This standard specifies the gas chromatography method for the determination of trace carbon monoxide and carbon dioxide in industrial ethylene and propylene. This standard is applicable to the determination of carbon monoxide with a concentration greater than 1 mL/m3 and carbon dioxide with a concentration greater than 5 mL/m3 in ethylene and propylene. GB/T 3394-1993 Gas chromatography method for the determination of trace carbon monoxide and carbon dioxide in industrial ethylene and propylene GB/T3394-1993 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Determination of traces of carbon monoxide and carbon dioxide in ethylene and propylene for industrial use by gas chromatography
Ethylent and propylene for industrial nseDetermination of traces of carbon monoxide and carbon dioxidetias chromatographic method
1 Subject content and scope of application
GB/T3394-93
Replaces GB3394B2
This standard specifies the gas chromatography method for the determination of trace carbon monoxide and carbon dioxide in ethylene and propylene for industrial use. This standard is applicable to the determination of carbon monoxide with a concentration greater than 1 mL/m3 and carbon dioxide with a concentration greater than 5 mL/m3 in ethylene and propylene. 2 Reference standards
GB/T13289T. Sampling method for liquid and gaseous ethylene for industrial use GB/T13290 Sampling method for gaseous propylene and butadiene for industrial use 3 Method summary
The gas sample is injected through the sample injection device and carried into the chromatographic column by the carrier gas to separate carbon monoxide and carbon dioxide from other components. It enters the catalytic hydrogenation column to convert carbon monoxide and carbon dioxide into methane, which is then detected by a nitrogen flame ionization detector and its chromatogram is recorded. The carbon monoxide and carbon dioxide content are calculated by the external standard method. The reaction formula for the conversion of carbon monoxide and carbon dioxide into methane is as follows: CO+3H:NI Catalyst
CH+H,O
Ni Catalyst
4 Materials and reagents
4.1 Carrier gas
Hydrogen; purity greater than 99.9%, dried and purified by silica gel and 5A molecular sieve. 4.2 Auxiliary gas
4.2.1 Nitrogen; purity greater than 99.99%, dried and purified with 5A molecular sieve-10. 4.2.2 Air; dried and purified with basic resin and 5A molecular sieve. 4.3 Carbon monoxide
Commercial carbon monoxide with purity greater than 99% can also be prepared as follows: Carbon monoxide obtained by dehydration with formaldehyde and concentrated acid in a water bath heated to 80°C is reacted with 5% alkali, then with gallic acid solution, purified and dried with calcium chloride and phosphorus pentoxide. After the air in the filter is exhausted, it can be collected, with a purity of more than 99%. 4.4 Carbon nitride
Commercial carbon diamine with a purity of more than 99% can also be used to prepare pure carbon dioxide: it is obtained by reacting sodium phosphate with dilute hydrochloric acid and drying with concentrated sulfuric acid. The purity can reach more than 99%: Approved by the State Bureau of Technical Supervision on July 21, 1993, and implemented on July 1, 1994
4.5 Preparation of nickel catalyst
GB/T 3394--93
Weigh 200g of nickel nitrate and dissolve it in 90mL of distilled water, add 80g of 6201 carrier (or other suitable carrier), boil for 5-10min, cool and remove the filtrate. Place it in an evaporator, dry it at 105°C, and then slowly heat it on an electric heater (it should be done in a distilled water tank). Heat until the red dinitrogen is completely eliminated, and then burn it in a nitrogen stream at 450°C for 7 hours to obtain a nickel oxide catalyst. Put it into a clean, dry stainless steel column, and pass hydrogen (about 50ml/min) at 350-380°C for 1 hour to form a reduced nickel catalyst for use. The prepared reduced nickel catalyst should be sealed to prevent contact with air to reduce the catalytic activity. 5 Instrument
It is a gas chromatograph equipped with a hydrogen flame ionization detector, a catalytic hydrogen device and a carrier gas backflush system. The peak height of carbon monoxide and carbon dioxide produced by this instrument at the minimum detection temperature specified in this standard should be twice that of the peak height of the instrument. 5.1 Sample protection system
Gas Injection valve fixed load tube volume 1~3ml
5.2 Chromatographic column
Recommended chromatographic column and typical operating conditions are shown in Table 1. Other chromatographic columns that can achieve the same separation efficiency can also be used. Table 1 Recommended chromatographic column Typical operating conditions Chromatographic column
Column tubing
Inner diameter, mam
Stationary phase particle size, mre
Carrier gas flow rate, ml./mir
Column temperature,
5.3 Catalytic column. Operating conditions are shown in Table 2. Column length, m
Inner diameter, nmm
Column material
Column temperature,
5.4 Detector
Flame ionization detector.
5.5 Recording device
Table 2 Catalytic hydrogenation column operating conditions
TDX-01 Or test 691
stainless steel
0, 177~-0,250
0. 1 ~-0. 2Www.bzxZ.net
stainless steel
350-380
6201,0. 420--0. 250mm(40-60 3)recorder, integrator or chromatographic data processor, 6 Sampling
Take samples according to the technical requirements specified in GB/T13289.GR/T13290, 7 Operating steps
GB/T3394·93
7.1 Setting operating conditions
After starting the chromatograph, make necessary adjustments to achieve the typical operating conditions in Tables 1 and 2, or other suitable conditions that can achieve the same separation. Once the instrument is stable, the measurement can be carried out. 7.2 Preparation of standard samples||t t||This standard adopts the external standard method for quantitative analysis. Prepare a standard gas sample with a roughly equivalent content of carbon monoxide and carbon dioxide in the sample in high-purity olefins (should be free of carbon monoxide and carbon dihydrogen) or pure chlorine (should be free of carbon monoxide and carbon dioxide). 7.3 Determination
7.3.1 Calibration
Use the gas injection valve to inject 1 to 3 ml of standard gas sample into the chromatograph under specified conditions, repeat the measurement twice, and measure the peak areas of carbon monoxide and carbon dioxide after the chromatographic peaks elute, which are used as the external calibration calculation standard. 7.3.2 Sample determination
Take a sample with the same volume as the standard gas sample, inject it into the chromatograph using the gas injection valve, repeat the measurement twice, record and measure the peak areas of carbon monoxide and carbon dioxide, and compare them with the corresponding external standard peak areas. 7.3.3 Chromatogram
A typical chromatogram is shown in Figure 1.
Figure 1 Typical chromatogram of TIDX-01 book
1-----Carbon monoxide; 2---Methane, 3 Carbon dioxide 7.4 Calculation
The contents of carbon monoxide and carbon dinitride in the sample are calculated according to the following formula: XE·
Wherein: X is the content of carbon monoxide or carbon dioxide in the sample, mL/m; E is the content of carbon monoxide or carbon dioxide in the standard gas sample, mL/m; A is the peak area of ​​carbon monoxide or carbon dioxide in the sample; A is the peak area of ​​carbon monoxide or carbon dioxide in the standard gas sample. 8.1 Analytical results The arithmetic mean of repeated determinations is taken as the analytical result, and the unit is volume per cubic meter of product (mlL). 8.2 Repeatability The same operator uses the same instrument and the same operating conditions to perform two repeated determinations on the same sample using normal and correct operating methods. Within the range of carbon dioxide concentration of 5~20ml/m* and carbon monoxide concentration of 10~20mL/m*, the difference between the measured values ​​should not be greater than 15% (95% confidence level) of the arithmetic mean of the two determinations according to FCB/T3394-93. 9. Test report The report should include the following: All information about the sample; batch number, date, time, sampling location, etc.; measurement results; abnormal phenomena observed in the test; any operation not included in this standard and a description of the operating conditions selected by the operator. Additional Notes:
This standard was proposed by China Petrochemical Corporation. This standard is under the jurisdiction of Petrochemical Standardization Technical Committee. This standard is funded by Gonghai Petrochemical Research Institute and the main drafters of this standard are Fang Zhide and Tang Qimin.
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