Some standard content:
HG/T2863-1997
This standard is a revision of the national standard GB7447-1987 "Gas for Bulbs and National Standard GB7448-1987 Inspection Methods for Argon for Bulbs", and after merging, it is adjusted to the industry standard for argon for bulbs. When revising GB7447-1987 and GB7447-1987, the main contents of GB7447-1987 and GB7448-1987 were retained, and two new chapters on scope and reference were added. The moisture content in the technical requirements was revised from the original 20×10" to 15×10~\, and the analysis method of oxygen content was added with "electrochemical method and yellow phosphorus luminescence method". The standard writing format is in accordance with GB/T1.1-1993. This standard shall be implemented from January 1, 1998. From the date of implementation, the original national standard GB7447-1987 "Argon for Bulbs" 、National Standard GB7448-1987 "Test Method for Hydrogen for Light Bulbs". Appendix A of this standard is the appendix of the standard.
This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Southwest Research Institute of Chemical Industry of the Ministry of Chemical Industry. The drafting units of this standard: Southwest Research Institute of Chemical Industry of the Ministry of Chemical Industry, Shanghai Biosi Gas Industry Co., Ltd. The main drafters of this standard: Yan Boju, Li Zongji. 663
1 Scope
Chemical Industry Standards of the People's Republic of China
Argon for Light Bulbs
Argon for glow lamp
This standard specifies the technical requirements, test methods, packaging, marking, etc. of hydrogen for bulbs. HG/T2863—1997
This standard applies to hydrogen for bulbs in steel cylinders prepared by cryogenic method with fluorine gas and nitrogen in the proportion specified in this standard, mainly used as filling gas for incandescent lamps.
Cited standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is released, the versions shown are valid. All standards will be revised, and the parties using this standard should explore the possibility of using the latest versions of the following standards. GB190---1990 Dangerous goods packaging mark GB50991994 Seamless steel gas cylinders
GB/T5831—1986 Determination of trace oxygen in gas by colorimetric method GB/T5832.1-1986 Determination of trace moisture in gas by electrolytic method GB/T 5832. 2--1986
Determination of trace moisture in gas-Dew point method
GB/T6285—1986
Determination of trace oxygen in gas-Electrochemical method
GB/T 7144: 1986
GB/T 8981—1988
Color marking of gas cylinders
Determination of trace hydrogen in gas
GB/T 8984. 2—1997
Gas chromatography
Determination of total content of carbon monoxide, carbon dioxide and hydrocarbons in gas-Gas chromatography
Determination of permanent gas filling
GB 14194—1993
GB/F 14852--1993
3 Requirements
Determination of trace oxygen in gas
Yellow phosphorus luminescence method
The quality of argon gas used in the bulb should meet the requirements of Table 1. Table 1
Hydrogen content, 10-3 (V/V)
Ammonia content, 10-2 (V/V)
Hydrogen content, 10-* (V/V)
Oxygen content, 10-(V/V)
Total carbon content (calculated as alkane), 10-6 (V/V)
Water content, 10-= (V/V)
Approved by Chemical Industry Bureau of the People's Republic of China on March 11, 1997 664
Technical requirements
Implemented on January 1, 1998
4 Test methods
4.1 Sampling
HG/T 2863—1997
4.1.1 Argon gas for bottled bulbs shall be sampled directly from the sample using a needle valve and a metal tube. Before sampling, the bottle valve, needle valve and pipeline shall be purged three times by the pressure increase and decrease method.
4.1.2 Hydrogen gas for bulbs shall be sampled and tested randomly according to Table 2 and accepted in batches. The number of bottles in each batch shall not exceed the number of bottles produced by one operating shift. If the test results show that one bottle does not meet the technical requirements of this standard, double sampling shall be conducted from the same batch of products. If there is still one bottle that does not meet the technical requirements of this standard, the batch of products shall be deemed unqualified. Table 2 Sampling table
Product batch, bottle
Sampling number, bottle
4.2 Determination of argon content:
Argon content is calculated according to formula (1)
Where: -Fluorine content, 10-2,
9 -Nitrogen content, 10-2
4.3 Determination of nitrogen content
The following two methods have equal validity.
4.3.1 Gas thermal conductivity method
4.3.1.1 Principle
9= 100 — 9
With a thermal conductivity cell as the detector, when the argon and nitrogen mixture to be measured enters the measuring arm of the thermal conductivity cell, due to the change in component concentration, it will take away constant heat from the thermistor and cause a change in the resistance of the thermistor. Therefore, a corresponding signal is immediately given at the output end of the measuring bridge, thereby determining the content of the nitrogen component.
4.3.1.2 Analytical Instruments
A gas thermal conductivity analyzer is used. The schematic flow chart of the gas thermal conductivity analyzer is shown in Figure 1: F
1-sample gas bottle or standard gas cylinder, 2-high pressure needle valve; 3-four-way valve; 4-platinum wire thermal conductivity cell; 5-measuring cell; 6-sealing gas reference. Rotor flowmeter: 8-water seal bottle; 9-power supply and measuring bridge; 10 recorder Figure 1 Schematic flow chart of gas thermal conductivity analyzer
4.3.1.3 Reference operating conditions
HG/T 2863-1997
The material of the thermistor element of the four-arm thermal conductivity cell is platinum wire, and the single-arm cold resistance is 13Q. The thermal conductivity cell is kept at a constant temperature of 60℃:
Working current: 200mA:
Sample gas or standard gas flow rate: 500mL/mins Recorder: Full scale 10 mV,
When the nitrogen content is 11×10-2～17×102+, the recorder scale should be greater than 100mm. 4.3.1.4 Determination method
Instrument start-up: Turn on the sample gas source, connect the thermal conductivity cell power supply to keep the cell body at a constant temperature of 60℃, and the instrument can be calibrated or measured after it stabilizes.
Instrument calibration: adjust the working current to 200mA, that is, the recorder pointer stably displays at 8nlV, and then use two bottles of standard gas with known nitrogen content (argon as the base gas) to continuously pass through the measuring arm of the instrument at a flow rate of 500mL/min, and adjust the "zero adjustment potentiometer" and the "range potentiometer" respectively to make the nitrogen content indicated by the instrument consistent with the nitrogen content of the standard gas. The calibration cycle is once a week. Determination: Open the sample gas cylinder valve, use the needle valve to adjust the measured gas flow to 500mL/min, fully replace the needle valve and the instrument pipeline, and continuously pass through the measuring arm of the instrument. After the recorder indication value is stable, read the nitrogen content measurement value. Repeat the determination twice, take the average value as the analysis result, and the relative deviation is not more than 5%.
4.3.2 Thermal conductivity gas chromatography
4.3.2.1 Principle
See 4.3.1.1.
4.3.2.2 Analytical Instruments
A gas chromatograph is used, and the argon carrier gas complies with the technical requirements of GB/T4842-1995 Chlorine. The schematic flow chart of the gas chromatograph is shown in Figure 2:
1-Carrier gas cylinder: 2-—Pressure reducing valve; 3-Pressure stabilizing valve; 4-Pressure gauge 5-Thermal conductivity cell; 6-Six-way valve; 7-Quantitative tube, 8-Chromatographic column, 9-Rotameter, 10-Sample gas or standard gas cylinder: 11-High-pressure needle valve; 12-Water seal bottle, 13- - Stabilized power supply and measuring bridge, 14—Recorder Figure 2 Schematic flow chart of gas chromatograph
4.3.2.3 Preparation of chromatographic column
Put 0.3mm~0.45mm13X molecular sieve or 5A molecular sieve for chromatographic analysis into a stainless steel tube with an inner diameter of 4mm and a length of about 0.7m, and activate it with fluorine gas at 300℃~350℃ for 3h~3.5h666
4.3.2.4 Reference operating conditions
Carrier gas flow rate: 20ml./min~30 ml./min; quantitative tube volume: about 3mI. :
Cold resistance of thermal conductivity cell single arm: greater than 60Ω;
Working current: 70mA;
Column temperature: room temperature;
HG/T 2863—1997
Recorder: full scale 5mV automatic balance potentiometer; Sensitivity attenuator: multiple gears. When selecting the attenuation gear, the instrument sensitivity is required to be at least 160mm when the nitrogen content is 16×10-2, and the instrument noise is less than 1mm.
4.3.2.5 Determination method
Instrument start-up: Turn on the carrier gas, adjust the flow rate to the specified value, connect the thermal conductivity cell source. Adjust the working current to about 70 mA, and analyze after the instrument is stable.
Calibration: Use air or nitrogen standard gas (fluorine gas as base gas), inject through the quantitative tube, measure the peak height and half-peak width of the nitrogen peak, calculate the peak area, and
determine; open the sample gas cylinder valve, use the high-pressure needle valve to adjust the flow, fully replace the red valve, pipeline and quantitative tube, then switch the six-way valve, use the quantitative tube to inject, measure the peak height and half-peak width of the nitrogen peak, and calculate the peak area. Repeat the injection twice, take the average value for calculation, and the relative deviation is no more than 5%.
4.3.2.6 Calculation method
Nitrogen content is calculated according to formula (2):
Where:
Nitrogen component content in sample gas, 10
Nitrogen component content in standard gas, 10-2;
AlNitrogen component peak area in sample gas, mm;
Nitrogen component peak area in standard gas, mm.
When the half-peak width remains unchanged, peak height can be used for quantification. 4.4 Measurement of hydrogen content
According to GB/T 8981.
4.5 Determination of oxygen content
According to GB/T5831 or GB/T6285 or GB/T14852 + but the arbitration method is GB/I5831. 4.6 Determination of total carbon content
According to GB/T8984.2.
4.7 Determination of moisture content
According to GB/T5832.1 or GB/T5832.2, the two methods have equal validity. 5 Packaging and marking
5.1 Packaging container
5.1.1 Gas cylinders for filling, storing and transporting argon gas for bulbs shall comply with the relevant provisions of GB 5099, GB 14194 and the "Regulations on Safety Supervision of Gas Cylinders".
5.1.2 Users return empty bottles to production! 5.2 Filling pressure and filling quantity
After confirming that the temperature of the fluorine gas for bulbs in the gas cylinder is equal to the ambient temperature, use a pressure gauge of not less than 2.5 to measure the gas pressure, which should be 15.0 MPa±1.0 MPa at 20°C. At 20°C, 101.3 kPa, the volume of oxygen for bulbs in the gas cylinder is calculated according to Appendix A (Appendix 667
).
5.3 Marking
HG/T 2863—1997
5.3.1 The steel stamp marking of argon gas cylinders for bulbs shall comply with the provisions of the "Gas Cylinder Safety Supervision Regulations". 5.3.2 The paint color marking of argon gas cylinders for bulbs shall comply with the provisions of GB7144. 5.3.3 The packaging marking of fluorine gas cylinders for bulbs shall comply with the provisions of GB190. 5.3.4 Argon gas products for bulbs should be accompanied by a quality certificate when leaving the factory, and the contents include: a) manufacturer name; b) product name; c) production date; d) volume and pressure of argon gas for bulbs; e) number of this standard; f) certificate number.
HG/T2863
Appendix A
(Appendix of the standard)
Calculation of the volume of nitrogen in steel cylinders and the compressibility coefficients of nitrogen and sensible gasA1 Calculation of the volume of stacked gas for bulbs in steel cylindersThe volume of hydrogen for bulbs in steel cylinders is calculated according to formula (A1) to (A3): V=K×V,
Wherein: V—the volume of argon for bulbs in steel cylinders, m\V,——-the water volume of the cylinder, I.;
K-...converted to the volume conversion coefficient of argon for bulbs at an overflow of 20℃ and a pressure of 101.3kPa. The coefficient K is calculated as follows: www.bzxz.net
where P-
gas pressure in the cylinder measured by the pressure gauge, kPa-gas temperature in the cylinder when measuring pressure, ℃; 293
7---compression coefficient of the argon and nitrogen mixture used in the bulb when the temperature is 1. The compression coefficient Z is calculated as follows:
Z - EY,Z
where: Y,--1 molecular fraction of component; z
compression coefficient of component.
A2Compression coefficient of nitrogen (see Table A1)
Compression coefficient of argon (see Table A2)
14 700
Where P-
Gas pressure in the cylinder measured by the pressure gauge, kPa-Gas temperature in the cylinder when measuring pressure, ℃; 293
7---Compression coefficient of the argon-nitrogen mixture used in the bulb when the temperature is 1. The compression coefficient Z is calculated as follows:
Z - EY,Z
Where: Y,—-1Molecular fraction of component; z
Compression coefficient of component.
A2Compression coefficient of nitrogen (see Table A1)
Compression coefficient of argon (see Table A2)
14 700
Where P-
Gas pressure in the cylinder measured by the pressure gauge, kPa-Gas temperature in the cylinder when measuring pressure, ℃; 293
7---Compression coefficient of the argon-nitrogen mixture used in the bulb when the temperature is 1. The compression coefficient Z is calculated as follows:
Z - EY,Z
Where: Y,—-1Molecular fraction of component; z
Compression coefficient of component.
A2Compression coefficient of nitrogen (see Table A1)
Compression coefficient of argon (see Table A2)
14 700
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