GB/T 33291-2016 PDF English
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Measurement method of pressure-composition-temperature for reversable hydrogen absorption and desorption of hydrides
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GB/T 33291-2016: PDF in English (GBT 33291-2016) GB/T 33291-2016
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 27.180
F 19
Measurement method of pressure-composition-temperature
for reversable hydrogen absorption & desorption of
hydrides
ISSUED ON: DECEMBER 13, 2016
IMPLEMENTED ON: JULY 01, 2017
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of the People's Republic of China.
Table of Contents
Foreword ... 4
1 Scope ... 5
2 Normative references ... 5
3 Terms and definitions... 5
4 Symbols and marks ... 6
5 Test method and principle ... 7
5.1 Test method ... 7
5.2 Test principle ... 7
6 Test device ... 8
6.1 Device composition ... 8
Figure 1 -- Test device composition diagram ... 9
6.2 Technical requirements for test system ... 9
6.2.1 Calibration of equipment and instruments ... 9
6.2.2 Pressure sensor ... 9
6.2.3 System leak rate ... 9
6.2.4 Connecting pipes ... 9
6.2.5 Temperature fluctuation ... 9
6.2.6 Hydrogen purity ... 9
6.2.7 Helium purity ... 9
6.3 Volume calibration of test system ... 10
7 Preparation before the test ... 11
7.1 Sample shape and sample size ... 11
7.1.1 Sample shape ... 11
7.1.2 Sample size ... 11
7.2 Filling of samples ... 11
7.3 Calibration of sample chamber volume ... 12
7.3.1 Calibration method ... 12
7.3.2 Calibration steps ... 12
7.3.3 Calibration times ... 13
7.4 Sample activation ... 13
7.4.1 Classification of the original state of the sample ... 13
7.4.2 Hydrogen-containing samples ... 13
7.4.3 Hydrogen-free samples ... 13
8 P-C-T tests ... 14
8.1 Temperature setting ... 14
8.2 Hydrogenation P-C-T test ... 14
8.3 Dehydrogenation P-C-T test ... 15
8.4 Determination of pressure balance ... 15
8.5 Processing of test results ... 16
8.6 Sample removal and storage ... 16
9 Calculation of hydrogenation/dehydrogenation capacity ... 16
9.1 One-step hydrogenation/dehydrogenation capacity ΔC(m)a/ΔC(m)d ... 16
9.2 Total hydrogenation/dehydrogenation capacity Ca/Cd ... 17
Annex A (informative) P-C-T curve test report ... 18
Annex B (informative) Typical P-C-T curve ... 19
Figure B.1 -- P-C-T curve of Ti-Mn metal hydride hydrogen storage materials under
different annealing conditions ... 19
Figure B.2 -- P-C-T curve of NaAlH4 complex hydride hydrogen storage materials ... 20
Bibliography... 21
Measurement method of pressure-composition-temperature
for reversable hydrogen absorption & desorption of
hydrides
1 Scope
This Standard specifies the measurement method of pressure-composition-temperature
for reversable hydrogen absorption & desorption of hydrides.
This Standard is applicable to testing the pressure-composition-temperature (P-C-T) of
metal hydrides, complex hydrides, chemical hydrides and physical adsorption hydrogen
storage materials that have reversible hydrogen absorption and desorption
characteristics within the range of which the temperature is 77K~873K and the pressure
is 0~75MPa.
2 Normative references
The following referenced documents are indispensable for the application of this
document. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
GB/T 3634.2, Hydrogen - Part 2: Pore hydrogen, high pure hydrogen and ultrapure
hydrogen
GB 4962-2008, Technical safety regulation for gaseous hydrogen use
GB/T 16943, Gas for electronic industry - Helium
GB/T 24499, Technology glossary for gaseous hydrogen, hydrogen energy and
hydrogen energy system
3 Terms and definitions
For the purposes of this document, the terms and definitions defined in GB/T 24499 as
well as the followings apply.
3.1 one-step hydrogenation capacity
After the hydride has undergone a pressure change at a constant temperature and
reached a steady state, the ratio of the hydrogen adsorbed in the hydride material to the
original mass of the hydride.
3.2 one-step dehydrogenation capacity
After the hydride has undergone a pressure change at a constant temperature and
reached a steady state, the ratio of the mass of hydrogen released in the hydride material
to the original mass of the hydride.
3.3 total hydrogenation capacity; Ca
The sum of multiple consecutive one-step hydrogenation capacity of the hydride.
3.4 total dehydrogenation capacity; Cd
The sum of multiple consecutive one-step dehydrogenation capacity of the hydride.
4 Symbols and marks
The following symbols apply to this document.
w - The mass of the hydride material, in g.
Tsam - The temperature of the sample chamber, in K.
Tsys - The ambient temperature of test system, in K.
Tcon - The sample connection pipe temperature, in K.
Psam - The pressure in the sample chamber, in MPa.
Psys - The test system pressure, in MPa.
Psys(n) - The system test pressure in the nth step test, in MPa, n=0,1,2,3….
Peq - The equilibrium pressure, in MPa.
Vsam - The volume of the sample chamber, in mL.
Vsys - The test system volume, in mL.
Vcon - The volume of the sample connection pipeline, in mL.
Vb - The volume of the steel ball, in mL.
Vx - The volume of the blank sample chamber in the unknown state, in mL.
Vi - The valve and number, i=1,2,3,4,5,6.
Pi - The measured pressure value during testing, i=1,2,3,4,5,6, x.
R - The ideal gas constant, R=8.314472J·mol-1 K-1.
Zsys - The hydrogen compression factor at pressure Psys and temperature Tsys.
Zsam - The compression factor of hydrogen gas at pressure Psam and temperature Tsam.
Zcon - The hydrogen compressibility factor at pressure Psam and temperature Tcon.
Z'sys - The hydrogen compressibility factor at pressure Peq and temperature Tsys.
Z'sam - The hydrogen compressibility factor at pressure Peq and temperature Tsam.
Z'con - The hydrogen compressibility factor at pressure Peq and temperature Tcon.
Mr - The relative molecular mass of hydrogen, in g/mol.
Ca - The total hydrogenation capacity, in wt%.
Cd - The total dehydrogenation capacity, in wt%.
ΔC(m)a - The one-step hydrogenation capacity, in wt%.
ΔC(m)d - The one-step dehydrogenation capacity, in wt%.
m - The number of steps to repeat the one-step hydrogenation/dehydrogenation
measurement process.
NOTE 1: Vsys refers to the sum of the volume of the internal connecting pipes when the accumulator
D and the valves V1, V2, V4, V5 and V6 are in the closed state.
NOTE 2: Vcon refers to the volume of the connecting pipe between the valve V3 and the constant
temperature zone of the sample chamber, as shown by the dotted box in Figure 1.
NOTE 3: Vsam refers to the empty volume in the sample chamber after filling with a sample of
which its mass is w.
5 Test method and principle
5.1 Test method
The test uses the isovolumic method.
5.2 Test principle
At a certain temperature, introduce hydrogen gas of known pressure into a container of
known volume. Connect the hydride reactor to the vessel. Hydrogenation or
Figure 1 -- Test device composition diagram
6.2 Technical requirements for test system
6.2.1 Calibration of equipment and instruments
The equipment and instruments used in this test method shall be regularly calibrated by
a qualified inspection agency in accordance with the relevant national standards.
6.2.2 Pressure sensor
The accuracy of the pressure sensor shall not be less than 0.5‰. The significant figures
of the test value under the highest working pressure shall be no less than 5 digits.
6.2.3 System leak rate
The pressure drop of the system under the maximum working pressure within 24h shall
not be greater than 0.1% of the maximum working pressure.
6.2.4 Connecting pipes
Connecting pipes shall be internally polished stainless-steel pipes. They shall comply
with the provisions of 4.4.4 in GB 4962-2008.
6.2.5 Temperature fluctuation
The fluctuation of the ambient temperature of the test system and the working
temperature of the sample chamber shall not exceed ±0.5K.
6.2.6 Hydrogen purity
The purity of hydrogen shall meet the requirements of high-purity hydrogen in GB/T
3634.2.
6.2.7 Helium purity
The purity of helium shall meet the requirements of high-purity helium in GB/T 16943.
7 Preparation before the test
7.1 Sample shape and sample size
7.1.1 Sample shape
7.1.1.1 Block sample
For block samples, it is advisable to use mechanical crushing method to make granular
samples of 0.5mm~1.0mm.
7.1.1.2 Fine powder sample
For fine powder samples, it is advisable to use the mechanical tableting method to make
them into flake samples. The tableting pressure shall not be lower than 20MPa.
7.1.2 Sample size
7.1.2.1 Metal hydride hydrogen storage materials
For metal hydride hydrogen storage material samples, the mass shall be 1.0g~2.0g. The
sample volume shall not exceed 50% of the sample chamber volume.
7.1.2.2 Other hydride hydrogen storage materials in this Standard
For other hydride hydrogen storage material samples in this Standard, the mass shall
not be less than 0.5g. The sample volume shall not exceed 50% of the sample chamber
volume.
7.1.2.3 Weighing accuracy of sample
It shall use a weighing tool with an accuracy of not less than 0.2mg to weigh the sample.
7.2 Filling of samples
The filling of the sample shall be carried out as follows:
a) Open valve V1 and valve V3. Fill the sample chamber with about 0.1MPa of
helium;
b) Close valve V1 and valve V3. Open the sample chamber H. Load the sample into
the sample chamber H. Seal the sample chamber H;
c) Open valve V3 and valve V5. Vacuum the sample chamber to better than 0.1Pa;
d) Close valve V5. Open valve V1. Fill the sample chamber with helium to the
maximum test pressure of the sample. Detect if the sample chamber has leakage;
e) When there is no leakage in the sample chamber, open valve V4. Reduce the
sample chamber pressure to about 0.1MPa. Close valve V4.
NOTE: For samples with high activity in the air, the filling of the samples shall be carried out in a
protective atmosphere.
7.3 Calibration of sample chamber volume
7.3.1 Calibration method
7.3.1.1 Sample chamber volume calibration for granular samples
For the samples made in 7.1.1.1, the volume of the sample chamber can be calibrated
at room temperature.
7.3.1.2 Sample chamber volume calibration for powdered samples
For samples made in 7.1.1.2, it shall start at room temperature. Carry out the calibration
of sample chamber volume Vsam at Tsam temperature every 20K~50K. The calibrated
maximum temperature shall not exceed the minimum temperature for the thermal
decomposition of the sample to release hydrogen. When the deviation of the sample
chamber volume measured at three consecutive temperature points is less than 1.5%,
the average value is taken as the final sample chamber volume Vsam.
7.3.2 Calibration steps
Calibration shall be performed as follows:
a) Open valve V3 and valve V5. After the system is evacuated to better than 0.1Pa,
close valve V5;
b) After the sample chamber temperature Tsam is stable, open the valve V1. Fill the
sample chamber with helium. After the pressure is stable, record the pressure P5
(P5 shall not be greater than 1.0MPa);
c) Close valve V3. Open valve V5. Evacuate the system to better than 0.1Pa. Close
valve V5;
d) Open valve V3. Record stable post-pressure P6. Calculate the sample chamber
volume Vsam according to formula (4).
the pressure is stable;
d) Open valve V3 to introduce hydrogen into the sample chamber. After the pressure
is stable, record the pressure Peq;
e) Use formula (5) to calculate the hydrogenation capacity of the sample;
f) Repeat steps a)~e). The activation is completed until the deviation of the
hydrogenation capacity obtained during the two consecutive activation processes
is less than 2%;
g) When the activation is completed, repeat step a). Wait for the P-C-T test.
8 P-C-T tests
8.1 Temperature setting
The temperature setting shall be carried out as follows:
a) Set the system temperature to (298±0.5)K;
b) Set the sample chamber temperature to the P-C-T test temperature Tsam and
maintain a constant temperature.
8.2 Hydrogenation P-C-T test
The hydrogenation P-C-T test shall be carried out according to the following steps:
a) Record the sample chamber pressure Psam. Close valve V3. Open valve V2. Fill the
system with hydrogen. After the system pressure is stable, record the system
pressure Psys(0);
b) Open valve V3. Connect the system and the sample chamber. When the pressure
meets the equilibrium condition of 8.4, record the equilibrium pressure Peq,
sample chamber temperature Tsam, and system temperature Tsys. Close valve V3.
Complete a one-step hydrogenation. The equilibrium pressure Peq is defined as
the sample chamber pressure Psam for the next hydrogenation test. Calculate the
one-step hydrogenation capacity ΔC(m) of the sample according to formula (5).
Obtain a set of pressure and hydrogenation capacity data.
c) Increase system pressure by ΔPsys. After the system pressure is stable, record the
system pressure Psys(n). Proceed to the one-step hydrogenation test according to
step b). If the difference ΔPeq between the (n+1)th and nth equilibrium pressures
is less than 0.5‰ of the full scale of the system, then the system pressure rise
ΔPsys shall be increased by 1.5 times in the (n+2)th one-step hydrogenation
measurement. Otherwise, continue to adjust the system pressure according to
ΔPsys.
d) Repeat the one-step hydrogenation steps. The number of steps shall not be less
than 10.
e) When the system equilibrium pressure reaches the maximum hydrogenation
pressure specified by the sample, the hydrogenation P-C-T test is completed.
8.3 Dehydrogenation P-C-T test
The dehydrogenation P-C-T test shall be carried out as follows:
a) Record the sample chamber pressure Psam. According to the sample chamber
pressure Psam, the system volume Vsys and the sample chamber volume Vsam,
adjust the initial pressure Psys(0) of the system;
b) Open valve V3. Connect the system and sample chamber. When the pressure
meets the equilibrium condition of 8.4, record the pressure Peq, the sample
chamber temperature Tsam, and the system temperature Tsys. Close valve V3. The
one-step dehydrogenation of the sample is completed. The pressure Peq is defined
as the new pressure Psam of the sample chamber for the next one-step
dehydrogenation. Calculate the one-step dehydrogenation capacity ΔC(m) of
hydride according to formula (5). Obtain a set of pressure and dehydrogenation
capacity data.
c) Proceed to the one-step dehydrogenation test according to step b). If the pressure
difference between the (n+1)th and nth times after stabilization ΔPeq=Peq(n)-Peq(n+1)
is less than 0.5‰ of the full scale of the system, then the system pressure variable
ΔPsys shall be increased by 1.5 times in the (n+2)th system one-step
dehydrogenation measurement. Otherwise, continue to adjust the system pressure
according to ΔPsys.
d) Repeat the one-step dehydrogenation steps. The number of steps shall not be less
than 10. Until the final pressure Peq is not greater than 0.5‰ of the full scale of
the system, the dehydrogenation P-C-T test is completed.
8.4 Determination of pressure balance
When the pressure change value within 30min is not greater than 0.5‰ of the full scale
of the system, the pressure is considered to be balanced. Otherwise, continue to
determine the pressure balance for the next 30min until the pressure balance is reached.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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