CN108956600A - The measuring method and its application of impurity copper content in a kind of zirconium aluminium powder - Google Patents
The measuring method and its application of impurity copper content in a kind of zirconium aluminium powder Download PDFInfo
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- CN108956600A CN108956600A CN201811189277.8A CN201811189277A CN108956600A CN 108956600 A CN108956600 A CN 108956600A CN 201811189277 A CN201811189277 A CN 201811189277A CN 108956600 A CN108956600 A CN 108956600A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
Abstract
The invention discloses the measuring methods and its application of impurity copper content in a kind of zirconium aluminium powder, the described method comprises the following steps: the volatile organic matter in S1, removal zirconium aluminium powder obtains sample to be tested；S2, the copper in sample to be tested is converted to copper ion, is reacted using dithizone as chelating agent with copper ion, colorimetric test solution is prepared；S3, preparation comparison blank solution；S4, with luminosity meter, contrastive colours test solution and the measurement of comparison blank solution and the percentage that copper content is calculated respectively.It can detect the copper content in zirconium aluminium powder sensitive and accurately using the measuring method, it is easy to operate, it is low in cost, the detection method is applied to microwave three, the detection application in tetreode to zirconium aluminium powder getter, it can be completed in microwave tube chemical treatment plant, the effectively content of detection copper impurity, to guarantee the performance of microwave three, tetreode.
Description
Technical field
The present invention relates to a kind of measurement sides of impurity copper content in the technical field of copper content testing more particularly to zirconium aluminium powder
Method and its application.
Background technique
Microwave triode and microwave tetrode are the microwave tubes based on Electrostatic Control principle.Including lighthouse tube, disk seal
Pipe, pencil tube, UHF transmitting tube, plate triode and titanium ceramics triode etc., common operating frequency range be 300~
16000 megahertzs.
Microwave three, tetrode can generally work to 3000 megahertzs or more of frequency, and continuous wave power is in watt grade to tens
Watt, pulse power is from several hectowatts to thousands of watts of magnitudes.They are widely used in communication, navigation, beacon, fuse, telemetering, survey height
In the radio instruments equipment such as meter and microwave signal source.The spy that HIGH-POWERED MICROWAVES three, tetrode have high gain, power capacity big
Point, in decimeter range continuous wave power up to tens of kilowatt, pulse power is widely used in TV, radar up to megawatt magnitude
With the engineerings such as accelerator.
Getter refer to can the effectively preparation or device of certain (kind) gas molecules of sorption common name, for obtaining or tieing up
Hold vacuum and purified gases etc..Getter has the diversified forms such as powdery, disk like, band-like, tubulose, ring-type, cup-shaped.At each
It is fitted with multiple getters in microwave three, tetreode, for maintaining the vacuum degree in pipe, creates good work for pipe
Environment stablizes the characteristic parameters of pipe, and performance and service life to pipe have important influence.
In many microwaves three, tetreode usually the porous structure made of zirconium aluminium powder compacting sintering as the suction in pipe
Gas agent.Zirconium aluminium powder used in microwave three, tetreode is higher to the content requirement of impurity, contains polymictic zirconium aluminium powder sintering
Made of porous structure inspiratory effects it is poor, influence the performance of pipe, and copper impurity is one of major impurity in zirconium aluminium powder, microwave
Three, impurity chemical component (%) content requirement is as follows in zirconium aluminium powder used in tetreode: iron≤0.15, silicon≤0.01, and copper≤
0.01, zinc≤0.01, volatile materials≤2%.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of measuring method of copper content in zirconium aluminium powder and
It is applied, and can detect the copper content in zirconium aluminium powder sensitive and accurately using the measuring method, easy to operate, low in cost,
The detection method is applied to microwave three, the detection application in tetreode to zirconium aluminium powder getter, is chemically treated vehicle in microwave tube
Between can complete, effectively detect copper impurity content, to guarantee the performance of microwave three, tetreode.
The measuring method of impurity copper content in a kind of zirconium aluminium powder proposed by the present invention, the described method comprises the following steps: S1,
The volatile organic matter in zirconium aluminium powder is removed, sample to be tested is obtained；
S2, the copper in sample to be tested is converted to copper ion, is reacted using dithizone as chelating agent with copper ion, prepared
Obtain colorimetric test solution；
S3, preparation comparison blank solution；
S4, with luminosity meter, contrastive colours test solution and the measurement of comparison blank solution and the percentage that copper content is calculated respectively
Than.
Preferably, detailed process is as follows by step S2: the sample to be tested being dissolved in hydrochloric acid, chloric acid is then added
Potassium evaporative crystallization, then crystallized product is dissolved in water, dissolved solution filters to get filtrate, and adds water to be configured to the filtrate
Mixed solution known to M volumetric concentration takes mixed solution described in V volume and places Congored test paper, adjusts the mixed solution
Acid-base property is blue to Congored test paper, then successively adds hydroxylamine hydrochloride solution and dithizone, the additive amount of dithizone to institute
Mixed solution is stated in green or aubergine, continues thereafter with and dithizone is added to mixed solution in stable green or stable purplish red
Color obtains the colorimetric test solution, wherein M >=V.
Preferably, comparing the preparation of colorimetric test solution in the preparation process and step S2 of blank solution in step S3
Journey is consistent, and difference is, compares and does not add the sample to be tested in the preparation process of blank solution.
Preferably, the hydroxylamine hydrochloride solution is the aqueous solution of mass concentration 10%, the hydroxylamine hydrochloride solution addition
Amount and the volume ratio of mixed solution described in V volume are 1:10-200ml.
Preferably, detailed process is as follows by step S4: carrying out colorimetric estimation using photometer, the colorimetric tests solution
Make test specimens and reference, the colorimetric test solution and the preceding mistake respectively of comparison blank solution test respectively with blank solution is compared
To remove moisture, the percentage of copper content is calculated according to the following formula for filter:
In formula: the content (g) for the copper equal with 1cm thick layer delustring amount that a-is found out by calibration curve；
The sample to be tested weight (g) being added in d-step S2；
Repeated measurement 2-3 times takes its average value.
Preferably, detailed process is as follows by step S1: by zirconium aluminium powder carbon tetrachloride filtration washing, after the completion of washing
It is 20-50 minutes dry at 80-100 DEG C, obtain sample to be tested.
Detection application of the measuring method of impurity copper content on microwave three, the effective getter of level Four in a kind of zirconium aluminium powder.
The present invention can quickly detect the copper content in aluminium powder, and entire detection method is easy to operate, and the detection used
Method and related reagent are swift in response, and phenomenon is obviously easy to observe and judge, thereby ensures that the accuracy of detection, can be effectively
Detect the copper content that mass concentration is lower than 0.01%, so that the quality standard for zirconium aluminium powder getter provides judgment basis, it will
The detection method is applied to microwave three, the detection application in tetreode to zirconium aluminium powder getter, effectively detects containing for copper impurity
Amount, to guarantee the performance of microwave three, tetreode.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.Agents useful for same of the present invention is uniform
Routine test or commercially available gained.In the present invention, it configures reagent and all uses distilled water and chemically pure reagent when being analyzed.
Embodiment 1
The measuring method of impurity copper content in a kind of zirconium aluminium powder, the described method comprises the following steps:
S1, by zirconium aluminium powder carbon tetrachloride filtration washing, after the completion of washing dry 20 minutes at 100 DEG C, obtain to
Test specimens；
S2, the sample to be tested is dissolved in hydrochloric acid, potassium chlorate evaporative crystallization is then added, then by crystallized product in water
Middle dissolution, dissolved solution filter to get filtrate, and add water to be configured to mixed solution known to M volumetric concentration the filtrate, take V
Mixed solution described in volume simultaneously places Congored test paper, and it is blue to Congored test paper to adjust the mixed solution acid-base property, with
Hydroxylamine hydrochloride solution and dithizone are successively added afterwards, additive amount to the mixed solution of dithizone is in green or aubergine, with
Dithizone is continuously added afterwards to mixed solution in stable green or stable aubergine, obtains the colorimetric test solution,
Middle M >=V；
S3, the preparation process for comparing blank solution are consistent with the colorimetric test preparation process of solution in step S2, and difference exists
In comparing and not adding the sample to be tested in the preparation process of blank solution；
S4, colorimetric estimation is carried out using photometer, the colorimetric test solution and comparison blank solution make test specimens respectively
And reference, it is filtered respectively before the colorimetric test solution and comparison blank solution test to remove moisture, the percentage of copper content
Than being calculated according to the following formula:
In formula: the content (g) for the copper equal with 1cm thick layer delustring amount that a-is found out by calibration curve；
The sample to be tested weight (g) being added in d-step S2；
Repeated measurement 3 times, take its average value.
Above-mentioned steps S1, S2, S3 and S4 are carried out repeating to test three times, calculates separately and show that three groups of copper contents are
0.002%, 0.004% and 0.003%, being averaged to obtain in embodiment 1 copper content in zirconium aluminium powder is 0.003%.
Detection application of the measuring method of impurity copper content on microwave three, the effective getter of level Four in zirconium aluminium powder, according to
The copper content of the zirconium aluminium getter is qualified known to data judgement.
Embodiment 2
The measuring method of impurity copper content in a kind of zirconium aluminium powder, the described method comprises the following steps:
S1, by zirconium aluminium powder carbon tetrachloride filtration washing, after the completion of washing dry 50 minutes at 80 DEG C, obtain to be measured
Sample；
S2, the sample to be tested is dissolved in hydrochloric acid, potassium chlorate evaporative crystallization is then added, then by crystallized product in water
Middle dissolution, dissolved solution filter to get filtrate, and add water to be configured to mixed solution known to M volumetric concentration the filtrate, take V
Mixed solution described in volume simultaneously places Congored test paper, and it is blue to Congored test paper to adjust the mixed solution acid-base property, with
Hydroxylamine hydrochloride solution and dithizone are successively added afterwards, additive amount to the mixed solution of dithizone is in green or aubergine, with
Dithizone is continuously added afterwards to mixed solution in stable green or stable aubergine, obtains the colorimetric test solution,
Middle M >=V；
S3, the preparation process for comparing blank solution are consistent with the colorimetric test preparation process of solution in step S2, and difference exists
In comparing and not adding the sample to be tested in the preparation process of blank solution；
S4, colorimetric estimation is carried out using photometer, the colorimetric test solution and comparison blank solution make test specimens respectively
And reference, it is filtered respectively before the colorimetric test solution and comparison blank solution test to remove moisture, the percentage of copper content
Than being calculated according to the following formula:
In formula: the content (g) for the copper equal with 1cm thick layer delustring amount that a-is found out by calibration curve；
The sample to be tested weight (g) being added in d- step S2；
Repeated measurement 2 times, take its average value.
Above-mentioned steps S1, S2, S3 and S4 are carried out repeating to test three times, calculates separately and show that three groups of copper contents are
0.003% and 0.005%, being averaged to obtain in embodiment 2 copper content in zirconium aluminium powder is 0.004%.
Detection application of the measuring method of impurity copper content on microwave three, the effective getter of level Four in zirconium aluminium powder, according to
The copper content of the zirconium aluminium getter is qualified known to data judgement.
Embodiment 3
The measuring method of impurity copper content in a kind of zirconium aluminium powder, the described method comprises the following steps:
S1, zirconium aluminium powder is placed in the funnel or crucible for being lined with porous filter plate, is rinsed 4 times, will be leaked with carbon tetrachloride
It after carbon tetrachloride in bucket or crucible is filtered dry only, is put into baking oven, toasts 30 minutes and take out at 90 DEG C, obtain sample to be tested；
S2,1 gram of sample to be tested is placed in the beaker that volume is 100ml, then dissolves in 20ml dilute hydrochloric acid, cover glass
Lid, heating is completely dissolved sample after sharply reaction stops, and adds 0.05g potassium chlorate.Evaporation process makes the substance in beaker
Start to crystallize, after crystallization inject 50ml pure water, heating dissolve crystal salt, with close filter paper will crystallize dissolved solution filter into
Volume is to be rinsed with water filter paper, solution is diluted at the scale of measuring bottle with water punching, and rocks measuring bottle 3 minutes in the measuring bottle of 250ml
It is that solution is uniform；100ml solution is sucked out with pipe is moved, is put into the beaker of 150ml.A small pieces Congored test paper is placed in solution,
Adjusting solution acid-basicity is blue to test paper, then solution is poured into the short glass-tube separatory funnel that volume is 250ml；To short glass-tube
The hydroxylamine hydrochloride aqueous solution and 3ml dithizone that 1.0ml mass concentration is 10% are added in separatory funnel, shakes separatory funnel to double
The green of sulphur hydrazone starts to be further continued for shaking 5 minutes when changing.It is the graduated amount of 10ml by the copper salt solution injection volume of dithizone
In cylinder or measuring bottle, then divide 3 times and 3ml dithizone solution or so is added altogether until the green of solution is stablized and do not change, obtains
Solution is tested to the colorimetric；
S3, the preparation process agents useful for same for comparing blank solution and quantity, the condition of test are consistent with step S2, difference
It is, the preparation process for comparing blank solution does not add sample to be tested, and the solution of blank test will distill after hydrochloric acid is added
It is substantially dry, in residue after the drying plus water, then solution is poured into rush in the measuring bottle of 200ml with water and dilute to scale and is shaken
It is even, take out with the isometric solution of colorimetric test solution, neutralized with ammonium hydroxide make the Congored test paper to blue start to take on a red color for
Only, dilute hydrochloric acid solution is then instilled to being in acid, then pours into separatory funnel plus 4ml dithizone and shakes up, and obtains comparison blank
Solution takes 10ml comparison blank solution stand-by；
S4, colorimetric estimation is carried out using photometer, the colorimetric test solution and comparison blank solution make test specimens respectively
And reference, it is filtered respectively before the colorimetric test solution and comparison blank solution test to remove moisture, the percentage of copper content
Than being calculated according to the following formula:
In formula: the content (g) for the copper equal with 1cm thick layer delustring amount that a- is found out by calibration curve；
The sample to be tested weight (g) being added in d- step S2；
Repeated measurement 3 times, take its average value；
The volume for the solution that V- takes out from the volumetric flask that volume is 250ml.
Above-mentioned steps S1, S2, S3 and S4 are carried out repeating to test three times, calculates separately and show that three groups of copper contents are
0.001%, 0.003% and 0.004%, being averaged to obtain in embodiment 3 copper content in zirconium aluminium powder is 0.0027%.
Detection application of the measuring method of impurity copper content on microwave three, the effective getter of level Four in zirconium aluminium powder, according to
The copper content of the zirconium aluminium getter is qualified known to data judgement.
Embodiment 4
The measuring method of impurity copper content in a kind of zirconium aluminium powder, the described method comprises the following steps:
S1, zirconium aluminium powder is placed in the funnel or crucible for being lined with porous filter plate, is rinsed 3 times, will be leaked with carbon tetrachloride
It after carbon tetrachloride in bucket or crucible is filtered dry only, is put into baking oven, toasts 40 minutes and take out at 88 DEG C, obtain sample to be tested；
S2,1 gram of sample to be tested is placed in the beaker that volume is 100ml, then dissolves in 20ml dilute hydrochloric acid, cover glass
Lid, heating is completely dissolved sample after sharply reaction stops, and adds 0.05g potassium chlorate.Evaporation process makes the substance in beaker
Start to crystallize, after crystallization inject 50ml pure water, heating dissolve crystal salt, with close filter paper will crystallize dissolved solution filter into
Volume is to be rinsed with water filter paper, solution is diluted at the scale of measuring bottle with water punching, and rocks measuring bottle 3 minutes in the measuring bottle of 250ml
It is that solution is uniform；25ml solution is sucked out with pipe is moved, is put into the beaker of 100ml.A small pieces Congored test paper is placed in solution, is adjusted
Section solution acid-basicity is blue to test paper, then solution is poured into the short glass-tube separatory funnel that volume is 100ml；To short glass-tube point
The hydroxylamine hydrochloride aqueous solution and 3ml dithizone that 1.0ml mass concentration is 10% are added in liquid funnel, shakes separatory funnel to double sulphur
The aubergine of hydrazone starts to be further continued for shaking 3 minutes when changing.It is the graduated amount of 10ml by the copper salt solution injection volume of dithizone
In cylinder or measuring bottle, then divide be added altogether for 2 times 3ml dithizone solution or so until solution it is purplish red it is colour-stable do not change until,
Obtain the colorimetric test solution；
S3, the preparation process agents useful for same for comparing blank solution and quantity, the condition of test are consistent with step S2, difference
It is, the preparation process for comparing blank solution does not add sample to be tested, and the solution of blank test will distill after hydrochloric acid is added
It is substantially dry, in residue after the drying plus water, then solution is poured into rush in the measuring bottle of 200ml with water and dilute to scale and is shaken
It is even, take out with the isometric solution of colorimetric test solution, neutralized with ammonium hydroxide make the Congored test paper to blue start to take on a red color for
Only, dilute hydrochloric acid solution is then instilled to being in acid, then pours into separatory funnel plus 4ml dithizone and shakes up, and obtains comparison blank
Solution takes 10ml comparison blank solution stand-by；
S4, colorimetric estimation is carried out using photometer, the colorimetric test solution and comparison blank solution make test specimens respectively
And reference, it is filtered respectively before the colorimetric test solution and comparison blank solution test to remove moisture, the percentage of copper content
Than being calculated according to the following formula:
In formula: the content (g) for the copper equal with 1cm thick layer delustring amount that a- is found out by calibration curve；
The sample to be tested weight (g) being added in d- step S2；
Repeated measurement 2 times, take its average value；
The volume for the solution that V- takes out from the volumetric flask that volume is 250ml.
Above-mentioned steps S1, S2, S3 and S4 are carried out repeating to test three times, calculates separately and show that three groups of copper contents are
0.04%, 0.05% and 0.03%, being averaged to obtain in embodiment 4 copper content in zirconium aluminium powder is 0.04%.
Detection application of the measuring method of impurity copper content on microwave three, the effective getter of level Four in zirconium aluminium powder, according to
The copper content of the zirconium aluminium getter is exceeded known to data judgement.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. the measuring method of impurity copper content in a kind of zirconium aluminium powder, which is characterized in that the described method comprises the following steps: S1, going
Except the volatile organic matter in zirconium aluminium powder, sample to be tested is obtained；
S2, the copper in sample to be tested is converted to copper ion, reacts, is prepared using dithizone as chelating agent with copper ion
Colorimetric tests solution；
S3, preparation comparison blank solution；
S4, with luminosity meter, contrastive colours test solution and the measurement of comparison blank solution and the percentage that copper content is calculated respectively.
2. the measuring method of impurity copper content in zirconium aluminium powder according to claim 1, which is characterized in that step S2's is specific
Process is as follows: the sample to be tested being dissolved in hydrochloric acid, potassium chlorate evaporative crystallization is then added, then by crystallized product in water
Dissolution, dissolved solution filter to get filtrate, add water to be configured to mixed solution known to M volumetric concentration the filtrate, take V body
The product mixed solution simultaneously places Congored test paper, and it is blue to Congored test paper to adjust the mixed solution acid-base property, then
Hydroxylamine hydrochloride solution and dithizone are successively added, additive amount to the mixed solution of dithizone is in green or aubergine, then
Dithizone is continuously added to mixed solution in stable green or stable aubergine, obtains the colorimetric test solution, wherein M
≥V。
3. the measuring method of impurity copper content in zirconium aluminium powder according to claim 2, which is characterized in that compared in step S3
The preparation process of blank solution is consistent with the colorimetric test preparation process of solution in step S2, and difference is, compares blank solution
Preparation process in do not add the sample to be tested.
4. the measuring method of impurity copper content in zirconium aluminium powder according to claim 2, which is characterized in that the hydroxylamine hydrochloride
Solution is the aqueous solution of mass concentration 10%, the volume ratio of mixed solution described in the hydroxylamine hydrochloride solution additive amount and V volume
For 1:10-200ml.
5. according to the measuring method of impurity copper content in zirconium aluminium powder described in claim 2-4 any one, which is characterized in that step
Detailed process is as follows by rapid S4: carrying out colorimetric estimation, the colorimetric test solution and comparison blank solution difference using photometer
Make test specimens and reference, is filtered respectively before the colorimetric test solution and comparison blank solution test to remove moisture, copper contains
The percentage of amount is calculated according to the following formula:
In formula: the content (g) for the copper equal with 1cm thick layer delustring amount that a-is found out by calibration curve；
The sample to be tested weight (g) being added in d-step S2；
Repeated measurement 2-3 times takes its average value.
6. the measuring method of impurity copper content in zirconium aluminium powder according to claim 5, which is characterized in that step S1's is specific
Process is as follows: it is 20-50 minutes dry at 80-100 DEG C after the completion of washing by zirconium aluminium powder carbon tetrachloride filtration washing, it obtains
To sample to be tested.
7. the measuring method of impurity copper content is in microwave three, the effective air-breathing of level Four in a kind of zirconium aluminium powder according to claim 6
Detection application in agent.
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2018
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| US4876068A (en) * | 1989-03-03 | 1989-10-24 | Chemetrics, Inc. | Test kit for colorimetric analysis |
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| US20130059391A1 (en) * | 2011-09-02 | 2013-03-07 | Sony Corporation | Test piece for heavy metal ion, process for detecting heavy metal ion, kit and sensor |
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| Title |
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