CN104568540A - Preparation method for wide-size-distribution standard particle solid sample - Google Patents
Preparation method for wide-size-distribution standard particle solid sample Download PDFInfo
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- CN104568540A CN104568540A CN201410813029.1A CN201410813029A CN104568540A CN 104568540 A CN104568540 A CN 104568540A CN 201410813029 A CN201410813029 A CN 201410813029A CN 104568540 A CN104568540 A CN 104568540A
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Abstract
The invention discloses a preparation method for a wide-size-distribution standard particle solid sample. The method is characterized by comprising the following steps: pre-determining the sizes and mixing proportion of narrow-distribution standard particles for proportioning for a wide size distribution index of the standard particles to be achieved; proportioning and mixing the narrow-distribution standard particles according to a corresponding proportion, and dispersing the mixed wide-size-distribution particles in a sample cell by adopting a dispersing agent; curing the dispersing agent to form the wide-size-distribution standard particle solid sample during the suspension and dispersion of the particles; sequentially determining the sizes of the particles in the solid sample to obtain the real size value and distribution of the standard particle solid sample for the calibration of a size analyzer by adopting a microscope. The preparation method has the benefits that the size value and distribution of the wide-size-distribution standard particle solid sample can be accurately known, the size distribution range is wide, flexible and controllable, and the wide-size-distribution standard particle solid sample is easily stored for a long time, and is reusable.
Description
Technical field
The present invention relates to a kind of preparation method of standard particle sample, particularly a kind of wide size-grade distribution, can be used for the granular solid sample and preparation method thereof that particle-size measuring instrument device demarcates.
Background technology
Grain graininess measurement demand is extensively present in the fields such as the energy, chemical industry, power, food, pharmacy, and Calibration of measuring equipment is of great significance the normal use of instrument and the accuracy tool of measurement result.The demarcation of current particle-size measuring instrument device generally adopts the standard particle sample of narrow ditribution, namely particle size distribution is more concentrated, the particulate samples being considered as single particle size can be similar to, and use gas or liquid as dispersion medium, gather corresponding signal when standard particle is suspended in or flow through measured zone; Along with the increasingly stringent of granulometry standard, measure the grain graininess of wide Size Distribution, namely grain size does not concentrate near a certain particle size values that the grain graininess measurement of wider distribution is had higher requirement.The standard model of wide size-grade distribution particle is generally obtained by the standard particle proportioning of narrow ditribution, and how to ensure the homogeneity that different-grain diameter particle disperses in the solution in measuring process and how to determine the True Data of measured zone grain graininess and distribution, be the difficult problem that the wide particle size distribution measurement of grain graininess instrument is demarcated.
Summary of the invention
In order to overcome the difficult problem that the wide particle size distribution measurement of grain graininess instrument is demarcated, the present invention proposes a kind of preparation method of solid sample of wide size-grade distribution standard particle, for the demarcation of grain graininess instrument when wide particle size distribution measurement, it has the following advantages: sample granularity value and distribution accurately known, particle size distribution range greatly and controlled flexibly, easily permanent preservation, reusable.
Ultimate principle of the present invention: for incomprehensiveness and the uncontrollability of routine wide distribution standard particulate samples fmer-granularity, adopt the method that spreading agent is solidified, standard model particle " is freezed " in spreading agent, microscope is then adopted to carry out the particle of " freezing " measuring the accurate particle diameter obtaining particle in sample, obtain accurate wide particle size distribution data, as the reference of grain graininess instrument calibration result; For the wide size-grade distribution index intending reaching, can be realized by the particle size and blending ratio regulating the narrow ditribution standard particle being used for proportioning; To the surveying instrument based on different principle, the solid sample of difformity and size can be prepared to adapt to the requirement of measurement zone.
Based on foregoing invention principle, technical scheme of the present invention is: a kind of preparation method of standard particle solid sample of wide size-grade distribution, is characterized in, the step of this preparation method is:
1. selection standard particle type as required, refers to the distribution intending the wide size-grade distribution standard particle reached
Mark, precalculates particle size and the blending ratio of the narrow ditribution standard particle determining proportioning;
2. narrow ditribution standard particle is carried out proportioning mixing according to determined ratio;
3. select spreading agent to make mixed particle dispersed in sample cell;
4. when composite grain suspends and be dispersed, spreading agent is solidified, form the standard particle of wide size-grade distribution
Solid sample, carries out the demoulding or sample surfaces polishing;
5. employing microscope measures the grain diameter in solid sample one by one, obtains this wide size-grade distribution standard and consolidates
The true granularity of aspect product and distribution, for the demarcation of particle-size analyzer.
The invention has the beneficial effects as follows the method by making spreading agent solidify, the position of wherein particle is fixed, form the solid sample of wide size-grade distribution standard particle, its granularity and distribution accurately known, particle size distribution range greatly and controlled flexibly, to be preserved easily for a long time, reusable.
Accompanying drawing explanation
Fig. 1 is rectangular parallelepiped sample schematic diagram of the present invention;
Fig. 2 is truncated cone-shaped sample schematic diagram of the present invention.
Embodiment
A preparation method for the standard particle solid sample of wide size-grade distribution, its preparation process is:
1. selection standard particle type as required, as polystyrene or beaded glass standard particle; To the distribution index intending the wide size-grade distribution standard particle reached, precalculate particle size and the blending ratio of the narrow ditribution standard particle determining proportioning; As supposed, a wide size-grade distribution index is d
10=20 μm (namely the particle of less than 20 μm accounts for 10% of total particle quality, as follows), d
40=50 μm, d
95=100 μm, then can select the standard particle of 20 μm, 50 μm, 100 μm and 110 μm, carry out proportioning according to the ratio of mass percent 0.1:0.3:0.55:0.05; When wide distribution index is stricter, the narrow ditribution grain diameter progression of needs is more;
2. narrow ditribution standard particle is proportionally entered mixing, select rectangular parallelepiped sample cell or truncated cone-shaped sample cell as mould;
3. select proportioning to be the standard particle that the bisphenol A epoxide resin AB glue of 1:2 mixes as dispersant; Use injector for medical purpose, extract the AB glue that proportioning is good, for preventing bubble to be mixed into, needle point can be pulled out, utilizing Action of Gravity Field that AB glue in syringe is slowly flowed in rectangular parallelepiped or truncated cone-shaped sample cell, finally bottom sample cell, forming colloid thin layer.Test shows, this AB glue viscosity 100 degrees Celsius time is minimum, should extract colloid as early as possible at this temperature and inject rectangular parallelepiped sample cell or truncated cone-shaped sample cell;
4. colloid thin layer is solidified at the temperature of 80 degrees Celsius, when it does not solidify completely, in mould, evenly drop into the particle of narrow size-grade distribution.Treat that this colloid thin layer solidifies, in same sample pond, repeat above step, multilayer colloid will bond voluntarily in preparation process, and the wide size-grade distribution standard particle solid sample of final formation, carries out the demoulding or sample surfaces polishing as required;
5. employing microscope measures the grain diameter in solid sample one by one, obtains true granularity and the distribution of this wide size-grade distribution standard particle solid sample, for the demarcation of particle-size analyzer.
Claims (1)
1. a preparation method for the standard particle solid sample of wide size-grade distribution, is characterized in that, this preparation method
Step be:
Selection standard particle type, to the distribution index intending the wide size-grade distribution standard particle reached, in advance
Calculate the particle size and the blending ratio that determine the narrow ditribution standard particle of proportioning;
(2) narrow ditribution standard particle is carried out proportioning mixing according to determined ratio;
(3) spreading agent is selected to make mixed particle dispersed in sample cell;
(4) when composite grain suspended dispersed, spreading agent is solidified, form the solid-state sample of standard particle of wide size-grade distribution
Product, carry out the demoulding or sample surfaces polishing;
(5) employing microscope measures the grain diameter in solid sample one by one, obtains true granularity and the distribution of this wide size-grade distribution standard particle solid sample, for the demarcation of particle-size analyzer.
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Cited By (6)
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CN106248462A (en) * | 2016-10-14 | 2016-12-21 | 北京海岸鸿蒙标准物质技术有限责任公司 | For wide distributed granule standard substance calibrating particle size analyzer and preparation method thereof |
CN106248463A (en) * | 2016-10-14 | 2016-12-21 | 北京海岸鸿蒙标准物质技术有限责任公司 | For calibrating the standard substance of PM2.5 sickle and preparation thereof and valued methods |
CN106596546A (en) * | 2016-11-11 | 2017-04-26 | 中国科学院广州地球化学研究所 | Method for placing and screening mineral single particle sample on a microscope slide |
CN108279152A (en) * | 2017-12-28 | 2018-07-13 | 东北大学秦皇岛分校 | A kind of pulveryte particle dispersing method |
CN109655384A (en) * | 2019-01-29 | 2019-04-19 | 南开大学 | PM2.5Model particulate matter preparation method and model particulate matter |
CN113405954A (en) * | 2021-05-10 | 2021-09-17 | 上海市计量测试技术研究院 | Method for determining value of wide-distribution solid particle size standard substance applied to dry dispersion system of laser diffraction particle size analyzer |
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---|---|---|---|---|
CN106248462A (en) * | 2016-10-14 | 2016-12-21 | 北京海岸鸿蒙标准物质技术有限责任公司 | For wide distributed granule standard substance calibrating particle size analyzer and preparation method thereof |
CN106248463A (en) * | 2016-10-14 | 2016-12-21 | 北京海岸鸿蒙标准物质技术有限责任公司 | For calibrating the standard substance of PM2.5 sickle and preparation thereof and valued methods |
CN106596546A (en) * | 2016-11-11 | 2017-04-26 | 中国科学院广州地球化学研究所 | Method for placing and screening mineral single particle sample on a microscope slide |
CN106596546B (en) * | 2016-11-11 | 2019-05-17 | 中国科学院广州地球化学研究所 | A method of mineral individual particle sample is disposed and screened on microscopic slide |
CN108279152A (en) * | 2017-12-28 | 2018-07-13 | 东北大学秦皇岛分校 | A kind of pulveryte particle dispersing method |
CN109655384A (en) * | 2019-01-29 | 2019-04-19 | 南开大学 | PM2.5Model particulate matter preparation method and model particulate matter |
CN113405954A (en) * | 2021-05-10 | 2021-09-17 | 上海市计量测试技术研究院 | Method for determining value of wide-distribution solid particle size standard substance applied to dry dispersion system of laser diffraction particle size analyzer |
CN113405954B (en) * | 2021-05-10 | 2023-06-23 | 上海市计量测试技术研究院 | Method for determining wide-distribution solid granularity standard substance of dry dispersion system applied to laser diffraction granularity analyzer |
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