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GB/T 3634.2-2011 PDF in English


GB/T 3634.2-2011 (GB/T3634.2-2011, GBT 3634.2-2011, GBT3634.2-2011)
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GB/T 3634.2-2011: PDF in English (GBT 3634.2-2011)

GB/T 3634.2-2011
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.20
G 86
Replacing GB/T 7445-1995
Hydrogen -- Part 2. Pure hydrogen, high pure
hydrogen and ultrapure hydrogen
ISSUED ON. DECEMBER 30, 2011
IMPLEMENTED ON. OCTOBER 1, 2012
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of the People’s Republic of China;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword ... 3 
1 Scope ... 5 
2 Normative references ... 5 
3 Requirements ... 5 
4 Inspection rules ... 6 
5 Test methods ... 7 
6 Packaging, marking, storage and transportation ... 8 
7 Safety requirements ... 9 
Annex A (Normative) Determination of oxygen + argon, nitrogen, carbon
monoxide, carbon dioxide, and methane in hydrogen using the gas
chromatography with helium ionization detector ... 10 
Annex B (Informative) Example of temperature-changing concentration injector
... 13 
Foreword
GB/T 3634 Hydrogen is divided into two parts.
Part 1. Industrial hydrogen;
Part 2. Pure hydrogen, high pure hydrogen and ultrapure hydrogen.
This is Part 2 of GB/T 3634.
This Part was drafted in accordance with the rules given in GB/T 1.1-2009.
This Part supersedes GB/T 7445-1995 Pure hydrogen, high purity hydrogen
and ultra pure hydrogen. Compared with GB/T 7445-1995, in addition to
editorial changes, the main technical changes are as follows.
— MODIFY the scope of application (SEE Chapter 1 of this edition, and
Chapter 1 of the 1995 edition);
— MODIFY the normative references (SEE Chapter 2 of this edition, and
Chapter 2 of the 1995 edition);
— MODIFY the argon component requirements (SEE Chapter 3 of this
edition, and Chapter 3 of the 1995 edition);
— SUPPLEMENT the inspection rules for container assembly and hydrogen
tanker loading products (SEE 4.2, 4.3 and 4.5 of this edition); MODIFY
the inspection rules for high purity hydrogen (SEE 4.2 and 4.3 of this
edition, and 5.4 of the 1995 edition);
— In the test methods, SUPPLEMENT the electrochemical method to
determine the oxygen content; SUPPLEMENT the gas chromatography
with helium ionization detector, and INCORPORATE the supplement in
Annex A of this edition; INTRODUCE a thermal conductivity gas
chromatograph to determine the contents of carbon monoxide, carbon
dioxide, and methane in hydrogen (SEE 5.2 of this edition, Annex A);
— MODIFY the temperature-changing concentration gas circuit for sample
injection; INCORPORATE the modification in Annex A (SEE Annex B of
this edition, and Figure 1 of the 1995 edition).
This Part was proposed by the China Petroleum and Chemical Industry
Federation.
This Part shall be under the jurisdiction of National Technical Committee for
Standardization of Gas (SAC/TC 206).
Hydrogen -- Part 2. Pure hydrogen, high pure
hydrogen and ultrapure hydrogen
1 Scope
This Part specifies the technical requirements, test methods, packaging,
marking, storage and transportation, and safety requirements for pure hydrogen,
high pure hydrogen and ultrapure hydrogen.
This Part is applicable to hydrogen produced by means of adsorption and
diffusion, loaded in bottles and containers, and transmitted by pipeline. It is
mainly used in the fields of electronics industry, petrochemical industry, metal
smelting, and scientific research.
Molecular formula. H2.
Relative molecular mass. 2.015 88 (according to international relative atomic
mass in 2007).
2 Normative references
The following documents are essential to the application of this document. For
dated references, only the editions with the dates indicated are applicable to
this document. For undated references, only the latest editions (including all the
amendments) are applicable to this document.
GB/T 3634.1-2006 Hydrogen -- Part 1. Industrial hydrogen
GB/T 5832.3 Determination of moisture in gases -- Part 3. The method of
cavity ring-down spectroscopy
GB/T 6285 Determination of trace oxygen in gases -- Electrochemical
method
3 Requirements
3.1 The technical requirements for pure hydrogen, high pure hydrogen and
ultrapure hydrogen shall meet the requirements of Table 1.
φ2 - Argon content (volume fraction),10-6;
φ3 - Nitrogen content (volume fraction), 10-6;
φ4 - Carbon monoxide content (volume fraction), 10-6;
φ5 - Carbon dioxide content (volume fraction), 10-6;
φ6 - Methane content (volume fraction), 10-6;
φ7 - Moisture content (volume fraction), 10-6.
5.2 Determination of contents of oxygen + argon, nitrogen, carbon
monoxide, carbon dioxide, and methane in hydrogen
5.2.1 USE gas chromatography with helium ionization detector to determine
the contents of oxygen + argon, nitrogen, carbon monoxide, carbon dioxide,
and methane in hydrogen. SEE Annex A.
5.2.2 It is allowed to use thermal conductivity gas chromatography to
determine the contents of oxygen + argon, and azane in hydrogen. It is allowed
to use flame ionization to determine the contents of carbon monoxide, carbon
dioxide, and methane in hydrogen. When the detection limit of the instrument
cannot meet the analysis requirements, the temperature-changing
concentration for sample injection may be adopted. SEE Annex B.
5.2.3 When there is any objection to the determination results of the above
methods, the gas chromatography with helium ionization detector is used as
the arbitration method.
5.2.4 DETERMINE the content of oxygen in hydrogen according to the
provisions of GB/T 6285. Other equivalent methods are allowed to determine
the content of oxygen in hydrogen. When there is any objection to the
determination results, the method specified in GB/T 6285 is used as the
arbitration method.
5.3 Determination of moisture content
PERFORM according to the provisions of GB/T 5832.3. Other equivalent
methods are allowed to determine the moisture content in hydrogen. When
there is any objection to the determination results, the method specified in GB/T
5832.3 is used as the arbitration method.
6 Packaging, marking, storage and transportation
The requirements for packaging, marking, storage and transportation of
hydrogen shall comply with the provisions of Chapter 5 in GB/T 3634.1-2006.
The operating parameters of the instrument are selected according to the
requirements of instrument specifications and detection limits.
A.5 Determination procedures
A.5.1 TURN on the instrument according to the instrument specifications.
REGULATE the operating parameters until the parameters of the instrument
are stable.
A.5.2 According to the analysis task, SELECT the appropriate
chromatographic conditions. These conditions include. carrier gas flow, sample
gas flow, setting of the time program for the operation control of one ten-way
valve and two six-way valves, selection of the instrument’s gas circuit balancing
conditions, etc.
A.5.3 CONNECT the standard sample to the instrument. INJECT the sample
after full replacement to obtain the representative sample. CARRY out the
determination in parallel at least twice until the relative deviation of the
chromatographic response values of the components to be determined
between the two adjacent assays is not more than 5%. TAKE the average.
A.5.4 Under the exact same conditions as the standard sample, CONNECT
the sample to be tested to the instrument. INJECT the sample after full
replacement to obtain the representative sample. CARRY out the determination
in parallel at least twice until the relative deviation of the chromatographic
response values of the components to be determined between the two adjacent
assays is not more than 5%. TAKE the average.
A.5.5 Under the same conditions, the determination shall be carried out in two
test conditions, oxygen removal from the sample and no oxygen removal from
the sample.
A.5.6 After completing the analysis operation, SHUT down according to the
relevant requirements of the specifications.
A.6 Result calculation
The calculation of the contents of oxygen + argon, argon, nitrogen, carbon
monoxide, carbon dioxide, and methane in hydrogen is specified in A.1.6 of
GB/T 3634.1-2006.
The same sample is not subjected to the deoxy column to determine the content
of oxygen + argon, and is subjected to the deoxy column to determine the
content of argon. The content of oxygen in the sample is obtained by subtracting
the argon content from the content of oxygen + argon.
B.4 Determination conditions
B.4.1 Carrier gas, and auxiliary gas
The carrier gas and auxiliary gas required for instrument operation refer to the
corresponding instrument specifications.
B.4.2 Concentration column
Concentration column 1. It is used to concentrate oxygen + argon, and nitrogen
components in the sample. A stainless steel tube with a length of approximately
30cm and an inner diameter of 4mm contains activated carbon with a grain size
of 0.25mm to 0.40mm; or other equivalent concentration columns. USE the
concentration column after hydrogen activation at 160°C for 4h. The
concentration temperature is liquid nitrogen temperature (liquid nitrogen bath).
The desorption temperature is room temperature water bath.
Concentration column 2. It is used to concentrate carbon monoxide, carbon
dioxide, and methane components in the sample. A stainless steel tube with a
length of approximately 30cm and an inner diameter of 4mm contains color-
changing silica with a grain size of 0.25mm to 0.40mm; or other equivalent
concentration columns. USE the concentration column after hydrogen
activation at 160°C for 4h. The concentration temperature is liquid nitrogen
temperature (liquid nitrogen bath). The desorption temperature is 80°C water
bath.
B.5 Concentrated injection procedures
B.5.1 Gas circuit system’s reliability check and determination of blank
value
CONNECT the temperature-changing concentrating device to the gas
chromatograph’s gas circuit system. TURN on the instrument according to the
instrument specifications until it is stable. After closing the concentration column,
PLACE a liquid nitrogen bath over it. After about 5 minutes of concentration,
REMOVE the liquid nitrogen bath. Quickly PLACE the concentration column in
a desorption water bath. The carrier gas is then passed through the
concentration column. RECORD the chromatographic signal. No
chromatographic signal is normal. Otherwise, CHECK the gas circuit system of
the concentration injector until there is no chromatographic signal. The carrier
gas is then passed through the concentration column. CONCENTRATE the
carrier gas for 5min, while observing and preventing the air inhalation of the
concentration injector. DETERMINE the blank value of the chromatographic
system. The blank value shall be lower than the corresponding indicator of high
pure hydrogen or ultrapure hydrogen in this Part.
B.5.2 Sampling
......
 
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.