GB/T 33291-2016 English PDF (GBT33291-2016)

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GB/T 33291-2016: Measurement method of pressure-composition-temperature for reversable hydrogen absorption and desorption of hydrides
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 and 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 and desorption of
hydrides
1 Scope
This Standard specifies the measurement method of pressure-composition-temperature
for reversable hydrogen absorption and 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