GB/T 24203-2024 PDF English
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Method for determination of bulk density, true density, true porosity and open porosity of carbon materials
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| GB/T 24203-2009 | English | 139 |
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Carbon materials -- Determination of the true density or true porous -- Boiling method
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GB/T 24203-2024: Method for determination of bulk density, true density, true porosity and open porosity of carbon materials
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GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 29.050
CCS Q 52
Replacing GB/T 24203-2009, GB/T 24528-2009, GB/T 24529-2009
Method for determination of bulk density, true density, true
porosity and open porosity of carbon materials
Issued on: SEPTEMBER 29, 2024
Implemented on: APRIL 01, 2025
Issued by. State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword... 3
1 Scope... 5
2 Normative references... 5
3 Terms and definitions... 5
4 Determination of bulk density... 5
5 Determination of true density... 7
6 Determination of true porosity... 15
7 Determination of open porosity... 16
8 Test report... 19
Method for determination of bulk density, true density, true
porosity and open porosity of carbon materials
1 Scope
This document specifies the method for determination of bulk density, true density, true
porosity and open porosity of carbon materials.
This document is applicable to the determination of bulk density, true density, true
porosity and open porosity of carbon materials at room temperature.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this
document and are indispensable for its application. For dated references, only the
edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
GB/T 1427, Sample method of carbon material
GB/T 1997, Coke-sampling and preparation of samples
GB/T 8170, Rules of rounding off for numerical values & expression and judgment
of limiting values
GB/T 8718, The terms of carbon materials
3 Terms and definitions
For the purpose of this document, terms and definitions given in GB/T 8718 apply.
4 Determination of bulk density
4.1 Instruments and apparatuses
4.1.1 Analytical balance. scale graduation 0.01 g.
4.1.2 Blast drying oven. equipped with an automatic temperature control device,
capable of maintaining the temperature at (110±5) °C.
4.1.3 Vernier caliper. measuring range (0~200) mm, graduation value 0.02 mm.
Where.
a – length of the rectangular test sample, in millimeters (mm);
b – width of the rectangular test sample, in millimeters (mm);
c – height of the rectangular test sample, in millimeters (mm).
4.4.3 Calculate the bulk density of the test sample (Db) according to Formula (3).
Where.
Db – bulk density of the test sample, in grams per cubic centimeter (g/cm3);
m1 – mass of the test sample, in grams (g);
4.4.4 The calculated value shall be rounded to two decimal places and the numerical
value shall be rounded off in accordance with the provisions of GB/T 8170.
4.5 Allowable error
The allowable error in bulk density determination shall not exceed 0.01 g/cm3.
5 Determination of true density
5.1 General
This Chapter specifies two methods for determining true density - Method 1 (boiling
method) and Method 2 (helium method).
5.2 Method 1.Boiling method
Warning – The absolute ethanol used in this method is flammable. When heated
on an electric stove, an asbestos mesh must be used and the heating temperature
shall be controlled.
5.2.1 Reagents
5.2.1.1 Absolute ethanol. not less than 99.7%, analytical grade or above.
5.2.1.2 Sulfuric acid. chemically pure or above.
5.2.1.3 Acetone. chemically pure or above.
5.2.2.5 Blast drying oven. equipped with automatic temperature control device, capable
of heating to 200 ℃.
5.2.2.6 Desiccator. containing desiccant.
5.2.2.7 Filter paper.
5.2.2.8 Electric hot plate or thermostatically controlled electric stove.
5.2.2.9 Thermometer. (0 ~ 50) ℃, graduation value 0.1 ℃.
5.2.2.10 Beakers. 300 mL, 500 mL, 1000 mL.
5.2.2.11 Sand bath.
5.2.2.12 Jaw crusher.
5.2.2.13 Crusher.
5.2.2.14 Square-hole standard sieve. pore size 0.15 mm.
5.2.3 Sample preparation
5.2.3.1 Take samples of carbon materials in accordance with GB/T 1427; if necessary,
crush the samples to less than 1 mm [If the samples are damp, they shall be first dried
in a blast drying oven at (150 ± 10) °C for 20 min]; reduce the samples to (50 ~ 60) g
by quartering; crush all to pass through a 0.15 mm square-hole standard sieve.
5.2.3.2 The number and mass of incremental samples of calcined coke and calcined
anthracite shall be in accordance with the industrial analysis samples in GB/T 1997,
and the laboratory preparation procedures shall be the same as above.
5.2.4 Test procedures
5.2.4.1 Calibration of density bottle
5.2.4.1.1 Determination of density bottle mass (m2).
First, soak the density bottle in a saturated solution of potassium dichromate in
concentrated sulfuric acid for (1 ~ 2) hours; then take it out (if it is a new density bottle
or it has not been used many times, inject hydrochloric acid solution to 2/3 of the bottle
and boil it on a sand bath for more than 30 minutes); use water to rinse it; then use
absolute ethanol and acetone to wash it respectively; use detergent powder to clean the
outer wall of the bottle. Finally, use distilled water to clean the inner wall of the bottle;
place it in a drying oven and dry it at 120 ℃ ± 5 ℃ for 2 h; take it out and place it in a
desiccator; cool it to room temperature; weigh it with the reading accurate to 0.000 1 g.
Repeat the above operation by using distilled water to clean the inner and outer walls
of the bottle several times and measure its mass. The weighing error shall be within
0.000 4 g for at least three times. Take the average value as the density bottle mass,
which is m2.
5.2.4.1.2 Determination of density bottle water value (mass m3 of density bottle plus
distilled water).
Fill bubble-free distilled water into the density bottle in 5.2.4.1.1 (distilled water can be
boiled before use) and place it together with the dropping bottle in a constant
temperature water bath. The water level in the water bath shall be slightly above the
scale line of the density bottle or level with the bottle mouth of the capillary density
bottle. Keep the temperature at (25 ± 0.2) ℃ for 20 minutes. When the scale line of the
density bottle is not exposed above the water surface, use a filter paper roll or a dropping
bottle to suck out or add distilled water in the density bottle so that the liquid level is
accurately at the scale line; wipe the inner wall above the liquid level clean (if a
capillary density bottle is used, the stopper shall be immediately covered). Take out the
density bottle; use a clean absorbent towel to carefully wipe the outside of the density
bottle; quickly weigh its mass with the reading accurate to 0.000 1 g. Repeatedly inject
distilled water and measure its mass according to the above operation. The weighing
error of the density bottle water value shall be no more than 0.002 4 g for at least 3
times. Take the average value, which is the density bottle water value, that is, m3.
5.2.4.1.3 The density bottle water value shall be calibrated every three months. If the
frequency of use is low, it can be delayed appropriately.
5.2.4.2 Determination of true density of test sample
5.2.4.2.1 Determination of true density of test sample wettable by distilled water
Weigh 3 g of the sample as m4, with the reading accurate to 0.000 2 g; place it in a clean
density bottle; fill bubble-free distilled water (distilled water can be boiled before use)
to 2/3 of the bottle and boil for 3 minutes; do not allow the sample to splash out at this
time. After removing the bottle, inject bubble-free distilled water (distilled water can be
boiled before use) to a level slightly above the scale line or to the same level as the
mouth of the capillary density bottle. Put it together with the dropping bottle injected
with distilled water into a constant temperature water bath. The water surface of the
water bath shall be slightly higher than the scale line of the density bottle. Keep at
(25±0.2) ℃ for more than 30 minutes. When the scale line on the density bottle is not
exposed above the water surface, use a filter paper roll or a dropping bottle to adjust the
distilled water level to the scale line and wipe the inner wall above the liquid surface (if
using a capillary density bottle, the stopper shall be covered immediately). After taking
it out, use a clean and absorbent towel to wipe the outside of the bottle carefully and
quickly weigh its mass, which is m5.
5.2.4.2.2 Determination of true density of test sample wettable by absolute ethanol
Weigh 3 g of the test sample, which is m4; read the value to the nearest 0.000 2 g; place
it in a dry density bottle. Boil the absolute ethanol in the beaker and inject it into a blank
5.3.2.6 Square-hole standard sieve. pore size 0.075 mm.
5.3.2.7 Drying oven. equipped with automatic temperature control and air blowing
device, and capable of maintaining the temperature within the range of (110±5) ℃.
5.3.2.8 Glass desiccator. containing color-changing silica gel or granular anhydrous
calcium chloride.
5.3.2.9 Analytical balance. scale graduation value not less than 0.000 1 g.
5.3.3 Test sample
5.3.3.1 Take samples in accordance with the provisions of GB/T 1427 or relevant
product standards.
5.3.3.2 Crush the samples to a size of less than 4 mm; mix thoroughly; use the quartering
method to separate at least 100 g of samples; grind all the samples to a particle size of
less than 0.075 mm.
5.3.3.3 Place the prepared samples in a drying oven and dry at (110 ± 5) °C for at least
2 h; remove the samples and place them in a desiccator to cool to room temperature
before testing (the desiccator must be placed in the same place as the true density tester).
5.3.4 Test procedures
5.3.4.1 Turn on the true density tester; introduce helium; preheat for at least 30 minutes;
check the air tightness of the gas line.
5.3.4.2 Calibrate the instrument using standard samples.
5.3.4.3 Place the samples in the sample cup, with the sample volume not less than 2/3
of the sample cup volume and not exceeding the scale line inside the sample cup. When
filling the samples, vibrate the sample cup to ensure that the samples are filled tightly;
remove the samples above the scale line on the inner wall of the sample cup and the
sample adhering to the outer wall; accurately weigh the mass of the samples to an
accuracy of 0.000 1 g.
5.3.4.4 Place the sample cup on the test stand and tighten it; enter the test parameters
according to the instrument manual; let it stand for 5 ~ 10 minutes before measuring.
5.3.5 Test data processing
5.3.5.1 Calculate the true density of the sample (Dt) according to Formula (8).
Where.
6 Determination of true porosity
Calculate the true porosity of the test sample according to Formula (10).
Where.
Pt – true porosity of the sample (volume fraction), %.
The result shall be rounded to two decimal places and the numerical value shall be
rounded off in accordance with the provisions of GB/T 8170.
7 Determination of open porosity
7.1 General provisions
This Chapter specifies two methods for determining open porosity - Method 1 (vacuum
method) and Method 2 (boiling method).
7.2 Method 1.Vacuum method
7.2.1 Instruments and apparatuses
7.2.1.1 Blast drying oven. equipped with automatic temperature control device, capable
of heating to 200 ℃.
7.2.1.2 Vacuuming device. The vacuum degree can reach 0.098 MPa (see Figure 3).
7.2.1.3 Analytical balance. provided with hanging hook, scale value (0.01 ~ 0.000 1) g.
7.2.1.4 Beaker. 1000 mL.
7.2.1.5 Square plate.
7.2.1.6 Grid. woven from metal mesh.
7.2.2 Test sample
7.2.2.1 Samples shall be sampled and processed in accordance with GB/T 1427.
7.2.2.2 The sample size shall be Φ(45±0.1) mm × (40±0.1) mm, Φ(40±0.1) mm ×
(40±0.1) mm; or other regular cylindrical or rectangular samples whose mass shall not
be less than 30 g.
7.2.3 Test procedures
7.2.3.1 Place the sample in a drying oven at (110 ± 5) °C and dry it to constant weight.
The error between 2 weighings shall not exceed 0.02 g. After cooling to room
temperature, weigh the sample to obtain m8.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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