This standard specifies the conditions and procedures for determining the particle distribution of ceramic raw materials and pigments by sedimentation analysis. This standard is applicable to the determination of the particle distribution of ceramic raw materials and ceramic pigments with a particle diameter not greater than 63μm. QB/T 1465-1992 Method for determining the particle distribution of ceramic raw materials and pigments QB/T1465-1992 Standard download decompression password: www.bzxz.net

Light Industry Industry Standard of the People's Republic of China
Method for Determining Particle Distribution of Ceramic Raw Materials and Pigments 1 Subject Content and Scope of Application
This standard specifies the conditions and steps for determining the particle distribution of ceramic raw materials and pigments by sedimentation analysis. QB/T1465-1992
This standard is applicable to the determination of particle distribution of ceramic raw materials and ceramic pigments with a particle diameter not exceeding 63 um. 2 Reference Standards
QB/T1010 Method for Determining True Density of Daily Ceramic Materials and Pigments 3 Principle and Test Conditions
3.1 Principle
According to Stoles's law, the particle distribution of the sample is determined by sedimentation analysis under stagnant flow conditions (i.e., Reynolds number is not greater than 0.3). 3.2 Test Conditions
3.2.1 The dispersion medium should be adapted to the sample properties and instrument characteristics, and its viscosity value should be adjusted according to the temperature changes to meet the requirements of 3.1. 3.2.2 During the test, the room temperature fluctuation shall not exceed ±2°C. 3.2.3 Before testing, the sample should be dried as required, and the true density of the sample should be measured according to QB/T1010. 4 Reagents
4. Sodium hexametaphosphate (AR).
4.2 Anhydrous ethanol (AR). Propylene glycol (AR). 5 Instruments
5.1 Two ampoule bottles with a volume of 500~600ml, 0~200mm scale, and a pipette bubble chamber with a volume of 10ml. or a particle analyzer designed based on the Stores sedimentation law. 5.2 An ultrasonic disperser.
5.3 A 0.1mg sensitivity platform.
5.4 A stopwatch.
5.5 Several thousand 250, 100, 50ml beakers, and a 100mlL measuring cylinder. 5.6 A drying oven.
5.7 A mercury thermometer with a graduation value of 1C. 6 Determination steps
6.1 Ampere flask method (arbitration method)
6.1.1 Instrument calibration
Insert a dry pipette into an ampere flask filled with distilled water to a certain height, turn the double-pass stopper to absorb the distilled water into the bubble chamber to the scale; then, turn the double-pass stopper to the liquid discharge position, carefully transfer the water into a 50ml beaker of known weight, and weigh it. Repeat three times, and take the average value as the volume of the bubble chamber
QB/T 1465—1992
Pour distilled water into the sedimentation bottle to the full scale, and use a measuring stick to measure the volume V of the distilled water injected. Pour distilled water into the sedimentation bottle to 180mm, insert a pipette, read the liquid level hl, and calculate the height increment by △h1-h1-180. When the liquid level is h1, take samples three times, read the liquid level height h2 at the end, and calculate the height of the sampled liquid level drop by △hz-(hl-h2)/3.
6.1.2 Weigh the sample according to the provisions of 3.2.3, and its mass is calculated according to formula (1): mo=nVp
Where: m1-mass of the sample, g;
n——viscosity value of water at the test temperature; V——volume of the sedimentation bottle at full scale, mL; P.·True density of the sample, g/cm2.
6.1.3 Determination of Samples
Transfer the sample to a 250mL beaker, add an appropriate amount of dispersion medium and an appropriate amount of 0.2% sodium hexametaphosphate solution according to the requirements of 3.2.1, soak for 3~5h, place the beaker in an ultrasonic disperser and fully oscillate and disperse for about 15min, and cool to room temperature. Transfer the dispersed and cooled sample to a sedimentation bottle without damage, fill the dispersion medium to the 200mm scale according to the requirements of 3.2.1, insert a pipette, repeatedly invert the sedimentation bottle for about 5min, 4~8 times/min, and let it stand. Immediately start the stopwatch and record the sedimentation start time. Calculate the corresponding sampling time according to the required Stoles diameter of each level of particle limit; (For the calculation method of t, see Appendix A). Sampling starts 10s before t and ends within 20s. Transfer the aspirated liquid to a 50mL beaker of known weight, wash the bubble chamber with distilled water, and allow the aspirated liquid to enter the beaker without damage.
Dry the absorbed liquid to constant weight at a temperature below 110°C, and weigh it to obtain mi. 6.1.4 Calculation of analytical results
The mass of sodium hexametaphosphate in the evaporation residue is calculated according to formula (2): mz-
Wherein: m?-mass of sodium hexametaphosphate in the evaporation residue, g; V,-volume of the pipette bubble chamber, mL;
V-volume of the sedimentation bottle when it is full scale, ml.;
Total amount of sodium hexametaphosphate added. g.
The cumulative percentage of particle distribution is calculated according to formula (3): P(%) =
Wherein: P: \-·Cumulative percentage of particle distribution (take three significant figures), %; m
The mass of the component less than the limiting Stoles diameter d (minus m) + g: m. Sample mass·g.
6.1.5 Deviation
The same sample is measured in parallel. The weight cumulative percentage of the same limiting Stoles diameter shall not be greater than 3%. 6.2 Instrumental methodbZxz.net
(2)
6.2.1 Prepare the sample according to the instrument requirements and determine the test conditions. 6.2.2 Place the sample in a 100mL beaker, add an appropriate amount of dispersion medium and an appropriate amount of 0.2% sodium hexametaphosphate solution according to the requirements of 3.2.1, and soak for about 5 hours.
6.2.3 Place the soaked sample in an ultrasonic disperser, fully oscillate and disperse for about 15 minutes, and then cool to room temperature. 6.2.4 Move the dispersed sample into the sample chamber of the instrument and circulate it for 3 minutes according to the instrument operating instructions to make the particles evenly distributed: measure the sample three times and take the average value as the test result. 137
6.2.5 Deviation
QB/T 1465 1992
When the same sample is tested three times, the weight cumulative percentage of the same limit of Stoles diameter shall not be greater than 5%. Test report
The test report shall include the following contents:
a. Sample name, true density;
b. Medium name, density and viscosity;
c. Test time, test temperature;
d. The percentage or cumulative percentage of each particle size of the sample, 138
QB/T 14651992
Appendix A
Calculation of sampling time corresponding to the limiting Stoles diameter of each level (supplement)
The sampling time corresponding to the required limiting Stoles diameter of each level is calculated according to formula (A1): AT
18·h·n
(p,- p)g+d?
Where: t,—sampling time corresponding to the limiting Stoles diameter of each level S: h, liquid level height at the time of the first sampling, cm; n——dispersion medium viscosity, Pa·s;
pi--true density of sample, g/cm
P2--medium density·g/cm\;
g—gravitational acceleration.980cm/s\;
d—-the limiting Stoles diameter required.cm. A2h, calculated according to formula (A2):
h; = (200 + Ah) -(i -- 1)Ahz Where: h, - height of liquid level at the time of i-th sampling, cm; i.1,2,3.+
Ah, Ahz see the introduction of the Amersfoort method.
Additional notes:
This standard is proposed by the Quality Standards Department of the Ministry of Light Industry. This standard is under the jurisdiction of the National Ceramic Standardization Center. This standard is drafted by the Ceramic Research Institute of the Ministry of Light Industry. The main drafters of this standard are Xu Lihua, Li Feng, and Ao Jingqiu. ·(AI)
·（A2)
From the date of implementation of this standard, the former Ministry of Light Industry standard QB898-1983 "Daily Ceramic Raw Materials, Pigment Particle Distribution Determination Method" shall be abolished.
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