample storage tube, step 2, pump stall 6 seconds, step 3, sample feeding pipe is transferred in current-carrying solution, stop 12 ~ 16 seconds through passage A, revolution speed 100rpm ~ 120rpm, import solution of potassium borohydride (1.6), carrier fluid (1.13) and solution (4.2) (4.3) (4.4), atomic fluorescence spectrometry is adopted to measure the atomic fluorescence intensity of tellurium in reagent blank Standard entertion working curve solution and test portion Standard entertion working curve solution, draw reagent blank Standard entertion working curve and test portion Standard entertion working curve respectively, reagent blank Standard entertion working curve checks in the Te quality of reagent blank, test portion Standard entertion working curve checks in the Te quality of test portion, deduct the Te quality of reagent blank by the Te quality of the test portion checked in, converting with following formula obtains Te content in the test portion recorded as atomic fluorescence spectrometry,
In formula:
M
1---the quality of the tellurium element checked on working curve, unit is microgram;
The quality of m---test portion, unit is gram.
(5), computation and measurement result, obtain tellurium content; The content of tellurium is 0.000057%.
Embodiment two
Measure tellurium content in IN738 high temperature alloy, adopt atomic fluorescence emission spectrometer, the measuring condition of instrument is as follows: atomic fluorescence emission spectrometer measuring condition, photomultiplier negative high voltage 340V ~ 380V; Atomization temperature 800 DEG C ~ 840 DEG C; Stove height 6.0mm ~ 10.0mm; Flow rate of carrier gas 500mL/min ~ 700mL/min; Shield gas flow speed 800mL/min ~ 1000mL/min; Lamp current 50mA ~ 80mA; Be equipped with the special hollow cathode lamp of tellurium, analytical line is 214.3nm;
(1) 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), perchloric acid, ρ 1.67g/mL; Top grade is pure;
(1.4), nitric acid, 1+1; Top grade is pure;
(1.5), citric acid solution, 400g/L;
Take 200g citric acid to be dissolved in 200mL water, being diluted with water to volume is 500mL;
(1.6), solution of potassium borohydride: 16g/L; In the sodium hydroxide solution of 4g/L, matching while using;
Take 2g NaOH to be dissolved in 500mL water, then add 8.0g potassium borohydride, shake is dissolved, if there is muddiness, filters rear use;
(1.7), tellurium standard solution A:0.100mg/mL; Take 0.1000g; > 99.995% tellurium powder, is placed in 100mL beaker, slowly adds 10mL nitric acid (1.4), heating for dissolving, after entirely molten, slightly cold, add 2mL perchloric acid (1.3), continue to be heated to emit white cigarette, take off slightly cold, add about 10mL water, heating for dissolving salt, take off after all dissolving, be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, shake up;
(1.8), tellurium standard solution B, 10.0 μ g/mL; Pipette 20.00mL tellurium standard solution A (1.7) in 200mL volumetric flask, add 10mL nitric acid (1.4), be diluted with water to scale, shake up;
(1.9), tellurium standard solution C, 1.0 μ g/mL; Pipette 20.00mL tellurium standard solution B (1.8) in 200mL volumetric flask, add 10mL nitric acid (1.4), be diluted with water to scale, shake up;
(1.10), tellurium standard solution D, 0.1 μ g/mL, matching while using; Pipette 20.00mL tellurium standard solution C (1.9) in 200mL volumetric flask, add 10mL nitric acid (1.4), be diluted with water to scale, shake up;
(1.11), nickel solution, 20mg/mL; Take 10.00g; > 99.99% metallic nickel, adds 65mL nitric acid (1.4), heating for dissolving, boils expeling nitrogen oxide, cooling, moves in 500mL volumetric flask, is diluted with water to scale, shakes up;
(1.12), cobalt liquor: 5mg/mL; Take 2.50g; > 99.98% metallic cobalt, adds 20mL nitric acid (1.4), and low-temperature heat is dissolved, and cooling moves in 500mL volumetric flask, is diluted with water to scale, shakes up;
(1.13), carrier fluid; In the port grinding bottle of 500mL, add 240mL water, then add 160mL hydrochloric acid (1.1), shake up, be cooled to room temperature, for subsequent use;
(2), sampling and sample preparation; The sample analyzed carries out sampling and sample preparation according to the requirement of HB/Z205;
(3) prepare before, analyzing
Co-existing element interference, 65 milligrams-85 milligrams, nickel, chromium 5 milligrams-30 milligrams, molybdenum are less than 20 milligrams, titanium is less than 15 milligrams, tantalum is less than 10 milligrams, hafnium is less than 10 milligrams, tantalum is less than 10 milligrams, tungsten is less than 15 milligrams, manganese tantalum is less than 7 milligrams;
Solution of potassium borohydride, matching while using;
(4), analytical procedure is as follows:
(4.1), test portion: take 0.10g sample, be accurate to 0.0001g;
(4.2), blank test solution: do blank test in company with test portion;
(4.3), prepare sample solution: the test portion of analytical procedure (4.1) is placed in 100mL beaker, add 15mL ~ 25mL hydrochloric acid (1.1), 1mL ~ 1.5mL nitric acid (1.2), on electric hot plate, low-grade fever is dissolved completely to test portion; Take off slightly cold from electric hot plate, add 5mL citric acid solution (1.5), electric furnace voltage is adjusted to 200V, and heating is boiled; Solution, to room temperature, moves in 50mL volumetric flask, is diluted with water to scale, shake up by cooling test solution;
(4.4), preparation standard adds working curve solution
(4.4.1) test portion Standard entertion working curve solution, is prepared; Take containing tantalum high temperature alloy test portion in 100mL beaker, add 15mL ~ 25mL hydrochloric acid (1.1), 1mL ~ 1.5mL nitric acid (1.2), on electric hot plate, low-grade fever is dissolved completely to test portion; Take off slightly cold from electric hot plate, add 5mL citric acid solution (1.5), electric furnace voltage is adjusted to 200V, and heating is boiled; Solution, to room temperature, moves in 50mL volumetric flask, adds 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL tellurium standard solution (1.10) successively, be diluted to scale, shake up with water by cooling test solution;
(4.4.2) reagent blank Standard entertion working curve solution, is prepared; Prepare reagent blank with sample operation repetitive, add 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL tellurium standard solution (1.10) successively, be diluted to scale with water, shake up, the Standard entertion serial solution of preparation reagent blank;
(4.5) concentration of tellurium in test solution, is measured, by condition of work, pump line parameter and injection procedure that atomic fluorescence emission spectrometer, Generation-Atomic Fluorescence Spectrometry hydride generator are selected, pump line parameter, passage A sample or carrier fluid solution, bore 2mm, channel B reductant solution, bore 1mm, channel C waste liquid, bore 2mm, on atomic fluorescence emission spectrometer, with special tellurium hollow cathode lamp, at Te214.3nm wavelength place, injection procedure setting steps one: sample feeding pipe inserts sample solution, stops 6 ~ 10 seconds through passage A, revolution speed 90rpm ~ 110rpm, meanwhile, reductive agent solution of potassium borohydride, stops 6 ~ 10 seconds through channel B, revolution speed 90rpm ~ 110rpm, now sample solution and reductive agent just enter the endless tube end of sample storage tube, step 2, pump stall 6 seconds, step 3, sample feeding pipe is transferred in current-carrying solution, stop 12 ~ 16 seconds through passage A, revolution speed 100rpm ~ 120rpm, import solution of potassium borohydride (1.6), carrier fluid (1.13) and solution (4.2) (4.3) (4.4), atomic fluorescence spectrometry is adopted to measure the atomic fluorescence intensity of tellurium in reagent blank Standard entertion working curve solution and test portion Standard entertion working curve solution, draw reagent blank Standard entertion working curve and test portion Standard entertion working curve respectively, reagent blank Standard entertion working curve checks in the Te quality of reagent blank, test portion Standard entertion working curve checks in the Te quality of test portion, deduct the Te quality of reagent blank by the Te quality of the test portion checked in, converting with following formula obtains Te content in the test portion recorded as atomic fluorescence spectrometry,
In formula:
M
1---the quality of the tellurium element checked on working curve, unit is microgram;
The quality of m---test portion, unit is gram.
(5), computation and measurement result, obtain tellurium content; The content of tellurium is 0.00015%.
Embodiment three
Measure tellurium content in single crystal super alloy, adopt atomic fluorescence emission spectrometer, the measuring condition of instrument is as follows: atomic fluorescence emission spectrometer measuring condition, photomultiplier negative high voltage 340V ~ 380V; Atomization temperature 800 DEG C ~ 840 DEG C; Stove height 6.0mm ~ 10.0mm; Flow rate of carrier gas 500mL/min ~ 700mL/min; Shield gas flow speed 800mL/min ~ 1000mL/min; Lamp current 50mA ~ 80mA; Be equipped with the special hollow cathode lamp of tellurium, analytical line is 214.3nm;
(1) 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), perchloric acid, ρ 1.67g/mL; Top grade is pure;
(1.4), nitric acid, 1+1; Top grade is pure;
(1.5), citric acid solution, 400g/L;
Take 200g citric acid to be dissolved in 200mL water, being diluted with water to volume is 500mL;
(1.6), solution of potassium borohydride: 16g/L; In the sodium hydroxide solution of 4g/L, matching while using;
Take 2g NaOH to be dissolved in 500mL water, then add 8.0g potassium borohydride, shake is dissolved, if there is muddiness, filters rear use;
(1.7), tellurium standard solution A:0.100mg/mL; Take 0.1000g; > 99.995% tellurium powder, is placed in 100mL beaker, slowly adds 10mL nitric acid (1.4), heating for dissolving, after entirely molten, slightly cold, add 2mL perchloric acid (1.3), continue to be heated to emit white cigarette, take off slightly cold, add about 10mL water, heating for dissolving salt, take off after all dissolving, be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, shake up;
(1.8), tellurium standard solution B, 10.0 μ g/mL; Pipette 20.00mL tellurium standard solution A (1.7) in 200mL volumetric flask, add 10mL nitric acid (1.4), be diluted with water to scale, shake up;
(1.9), tellurium standard solution C, 1.0 μ g/mL; Pipette 20.00mL tellurium standard solution B (1.8) in 200mL volumetric flask, add 10mL nitric acid (1.4), be diluted with water to scale, shake up;
(1.10), tellurium standard solution D, 0.1 μ g/mL, matching while using; Pipette 20.00mL tellurium standard solution C (1.9) in 200mL volumetric flask, add 10mL nitric acid (1.4), be diluted with water to scale, shake up;
(1.11), nickel solution, 20mg/mL; Take 10.00g; > 99.99% metallic nickel, adds 65mL nitric acid (1.4), heating for dissolving, boils expeling nitrogen oxide, cooling, moves in 500mL volumetric flask, is diluted with water to scale, shakes up;
(1.12), cobalt liquor: 5mg/mL; Take 2.50g; > 99.98% metallic cobalt, adds 20mL nitric acid (1.4), and low-temperature heat is dissolved, and cooling moves in 500mL volumetric flask, is diluted with water to scale, shakes up;
(1.13), carrier fluid; In the port grinding bottle of 500mL, add 240mL water, then add 160mL hydrochloric acid (1.1), shake up, be cooled to room temperature, for subsequent use;
(2), sampling and sample preparation; The sample analyzed carries out sampling and sample preparation according to the requirement of HB/Z205;
(3) prepare before, analyzing
Co-existing element interference, 65 milligrams-85 milligrams, nickel, chromium 5 milligrams-30 milligrams, molybdenum are less than 20 milligrams, titanium is less than 15 milligrams, tantalum is less than 10 milligrams, hafnium is less than 10 milligrams, tantalum is less than 10 milligrams, tungsten is less than 15 milligrams, manganese tantalum is less than 7 milligrams;
Solution of potassium borohydride, matching while using;
(4), analytical procedure is as follows:
(4.1), test portion: take 0.10g sample, be accurate to 0.0001g;
(4.2), blank test solution: do blank test in company with test portion;
(4.3), prepare sample solution: the test portion of analytical procedure (4.1) is placed in 100mL beaker, add 15mL ~ 25mL hydrochloric acid (1.1), 1mL ~ 1.5mL nitric acid (1.2), on electric hot plate, low-grade fever is dissolved completely to test portion; Take off slightly cold from electric hot plate, add 5mL citric acid solution (1.5), electric furnace voltage is adjusted to 200V, and heating is boiled; Solution, to room temperature, moves in 50mL volumetric flask, is diluted with water to scale, shake up by cooling test solution;
(4.4), preparation standard adds working curve solution
(4.4.1) test portion Standard entertion working curve solution, is prepared; Take containing tantalum high temperature alloy test portion in 100mL beaker, add 15mL ~ 25mL hydrochloric acid (1.1), 1mL ~ 1.5mL nitric acid (1.2), on electric hot plate, low-grade fever is dissolved completely to test portion; Take off slightly cold from electric hot plate, add 5mL citric acid solution (1.5), electric furnace voltage is adjusted to 200V, and heating is boiled; Solution, to room temperature, moves in 50mL volumetric flask, adds 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL tellurium standard solution (1.10) successively, be diluted to scale, shake up with water by cooling test solution;
(4.4.2) reagent blank Standard entertion working curve solution, is prepared; Prepare reagent blank with sample operation repetitive, add 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL tellurium standard solution (1.10) successively, be diluted to scale with water, shake up, the Standard entertion serial solution of preparation reagent blank;
(4.5) concentration of tellurium in test solution, is measured, by condition of work, pump line parameter and injection procedure that atomic fluorescence emission spectrometer, Generation-Atomic Fluorescence Spectrometry hydride generator are selected, pump line parameter, passage A sample or carrier fluid solution, bore 2mm, channel B reductant solution, bore 1mm, channel C waste liquid, bore 2mm, on atomic fluorescence emission spectrometer, with special tellurium hollow cathode lamp, at Te214.3nm wavelength place, injection procedure setting steps one: sample feeding pipe inserts sample solution, stops 6 ~ 10 seconds through passage A, revolution speed 90rpm ~ 110rpm, meanwhile, reductive agent solution of potassium borohydride, stops 6 ~ 10 seconds through channel B, revolution speed 90rpm ~ 110rpm, now sample solution and reductive agent just enter the endless tube end of sample storage tube, step 2, pump stall 6 seconds, step 3, sample feeding pipe is transferred in current-carrying solution, stop 12 ~ 16 seconds through passage A, revolution speed 100rpm ~ 120rpm, import solution of potassium borohydride (1.6), carrier fluid (1.13) and solution (4.2) (4.3) (4.4), atomic fluorescence spectrometry is adopted to measure the atomic fluorescence intensity of tellurium in reagent blank Standard entertion working curve solution and test portion Standard entertion working curve solution, draw reagent blank Standard entertion working curve and test portion Standard entertion working curve respectively, reagent blank Standard entertion working curve checks in the Te quality of reagent blank, test portion Standard entertion working curve checks in the Te quality of test portion, deduct the Te quality of reagent blank by the Te quality of the test portion checked in, converting with following formula obtains Te content in the test portion recorded as atomic fluorescence spectrometry,
In formula:
M
1---the quality of the tellurium element checked on working curve, unit is microgram;
The quality of m---test portion, unit is gram.
(5), computation and measurement result, obtain tellurium content; The content of tellurium is 0.00045%.
Claims (2)
1. an AFS DETERMINATION is containing the analytical approach of tellurium in tantalum high temperature alloy, it is characterized in that: adopt atomic fluorescence emission spectrometer, the measuring condition of instrument is as follows: atomic fluorescence emission spectrometer measuring condition, photomultiplier negative high voltage 340V ~ 380V; Atomization temperature 800 DEG C ~ 840 DEG C; Stove height 6.0mm ~ 10.0mm; Flow rate of carrier gas 500mL/min ~ 700mL/min; Shield gas flow speed 800mL/min ~ 1000mL/min; Lamp current 50mA ~ 80mA; Be equipped with the special hollow cathode lamp of tellurium, analytical line is 214.3nm;
(1) 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), perchloric acid, ρ 1.67g/mL; Top grade is pure;
(1.4), nitric acid, 1+1; Top grade is pure;
(1.5), citric acid solution, 400g/L;
Take 200g citric acid to be dissolved in 200mL water, being diluted with water to volume is 500mL;
(1.6), solution of potassium borohydride: 16g/L; In the sodium hydroxide solution of 4g/L, matching while using;
Take 2g NaOH to be dissolved in 500mL water, then add 8.0g potassium borohydride, shake is dissolved, if there is muddiness, filters rear use;
(1.7), tellurium standard solution A:0.100mg/mL; Take 0.1000g; > 99.995% tellurium powder, is placed in 100mL beaker, slowly adds 10mL nitric acid (1.4), heating for dissolving, after entirely molten, slightly cold, add 2mL perchloric acid (1.3), continue to be heated to emit white cigarette, take off slightly cold, add about 10mL water, heating for dissolving salt, take off after all dissolving, be cooled to room temperature, move in 1000mL volumetric flask, be diluted with water to scale, shake up;
(1.8), tellurium standard solution B, 10.0 μ g/mL; Pipette 20.00mL tellurium standard solution A (1.7) in 200mL volumetric flask, add 10mL nitric acid (1.4), be diluted with water to scale, shake up;
(1.9), tellurium standard solution C, 1.0 μ g/mL; Pipette 20.00mL tellurium standard solution B (1.8) in 200mL volumetric flask, add 10mL nitric acid (1.4), be diluted with water to scale, shake up;
(1.10), tellurium standard solution D, 0.1 μ g/mL, matching while using; Pipette 20.00mL tellurium standard solution C (1.9) in 200mL volumetric flask, add 10mL nitric acid (1.4), be diluted with water to scale, shake up;
(1.11), nickel solution, 20mg/mL; Take 10.00g; > 99.99% metallic nickel, adds 65mL nitric acid (1.4), heating for dissolving, boils expeling nitrogen oxide, cooling, moves in 500mL volumetric flask, is diluted with water to scale, shakes up;
(1.12), cobalt liquor: 5mg/mL; Take 2.50g; > 99.98% metallic cobalt, adds 20mL nitric acid (1.4), and low-temperature heat is dissolved, and cooling moves in 500mL volumetric flask, is diluted with water to scale, shakes up;
(1.13), carrier fluid; In the port grinding bottle of 500mL, add 240mL water, then add 160mL hydrochloric acid (1.1), shake up, be cooled to room temperature, for subsequent use;
(2), sampling and sample preparation; The sample analyzed carries out sampling and sample preparation according to the requirement of HB/Z 205;
(3) prepare before, analyzing
Co-existing element interference, 65 milligrams-85 milligrams, nickel, chromium 5 milligrams-30 milligrams, molybdenum are less than 20 milligrams, titanium is less than 15 milligrams, tantalum is less than 10 milligrams, hafnium is less than 10 milligrams, tantalum is less than 10 milligrams, tungsten is less than 15 milligrams, manganese tantalum is less than 7 milligrams;
Solution of potassium borohydride, matching while using;
(4), analytical procedure is as follows:
(4.1), test portion: take 0.10g sample, be accurate to 0.0001g;
(4.2), blank test solution: do blank test in company with test portion;
(4.3), sample solution is prepared: the test portion of analytical procedure (4.1) is placed in 100mL beaker, add 15mL ~ 25mL hydrochloric acid (1.1), 1mL ~ 1.5mL nitric acid (1.2), on electric hot plate, low-grade fever is dissolved completely to test portion; Take off slightly cold from electric hot plate, add 5mL citric acid solution (1.5), electric furnace voltage is adjusted to 200V, and heating is boiled; Solution, to room temperature, moves in 50mL volumetric flask, is diluted with water to scale, shake up by cooling test solution;
(4.4), preparation standard adds working curve solution
(4.4.1) test portion Standard entertion working curve solution, is prepared; Take containing tantalum high temperature alloy test portion in 100mL beaker, add 15mL ~ 25mL hydrochloric acid (1.1), 1mL ~ 1.5mL nitric acid (1.2), on electric hot plate, low-grade fever is dissolved completely to test portion; Take off slightly cold from electric hot plate, add 5mL citric acid solution (1.5), electric furnace voltage is adjusted to 200V, and heating is boiled; Solution, to room temperature, moves in 50mL volumetric flask, adds 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL tellurium standard solution (1.10) successively, be diluted to scale, shake up with water by cooling test solution;
(4.4.2) reagent blank Standard entertion working curve solution, is prepared; Prepare reagent blank with sample operation repetitive, add 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL tellurium standard solution (1.10) successively, be diluted to scale with water, shake up, the Standard entertion serial solution of preparation reagent blank;
(4.5) concentration of tellurium in test solution, is measured, by condition of work, pump line parameter and injection procedure that atomic fluorescence emission spectrometer, Generation-Atomic Fluorescence Spectrometry hydride generator are selected, pump line parameter, passage A sample or carrier fluid solution, bore 2mm, channel B reductant solution, bore 1mm, channel C waste liquid, bore 2mm, on atomic fluorescence emission spectrometer, with special tellurium hollow cathode lamp, at Te 214.3nm wavelength place, injection procedure setting steps one: sample feeding pipe inserts sample solution, stops 6 ~ 10 seconds through passage A, revolution speed 90rpm ~ 110rpm, meanwhile, reductive agent solution of potassium borohydride, stops 6 ~ 10 seconds through channel B, revolution speed 90rpm ~ 110rpm, now sample solution and reductive agent just enter the endless tube end of sample storage tube, step 2, pump stall 6 seconds, step 3, sample feeding pipe is transferred in current-carrying solution, stop 12 ~ 16 seconds through passage A, revolution speed 100rpm ~ 120rpm, import solution of potassium borohydride (1.6), carrier fluid (1.13) and solution (4.2) (4.3) (4.4), atomic fluorescence spectrometry is adopted to measure the atomic fluorescence intensity of tellurium in reagent blank Standard entertion working curve solution and test portion Standard entertion working curve solution, draw reagent blank Standard entertion working curve and test portion Standard entertion working curve respectively, reagent blank Standard entertion working curve checks in the Te quality of reagent blank, test portion Standard entertion working curve checks in the Te quality of test portion, deduct the Te quality of reagent blank by the Te quality of the test portion checked in, converting with following formula obtains Te content in the test portion recorded as atomic fluorescence spectrometry,
In formula:
M
1---the quality of the tellurium element checked on working curve, unit is microgram;
The quality of m---test portion, unit is gram.
2. a kind of AFS DETERMINATION according to claim 1 is containing the analytical approach of tellurium in tantalum high temperature alloy, it is characterized in that: use the standard solution of same single treatment to measure the same trade mark test solution that front and back process for twice respectively, control final sample solution volume and unanimously namely control solution acidity unanimously, reduce analytical error.
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| CN101344486A (en) * | 2007-07-10 | 2009-01-14 | 中国船舶重工集团公司第七二五研究所 | Hydride-atomic fluorescence optical spectrum rapid measuring method for micro-trace amount of tellurium in hull steel |
| CN102879373A (en) * | 2012-10-12 | 2013-01-16 | 中国航空工业集团公司北京航空材料研究院 | Method for determining selenium and tellurium content of pure chromium by using atomic fluorescence spectrometry |
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| CN1437013A (en) * | 2002-02-04 | 2003-08-20 | 李学璧 | Sample entering method for atomic spectrometer |
| CN101344486A (en) * | 2007-07-10 | 2009-01-14 | 中国船舶重工集团公司第七二五研究所 | Hydride-atomic fluorescence optical spectrum rapid measuring method for micro-trace amount of tellurium in hull steel |
| CN102879373A (en) * | 2012-10-12 | 2013-01-16 | 中国航空工业集团公司北京航空材料研究院 | Method for determining selenium and tellurium content of pure chromium by using atomic fluorescence spectrometry |
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| 氢化物—无色散原子荧光法测定地质样品中微量硒及碲;郭小伟,张文琴,杨密云;《岩石矿物及测试》;19981231;第2卷(第4期);第290页右栏第1段-第291页左栏第1段 * |
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