Preparation process of multi-particle-size standard particle calibration solution

Abstract

The present application relates to the technical field of preparation of particle size standard calibration solution, and particularly relates to a preparation process of multi-particle size standard particle calibration solution, which comprises the following steps: putting multi-particle size standard particles with traceability diameter size into a prepared blank reference solution; simultaneously adding antioxidants, water absorbents, dispersants and flocculants; preparing through temperature rising-constant temperature-temperature lowering isothermal control cycle and stirring process; cross testing and evaluating the multi-particle size standard particle calibration solution in preparation through a particle counter with traceability; comparing and obtaining threshold spectrum and pulse wave spectrum corresponding to particle size in the multi-particle size standard particle calibration solution; and finally obtaining the multi-particle size standard particle calibration solution with traceability value transmission.

Description

Technical Field

[0001] This invention relates to the field of particle size standard calibration solution preparation technology, and in particular to a preparation process of multi-particle size standard particle calibration solution. Background Technology

[0002] Liquid particle counters are used to detect parameters such as particle size and quantity in liquids. Based on the principle of optical obscuration, a laser beam disappears after passing through the particles being measured, and the laser receiver, unable to receive the signal, tracks and records it. The laser receiver converts the received light signal into a voltage signal. By amplifying, processing, and removing impurities from threshold spectrum and pulse spectrum data using an industrial control computer, the correlation between particle size and quantity is obtained, thus determining the particle size and quantity in the liquid.

[0003] The disadvantages of existing technologies are: 1. The particle size standard calibration solution has few particle size points and large intervals between calibration points, resulting in a large difference between the curve fitting after instrument calibration and the actual situation; 2. The concentration range is small, making it impossible to form a three-dimensional model, resulting in poor traceability; 3. According to the calibration and verification specifications, metrologists need to configure it themselves, which is complicated to operate, and the different skill levels of personnel lead to large individual differences. Summary of the Invention

[0004] The purpose of this invention is to provide a preparation process for a multi-size standard particle calibration solution, thereby addressing the shortcomings of existing technologies.

[0005] Solution to the technical problem of the present invention:

[0006] This invention provides a process for preparing a calibration solution of multi-size standard particles, the process comprising the following steps:

[0007] A process for preparing a calibration solution of multi-size standard particles, characterized by comprising the following steps:

[0008] Step 1: Prepare the preparation tools;

[0009] Step 2: Prepare blank reference solution and purify the blank reference solution to remove impurities;

[0010] Step 3: Prepare a multi-size standard particle calibration solution from the solution obtained in Step 2 using a temperature-controlled cycle of heating-constant temperature-cooling.

[0011] Step 4: When preparing the multi-size standard particle calibration solution in step 3, perform cross-testing and evaluation on the solution obtained in step 3 to obtain the threshold spectrum and pulse spectrum corresponding to the particle size in the multi-size standard particle calibration solution.

[0012] Step 5: Compare the threshold spectrum and pulse spectrum corresponding to the particle size in the obtained multi-size standard particle calibration solution until the requirements are met, and obtain a multi-size standard particle calibration solution with traceable value transfer.

[0013] Preferably, the temperature control cycle preparation process of heating-constant temperature-cooling is as follows:

[0014] Increase the temperature by raising the blank standard solution from room temperature at a rate of 1℃ / min until it reaches 82℃;

[0015] After maintaining a constant temperature, add multi-size standard particles with traceable diameters. After maintaining a constant temperature for 2 hours, add antioxidants, water absorbents, and dispersants. Then, raise the temperature to 100°C at a rate of 1°C / min and maintain a constant temperature for 2 hours.

[0016] Cooling: The temperature was lowered from 100℃ to 82℃ at a rate of 1℃ / min and held for 2 hours. Then flocculant was added, and the temperature was lowered from 82℃ to 42℃ at a rate of 1℃ / min and held for 2 hours. Finally, the temperature was lowered to room temperature.

[0017] Preferably, the diameters of the multi-size standard particles with traceable diameters are 0.5μm to 100μm and 1μm to 70μm.

[0018] Preferably, the mass ratio of the multi-size standard particles with traceable diameter to the antioxidant is 1:155 to 255.

[0019] Preferably, the mass ratio of the antioxidant, water absorbent and dispersant is 1:4.5-5.5:1.5-2.5.

[0020] Preferably, the mass ratio of the flocculant to the dispersant is 1:1.

[0021] Preferably, step 4 specifically includes:

[0022] The solution obtained in step 3 was cross-tested and evaluated using a traceable particle counter to obtain the corresponding threshold spectrum and pulse spectrum.

[0023] Preferably, the traceable particle counter is a PLD-0201 liquid particle counter.

[0024] The beneficial effects of this invention are: by preparing a multi-size standard particle calibration solution, a traceable measurement value transfer multi-size standard particle calibration solution is obtained, which improves the accuracy, repeatability and stability of liquid particle counter calibration, eliminates the interference of the standard equipment's own error and the uneven distribution of particles in the liquid on the calibration results; and realizes automated calibration of multiple particle size points, improving calibration efficiency. Attached Figure Description

[0025] Figure 1 A flowchart illustrating the preparation process of a multi-size standard particle calibration solution provided for the implementation of this invention. Detailed Implementation

[0026] To facilitate understanding of this application, a more complete description will be provided below with reference to the accompanying drawings. Preferred embodiments of this application are shown in the drawings. However, this application can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a more thorough and complete understanding of the disclosure of this application.

[0027] refer to Figure 1 This invention provides a process for preparing a calibration solution of multi-size standard particles, which includes the following steps:

[0028] Step 1: Prepare the preparation tools;

[0029] Step 2: Prepare blank reference solution and purify the blank reference solution to remove impurities;

[0030] Step 3: Prepare a multi-size standard particle calibration solution from the solution obtained in Step 2 using a temperature-controlled cycle of heating-constant temperature-cooling.

[0031] Step 4: When preparing the multi-size standard particle calibration solution in step 3, perform cross-testing and evaluation on the solution obtained in step 3 to obtain the threshold spectrum and pulse spectrum corresponding to the particle size in the multi-size standard particle calibration solution.

[0032] Step 5: Compare the threshold spectrum and pulse spectrum corresponding to the particle size in the obtained multi-size standard particle calibration solution until the requirements are met, and obtain multi-size standard particle calibration with traceable value transfer.

[0033] Specifically, the preparation of 10L of a 5mg / L multi-size standard particle calibration solution will be used as an example:

[0034] Step 1: The preparation tools can include a reaction vessel, stirrer, temperature sensor, pressure sensor, flow meter, power pump, pipette, and beaker. At the same time, the above preparation tools need to be cleaned, such as the reaction vessel, pipette, and beaker, so that the preparation tools meet the process requirements of ISO 3722 "Hydraulic transmission - Identification of cleaning methods for sampling containers".

[0035] Step 2: Use a power pump to transfer the polyalphaolefin to the reactor. In the reactor, the polyalphaolefin is dehydrated, purified and impurities removed to obtain 10L of blank reference solution that meets the requirements. Continue stirring with a stirrer, measure the temperature with a temperature sensor, measure the pressure in the reactor with a pressure sensor, and measure the purification flow rate during the purification process with a flow meter.

[0036] The purification and impurity removal requirements are as follows: no precipitable impurities or components should be introduced; purity ≥ 99.9%; water content ≤ 0.01%; mechanical impurities ≤ 0.1%; and 0.5μm particle size ≤ 2 particles / ml.

[0037] Step 3 includes the following steps:

[0038] Heating: Place 10L of blank standard solution into the preparation container, and then increase the temperature from room temperature at 1℃ / min until it reaches 82℃;

[0039] The sample was kept at a constant temperature. Then, using a beaker, 5 mg of traceable, multi-size standard particles of various diameters were placed into the preparation container. The traceability standard was certified by the National Institute of Standards and Technology (NIST) as SRM-2806b, conforming to ISO ACFTD or MTD standards. The diameters of the traceable standard particles ranged from 0.5 μm to 100 μm and from 1 μm to 70 μm, with at least 15 different particle sizes. The concentration added was sufficient to cover the maximum detection range of the liquid particle counter. Next, 1 g of antioxidant, 5 g of desiccant, 2 g of dispersant, and 2 g of flocculant were added to the preparation container using a pipette. The antioxidant was IRGANOX B225 (antioxidant 1010) from Germany. Finally, the temperature was increased to 100 °C at a rate of 1 °C / min and held for 2 hours.

[0040] Cooling: The temperature was lowered from 100℃ to 82℃ at a rate of 1℃ / min and held for 2 hours. Then, 2g of flocculant was added, and the temperature was lowered to 42℃ and held for 2 hours in a sealed container. Finally, the temperature was lowered to room temperature in a sealed container.

[0041] Step 4: Cross-test and evaluate the prepared multi-size standard particle calibration solution using a traceable PLD-0201 particle counter. The PLD-0201 particle counter is traceable to standard materials from the Institute of Chemical Metrology and Analysis, National Center for Standard Materials Research, China National Institute of Metrology, and to standard materials from the National Institute of Standards and Technology (NIST), USA. By obtaining a traceable multi-size standard particle calibration solution, the liquid particle counter can be used for effective traceable metrological calibration applications.

[0042] Step 5: Compare the threshold spectrum and pulse spectrum corresponding to the particle size in the obtained multi-size standard particle calibration solution until the requirements are met, and obtain a multi-size standard particle calibration solution with traceable value transfer.

[0043] The specific number of threshold spectra of multi-size standard particles is obtained as the standard particle size value, and the specific number of pulse spectra of multi-size standard particles is obtained as the standard particle quantity value.

[0044] The method allows for comparison and acquisition of threshold spectra and pulse spectra corresponding to the particle sizes in the calibration solution of multi-size standard particles.

[0045] Threshold spectra were used to establish the particle size model relationship between the standard materials of the Institute of Chemical Metrology and Analytical Science (National Center for Standard Materials Research) of the National Institute of Metrology, China, and the particle size model relationship between the standard materials of the National Institute of Standards and Technology (NIST) of the United States and the particle size model relationship between the standard materials of the National Institute of Standards and Technology (NIST) of the United States, ... standard materials of the standard materials.

[0046] Threshold spectra and pulse spectra corresponding to the particle sizes in the multi-size standard particle calibration solution were compared and obtained; finally, 10L of multi-size standard particle calibration solution with a 5mg / L concentration and traceable value transfer was obtained.

[0047] By obtaining a 5 mg / L multi-size standard particle calibration solution with traceable metrological transfer, effective traceable metrological calibration applications can be performed on liquid particle counters.

Claims

1. A preparation process for a calibration solution of multi-size standard particles, characterized in that, Includes the following steps: Step 1: Prepare the preparation tools; Step 2: Prepare a blank reference solution and purify it to remove impurities. The purification and impurity removal shall meet the following requirements: no precipitating impurities or components shall be introduced, purity ≥ 99.9%, water content ≤ 0.01%, mechanical impurities ≤ 0.1%, and 0.5 μm particle size ≤ 2 particles / ml. Step 3: Prepare a multi-size standard particle calibration solution from the solution obtained in Step 2 using a temperature-controlled cycle of heating-isothermal-cooling; the specific process of the temperature-controlled cycle of heating-isothermal-cooling is as follows: Increase the temperature by raising the blank standard solution from room temperature at a rate of 1℃ / min until it reaches 82℃; The sample was kept at a constant temperature. Multi-size standard particles with traceable diameters were added. After keeping the sample at a constant temperature for 2 hours, antioxidants, water-absorbing agents, and dispersants were added. The temperature was then increased to 100°C at a rate of 1°C / min and kept at a constant temperature for 2 hours. The diameters of the multi-size standard particles with traceable diameters were 0.5μm~100μm and 1μm~70μm. Cooling: The temperature was lowered from 100℃ to 82℃ at a rate of 1℃ / min and held for 2 hours. Then flocculant was added, and the temperature was lowered from 82℃ to 42℃ at a rate of 1℃ / min and held for 2 hours. Finally, the temperature was lowered to room temperature. Step 4: When preparing the multi-size standard particle calibration solution in step 3, perform cross-testing and evaluation on the solution obtained in step 3 to obtain the threshold spectrum and pulse spectrum corresponding to the particle size in the multi-size standard particle calibration solution. Step 5: Compare the threshold spectrum and pulse spectrum corresponding to the particle size in the obtained multi-size standard particle calibration solution until the requirements are met, and obtain a multi-size standard particle calibration solution with traceable value transfer.

2. The preparation process of a multi-size standard particle calibration solution according to claim 1, characterized in that, The mass ratio of the multi-size standard particles with traceable diameter to the antioxidant is 1:155~255.

3. The preparation process of a multi-size standard particle calibration solution according to claim 2, characterized in that, The mass ratio of the antioxidant, water absorbent, and dispersant is 1:4.5~5.5:1.5~2.

5.

4. The preparation process of a multi-size standard particle calibration solution according to claim 3, characterized in that, The mass ratio of the flocculant to the dispersant is 1:

1.

5. The preparation process of a multi-size standard particle calibration solution according to claim 4, characterized in that, Step 4 specifically involves: The solution obtained in step 3 was cross-tested and evaluated using a traceable particle counter to obtain the corresponding threshold spectrum and pulse spectrum.

6. The preparation process of a multi-size standard particle calibration solution according to claim 5, characterized in that, The traceable particle counter is a PLD-0201 liquid particle counter.

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