CN102890044A - Method for testing granularity of cast auxiliary materials - Google Patents
Method for testing granularity of cast auxiliary materials Download PDFInfo
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- CN102890044A CN102890044A CN2012103397907A CN201210339790A CN102890044A CN 102890044 A CN102890044 A CN 102890044A CN 2012103397907 A CN2012103397907 A CN 2012103397907A CN 201210339790 A CN201210339790 A CN 201210339790A CN 102890044 A CN102890044 A CN 102890044A
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Abstract
The invention belongs to the technical field of chemical analysis, and relates to a method for testing granularity of cast auxiliary materials. The method comprises the steps of: analyzing the granularity of the cast auxiliary material powder by a laser granularity analyzer, fully and evenly dispersing and transmitting samples to a main machine through an equipment accessory (a sample feeder), and selecting proper parameters to determine the granularity of the auxiliary material powder. The determination process is fast, simple and convenient, the sample consumption amount is few, the measurement range is from 0.1 to 2000micrometers, the result can be fast generated within one minute, the whole sample can be measured, even if measured samples (usually 4-10g of dried powder) are few, and all granules can still pass through laser bundles to obtain the diffraction of all samples.
Description
Technical field
The invention belongs to the chemical analysis technology field, relate to a kind of for the method for casting with the test of auxiliary material powder size.
Background technology
Laser diffraction technology is based on following principle: particle produces scattered light and the light intensity map that forms depends on particle size in all directions.In certain limit, the scatter graph of serial particle is equal to the stack of each particle scattering figure.By using mathematics overlay technique program to use optical model unit of account volume particles at the scatter diagram of selected grain size intervals, just can calculate the volume particle size distribution of particle.
At present, for this type of powder class, ball class granulometry sieve method commonly used, the method detection limit is of a size of 45 microns; When measuring dried powder, because particle is small and light, some powder can stick on the screen cloth, even in the process of sieve of shaking, and also have a small amount of powder screen cloth that flies out, thereby cause the reduction of analysis result accuracy; In addition, because the difference on the particle microscopic pattern, therefore sieve method can not obtain the size-grade distribution result of pin-point accuracy closer to the reduced size of measuring particle, and sieve method to have process loaded down with trivial details, length consuming time, the shortcoming such as amount of samples is large.
Summary of the invention
The purpose of this invention is to provide a kind of size-grade distribution result that can access pin-point accuracy, and weak point consuming time, the method that is used for casting usefulness auxiliary material testing graininess that amount of samples is little.Technical solution of the present invention is,
1) opens main frame and the injector power supply of laser particle analyzer, carry out the preliminary work of experiment;
2) preheating 20-50 minute, guarantee that the background of instrument and light intensity are in steady state (SS);
3) start injector, add entry and water is circulated in sampling system, sampling system is cleaned;
4) the instrument control software on the computing machine of click laser particle analyzer moves this control software, and instrument is connected with software;
5) instrument of opening on the computing machine is controlled the file that the record in the software is deposited, and is convenient to search in the future;
6) click hand push button in the measurement menu in the control software on the computing machine, enter measurement window, this moment observable whether measure background normal; If undesired then tackle sampling system and optical mirror slip cleans;
7) enter options menu in the control software on the computing machine, the input sample message, sample message comprises: sample refractive index, granule absorbance, obscurity, and record the information in the file that the record on the computing machine deposits;
8) pump speed of adjustment injector is 2700-3250 rev/min, the start button of clicking in the measurement window is measured sample, in injector, add sample size to the obscurity of control according to prompting, again click the start button in the measurement window, measure the granularity of sample, measurement result can be deposited in the file of step 5) selection by number automatically;
9) after measurement is finished, outwell the water in the injector, it is normal to measuring background to change clear water wash cycles sampling system;
10) shut down computer successively, injector, host power supply.
Described sample is zirconium English powder, Al
2O
3, glass dust or zirconium English powder and glass dust mixed powder, blending ratio is 1:1, the refractive index of zirconium English powder is 1.4 or 1.6 or 1.97, granule absorbance is 0.01 or 0.5 or 1.0, Al
2O
3Refractive index be 1.765 or 1.768 or 1.304, granule absorbance is 0.1 or 0.01, and the refractive index of glass dust is 1.466 or 1.458 or 1.452, and granule absorbance is 0.1, the refractive index of mixed powder is 1.730 or 1.830 or 1.930, and granule absorbance is 0.01 or 0.5 or 1.0.
The advantage that the present invention has and beneficial effect, the present invention adopts laser particle size analyzer that casting is analyzed with the auxiliary material powder size, sample fully is uniformly dispersed and is sent to main frame by equipment appurtenance (injector), select suitable parameter that the granularity of auxiliary material powder is measured, the mensuration process is fast and convenient, amount of samples is few, from 0.1 to 2000 micron of measurement range, within one minute, can bear results fast, and it can measure whole sample, even amount sample few (usually dried powder 4-10 gram), thereby still can make all particles obtain the diffraction of whole samples by laser beam.
Embodiment
This method realizes by following step:
1) opens main frame and the injector power supply of laser particle analyzer, carry out the preliminary work of experiment;
2) preheating 20-50 minute, guarantee that the background of instrument and light intensity are in steady state (SS);
3) start injector, add entry and water is circulated in sampling system, sampling system is cleaned;
4) the instrument control software on the computing machine of click laser particle analyzer moves this control software, and instrument is connected with software;
5) instrument of opening on the computing machine is controlled the file that the record in the software is deposited, and is convenient to search in the future;
6) click hand push button in the measurement menu in the control software on the computing machine, enter measurement window, this moment observable whether measure background normal; If undesired then tackle sampling system and optical mirror slip cleans;
7) enter options menu in the control software on the computing machine, the input sample message, sample message comprises: sample refractive index, granule absorbance, obscurity, and record the information in the file that the record on the computing machine deposits;
8) pump speed of adjustment injector is 2700-3250 rev/min, the start button of clicking in the measurement window is measured sample, in injector, add sample size to the obscurity of control according to prompting, again click the start button in the measurement window, measure the granularity of sample, measurement result can be deposited in the file of step 5) selection by number automatically;
9) after measurement is finished, outwell the water in the injector, it is normal to measuring background to change clear water wash cycles sampling system;
10) shut down computer successively, injector, host power supply.
Embodiment one
1. start: open instrument host and injector power supply.
2. preheating time: 30 minutes.
3. starting injector after preheating finishes gets up by the dispersion medium water circulation.
4. startup computing machine, double click operation software enters function software.
5. open existing file or new files, record is left under your the needed file.
6. click " manually " button in " measurement " menu, enter measurement window.
7. determine that background state is normal, can measure.
8. enter " option " menu: input following parameter:
Sample introduction pump speed: 3250 rev/mins; The sample measurement time: 10 seconds; Background Measuring Time: 5 seconds; Postpone between the measurement: 5 seconds; Particle shape: irregular; Spreading agent: water; Analytical model: general.Enter " document " menu, the information such as input sample title and lot number.
9. after setting up, click START button, system begins to measure by step.
10. when having surveyed background and prompting adding sample, add sample in the obscurity scope of control, then click " beginning " and measure sample.Every measurement once, the result can exist in the file by record number.Click " measurement sample ", the duplicate measurements secondary.
11. after measurement is finished, sample solution is outwelled, is used clear water wash cycles one to secondary (normally being as the criterion with background).
12. shutdown: close first computing machine, close again injector and main frame.
Embodiment two
1. start: open instrument host and injector power supply.
2. preheating time: 50 minutes.
3. starting injector after preheating finishes gets up by the dispersion medium water circulation.
4. startup computing machine, double click operation software enters function software.
5. open existing file or new files, record is left under your the needed file.
6. click " manually " button in " measurement " menu, enter measurement window.
7. determine that background state is normal, can measure.
8. enter " option " menu: input following parameter:
Sample introduction pump speed: 2950 rev/mins; The sample measurement time: 6 seconds; Background Measuring Time: 7 seconds; Postpone between the measurement: 10 seconds; Particle shape: irregular; Spreading agent: water; Analytical model: general.Enter " document " menu, the information such as input sample title and lot number.
9. after setting up, click START button, system begins to measure by step.
10. when having surveyed background and prompting adding sample, add sample in the obscurity scope of control, then click " beginning " and measure sample.Every measurement once, the result can exist in the file by record number.Click " measurement sample ", duplicate measurements three times.
11. after measurement is finished, sample solution is outwelled, is used clear water wash cycles two to four times (normally being as the criterion with background).
12. shutdown: close first computing machine, close again injector and main frame.
Embodiment three
1. start: open instrument host and injector power supply.
2. preheating time: 40 minutes.
3. starting injector after preheating finishes gets up by the dispersion medium water circulation.
4. the startup computing machine is double-clicked the Mastersizer2000 function software, enters function software.
5. open existing file or new files, record is left under your the needed file.
6. click " manually " button in " measurement " menu, enter measurement window.
7. determine that background state is normal, can measure.
8. enter " option " menu: input following parameter:
Sample introduction pump speed: 2850 rev/mins; The sample measurement time: 6 seconds; Background Measuring Time: 6 seconds; Postpone between the measurement: 10 seconds; Particle shape: irregular; Spreading agent: water; Analytical model: general.Enter " document " menu, the information such as input sample title and lot number.
9. after setting up, click START button, system begins to measure by step.
10. when having surveyed background and prompting adding sample, add sample in the obscurity scope of control, then click " beginning " and measure sample.Every measurement once, the result can exist in the file by record number.Click " measurement sample ", duplicate measurements four times.
11. after measurement is finished, sample solution is outwelled, is used clear water wash cycles two to three times (normally being as the criterion with background).
12. shutdown: close first computing machine, close again injector and main frame.
Claims (2)
1. one kind is used for casting with the method for auxiliary material testing graininess, it is characterized in that,
1) opens main frame and the injector power supply of laser particle analyzer, carry out the preliminary work of experiment;
2) preheating 20-50 minute, guarantee that the background of instrument and light intensity are in steady state (SS);
3) start injector, add entry and water is circulated in sampling system, sampling system is cleaned;
4) the instrument control software on the computing machine of click laser particle analyzer moves this control software, and instrument is connected with software;
5) instrument of opening on the computing machine is controlled the file that the record in the software is deposited, and is convenient to search in the future;
6) click hand push button in the measurement menu in the control software on the computing machine, enter measurement window, this moment observable whether measure background normal; If undesired then tackle sampling system and optical mirror slip cleans;
7) enter options menu in the control software on the computing machine, the input sample message, sample message comprises: sample refractive index, granule absorbance, obscurity, and record the information in the file that the record on the computing machine deposits;
8) pump speed of adjustment injector is 2700-3250 rev/min, the start button of clicking in the measurement window is measured sample, in injector, add sample size to the obscurity of control according to prompting, again click the start button in the measurement window, measure the granularity of sample, measurement result can be deposited in the file of step 5) selection by number automatically;
9) after measurement is finished, outwell the water in the injector, it is normal to measuring background to change clear water wash cycles sampling system;
10) shut down computer successively, injector, host power supply.
2. according to claim 1 a kind of for the method for casting with the auxiliary material testing graininess, it is characterized in that described sample is zirconium English powder, Al
2O
3, glass dust or zirconium English powder and glass dust mixed powder, blending ratio is 1:1, the refractive index of zirconium English powder is 1.4 or 1.6 or 1.97, granule absorbance is 0.01 or 0.5 or 1.0, Al
2O
3Refractive index be 1.765 or 1.768 or 1.304, granule absorbance is 0.1 or 0.01, and the refractive index of glass dust is 1.466 or 1.458 or 1.452, and granule absorbance is 0.1, the refractive index of mixed powder is 1.730 or 1.830 or 1.930, and granule absorbance is 0.01 or 0.5 or 1.0.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020071119A1 (en) * | 2000-12-08 | 2002-06-13 | Horiba, Ltd. | Particle size distribution measuring apparatus |
| US20020180972A1 (en) * | 1999-12-06 | 2002-12-05 | Ansari Rafat Razak | Particle sizing of flowing fluids, dispersion, and suspension |
| CN101598656A (en) * | 2009-07-21 | 2009-12-09 | 长沙东星仪器有限责任公司 | Fineness measurement device for pulverized coal |
| CN102252944A (en) * | 2011-05-06 | 2011-11-23 | 清华大学 | Measurement method for particle size |
-
2012
- 2012-09-14 CN CN2012103397907A patent/CN102890044A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020180972A1 (en) * | 1999-12-06 | 2002-12-05 | Ansari Rafat Razak | Particle sizing of flowing fluids, dispersion, and suspension |
| US20020071119A1 (en) * | 2000-12-08 | 2002-06-13 | Horiba, Ltd. | Particle size distribution measuring apparatus |
| CN101598656A (en) * | 2009-07-21 | 2009-12-09 | 长沙东星仪器有限责任公司 | Fineness measurement device for pulverized coal |
| CN102252944A (en) * | 2011-05-06 | 2011-11-23 | 清华大学 | Measurement method for particle size |
Non-Patent Citations (4)
| Title |
|---|
| 张训彪等: "《中华人民共和国国家标准 GB/T 19077.1-2008》", 16 April 2008, article "粒度分析 激光衍射法 第1部分：通则" * |
| 赵云普等: "《中华人民共和国有色金属行业标准 YS/T 617.7-2007》", 13 April 2007, article "铝、镁及合金粉理化性能测定方法 第7部分：粒度分布的测定 激光散射/衍射法" * |
| 陈强等: "《中华人民共和国国家标准 GB/T 21779-2008》", 12 May 2008, article "金属粉末和相关化合物粒度分布的光散射试验方法" * |
| 黄宁等: "《中华人民共和国国家标准 GB/T 21782.13-2009》", 2 June 2009, article "粉末涂料 第13部分：激光衍射法分析粒度" * |
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Application publication date: 20130123 |