CN113295493A - Sample preparation method for counting particles of high-purity titanium - Google Patents
Sample preparation method for counting particles of high-purity titanium Download PDFInfo
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 117
- 239000010936 titanium Substances 0.000 title claims abstract description 117
- 239000002245 particle Substances 0.000 title claims abstract description 41
- 238000005464 sample preparation method Methods 0.000 title claims abstract description 39
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000002253 acid Substances 0.000 claims abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000001514 detection method Methods 0.000 claims abstract description 27
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 238000005260 corrosion Methods 0.000 claims abstract description 19
- 230000007797 corrosion Effects 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 238000005530 etching Methods 0.000 claims abstract description 17
- 239000006185 dispersion Substances 0.000 claims description 43
- 238000000120 microwave digestion Methods 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 15
- 238000007514 turning Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 11
- 238000005070 sampling Methods 0.000 claims description 9
- 238000005554 pickling Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 20
- 239000000243 solution Substances 0.000 description 50
- 230000000052 comparative effect Effects 0.000 description 27
- 239000000523 sample Substances 0.000 description 27
- 238000000034 method Methods 0.000 description 19
- 239000010419 fine particle Substances 0.000 description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 10
- 238000011109 contamination Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000004408 titanium dioxide Substances 0.000 description 5
- 239000012488 sample solution Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- 239000003732 agents acting on the eye Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229940023490 ophthalmic product Drugs 0.000 description 1
- 229940054534 ophthalmic solution Drugs 0.000 description 1
- 239000002997 ophthalmic solution Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/10—Investigating individual particles
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/10—Investigating individual particles
- G01N2015/1024—Counting particles by non-optical means
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Dispersion Chemistry (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a sample preparation method for counting particles of high-purity titanium, which comprises the steps of pretreating the high-purity titanium; mixing the pretreated high-purity titanium with a corrosion solution, and dispersing to obtain a solution to be detected; the etching solution comprises a mixed acid; the mixed acid comprises nitric acid and hydrofluoric acid; the corrosive solution also comprises pure water; the volume ratio of the mixed acid to the pure water in the corrosion solution is (1-1.2) to 1; the proportion of the high-purity titanium to the corrosive solution is (0.04-0.06) g:1mL, the sample preparation method shortens the corrosion time of a high-purity titanium material sample, improves the detection efficiency, reduces the possibility of sample liquid pollution, and enables data to be more stable.
Description
Technical Field
The invention relates to the technical field of particle calculation, in particular to a sample preparation method for counting particles of high-purity titanium.
Background
The liquid particle counter is mainly used for measuring the quantity of insoluble particles in liquid, adopts the principle of a light resistance method, and when insoluble particles pass through a sensor, the sensor can detect corresponding photoelectric signals because the signals fluctuate due to the obstruction of laser light, thereby realizing counting based on the photoelectric signals and calibrated voltage. The liquid particle counter is used in the fields of pharmacy, filtration detection, electronic information and the like, and has a wide application range.
CN107219162A discloses a method for detecting filtering performance of a filter, which at least comprises the following steps: preparing a detection test solution for simulating water quality; preprocessing a filter to be detected; connecting one or more pretreated filters to be tested into a test waterway, and introducing a detection test solution into the test waterway; taking an inlet water sample at a water inlet of each filter to be tested of the test waterway, and simultaneously taking an outlet water sample at a water outlet of each filter to be tested; respectively carrying out homogenization treatment on the taken water inlet sample and the taken water outlet sample; the method comprises the steps of measuring the number of particles in an inlet water sample and an outlet water sample, and calculating the removal rate of the particles according to the number of the particles in the inlet water sample and the number of the particles in the outlet water sample, but the method does not relate to the particle counting of the high-purity titanium material.
CN112672727A discloses a dispersion of precursor titanium dioxide particles having an intensity average peak particle size, as measured by DLS as described herein or a number average peak particle size, as measured by DLS as described herein, in a dispersing medium of from 0.2 to 2.0 μm, wherein the particle size distribution of the titanium dioxide particles in the dispersion is narrower than the particle size distribution of the precursor titanium dioxide particles, but not related to the particle count of the high purity titanium material.
CN111982761A discloses a method for detecting the dispersibility of titanium dioxide in aqueous color paste, which comprises the following steps: adopting covering power test paper, placing the prepared titanium dioxide water-based color paste on the top end of the test paper, wherein the width of the test paper is the same as that of a sample scraping groove of a wet film preparation device, and automatically scraping a plate from top to bottom by using the wet film preparation device with the wet film thickness of 120 +/-4 mu m; placing the scraped sample plate into a thermostat with the temperature of 50 +/-5 ℃, and drying for 20 +/-1 min; the black particles in the white blade area were counted from the black and white grid boundary lines of the hiding power test paper by irradiating from the back of the sample plate with a cell light, but the particle count of the high purity titanium material was not involved.
Disclosure of Invention
In order to solve the technical problems, the invention provides a sample preparation method for counting particles of high-purity titanium, which comprises the steps of mixing a mixed acid containing nitric acid and hydrofluoric acid with pure water according to a certain proportion, reacting with a high-purity titanium material in a microwave digestion device at a certain temperature, dispersing the high-purity titanium material in the mixed acid to obtain a solution to be detected, and further analyzing and calculating the granularity of the high-purity titanium material in the solution to be detected.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a sample preparation method for counting particles of high-purity titanium, which comprises the steps of pretreating the high-purity titanium; mixing the pretreated high-purity titanium with a corrosion solution, and dispersing to obtain a solution to be detected; the etching solution comprises a mixed acid; the mixed acid comprises nitric acid and hydrofluoric acid; the corrosive solution also comprises pure water; the volume ratio of the mixed acid to the pure water in the corrosion solution is (1-1.2) to 1; the proportion of the high-purity titanium to the corrosion solution is (0.04-0.06) g:1 mL.
According to the invention, the high-purity titanium and the corrosive solution are mixed according to a certain proportion, and the mixed acid in the corrosive solution and the pure water are mixed according to a certain proportion, so that the high-purity titanium can be efficiently dispersed in the mixed acid, the sampling amount of a high-purity titanium material is reduced, the dispersion speed is high, the corrosion time of a high-purity titanium material sample is shortened, and the detection efficiency is improved; the method reduces the possibility of sample liquid pollution, makes data more stable, conveniently and quickly obtains the granularity of the high-purity titanium in the liquid, and avoids introducing impurities due to long corrosion period, so that the result is unstable.
The method comprises the steps of turning a high-purity titanium target into a filamentous sample, dispersing the sample in acid liquor through the steps of pickling, corroding and the like to form mixed sample liquid, detecting the granularity of the sample liquid, and calculating to obtain a final result. The high-purity titanium is filamentous, so that the sample preparation time can be shortened, and the detection efficiency can be improved.
The high-purity titanium material generally refers to a titanium material with the purity of more than or equal to 99.9 wt%.
Wherein the volume ratio of the mixed acid to the pure water in the etching solution is (1-1.2): 1, and the volume ratio can be 1:1, 1:1.12, 1:1.14, 1:1.16, 1:1.18 or 1:2, for example; the ratio of the high-purity titanium to the mixed acid is (0.04 to 0.06) g:1mL, and may be, for example, 0.04g:1mL, 0.042g:1mL, 0.044g:1mL, 0.046g:1mL, 0.048g:1mL, 0.05g:1mL, 0.052g:1mL, 0.054g:1mL, 0.056g:1mL, 0.058g:1mL, or 0.06g:1 mL.
In the dispersion process, the liquid which reacts violently is prevented from overflowing in a large polytetrafluoroethylene beaker, and the sample is put into a microwave digestion device to be heated, so that the corrosion speed of the sample is accelerated.
Preferably, the pretreatment comprises turning, pickling and drying the high-purity titanium in sequence.
Preferably, the turning comprises turning the high purity titanium into a wire.
Preferably, the width of the high-purity titanium after turning is 5-15 mm, and may be 5mm, 6mm, 7mm, 8mm, 9mm, 10mm, 11mm, 12mm, or 5mm, for example.
Preferably, the acid washing comprises washing the high purity titanium with a washing liquid.
Preferably, the washing time is 3-5 min, for example, 3min, 3.2min, 3.4min, 3.6min, 3.8min, 4min, 4.2min, 4.4min, 4.6min, 4.8min or 5 min.
Preferably, the washing solution is a mixed acid.
Preferably, the drying comprises taking place under a sun light.
The volume ratio of the nitric acid to the hydrofluoric acid in the mixed acid is preferably 1 (0.8-1.2), and may be, for example, 1:0.8, 1:0.85, 1:0.9, 1:0.95, 1:1, 1:15, 1:2, or the like.
Preferably, the concentration of the nitric acid is 62 to 68 wt%, and for example, may be 62 wt%, 63 wt%, 64 wt%, 65 wt%, 66 wt%, 67 wt%, 68 wt%, or the like.
Preferably, the concentration of the hydrofluoric acid is 37 to 43 wt%, for example, 37 wt%, 38 wt%, 39 wt%, 40 wt%, 41 wt%, 42 wt%, 43 wt%, or the like.
Preferably, the purity of the high-purity titanium is 99.9 wt% or more, and may be, for example, 99.9 wt%, 99.93 wt%, 99.95 wt%, 99.97 wt%, 99.99 wt%, 99.993 wt%, 99.995 wt%, 99.997 wt%, 99.999 wt%, or the like.
Preferably, the temperature of the dispersion is 87 to 97 ℃, for example, 87 ℃, 88 ℃, 89 ℃, 90 ℃, 91 ℃, 92 ℃, 93 ℃, 94 ℃, 95 ℃, 96 ℃ or 97 ℃ and the like.
Preferably, the dispersing time is 3-5 h, for example, 3h, 3.2h, 3.4h, 3.6h, 3.8h, 4h, 4.2h, 4.4h, 4.6h, 4.8h or 5 h.
Preferably, the dispersion is carried out in a microwave digester.
Preferably, the microwave digestion device is preheated before the dispersion.
Preferably, the preheated final temperature is the temperature of dispersion.
Preferably, the solution to be detected is subjected to sampling, on-machine detection and data processing in sequence to obtain the granularity of the high-purity titanium.
Sampling, on-machine detection and data processing are carried out on a solution to be detected in sequence, namely impurities in the solution to be detected are filtered, an upper layer of clear solution is taken to form a mixed sample solution, 10ml of sample solution and 90ml of pure water are taken to be on-machine detected, the detection is carried out on the sample solution and the pure water in parallel for more than three times, and an average value is taken; mixing the mixed acid and the pure water according to the same volume ratio to form a control solution with the same ratio as the sample solution, taking 10ml of the control solution and 90ml of the pure water to carry out machine detection, taking an average value in parallel three times, and calculating the granularity of the sample by using a formula.
The invention provides a sample preparation method for counting the particles of high-purity titanium, which can be applied to insoluble particles in an ophthalmic solution and drug preparation, such as counting of insoluble particles in a sterile preparation, an injection and an injection liquid.
As a preferable technical scheme of the invention, the sample preparation method comprises the following steps:
(1) turning high-purity titanium with the purity of more than or equal to 99.9 wt% into a filament shape with the width of 5-15 mm, washing the turned high-purity titanium for 3-5 min by using mixed acid with the volume ratio of nitric acid to hydrofluoric acid being 1 (1.5-2.5), wherein the concentration of the nitric acid is 62-68 wt%, the concentration of the hydrofluoric acid is 37-43 wt%, and drying under a solar lamp to obtain pretreated high-purity titanium;
(2) mixing the mixed acid and pure water according to the volume ratio of (1-1.2) to 1 to obtain a corrosive solution, mixing the pretreated high-purity titanium and the corrosive solution obtained in the step (1) according to the ratio of (0.04-0.06) g:1mL, dispersing in a microwave digestion device at 87-97 ℃ for 3-5 hours, and preheating the microwave digestion device to the dispersing temperature before dispersion to obtain a solution to be detected;
(3) and (3) sequentially sampling, carrying out on-machine detection and carrying out data processing on the solution to be detected in the step (2) to obtain the granularity of the high-purity titanium.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the invention provides a sample preparation method for counting particles of high-purity titanium, which comprises the steps of mixing mixed acid containing nitric acid and hydrofluoric acid with pure water according to a certain proportion, reacting with a high-purity titanium material in a microwave digester at a certain temperature, dispersing the high-purity titanium material in the mixed acid to obtain a solution to be tested, and further analyzing and calculating the granularity of the high-purity titanium material in the solution to be tested, wherein the sample preparation method shortens the corrosion time of a high-purity titanium material sample, improves the detection efficiency, reduces the possibility of sample liquid pollution, enables the data to be more stable, ensures that the dispersion time of the high-purity titanium is less than or equal to 8.5 hours, ensures that the standard deviation of test result data is less than or equal to 7.02, ensures that the dispersion time of the high-purity titanium is less than or equal to 5 hours and the standard deviation is less than or equal to 4.56 under the optimal condition;
(2) the sample preparation method for counting the particles of the high-purity titanium is simple and easy to operate.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
First, an embodiment
Example 1
The embodiment provides a sample preparation method for counting particles of high-purity titanium, which comprises the following steps:
(1) turning high-purity titanium with the purity of 99.9 wt% into a wire shape with the width of 10mm, washing the turned high-purity titanium for 4min by adopting mixed acid with the volume ratio of nitric acid to hydrofluoric acid being 1:1, wherein the concentration of the nitric acid is 65 wt% and the concentration of the hydrofluoric acid is 40 wt%, and drying under a solar lamp to obtain pretreated high-purity titanium;
(2) mixing the mixed acid and pure water according to the volume ratio of 1:1 to obtain an etching solution, mixing the pretreated high-purity titanium obtained in the step (1) and the etching solution according to the ratio of 0.05g:1mL, dispersing for 4 hours at the temperature of 92 ℃ in a microwave digestion device, and preheating the microwave digestion device to the dispersing temperature before dispersion to obtain a solution to be detected;
(3) and (3) sequentially sampling, carrying out on-machine detection and carrying out data processing on the solution to be detected in the step (2) to obtain the granularity of the high-purity titanium.
In this example, the top-up detection process used a liquid particle counter model Beckman HIAC 9703 +.
Example 2
The embodiment provides a sample preparation method for counting particles of high-purity titanium, which comprises the following steps:
(1) turning high-purity titanium with the purity of 99.9 wt% into a filament shape with the width of 5mm, washing the turned high-purity titanium for 3min by adopting mixed acid with the volume ratio of nitric acid to hydrofluoric acid of 1:0.8, wherein the concentration of nitric acid is 62 wt% and the concentration of hydrofluoric acid is 37 wt%, and drying under a solar lamp to obtain pretreated high-purity titanium;
(2) mixing the mixed acid and pure water according to the volume ratio of 1.1:1 to obtain an etching solution, mixing the pretreated high-purity titanium obtained in the step (1) and the etching solution according to the volume ratio of 0.04g:1mL, dispersing for 5 hours at 87 ℃ in a microwave digestion device, and preheating the microwave digestion device to the dispersing temperature before dispersion to obtain a solution to be detected;
(3) and (3) sequentially sampling, carrying out on-machine detection and carrying out data processing on the solution to be detected in the step (2) to obtain the granularity of the high-purity titanium.
In this example, the top-up detection process used a liquid particle counter model Beckman HIAC 9703 +.
Example 3
The embodiment provides a sample preparation method for counting particles of high-purity titanium, which comprises the following steps:
(1) turning high-purity titanium with the purity of 99.9 wt% into a wire shape with the width of 15mm, washing the turned high-purity titanium for 5min by adopting mixed acid with the volume ratio of nitric acid to hydrofluoric acid of 1:1.2, wherein the concentration of the nitric acid is 68 wt% and the concentration of the hydrofluoric acid is 43 wt%, and drying under a solar lamp to obtain pretreated high-purity titanium;
(2) mixing the mixed acid and pure water according to the volume ratio of 1.2:1 to obtain an etching solution, mixing the pretreated high-purity titanium obtained in the step (1) and the etching solution according to the volume ratio of 0.06g:1mL, dispersing for 3 hours at 97 ℃ in a microwave digestion device, and preheating the microwave digestion device to the dispersing temperature before dispersion to obtain a solution to be detected;
(3) and (3) sequentially sampling, carrying out on-machine detection and carrying out data processing on the solution to be detected in the step (2) to obtain the granularity of the high-purity titanium.
In this example, the top-up detection process used a liquid particle counter model Beckman HIAC 9703 +.
Example 4
This example provides a sample preparation method for counting fine particles of high purity titanium, which is different from example 1 only in that the volume ratio of nitric acid and hydrofluoric acid in the mixed acid of step (1) is 1:0.6, and the rest is the same as example 1.
Example 5
This example provides a sample preparation method for counting fine particles of high purity titanium, which is different from example 1 only in that the volume ratio of nitric acid to hydrofluoric acid in the mixed acid of step (1) is 1:1.4, and the rest is the same as example 1.
Example 6
This example provides a sample preparation method for counting fine particles of high purity titanium, which is different from example 1 only in that the dispersion temperature in step (2) is 80 ℃, and the rest is the same as example 1.
Example 7
This example provides a sample preparation method for counting fine particles of high purity titanium, which is different from example 1 only in that the dispersion temperature in step (2) is 100 ℃, and the rest is the same as example 1.
Example 8
This example provides a sample preparation method for counting fine particles of high purity titanium, which is different from example 1 only in that the microwave digestion device is not preheated to the temperature for dispersion before the dispersion in step (2), and the rest is the same as example 1.
Second, comparative example
Comparative example 1
This comparative example provides a sample preparation method for counting fine particles of high purity titanium, which is different from example 1 only in that the volume ratio of the mixed acid and pure water in step (2) is 0.8:1, and the rest is the same as example 1.
Comparative example 2
This comparative example provides a sample preparation method for counting fine particles of high purity titanium, which is different from example 1 only in that the volume ratio of the mixed acid and pure water in step (2) is 1.4:1, and the rest is the same as example 1.
Comparative example 3
This comparative example provides a sample preparation method for counting fine particles of high purity titanium, which is different from example 1 only in that the mixing ratio of the high purity titanium after pretreatment in step (2) to the etching solution was 0.03g:1mL, and the rest was the same as example 1.
Comparative example 4
This comparative example provides a sample preparation method for counting fine particles of high purity titanium, which is different from example 1 only in that the mixing ratio of the high purity titanium after pretreatment in step (2) to the etching solution was 0.07g:1mL, and the rest was the same as example 1.
The time for dispersing the high-purity titanium in the etching solution in this comparative example becomes long.
Comparative example 5
This comparative example provides a sample preparation method for counting fine particles of high purity titanium, which is different from example 1 only in that nitric acid is replaced with pure water in a mixed acid, and the rest is the same as example 1.
Comparative example 6
This comparative example provides a sample preparation method for counting fine particles of high purity titanium, which is different from example 1 only in that hydrofluoric acid was replaced with pure water in a mixed acid, and the rest is the same as example 1.
In comparative examples 5 to 6, high-purity titanium could not be dispersed, and the solution to be measured could not be obtained, and the process of counting particles could not be performed.
Third, test and results
Standard deviation test method: the standard deviation was calculated by performing 5 times of counting of the fine particles of high purity titanium.
The test results of the above examples and comparative examples are shown in table 1.
TABLE 1
| Standard deviation of | Dispersion time (h) | |
| Example 1 | 4.56 | 4 |
| Example 2 | 4.23 | 3 |
| Example 3 | 4.36 | 5 |
| Example 4 | 6.65 | 5.4 |
| Example 5 | 6.26 | 6.2 |
| Example 6 | 6.78 | 8.5 |
| Example 7 | 7.02 | 5.5 |
| Example 8 | 6.45 | 8.4 |
| Comparative example 1 | 16.45 | 12.5 |
| Comparative example 2 | 17.23 | 4.4 |
| Comparative example 3 | 16.47 | 3.5 |
| Comparative example 4 | 16.84 | 12.5 |
From table 1, the following points can be seen:
(1) the invention provides a sample preparation method for counting particles of high-purity titanium, which shortens the corrosion time of a high-purity titanium material sample, improves the detection efficiency, reduces the possibility of sample liquid pollution, and makes data more stable, specifically, the dispersion time of the high-purity titanium in examples 1-9 is less than or equal to 8.5h, the standard deviation of the test result data is less than or equal to 7.02, the dispersion time of the high-purity titanium is less than or equal to 5h and the standard deviation is less than or equal to 4.56 under the optimal condition;
(2) as can be seen from the combination of the embodiment 1 and the embodiments 4 to 5, the volume ratio of the nitric acid to the hydrofluoric acid in the mixed acid of the step (1) in the embodiment 1 is 1:1, compared with the volume ratios of the nitric acid to the hydrofluoric acid in the mixed acid of the step (1) in the embodiments 4 to 5 of 1:0.6 and 1:1.4, respectively, the dispersion time of the embodiment 1 is 4 hours, the standard deviation of the test result data is 4.56, the dispersion times of the embodiments 4 to 5 are 5.4 hours and 6.2 hours, respectively, and the standard deviation of the test result data is 6.65 and 6.26, respectively, which indicates that the volume ratio of the nitric acid to the hydrofluoric acid in the mixed acid is controlled within a certain range, so as to further shorten the corrosion time of the high-purity titanium, improve the detection efficiency, further reduce the possibility of contamination of the solution to be detected, and stabilize the data;
(3) as can be seen from the combination of the embodiment 1 and the embodiments 6 to 7, the dispersion temperature of the step (2) in the embodiment 1 is 92 ℃, compared with the dispersion temperatures of the step (2) in the embodiments 6 to 7 of 80 ℃ and 100 ℃, the dispersion time of the embodiment 1 is 4 hours, the standard deviation of the test result data is 4.56, the dispersion times of the embodiments 6 to 7 are 8.5 hours and 5.5 hours, respectively, and the standard deviations of the test result data are 6.78 and 7.02, respectively, which indicates that the dispersion temperature is controlled in a certain range, so that the corrosion time of the high-purity titanium can be further shortened, the detection efficiency is improved, the possibility of contamination of the solution to be detected is further reduced, and the data is more stable;
(4) as can be seen from the combination of example 1 and example 8, the microwave digestion device is preheated to the dispersing temperature before dispersion in example 1, and compared with the microwave digestion device which is not preheated to the dispersing temperature before dispersion in example 8, the dispersing time in example 1 is 4 hours, the standard deviation of the test result data is 4.56, the dispersing time in example 8 is 8.4 hours, and the standard deviation of the test result data is 6.45, so that the method provided by the invention preheats the microwave digestion device to the dispersing temperature before dispersion, can further shorten the corrosion time of high-purity titanium, improve the detection efficiency, and further reduce the possibility of contamination of the solution to be detected, and make the data more stable;
(5) as can be seen from the combination of example 1 and comparative examples 1 to 2, the volume ratio of the mixed acid and the pure water in step (2) in example 1 is 1:1, the dispersion time of example 1 is 4 hours, the standard deviation of the test result data is 4.56, the dispersion time of comparative examples 1 to 2 is 12.5 hours and 4.4 hours, and the standard deviation of the test result data is 16.45 and 17.23, compared with the volume ratio of the mixed acid and the pure water in step (2) in comparative examples 1 to 2 of 0.8:1 and 1.4:1, respectively, which indicates that the present invention can reduce the corrosion time of high-purity titanium, improve the detection efficiency, reduce the possibility of contamination of the solution to be detected, and stabilize the data by controlling the volume ratio of the mixed acid and the pure water within a certain range;
(6) as can be seen from the combination of example 1 and comparative examples 3 to 4, the mixing ratio of the high purity titanium pretreated by step (2) in example 1 to the etching solution is 0.05g:1mL, and the dispersion time of example 1 is 4 hours, the standard deviation of the test result data is 4.56, and the dispersion time of comparative example 4 is 12.5 hours, compared to the mixing ratio of the high purity titanium pretreated by step (2) in comparative examples 3 to 4 to the etching solution is 0.03g:1mL and 0.07g:1mL, respectively, and the standard deviation of the test result data in comparative examples 3 to 4 is 16.47 and 16.84, respectively, which shows that the present invention can control the mixing ratio of the pretreated high purity titanium to the etching solution within a certain range, can shorten the etching time of the high purity titanium, improve the detection efficiency, and reduce the possibility of contamination of the solution to be detected, thereby stabilizing the data.
In summary, the invention provides a sample preparation method for counting particles of high-purity titanium, which comprises the steps of mixing a mixed acid containing nitric acid and hydrofluoric acid with pure water according to a certain proportion, reacting with a high-purity titanium material in a microwave digestion device at a certain temperature, dispersing the high-purity titanium material in the mixed acid to obtain a solution to be tested, and further analyzing and calculating the granularity of the high-purity titanium material in the solution to be tested, wherein the sample preparation method shortens the corrosion time of a high-purity titanium material sample, improves the detection efficiency, reduces the possibility of sample liquid pollution, enables data to be more stable, ensures that the dispersion time of the high-purity titanium is less than or equal to 8.5 hours, the standard deviation of test result data is less than or equal to 7.02, under an optimal condition, the dispersion time of the high-purity titanium is less than or equal to 5 hours, and the standard deviation is less than or equal to 4.56.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A sample preparation method for counting particles of high-purity titanium is characterized by comprising the steps of pretreating the high-purity titanium; mixing the pretreated high-purity titanium with a corrosion solution, and dispersing to obtain a solution to be detected;
the etching solution comprises a mixed acid;
the mixed acid comprises nitric acid and hydrofluoric acid;
the corrosive solution also comprises pure water;
the volume ratio of the mixed acid to the pure water in the corrosion solution is (1-1.2) to 1;
the proportion of the high-purity titanium to the corrosion solution is (0.04-0.06) g:1 mL.
2. The sample preparation method according to claim 1, wherein the pretreatment comprises turning, pickling and drying of the high-purity titanium in sequence;
preferably, the turning comprises turning the high purity titanium into filaments;
preferably, the width of the turned high-purity titanium is 5-15 mm;
preferably, the acid washing comprises washing the high-purity titanium by using a washing liquid;
preferably, the washing time is 3-5 min;
preferably, the washing solution is a mixed acid;
preferably, the drying comprises drying under a sun light.
3. The sample preparation method according to claim 1 or 2, wherein the volume ratio of the nitric acid to the hydrofluoric acid in the mixed acid is 1 (0.8-1.2).
4. A sample preparation method as claimed in any one of claims 1 to 3, wherein the concentration of nitric acid is 62 to 68 wt%;
preferably, the concentration of the hydrofluoric acid is 37-43 wt%.
5. A sample preparation method as claimed in any one of claims 1 to 4, wherein the purity of the high-purity titanium is not less than 99.9 wt%.
6. A sample preparation method as claimed in any one of claims 1 to 5, wherein the temperature of dispersion is 87 to 97 ℃.
7. A sample preparation method as claimed in any one of claims 1 to 6, wherein the dispersion time is 3 to 5 hours.
8. A sample preparation method as claimed in any one of claims 1 to 7, wherein said dispersion is carried out in a microwave digestion apparatus.
9. A sample preparation method as claimed in claim 8, wherein the microwave digestion device is preheated before the dispersion;
preferably, the preheated final temperature is the temperature of dispersion;
preferably, the solution to be detected is subjected to sampling, on-machine detection and data processing in sequence to obtain the granularity of the high-purity titanium.
10. The sample preparation method according to any one of claims 1 to 9, comprising the steps of:
(1) turning high-purity titanium with the purity of more than or equal to 99.9 wt% into a filament shape with the width of 5-15 mm, washing the turned high-purity titanium for 3-5 min by using mixed acid with the volume ratio of nitric acid to hydrofluoric acid being 1 (1.5-2.5), wherein the concentration of the nitric acid is 62-68 wt%, the concentration of the hydrofluoric acid is 37-43 wt%, and drying under a solar lamp to obtain pretreated high-purity titanium;
(2) mixing the mixed acid and pure water according to the volume ratio of (1-1.2) to 1 to obtain a corrosive solution, mixing the pretreated high-purity titanium obtained in the step (1) with the corrosive solution according to the ratio of (0.04-0.06) g:1mL, dispersing in a microwave digestion device at 87-97 ℃ for 3-5 hours, and preheating the microwave digestion device to the dispersing temperature before dispersion to obtain a solution to be detected;
(3) and (3) sequentially sampling, carrying out on-machine detection and carrying out data processing on the solution to be detected in the step (2) to obtain the granularity of the high-purity titanium.
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