氢气 Hydrogen
第2部分:纯氢、高纯氢和超纯氢
Part 2: Pure hydrogen, high pure hydrogen and ultrapure
hydrogen
1. 范围Scope
本部分规定了纯氢、高纯氢和超纯氢的技术要求、试验方法、包装标志、贮运及安全要求。
This section provides the technical requirements, test methods,
packing marks and store safety requirements of pure hydrogen,
high purity hydrogen and ultra-pure hydrogen.
本部分适用于经吸附法、扩散法等制取的瓶装、集装格装和管道输送的氢气。它主要用于电子工业、石油化工、金属冶炼和科学研究等领域。
This section applies to the bottled, container loaded and pipeline
transferred hydrogen making with adsorption and diffusion method.
It is mainly used in electronic industry, petrochemical industry,
metal smelting and scientific research, etc.
分子式:Molecular formula: H2.
相对分子质量:2.01588(按2007年国际相对原子质量)。
Molecular weight: 2.01588 (as per 2007 international relative
atomic mass)
2. 规范性引用文件
The reference file
下列文件对于本文件的应用是必不可少的。凡是注日期的引用文件,仅注日期的版本适用于本文件。凡是不注日期的引用文件,其最新版本(包括所有的修改单)适用于本文件。
The following documents for this application is indispensable.
Every noted date reference documents, only version with noted
date is suitable for this article. Any reference documents without
noted date, the latest version (including all the modifications)
applies to this document.
GB/T 3634. 1-2006氢气第1部分:工业氢
GB/T 3634. 1-2006 Hydrogen- Part 1: Industrial Hydrogen
GB/T5832. 3 气体中微量水分的测定 第3部分:光腔衰荡光谱法
GB/T5832. 3 Determination of trace moisture in gas
Part 3: Optical cavity ring-down spectroscopy
GB/T 6285气体中微量氧的测定电化学法
GB/T 6285 Determination
electrochemical method of trace O2 in
gas
3 要求 Requirement
3.1 纯氢、高纯氢和超纯氢的技术要求应符合表1的规定。
Technical requirement of pure hydrogen, high pure hydrogen and
ultrapure hydrogen shall meet requirement of Table 1.
表1 纯氢、高纯氢和超纯氢的技术要求
Table1 Technical requirement of pure hydrogen, high pure
hydrogen and ultrapure hydrogen
Name Specification
Pure H2
H2 purity(MVF) / 10-2
≥
O2 concentration
(MVF) / 10-6
Ar.
concentration
(MVF) /
10-6
99.99
5
Hi pure H2
99.999
1
Determine by
Vendor
5
1
1
1
3
10
Ultrapure H2
99.999 9
0.2
0.2
≤
≤
Determine by
vendor
N2 concentration
(MVF) / 10-6
≤
60
Co concentration
(MVF) / 10-6
≤
5
CO2 concentration
(MVF) / 10-6
≤
5
CH4 concentration
(MVF) / 10-6
≤
10
H2O concentration
(MVF) / 10-6
≤
10
--
Total Impurity (MVF) / 10-6
≤
0.4
0.1
0.1
0.2
0.5
1
3.2 除超纯氢外,由供需双方商定氩含量是否列人纯度计算。
In addition to the ultrapure hydrogen, whether argon concentration
will be listed in purity calculation can be defined by both supplier
and buyer.
4 规则Rule
4.1 连续、稳定生产的瓶装(或集装格装)纯氢、瓶装高纯氢以生
产厂一个操作班生产的或一次充灌的产品组批,用户以同一车载里或同批进货量组批。每批产品的瓶数(或格数)不应超过300.
Continuous and stable production of bottled (or container cased)
pure hydrogen, bottled high purity hydrogen will be a batch
produced by manufacturer’s one operation shift or once filling
products, users will set the batched product with the same truck or
same batch material. Every batch of bottles number should not
exceed 300.
4.2 瓶装或集装格装纯氢和瓶装高纯氢产品按表2规定的批量随机抽样检验,成批验收。当有任何一项指标的检验结果不符合本部分技术要求时,应重新加倍随机抽样检验,如果仍有任何一项指标不符
合本部分技术要求时,则判该批产品不合格。
4.2 Bottled or container cased pure hydrogen and bottled high
purity hydrogen product will be random sampling inspection as
stipulated in the table 2, acceptance by batch. If any test result
does not conform to the technical specification, it should be double
random sampling inspection; any indication that it still has the
discrepancy with the technical requirements, this batch of product
is deemed as unqualified.
表2 瓶装或集装格装纯氢和瓶装高纯氢抽样表
Table 2 Bottled or container cased pure hydrogen and bottled high
purity hydrogen random check list
Bottle no. ( Each
batch)
Min. check bottle
(pure H2)
Min. check bottle(Hi
pure H2)
1 2 3-8 9-15 16-25 26-50 51-150 ≻150
1 2 2 3 4 5 6 7
1 2 3 5 7 9 11 13
4.3 集装格装高纯氢气产品应逐格检验验收。当检验结果有任何一项指标不符合本部分技术要求时,则判该产品不合格。
Container cased high purity hydrogen product should be inspected
for acceptance by each case. Any indication that the result has
discrepancy with the technical requirements, this batch of product
is deemed as unqualified.
4.4 超纯氢产品应逐一检查验收。当检验结果有任何一项指标不符合本标准技术要求时则判该产品不合格。
Ultrapure hydrogen product should be inspected for acceptance
one by one. Any indication that the result has discrepancy with the
technical requirements, this batch of product is deemed as
unqualified.
4.5 大容积无缝钢瓶装氢气产品应逐车检验并验收。当检验结果有任何一项指标不符合本标准技术要求时则判该车产品不合格。
Large volume of seamless steel bottled H2 product shall be
inspected for acceptance by each truck. Any indication that the
result has the discrepancy with the technical requirements, this
batch of product is deemed as unqualified.
4.6 稳定生产的管道输送的氢气每4h抽样检验一次。当检验结果有任何一项指标不符合本标准技术要求时则判该4h内产品不合格。
Pipelined H2 during stable operation shall be random inspected
every 4 hours. Any indication that the result has the discrepancy
with the technical requirements, this batch of product within this 4
hours is deemed as unqualified.
5 试验方法test method
5. 1 氢纯度 H2 purity
氢气纯度按式(1)计算:
H2 purity calculation based on formula (1)
φ=100 -(φ1 +φ2 +φ3 +φ4 +φ5 +φ6 +φ7) X10-.4
( 1 )式中:in formula(1)
φ―氢气纯度(体积分数),10-2;
φ- H2 purity(MVF), 10-2
φI 氧含量(体积分数),10-6;
φI
O2 concentration (MVF), 10-6;
φ2氩含量(体积分数),10-6;
φ2
AR concentration (MVF), 10-6
φ3氮含量(体积分数),10-6;
φ3
N2 concentration (MVF), 10-6;
φ4―一氧化碳含量(体积分数),10-6;
φ4
– Co concentration (MVF), 10-6
φ5―二氧化碳含量(体积分数),
106;
φ5
– CO2 concentration (MVF), 106
φ6―甲烷含量(体积分数),10-6;
φ6
– CH4 concentration (MVF), 10-6
φ7―水分含量(体积分数),10-6
φ7
– moisture concentration (MVF), 10-6
5.2 氢中氧+氩,氮、一氧化碳、二氧化碳和甲烷含量的测定
Determination of oxygen + argon, nitrogen, carbon monoxide,
carbon dioxide and methane concentration in hydrogen
5.2.1
采用氮离子化气相谱法测定氢中氧+氩、氮、一氧化碳、二氧化碳和甲烷的含量。见附录A.
Determination of oxygen + argon, nitrogen, carbon monoxide,
carbon dioxide and methane concentration in hydrogen by nitrogen
Ionization gas chromatography. See Appendix A.
5.2.2 允许采用热导气相谱法测定氢中氧+氩,氮烷含量;允许采用火焰离子化法测定氢中一氧化碳、二氧化碳和甲烷的含量。当仪器检测限无法满足分析要求时,可采用变温浓缩进样。参见附录B.
Determination of oxygen + argon, nitrogen and methane
concentration in oxygen by thermal conductivity gas
chromatography is allowed; Determination of carbon monoxide,
carbon dioxide and methane concentration in hydrogen by flame
ionization method is allowed. When the instrument detection limit
cannot meet analysis requirement, variable temperature
condensation sampling can be used. See appendix B.
5.2.3 当以上方法的测定结果有异议时,以氮离子化气相谱法为仲裁法。
When any objection to the above methods of measured results,
the nitrogen ionization gas chromatography will be used as the
arbitration method.
5.2.4 按GB/T6285的规定测定氢中氧含量。允许采用其他等效方法测定氢中氧含量。当测定结果存在异议时,以GB/T6285规定的方法为仲裁法。
Determination of oxygen concentration in hydrogen by the
provisions of GB/T6285. The other equivalent method to measure
oxygen concentration in the hydrogen is allowed. When the results
of the determination with objections, GB/T6285 will be used as
arbitration method.
5. 3水分含量的测定 Moisture determination
按GB/T5832. 3的规定执行。允许采用其他等效的方法测定氢中水分含量,当测定结果有异议时,以GB/T5832.3规定的方法为仲裁方法。
As per GB/T5832. The other equivalent method to measure the
moisture concentration in the hydrogen is allowed. When the
results of the determination with objections, GB/T5832.2 will be
used as arbitration method.
包装、标志及贮运 Packing, marking and shipping
氢气的包装、标志及贮运的要求应符合GB/T3634. 1-2006第5章的规定。
Requirements of hydrogen packing, marking and shipping should
be in comply with the provisions of chapter 5. In GB/T3634. 1-2006.
安全要求 Safety requirement
氢气的安全要求应符合GB/T3634. 1-2006第6章的规定。
Hydrogen safety requirement shall be in comply with the provisions
of chapter 6 In GB/T3634. 1-2006.
附录A Appendix A
(规范性附录)(normative appendixes)
氮离子化气相谱法测定氢中氧+氩、氮、一氧化碳、二氧化碳和甲烷
Determination of oxygen + argon, nitrogen, carbon monoxide,
carbon dioxide and methane in nitrogen by nitrogen Ionization gas
chromatography.
A. 1方法 method
采用氮离子化气相谱法测定氢中氧+氩、氮、一氧化碳、二氧化碳和甲烷的含量。
Determination of oxygen + argon, nitrogen, carbon monoxide,
carbon dioxide and methane concentration in nitrogen by nitrogen
Ionization gas chromatography.
A. 2仪器 Instrument
要求所采用的仪器对待测组分的检测限分别应低于本部分表1所列相应技术指标的1/4。推荐采用配备气路切割装置和柱切换装置的氮离子化气相谱仪。当分析超纯氢时,应配备脱氧装置。
It is required that detection limits for adopted instrument should be
respectively lower than 1/4 of technical indicators listed in table 1.
Nitrogen ionization gas chromatograph with pneumatic cutting
device and column switching device are recommended to be used.
When analyzing ultrapure hydrogen, de-oxidation device shall be
equipped.
图A.1给出了参考的配备气路切割、脱氧柱和柱切换装置的氮离子化气相谱仪的气路流程示意图。
Fig. A 1 gives the flow diagram of nitrogen ionization gas
chromatograph referenced for the pneumatic cutting, deoxidization
column and column switching device.
说明:Illustration:
1―高纯沉载气钢瓶; High purity heavy carrier gas cylinder;
2―钢瓶减压器; Cylinder pressure reducer
3载气稳压阀; Carrier gas regulator valve
4―压力表;
Pressure gauge
5载气净化器; Carrier gas purifier
6―定体积进样管; Volume sampling pipe
7―样气流量计; Sampling gas flow meter
8―样气入口; Sampling gas inlet
9―十通阁;
Ten-way valve
10―气路平衡调节阀;Pneumatic balance regulator
n―预分离柱; Pre- separator column
12―切割路载气流量计;Cutting carrier flow meter
13―脱氧柱; De -oxygen column
14―六通切换阀; 6-way switch valve
15―谱分析柱1; GC column 1
16―谱分析柱2; GC column 2
17-氮离子化检测器;N2 ion monitor
18-检测器路载气流童计.Monitor carrier gas flow meter
.
图A. 1气路流程示意图 Fig. A 1 Pneumatic flow meter sketch
A. 3 气体标准样品 Gas standard sample
采用以氢气作平衡气的气体标准样品。标准样品中的组分含量应与被测组分含量相近;当被测组分的含量(体积分数)不大于1x10-6时,宜采用相应组分含量为1x10-6一5X10-6的标准样品。
Gas standard samples will be balanced by hydrogen. The
component of standard sample gas should be close to measured
component; when the measured components (volume fraction) is
not greater than 1 x10-6, the corresponding components of 1x10-6-
5 x10-6 standard sample can be used.
A. 4 仪器条件 instrument
A. 4. 1 谱柱 GC
A.4.1.1 预分离柱:用于分离氢和其他组分。长0. 6m、内径2mm的不锈钢管,内装粒度为0. 25mm-0. 40mm的TDX-01。通载气在180℃活化3h后备用。允许采用其他等效预分离柱。
Pre separation column: used to separate hydrogen and other
components. With long 0. 6 m, inner diameter 2 mm stainless steel
pipe, built-in TDX – 01 with granularity of 0. 25 mm - 0. 40 mm.
Carrier gas will be used as backup after activation at 180 ℃ for 3
h. The other equivalent pre-separation column is allowed.
A.4.1.2 谱分析柱1:用于氧(氩)、氮、甲烷的分离。长2m、内径2mm的不锈钢管,内装粒度为0. 25mm-0. 40mm的5A分子筛。通载气在180℃活化3h后备用。谱柱使用温度:40C。允许采用其他等效谱柱。
GC analysis column 1: used to separate O2 (Ar), N2
and Ch4. With
long 2 m, inner diameter 2 mm stainless steel pipe, built-in 5A
molecular sieve with granularity of 0. 25 mm - 0. 40 mm. Carrier
gas will be used as backup after activation at 180 ℃ for 3 h.
Chromatographic column temperature: 40C. The other equivalent
chromatographic column is allowed.
A.4. 1.3 谱分析柱2:用于一氧化碳、二氧化碳、甲烷的分离。长2m、内径约2mm的不锈钢管,内装粒度为0.25mm-0. 40mm的活性炭。通载气在150℃活化2h后备用,谱柱使用温度:40C。允许采用其他等效谱柱。
GC analysis column 2:used to separate CO,CO2 and CH4。With long 2 m, inner diameter about 2 mm stainless steel pipe,
built-in active carbon with granularity of 0. 25 mm - 0. 40 mm.
Carrier gas will be used as backup after activation at 180 ℃ for 3
h. Chromatographic column temperature: 40C. The other
equivalent chromatographic column is allowed.
A.4.1.4 脱氧柱:当需要测定氩组分含量时,可采用脱氧柱脱除样品气中的氧组分。脱氧柱中的脱氧剂应确保能彻底脱除样品气中的氧组分。推荐采用长1m、内径约3mm的不锈钢管,内装粒度为
0. 25mm一0. 40mm的105钯催化剂。催化剂在使用前应按生产厂家提供的条件活化处理。
De-oxidation column: when argon composition need to be
measured, oxygen components in the sample gas can be
removed by de-oxidation column. Deoxidizer in deoxidization
column should ensure that oxygen components in the sample
gas can be completely removed. Long 1 m and inner diameter
about 3 mm stainless steel pipe are recommended, built-in 105
palladium catalyst with granularity of 25 mm-0. 40 mm. The
catalyst should be activated according to the vendor’s supply
conditions before usage.
A. 4.2操作参数 Operation parameters
仪器各操作参数按仪器说明书和检测限要求选定。
Instrument operation parameters selected according to the
requirements of spec and instrument detection limit.
A. 5测定步骤 Determination procedure
A.5.1按仪器说明书开启仪器,调节各操作参数,至仪器的各参数稳定。
Start instrument according to the instrument manual and adjust the
operating parameters to the instrument stability parameter.
A.5.2 根据分析任务,选定适当的谱条件。这些条件包括:载气流量,样气流量,控制1只十通阀、2只六通阀运转的时间程序的设置,仪器气路平衡条件的选择等。
According to the analysis assignment to select suitable
chromatographic conditions. These conditions include: carrier gas
flow rate, sample gas flow rate, control operating time setting of 1
ten-ways valve, 2 six –ways valve and the choice of instrument
pneumatic balance condition etc.
A.5.3 将标准样品接入仪器,在充分置换取得代表样后进样。平行测定至少两次,直至相邻两次测定的待测组分的谱响应值的相对偏差不大于5%,取其平均值。
Connect standard sample to the instrument and introduce sample
gas when representative sample in full replacement. Parallel
determination for at least two times until the adjacent two
chromatographic response values’ relative deviation is not more
than 5%, take the average value.
A.5.4 在与标准样品完全相同的条件下,将待测样品接入仪器,在充分置换取得代表样后进样。平行测定至少两次,直至相邻两次测定的待测组分的谱响应值的相对偏差不大于5%,取其平均值。
Under the condition of identical with standard sample, connect to
be determined sample to the instrument and introduce sample gas
when representative sample in full replacement. Parallel
determination for at least two times until the adjacent two
chromatographic response values’ relative deviation is not more
than 5%, take the average value.
A.5.5 在同样条件下,采用脱除样品气中氧和不脱除样品气中氧的两种测试状态进行测定。
Under the same conditions, it will be two ways of
removal oxygen in the sample gas and non- removal of oxygen in
the sample gas.
A.5.6 完成分析操作后,按说明书的相关要求停机。
Stop the instrument according to the specification requirements
after completion of analysis.
A. 6结果计算 Result calculation
氢中氧+氩、氩、氮、一氧化碳、二氧化碳和甲烷含量的计算见GB/T3634. 1-2006中A.1.6的规定。
Calculation of oxygen + argon, argon, nitrogen, carbon monoxide,
carbon dioxide and methane concentration in hydrogen see the
provisions of A.1.6 in GB/T3634. 1-2006.
同一样品不经过脱氧柱测定氧+氩的含量,通过脱氧柱测定氩含量。用氧+氩含量减去氩含量得到该样品的氧含量。
The same samples without determination the concentration of
oxygen + argon by de-O2 column, but the argon concentration
determined by a de-O2 column. Sample’s oxygen concentration
can be got by oxygen + argon concentration minus the argon
concentration.
附 录B(资料性附录)
Appendix B (Informative appendixes)
变温浓缩进样装置示例
Variable temperature concentration sample injection device
B. 1方法 method
采用液氮浴温度浓缩已知体积的样品,在常温下解吸样品,用载气把浓缩后的待测组分带入气相谱仪的谱柱,分离后进入检测器进行测定。
Using known volume sample with liquid nitrogen bath temperature
concentration, desorption samples at normal temperature, bring
the concentrated to be measured component into chromatograph
column of gas chromatography by carrier gas, determined by
detector after separation.
B. 2 仪器 Instrument
采用热导气相谱仪或氢火焰气相谱仪,配备液氮浴变温浓缩进样装置。实现成套仪器对氢中待测组分的检测限分别应低于本部分表1所列相应技术指标的1/4。图B. 1给出了变温浓缩进样装置的气路
流程示意图。
Using thermal conductivity gas chromatograph or hydrogen flame gas
chromatograph, equipped with liquid nitrogen bath temperature concentrated
sampling device. Implementation of detection limit between packaged
instruments to the component to be tested in hydrogen should be lower
than1/4 respectively for technical specification listed in table 1. Figure B.1
shows the temperature condensed sample pneumatic flow diagram. aux
说明:Illustration
1―样气瓶;Sample gas cylinder
2--载气入口;Carrier gas inlet
3―气路平衡调节阀,Pneumatic balance regulator
4---/L通阀; 8-ways valve
5--载气出口,carrier gas outlet
6―流量计; Flow meter
7―三通阀;3-way valve
8―液氮容器或水容器;Liquid N2 vessel or water vessel
9―液氮或水;Liquid N2 or water
10―浓缩柱,condensed column
n ―鼓泡器;Bubbler
12―三通阀;3-way valve
13―针形取样阀。Needle sampling valve
图B.1参考的变温浓缩气路流程示意圈
Referenced temperature condensed pneumatic flow sketch
B. 3 气体标准样品 Standard sample gas
推荐采用以氢气作为平衡气的气体标准样品。气体标准样品中组分含量应与样品气浓缩后的相应组分含量相近。
Gas balance with hydrogen is recommended for the standard
sample. Component content in standard samples should be close
to the corresponding components content in sample gas after
concentration
标准样品气不经过浓缩直接进样分析。
Standard sample gas goes directly into the analysis without
concentration.
B. 4测定条件Determination condition
B. 4. 1载气、辅助气 Carrier gas, aux. gas
仪器工作所需载气和辅助气参照相应的仪器说明书。
Take reference to instrument instruction for carrier and auxiliary
gas used in Instrument
B. 4.2 浓缩柱condensed column
浓缩柱1:用于浓缩样品中氧+氩、氮组分。长约30cm、内径4mm的不锈钢管,内装粒度为0. 25mm-0. 40mm的活性炭;或其他等效浓缩柱。浓缩柱通氢气在160℃活化4h后使用,浓缩温度为液氮温度(液氮浴),脱附温度为室温水浴。
Condensed column 1: used in O2+AR and N2
components
in
condensed sample. Stainless steel pipe with about 30cm long,
4mm inner diameter, built-in granulate 0. 25mm-0. 40mm active
carbon; or other equivalent condensed column. Through hydrogen
condensed column to be used after activate 4 h in 160 ℃,
condensed temperature is liquid nitrogen temperature (liquid
nitrogen bath), stripping temperature is room water bath
temperature.
浓缩柱2:用于浓缩样品中一氧化碳、二氧化碳和甲烷组分。长约30cm、内径4mm的不锈钢管,内装粒度为。.25mm-0. 40mm的变硅胶;或其他等效浓缩柱。浓缩柱通氢气在160℃活化4h后
使用,浓缩温度为液氮温度(液氮浴),脱附温度为80℃水浴。
Condensed column 2: used in CO, CO2 and CH4 components in
condensed sample. Stainless steel pipe with 30 cm long, 4mm
inner diameter, built-in granulate 0. 25mm-0. 40mm allochroic
silicone; or other equivalent condensed column. Through hydrogen
condensed column to be used after activate 4 h in 160 ℃,
condensed temperature is liquid nitrogen temperature (liquid
nitrogen bath), stripping temperature is 80o
C water bath
temperature.
B. 5浓缩进样步骤 Condensed sampling procedure
B. 5. 1 气路系统可靠性检查和空白值的测定
Pneumatic system reliability inspection and determination of blank value
把变温浓缩装置接入气相谱仪气路系统,按仪器说明书开启仪器至稳定。关闭浓缩柱后在其上套上液氮浴浓缩约5min后,取下液氮浴,并迅速使浓缩柱处于脱附水浴中,然后将载气通过浓缩柱,记录谱信号,无谱信号为正常。否则,应当检查浓缩进样装置气路系统直至无谱信号。此后使载气通过浓缩柱,注意观察并严防空气吸入浓缩进样装置的情况下浓缩载气5min,测定谱系统空白值,空白值应低于本部分高纯氢或超纯氢的相应指标。
Connect variable temperature concentration device to the
chromatograph pneumatic system, start instrument to stable as per
instrument manual. Put on liquid nitrogen bath condensed for
about 5 min after closing the condense column, remove the liquid
nitrogen bath, and quickly make condensed column in stripping
water bath, and then carrier gas goes through the condensed
column, recording the chromatographic signal, regards no
chromatographic signals as normal. Otherwise, shall check the
condensed sampling device until the system without
chromatographic signals. Then make the carrier through
condensed column, observe and beware of no air suction into
condensed sampling device, condensed the carrier gas for 5 min,
determination of blank value in chromatographic systems; blank
value should be lower than the corresponding values of high purity
hydrogen or ultra-pure hydrogen in the text.
B. 5. 2取样 Sampling
选取适当的针形取样阀,把样品气接入浓缩进样系统,充分置换取样管路,使所取样品气具有代表性。
Select appropriate sampling needle valve, introduce the sample
gas into condensed sampling system, full replacement sampling
pipe, makes the sample more representative.
B. 5 . 3 浓缩concentration
调节样品气以1. 0L/min-1. 5L/min的流速通过浓缩柱,置换浓缩柱2min-3min后关闭浓缩柱出口,然后将浓缩柱缓慢套上液氮浴,待垫气结束后打开浓缩柱出口,使样品气流经流量计后放空。
样品气的浓缩体积由被测组分含量和仪器的检测限确定。样品气的体积由流量计计量。
Adjusting the sample gas makes it goes through the condensed
column by 1. 0 L/min - 1. 5 L/min flow rate, after replacement
condensed column for 2 min -3 min close the column outlet, then
slowly put on liquid nitrogen bath on condensed column, open
column outlet wait until the cushion gas over, empty sample gas
flow through the flow meter.
The sample gas condensed volume is determined by the
measured component content and instrument detection limit. The
volume of the sample gas is by flow meter measurement.
B. 5. 4进样 Introducing sampling
浓缩完毕,关闭浓缩柱入口,取下液氮浴,在室温水浴下放掉解吸的氢,解吸的这部分氢也要流经流量计计量,关闭浓缩柱出口,载气通过浓缩柱把待测组分带入谱分析柱。
Close condensed column inlet after concentration completed;
remove the liquid nitrogen bath, drain the desorbed hydrogen at
room temperature water bath; the desorbed hydrogen will be
metering through the flow meter; close the column outlet; to be
measured component will be introduced into chromatographic
column through condensed column by carrier gas.
平行测定气体标准样品和样品气至少两次,直至相邻两次测定的待测组分的谱响应值的相对偏差不大于10X10-2,取其平均值。
Parallel measuring the gas standard samples and sample gas at
least twice until the adjacent two chromatographic response values
of the relative deviation is not more than 10 x10-2, taked the
average value.
B. 6 结果计算 Result calculation
采用峰面积(或峰高)定量,用外标法计算结果。用变温浓缩进样法测定氢中氧+氩、氮、一氧化碳、二氧化碳和甲烷含量时按式(B.1)计算:
The peak area or peak height, quantitative calculation results by
external standard method. As per (B. 1) calculation to determine
oxygen + argon, nitrogen, carbon monoxide, carbon dioxide and
methane content in the hydrogen with variable temperature
condensed sampling method.
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