GB/T 3394-2023_English: PDF (GB/T3394-2023)
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Determination of trace carbon monoxide, carbon dioxide and acetylene of ethylene and propylene for industrial use -- Gas chromatographic method
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GB/T 3394-2023
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| GB/T 3394-2009 | English | 160 |
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Ethylene and propylene for industrial use -- Determination of trace carbon monoxide, carbon dioxide and acetylene -- Gas chromatographic method
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GB/T 3394-2009
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| GB/T 3394-1993 | English | 239 |
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Ethylene and propylene for industrial use. Determination of trace of carbon monoxide and carbon dioxide. Gas chromatographic method
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GB/T 3394-1993
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| Standard ID | GB/T 3394-2023 (GB/T3394-2023) | | Description (Translated English) | Determination of trace carbon monoxide, carbon dioxide and acetylene of ethylene and propylene for industrial use -- Gas chromatographic method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | G16 | | Classification of International Standard | 71.080.10 | | Word Count Estimation | 14,159 | | Date of Issue | 2023-11-27 | | Date of Implementation | 2024-06-01 | | Older Standard (superseded by this standard) | GB/T 3394-2009 | | Drafting Organization | Sinopec (Shanghai) Petrochemical Research Institute Co., Ltd. | | Administrative Organization | National Chemical Standardization Technical Committee (SAC/TC 63) | | Proposing organization | China Petroleum and Chemical Industry Federation | | Issuing agency(ies) | State Administration for Market Regulation, National Standardization Administration | | Standard ID | GB/T 3394-2009 (GB/T3394-2009) | | Description (Translated English) | Ethylene and propylene for industrial use. Determination of trace carbon monoxide, carbon dioxide and acetylene. Gas chromatographic method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | G16 | | Classification of International Standard | 71.080.10 | | Word Count Estimation | 10,186 | | Date of Issue | 2009-10-30 | | Date of Implementation | 2010-06-01 | | Older Standard (superseded by this standard) | GB/T 3394-1993; GB/T 3395-1993 | | Quoted Standard | GB/T 3723; GB/T 8170; GB/T 13289; GB/T 13290 | | Adopted Standard | ASTM D2505-1988 (2004), NEQ | | Drafting Organization | China Petroleum & Chemical Corporation Shanghai Research Institute of Petrochemical | | Administrative Organization | National Petrochemical Standardization Technical Committee Technical Committee | | Regulation (derived from) | National Standard Approval Announcement 2009 No.12 (Total No.152) | | Proposing organization | China Petroleum & Chemical Corporation | | Issuing agency(ies) | Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China; Standardization Administration of China | | Summary | This standard specifies the determination of industrial ethylene, propylene trace of carbon monoxide, levels of carbon dioxide and acetylene gas chromatography. This standard applies to ethylene, propylene content of not less than 1 mL/m3 of carbon monoxide, carbon dioxide is not less than 5 mL/m3 and not less than acetylene measured 1 mL/m3 of. This standard is not intended to illustrate its use of all safety -related issues. Users are responsible for taking appropriate safety and health practices to ensure compliance with the relevant national regulations. | | Standard ID | GB/T 3394-1993 (GB/T3394-1993) | | Description (Translated English) | Ethylene and propylene for industrial use. Determination of trace of carbon monoxide and carbon dioxide. Gas chromatographic method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | G16 | | Classification of International Standard | 71.080.10 | | Word Count Estimation | 6,631 | | Date of Issue | 1993/7/21 | | Date of Implementation | 1994/7/1 | | Older Standard (superseded by this standard) | GB 3394-1982 | | Regulation (derived from) | Announcement of Newly Approved National Standards 2009 No. (No. 152 overall) 12 | | Proposing organization | China Petrochemical Corporation | | Issuing agency(ies) | State Bureau of Technical Supervision |
GB/T 3394-2023: Determination of trace amounts of carbon monoxide, carbon dioxide and acetylene in ethylene and propylene for industrial use by gas chromatography
ICS 71:080:10
CCSG16
National Standards of People's Republic of China
Replace GB/T 3394-2009
Trace amounts of carbon monoxide in industrial ethylene and propylene,
Determination of carbon dioxide and acetylene
gas chromatography
Published on 2023-11-27
2024-06-01 Implementation
State Administration for Market Regulation
Released by the National Standardization Administration Committee
Preface
This document complies with the provisions of GB/T 1:1-2020 "Standardization Work Guidelines Part 1: Structure and Drafting Rules of Standardization Documents"
Drafting:
This document replaces GB/T 3394-2009 "Determination of trace amounts of carbon monoxide, carbon dioxide and acetylene in industrial ethylene and propylene in gas phase
"Chromatography", compared with GB/T 3394-2009, in addition to structural adjustments and editorial changes, the main technical changes are as follows:
a) Changed the scope (see Chapter 1, Chapter 1 of the:2009 edition);
b) The gas used for preparing standard samples has been deleted (see 4:4 of the:2009 edition);
c) Change the chromatographic column and measurement conditions for carbon monoxide and carbon dioxide analysis (see Chapter 4, Chapter 5 and 7 of the:2009 edition)
chapter);
d) The chromatographic column and measurement conditions for acetylene analysis have been changed (see Chapter 5, Chapter 5 and Chapter 7 of the:2009 edition);
e) The repeatability limits of the method have been re-determined (see Chapter 7, Chapter 9 of the:2009 edition);
f) Added quality assurance and control (see Chapter 8):
Please note that some content in this document may be subject to patents: The publisher of this document assumes no responsibility for identifying patents:
This document is proposed by China Petroleum and Chemical Industry Federation:
This document is under the jurisdiction of the National Chemical Standardization Technical Committee (SAC/TC63):
This document was drafted by: Sinopec (Shanghai) Petrochemical Research Institute Co:, Ltd:
The main drafters of this document: Song Shiyao, Li Jiwen, Jiang Liyan, Li Chengwei, and Wang Chuan:
The previous versions of this document and the documents it replaces are as follows:
---First published as GB/T 3394-1982 in 1982, first revised in:1993;
---In the second revision in:2009, GB/T 3395-1993 "Determination of Trace Acetylene in Industrial Ethylene by Gas Chromatography"
The contents of the Law (the previous versions of GB/T 3395-1993 are released as: GB/T 3395-1982);
---This is the third revision:
Trace amounts of carbon monoxide in industrial ethylene and propylene,
Determination of carbon dioxide and acetylene
gas chromatography
Warning---This document is not intended to address all safety issues related to its use: It is the user's responsibility to take appropriate safety and
health measures to ensure compliance with relevant national laws and regulations:
1 Scope
This document specifies the use of gas chromatography for the determination of trace amounts of carbon monoxide, carbon dioxide and acetylene in industrial ethylene and propylene:
This document is applicable to the determination of carbon monoxide, carbon dioxide and acetylene with a content of not less than 0:5mL/m3 in ethylene and propylene:
2 Normative reference documents
The contents of the following documents constitute essential provisions of this document through normative references in the text: Among them, the dated quotations
For undated referenced documents, only the version corresponding to that date applies to this document; for undated referenced documents, the latest version (including all amendments) applies to
this document:
GB/T 3723 General Safety Principles for Sampling Industrial Chemical Products
GB/T 8170 Numerical rounding rules and expression and determination of limit values
GB/T 13289 Sampling method for liquid and gaseous ethylene for industrial use
GB/T 13290 Liquid sampling method for propylene and butadiene for industrial use
3 Terms and definitions
There are no terms or definitions to be defined in this document:
4 Determination of carbon monoxide and carbon dioxide
4:1 Summary of methods
Inject the gas (or liquid after vaporization) sample into the chromatograph through the sampling device and bring it into the packed column with carrier gas to make carbon monoxide and carbon dioxide
Separated from other components, carbon monoxide and carbon dioxide are converted into methane through a catalytic hydrogenation column: Detected with a hydrogen flame ionization detector (FID),
Record the chromatographic peaks of each impurity component and use the external standard method for quantification:
The reaction principle of converting carbon monoxide and carbon dioxide into methane is as follows:
CO 3H2
350℃~400℃
Ni catalyst→CH4 H2O
CO2 4H2
350℃~400℃
Ni catalyst→CH4 2H2O
4:2 Reagents and materials
Warning---The gas in 4:2 is a high-pressure compressed gas or an extremely flammable gas, so please pay attention to its safe use:
4:2:1 Carrier gas and auxiliary gas
High-purity nitrogen, with a purity of not less than 99:999% (volume fraction), dried and purified through silica gel and 5A molecular sieves:
......
GB/T 3394-2009
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.080.10
G 16
Replacing GB/T 3394-1993, GB/T 3395-1993
Ethylene and Propylene for Industrial Use
– Determination of Trace Carbon Monoxide, Carbon
Dioxide and Acetylene – Gas Chromatographic Method
ISSUED ON: OCTOBER 30, 2009
IMPLEMENTED ON: JUNE 01, 2010
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative References ... 4
3 Summary of Method ... 5
4 Reagents and Materials ... 5
5 Instruments ... 6
6 Sampling ... 11
7 Analysis Procedures ... 11
8 Presentation of Analysis Results ... 12
9 Precision ... 12
10 Test Report ... 13
Ethylene and Propylene for Industrial Use
– Determination of Trace Carbon Monoxide, Carbon
Dioxide and Acetylene – Gas Chromatographic Method
1 Scope
This Standard specifies a gas chromatographic method for the determination of trace carbon
monoxide, carbon dioxide and acetylene in ethylene and propylene for industrial use.
This Standard applies to the determination of carbon monoxide with content no less than
1mL/m3, carbon dioxide with content no less than 5mL/m3, and acetylene with content no less
than 1mL/m3 in ethylene and propylene.
This Standard is not intended to address all safety issues related to its use. It is the user's
responsibility to take appropriate safety and health measures to ensure compliance with the
relevant state regulations.
2 Normative References
The provisions in following documents become the provisions of this Standard through
reference in this Standard. For dated references, the subsequent amendments (excluding
corrigendum) or revisions do not apply to this Standard, however, parties who reach an
agreement based on this Standard are encouraged to study if the latest versions of these
documents are applicable. For undated references, the latest edition of the referenced document
applies.
GB/T 3723 Sampling of Chemical Products for Industrial Use – Safety in Sampling (GB/T
3723-1999, idt ISO 3165:1976)
GB/T 8170 Rules of Rounding off for Numerical Values & Expression and Judgement of
Limiting Values
GB/T 13289 Ethylene for Industrial Use - Sampling in the Liquid and the Gaseous Phase
(GB/T 13289-1991, neq ISO 7382:1986)
GB/T 13290 Propylene and Butadiene for Industrial Use - Sampling in the Liquid Phase
(GB/T 13290-1991, neq ISO 8563:1987)
concentrated sulfuric acid; then it is treated with 50% lye, pyrogallic acid-based solution, and
then the calcium chloride and phosphorus pentoxide to purify and dry. After the air in the
container is exhausted, it can be collected, and the purity is over 99%.
4.4.4 Carbon dioxide: commercial carbon dioxide with a purity (volume fraction) greater than
99%, pure carbon dioxide can also be prepared by the following method: use the carbonate
sodium to react with dilute hydrochloric acid, and obtain it after drying with concentrated
sulfuric acid. The purity can reach over 99%.
4.4.5 Acetylene: the purity (volume fraction) is greater than 99%. It may use the commercial
acetylene with a purity of more than 99%, and pure acetylene can also be prepared by the
following method: take tens of grams of calcium carbide; put it into a 500mL three-necked flask;
pour an appropriate amount of water into the separatory funnel on the three-necked flask; and
add dropwise to the three-necked flask. The produced acetylene needs to be purified by 20%
(mass fraction) sodium hydroxide solution and 20% (mass fraction) chromic anhydride solution.
After the air in the container is exhausted, it can be collected. The purity of acetylene can reach
over 99%.
4.5 Standard sample
Carbon monoxide, carbon dioxide or acetylene standard samples can be purchased from the
market for the certified standard samples or self-prepared. If the base gas is nitrogen or ethylene
(4.4.1), it shall not contain carbon monoxide, carbon dioxide or acetylene; otherwise, it shall
be corrected. The content of carbon monoxide, carbon dioxide or acetylene in the standard
sample shall be close to the concentration in the sample to be tested.
5 Instruments
5.1 Gas chromatograph: equipped with a ten-port valve sample-injecting device (quantitative
tube volume of 1 mL ~ 3 mL), a backflushing device, a split sample-injecting system and a
flame ionization detector (FID); and the dual gas path gas chromatography that can be operated
under the conditions of Tables 1 or 3. The determination of carbon monoxide and carbon
dioxide also needs to be equipped with a nickel reformer catalytic hydrogenation device. The
peak height produced by the instrument for the minimum detection concentration of impurities
specified in this Standard shall be at least twice the noise. The ten-port valve connection and
backflushing device of the instrument are shown in Figures 1 and 2. Other sample-injecting and
backflushing devices that meet the separation and quantification effects of this Standard may
also be used.
the determination of acetylene are shown in Table 3; and the typical chromatograms are shown
in Figures 5 and 6. Other chromatographic columns and analytical conditions that give
equivalent separation and quantification may also be used.
5.3 Nickel reformer: The nickel reformer is a device that converts carbon monoxide and carbon
dioxide into methane by catalytic hydrogenation; and consists of a nickel catalytic
hydrogenation column and a heating device. The recommended operating conditions of the
nickel catalytic hydrogenation column are shown in Table 2 (the operating conditions of the
packed column and capillary column are the same).
The nickel catalytic hydrogenation column is prepared as follows: Weigh 200g of nickel nitrate
and dissolve it in 90mL of distilled water; add 80g of 6201 chromatographic carrier or other
suitable carriers; boil for (5~10) min; cool off; filter; and place the carrier in an evaporating
dish. Dry at 105 ℃; and then placed on an electric furnace to heat slowly (shall be in a fume
hood) until the reddish-brown nitrogen dioxide is exhausted. After burning at 450℃ for 7 h
under nitrogen-injecting state; cool off; and obtain a nickel oxide catalyst. Put it into a clean
and dry stainless steel column tube; and inject hydrogen gas (flow rate is about 50 mL/min) at
350 ℃ ~ 380 ℃ for 4 h to reduce it to nickel catalyst and it can be used. The prepared nickel
catalytic hydrogenation column shall be sealed and stored to prevent the activity of the catalyst
from being reduced after contact with air and water.
NOTE: Standard samples shall be used to check the reactivity of the nickel catalytic hydrogenation
column regularly.
5.4 Recording device: electronic integrator or chromatographic data processing device.
Take the gas sample with the same injection volume as the standard sample; inject it into the
chromatograph by the gas sample-injecting valve; repeat the measurement twice; record the
peak area of carbon monoxide, carbon dioxide or acetylene; and compare it with the
corresponding external standard peak area.
NOTE: When injecting liquid propylene sample, measures shall be taken to ensure that the liquid
propylene is completely vaporized. It can also be vaporized by means of a flash evaporating injector or
a water bath.
8 Presentation of Analysis Results
8.1 Calculation
8.1.1 The content, φi, of carbon monoxide, carbon dioxide or acetylene, measured in milliliters
per cubic meter (mL/m3), shall be calculated according to Formula (1):
Where:
φs - the content of carbon monoxide, carbon dioxide or acetylene in the standard sample, in
milliliters per cubic meter (mL/m3);
Ai - the peak area of carbon monoxide, carbon dioxide or acetylene in the tested sample;
As - the peak area of carbon monoxide, carbon dioxide or acetylene in the standard sample.
8.2 Presentation of results
8.2.1 The numerical value of the analysis result shall be rounded off according to the provisions
of GB/T 8170; and the arithmetic mean of the results of two repeated determinations shall be
taken to represent the analysis result.
8.2.2 Report the content of carbon monoxide, carbon dioxide or acetylene, and accurate to
1mL/m3.
9 Precision
9.1 Repeatability
In the same laboratory, the absolute difference between the two independent test results
obtained by the same operator using the same equipment, according to the same test method,
and testing the same test object independently of each other in a short period of time shall not
exceed the values listed in Table 4. The given repeatability limit (r) is premised on the condition
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