1.1 This standard specifies the determination of methane, ethane, propane, butane, isobutane, propylene, acetylene, propadiene, cis-2-butene, 1-butene, isobutylene, trans-2-butene, methylacetylene and 1,3-butadiene in industrial ethylene by gas chromatography. Since this standard cannot determine all possible impurities such as CO, CO1, HzO, alcohols, NO and alkyl sulfides, as well as hydrocarbons higher than decane, other test methods are required to fully characterize the ethylene sample. 1.2 This standard does not purport to address all safety issues associated with its use. Therefore, the user of this standard should have the responsibility to establish appropriate safety and protection measures and determine appropriate regulations in advance. GB/T 3391-2002 Determination of hydrocarbon impurities in industrial ethylene by gas chromatography GB/T3391-2002 Standard download decompression password: www.bzxz.net

Ics 71. 080. 01
National Standard of the People's Republic of China
CB/33912002
Ethylcnc for industrial usc
Determination of hydrocarhon impurities-Gas chromatographic Method
2002-10-15 Issued
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
2003-04-01 Implementation
GB/T33912002
This standard is equivalent to ASTM D519, Standard for the determination of hydrocarbon impurities in 1991 sieves by colorimetric method CB133911991. The differences between this standard and ASTM D55:7 are as follows: 1. The double-rod coupling system recommended in the standard is changed to a chromatograph; 2. The detection conditions that can also be used as the standard are added; 5. The standard is determined by the user; this standard is a revision of the original standard. The main contents of the revision are: using AI and PT capillary tubes to replace the original standard aluminum filling rate, and the original standard text has been fully revised. This standard is G/T3391191: This standard is issued by China National Chemical Standardization Co., Ltd. This standard is the responsibility of the National Chemical Standardization Technical Committee, Shanghai Institute of Chemical Technology: Wang Chao, Lin Weisheng, Zhi Liumin. This standard was first issued in December 2012, and the scope of the revision is as follows: National Standard of the People's Republic of China Determination of hydrocarbon impurities in industrial olefins Gas chromatography Ethylene Far indistrial uke-
Determinatinn of hydracarhnn impuriticsGax chromatographic.methrd
GH/T3391—2002
Generation (H/T:31-1
1 standard) established European gas chromatography for the determination of ethylene, methane, acetylene, butane, isobutylene, propylene, acetylene, succinimide, cis-2-butylene, butylene, trans-2-butene, and 1.3-butylene. This standard cannot be used to identify all the impurities such as H), hydroxyl groups, and the characteristics of the bases, as well as the requirements of high-density alkanes, so it is necessary to use other test methods to screen the products.
"? This standard does not explain all safety issues related to its exclusive use. Therefore, the use of the standard should first be responsible for establishing appropriate drug safety and protection measures and determining appropriate regulations. 2 Reference standards
The following standards contain provisions: By reference in this standard, they constitute the provisions of this standard. This standard is valid for all editions. All parties who will use this standard should discuss the use of the following standards when the new edition is required. 133-192 Industrial carbon dioxide and trace carbon dioxide in propylene and propylene gas phase color (6415) 6381.1981)
GB5S87, above
B/T9170-1!87 numerical revision specification
Industrial propylene G1329-1991 Industrial Use of Ethylene in Liquid and Gas (1507382:96)3 Method for Sampling Trace Amounts of Ethylene in Liquid State. The detailed requirements are as follows: After the sample is delivered, it can be measured by injecting the transported volume into the fine arm of the chromatograph, and then using a high pressure rapid separation device (F) for effective measurement. The maximum content of impurities can be determined by the external standard method, and the total impurities content can be obtained by reducing the pressure by 100%.
2 Instruments
4.1 Gas chromatograph and () instrument: should be equipped with a true ionization detector 4.2 Ionization detector: should be equipped with 1ID. The process listed in 1.1 has a daily drug compound of about 2.01/1 or low temperature. 4.3 Gas chromatograph: should only be used with standard operating procedures and can withstand temperature protection. The recommended storage conditions are listed in .1. Please restore the process! , the program temperature rise rate test is sufficient to ensure that the decomposition time can reach (.> repeat
The General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China approved 23-C4-01 on October 15, 2002
H/T33912002
4.4 Ribbon K deactivation time A length 5m inner diameter 53m or other suitable inner diameter. Other cases or other special methods for deactivation O, PL process Du can also be used. The peak order and relative window of the normal quality depend on the deactivation method, which must be determined with standard samples Note: In practice, the induction and the teeth on the upper part are not good. You can use a base frame with a length of m. inner diameter n.53mm, thickness 5n). This can improve the separation of the induction. 4.5 Injection system: Use a 1.6mm head to let the gas pass through the sample room and place it on the unheated K area of ​​the gas phase chromatograph. Both the split bed and the non-split flow inlet method are possible.
4.5.1 Details of the non-split flow inlet method; use a volume of 1~, Figure 1 and Figure 2 are typical Amphitheater diagrams of the poor. When reading the connection, care should be taken to avoid dead parts, cold spots, too long connections and uneven heating. Sample in
Select product outlet
Set the treatment center
New product scholars
Figure 2 for details
4.5.2 The splitter is heated by an adjustable controller. The split ratio is 59:1 to 1:1 at 153 (to 29 (). A quantitative tube of 2.500-500 l is used. The typical operation table is shown in Figures 3 and 4. The splitter is used to monitor its performance. At the split ratio of 0:1, 7:1:1, the standard mixture is measured and corrected. The cross-linking cannot exceed 1%:
Quantitative form 9
GB/T3391-2002
And exit
Foreign benefit export
Due to the sample number
Exit of sampling station
Color language busy
Figure 4 Sample
1.6 Data collection system, integration or computer data acquisition system. 5 Reagents and materialsbzxZ.net
5.1 Rapid standard sample: Prepare gas standard by recording method: The concentration level of impurity components in your sample is 2/kg-204mgkg: 4ml./m.~4ml./m: The prepared standard should be verified by analysis to ensure that the difference between the analytical data and the standard content prepared by gravity or method is within 1% Collection: The concentration of impurity components in this standard should be no higher than 2950% of the test sample. 5.2 Reduction gas: The volume fraction of the concentration is 99.999% or higher, the total concentration should be less than 1mL/m, when using hydrogen as carrier, use gas as collection gas To avoid damage and the above industry. Note: The compressed oxygen cylinder gas is a high-pressure gas. 5.3 Method for selling hydrogen + detector fuel gas (class impurities 1m/m\) Note: Emulsion is a kind of flammable high-pressure gas. 5. Gas: When using currency F: Floating air with a diameter of 1m and impurities 6 sampling
According to the technical requirements of 1, if the sample is full of impurities, the corresponding chemical device should be used: Before the sampling, the gas and other respirators present in the steel storage should be caught, and the application of the bottom impact steel point: Instrument preparation
GB/T3391—2002
7.1 Instrument conditions: According to the following corrections Instrument parameters: Hanging: Humidity: 35C Humidity holding time: 2. (rm rise rate: 4Cmi: Final overflow: 1 C: Final temperature holding time: 1: min Gas: atmospheric air Ammonia .5mt/min-AnL/in
Separation sampling system: quantitative collection volume during sampling: 200l.-550 called 1. Inlet temperature: 5~4, split sample humidity: 15C~.200℃, split ratio: 0:1~.10:1FD backflow: 30 air .500ml/min. Oxygen: aml/mi-. Tail gas N..20mL/ain
Flexibility: set to a suitable value that can obtain the mass measurement value. Unfiltered inlet system Inlet network setting volume: 10.-I Inlet valve flow: 351-4 (calculation: 1 heat energy can be naturally changed.
? The air and hydrogen safety can be set according to the built-in modification of the device core production 7.? When the device is stabilized, it is called retrograde analysis.1. The gas standard and the gas are sent to the gas push-in part and the wellbore is connected to the quantitative part 303. Then the standard sample is pushed to the outlet of the plate. When the pressure drops to the pressure, the main sample flows out and the valve is turned to inject the standard sample. The standard analysis should be carried out at least three times to obtain the measurement value.
8.2 Calculation of correction factor According to formula (1), the correction factor of the standard sample is calculated: f = A
A correction factor,
Select the standard sample! The smaller the
, the smaller the number of samples and the pressure! The whole value of the sample, the measurement step
must be measured after the sample is wetted with the gas standard agent and under pressure. 9.2 Connect the gas sample port on the copper cylinder of the gas product to the gas well and stop the flow of the mechanical pipe: then close the outlet valve of the gas cylinder. When the pressure drops to normal and there is no gas flow, turn the valve immediately. Then analyze the peak value of the gas by comparing it with the original gas flow. Typical detailed product diagram is shown in Figure 5: PA
10 Calculation
GBT3391-2DD2
1-alkane 2--ethane 13-internal flame: 1-internal sieve; 5-and" annoyance: 6-effect: 7-di-tri-ethane: -2 t-1C-1 F:1 good: 13-- 2 "life: 13-μ to ethane; 11. " Milk 5 Figure
10.1 According to the formula: the concentration of the sieve quality is corrected to "ml./m" according to the provisions of GB91\. fxA.
In:
The concentration of impurities in a sample: rl,/r
The test quality calculated by the formula, the correction factor:
The system shows the product of drug impurities: mln
1℃.2 Add up the indicated contents of each element to get the total impurity content: the ethylene purity score can be obtained by calculating the total major impurity content of 100.0. If the impurities such as C), C0:), NII) and alcohols cannot be analyzed by manual standards, they can be analyzed according to GB/T 339, Appendix 771·187 AG/T127C and other local methods. When calculating the purity of part B, divide them by:
11 grams of weight
In the same laboratory, with the same equipment and device, the same sample is processed in two different ways. Under the conditions of the equipment, the difference between the following figures is not much: the net mass concentration/m3 is its average value! Quality control: The report of the test results shall include the following contents: GB/T3391—2002 1) Complete information of the sample, such as the name of the sample, batch number, sampling point, date of purchase, time of arrival, etc. 2) Code of this standard. 3) Description of the test results. 4) Details and explanation of any abnormal phenomena observed during the test. 5) Name and date of the analyst, etc.
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