Some standard content:
Chemical Industry Standard of the People's Republic of China
HG 2685-95
Medical Nitrous Oxide
Published in April 1995
Ministry of Chemical Industry of the People's Republic of China
Implementation on January 1, 1996
Chemical Industry Standard of the People's Republic of China
Medical Oxygen
1: Subject content and scope of application
HG2685 95
This standard specifies the technical requirements, test methods, inspection rules, packaging, labeling, storage and transportation of medical nitrous oxide. This standard applies to nitrous oxide prepared by the thermal decomposition process of ammonium nitrate. For surgical anesthesia, analgesia and other medical purposes, molecular formula: N, O
Relative molecular mass: 44.01 (according to the international relative molecular mass in 1991) 2 Reference standards
GB190 Dangerous goods packaging mark
GB601 Preparation of standard solution for full determination analysis (volumetric analysis) of chemical reagents GB/T5832.1 Determination of trace moisture in gas-Electrolytic method GB/T5832.2 Determination of trace moisture in blood-Dew point method
GB7144 Color marking of gas cylinders
GB8986 Test method for medical and aviation breathing oxygen GB/T14600 Nitrous oxide gas for electronics industry HG/T2537 Carbon dioxide for welding
3 Technical requirements
The quality of medical nitrous oxide products shall meet the requirements of Table 1: Fur
Content of ammonia fluoride. 10~1 (V / )
--Chemical limit, 10 (V/V
Dioxide content 10- (V/V)
Gaseous acids and alkalis
Halide (halogen)
Easily reducible
Easily oxidized
Oxygen, phosphide
Water content, g / m
Ministry of Chemical Industry of the People's Republic of China1995-04-05Approved 99.0bzxz.net
Conformity inspection
Conformity inspection
Conformity inspection
Conformity inspection
Conformity inspection
Implemented on January 1, 1996
Retest method
HG 2685 -- 95
The reagents used in this test are analytically pure reagents unless otherwise specified. 4.1 Determination of oxidation rate content
4.1.1 Method summary
Take 100m3 of nitrous oxide sample gas and absorb it with freshly boiled distilled water or deionized water. Read the volume of the sample gas less alkali from the analyzer, which is the nitrous oxide content.
4.1. 2 Reagents and materials
a, distilled water or deionized water without carbon dioxide; b. Empty fat
Instruments and equipment
Nitrous oxide analyzer: its gas tube volume is 100mL, the minimum graduation value is 0.1mL, see Appendix B Figure E1. Water storage bottle: a glass bottle with a bottom opening or equipped with a siphon. b.
4.1.4 Preparation before analysis
Boil the water for analysis for more than 10 minutes, and transfer it to the water storage bottle after cooling to room temperature for use. 4. 1. 5 Determination
4.1.5.1 Apply vacuum piston grease to the glass piston of the analyzer to ensure that there is no air leakage. Connect the outlet pipe of the water storage bottle to branch pipe E with a latex tube, turn the analyzer upside down, open piston C, close piston B, lift the analyzer, make piston B above the liquid level of the water storage bottle, open piston B again, let the piston hole be filled with water, then close it immediately, put the instrument straight, rotate piston B to connect branch pipe D with A, 4.1.5.2 Open the valve of the sample gas cylinder, and use the sample After the gas fully replaces the sampling valve and pipeline by the method of increasing and decreasing pressure at least three times, it enters the analyzer through branch pipe F or G, and purges with sample gas more than ten times the volume of the analyzer. Quickly close the valves C and B, turn piston B to connect the water outlet pipe of the water storage bottle with tube A, and close the pipe after water flows into tube A. Shake the analyzer to allow the water to fully absorb nitrous oxide. 4.1.5.3 Open piston C, release most of the water in tube A, close it, and then open piston B, let water in and shake. Repeat this process several times until tube A is full. 41.5.4 Close pistons B and C, remove the outlet pipe of the water bottle and connect it to branch pipe F or G, use water to exhaust the air in the C support channel, lift the instrument to open piston C, and close C when the liquid level in the analyzer is equal to the liquid level in the water storage bottle. Read the volume of gas reduced by water to obtain the content of nitrous oxide.
4.1.5.5 Repeat the determination twice. The difference between the two determination results is not more than 0.05%. Take the average value as the determination result. 4.1.6 It is allowed to use the method of subtracting the mass content to determine the purity of nitrous oxide. The determination method is shown in Appendix A. When the determination results of the two methods are inconsistent, the water absorption method is used as the arbitration method. 4.2 Determination of carbon monoxide
-4.2.1 Summary of the method
Carbon monoxide is oxidized to carbon dioxide and iodine by diiodine pentoxide at 120℃. The precipitated iodine forms a water-soluble solution with excess potassium iodide. Titrate with sodium thiosulfate standard solution and calculate the amount of carbon supported by determining the iodine content. 4.2.2 Reagents and solutions
, diiodine pentoxide;
b. Potassium iodide (GB T 1272), 160 g/L solution is called potassium iodide 16:0 g, dissolved in appropriate amount of water and diluted to 100 ml and stored in a brown bottle.
C Sodium thiosulfate (GB/T637) standard titration solution, (NazS0)=0.002mot/E:
C Na,S0=0. 1 mol/L standard solution is diluted with freshly boiled water before use to obtain, c(Na,S,0)-0.1 mol/L Preparation of sodium thiosulfate standard solution: according to the provisions of GB/T601.d, EGB/T 625), chemically pure:
C Sodium thiosulfate (GB/T3934), chemically pure. Acid solution: Take solid chromium trioxide and add it to the acid until it is saturated. HG 2685- 95 Starch indicator solution: Take 0.5g of soluble starch, add 5mL of water and stir: slowly pour into 100mL of boiling water, stir constantly, continue to boil for 2min, cool and take the upper clear liquid. The shelf life of this solution is two weeks. 4.2.3 Instruments and equipment. Absorption tube: filled with iodine pentoxide; b. Gas flowmeter; c. Heating furnace: controllable temperature 200±0.5℃, 4.2.4 Preparation before analysis 8. Dry the iodine pentoxide at 200℃ for 2h; b. Place chromium trioxide saturated mercaptic acid solution, solid potassium hydroxide and phosphorus pentoxide into three washing bottles respectively and connect them in order to form a washing device system.
4.2.5 Determination
4.2.5.1 Blank test. Take 5000mL of nitrogen (or air) without carbon monoxide and use the same reagents, dosages and determination steps as the sample for blank test.
4.2.5.2 After fully replacing the sampling pipeline with the sample gas, connect it to the absorption device system and let 5000mL of nitrous oxide gas pass through (1) chromium trioxide saturated sulfuric acid solution, (2) solid potassium hydroxide and (3) phosphorus pentoxide at a rate of about 100mL/min. Then pass through the diiodine pentoxide absorption tube at a constant temperature of 120℃. The precipitated iodine vapor is introduced into the iodine volumetric flask containing potassium iodide solution.
4.2.5.3 After the sample is passed, pass about 5000mL of hydrogen (or air) without carbon monoxide to drive away the iodine vapor remaining in the diiodine pentoxide absorption tube, and then continue to lead it into the potassium iodide solution for absorption. 4.2.5.4 Remove the iodine volume bottle. 2~3mL of human starch indicator solution is filtered with c(NazS,0,)=0.002 mol/L sodium thiosulfate standard solution until colorless, and its usage is recorded. 4.2.6 Calculation of results
Carbon dioxide content (p) is calculated according to formula (1): (V, - V,)× 0.112
Wherein: V—the usage of sodium thiosulfate standard solution in blank determination, mL; V—the usage of sodium thiosulfate standard solution in sample determination, mL; ——the volume of nitrous oxide gas (converted to standard conditions), L; (1)
0.112—under standard conditions, with 1 mLc(NazS,0,)=0.002 nmo1 / L Sodium thiosulfate standard solution equivalent to carbon monoxide, mL
4.2.7 It is allowed to determine the carbon monoxide content in medical nitrous oxide according to the test method specified in Article 4.4 of GB/T14600 "Gas Nitrous Oxide for Electronic Industry". It is allowed to use hydrogen or nitrogen as the cutting gas. When the results of the two methods are inconsistent, the iodine titration method shall be used as the arbitration method.
·4. 3 Determination of nitrous oxide
4.3.1 Reagents and solutions
. Barium hydroxide (GB/T630), 50g/L solution: Dissolve 5g of barium hydroxide in 100mL of water, filter quickly, and store in a sealed container. "Avoid contact with carbon dioxide in the air. b. Sodium bicarbonate (GB/T640). 10g/L solution: Dissolve 1.0g sodium bicarbonate in 100mL of freshly boiled water cooled to room temperature. c. Distilled water or deionized water: To remove carbon dioxide, boil for more than 10 s. 3.2 Instruments and equipment HG 2685 -- 95 Colorimetric tube: capacity 100mL, see Figure B2 in Appendix B; b. Gas flow meter. 4. 3. 3 Determination Add 50mL of clear barium hydroxide solution to each of the two colorimetric tubes, and then add 1.05mL of sodium bicarbonate solution to colorimetric tube No. 1 (equivalent to 300×10- of C0,) with a volume of about 100mL/L. Pass 1000 mL of nitrous oxide gas into tube 2 at a rate of 1:1. The turbidity produced shall not be deeper than that of tube 1. 4.4 Determination of hydrogen nitrate and alkali
According to the determination method of gaseous acid and alkali content in Chapter 6 of GB8986. 4.5 Determination of halides
4.5.1 Reagents and solutions
a Silver phosphate (GB/T 670), 17 g/L solution: weigh 17.0 g of nitric acid, dissolve in 1000 mL of water, shake the spoon and store in a brown bottle.
b. Nitric acid (GB 626)
4.5.2 Instruments
According to the provisions of Article 4.3.2.
4.5. 3 Determination
Add 1mL silver nitrate solution, 50mL water and several drops of concentrated nitric acid to two colorimetric tubes respectively, and pass 3000mL of nitrous oxide gas into one of the tubes at a speed of about 100mL/min. When the liquids in the two tubes are equally clear, it is considered that the halogen content in the medical nitroamine oxide product meets the requirements.
4.6 Determination of easily reducible substances
4.6.1 Reagents and solutions
. Glacial acid (GB/T 676):
b. Starch;
c Potassium iodide (GB/T1272) Starch indicator solution: weigh 1g of starch, add 10mL of water to dissolve, and then transfer to 200mL of boiling water, slowly boil for 5min, and add 0.5~1g of potassium iodide after cooling. 4.6.2 Instruments and equipment
According to the provisions of Article 4.3.2,
4. 6. 3 Determination
Add 50mL potassium iodide starch indicator solution and 1 drop of glacial acetic acid to two colorimetric tubes respectively, and pass 3000mL of nitrous oxide gas into one of the tubes at a rate of 100mL/min. When the colors of the solutions in the two tubes are the same, it is considered that the content of easily reducible substances in the medical nitrous oxide product meets the requirements.
4.7 Determination of easily fluorinated substances
4.7.1 Reagents and solutions
#. Potassium permanganate (GB/ T 643), 3.27L solution: weigh 3.2g potassium permanganate, add 1000mL of water and boil for 15 minutes, seal, let stand for more than 2 days, filter and put into a dry brown bottle, b. Sulfuric acid (GB/ T 625).
4.7.2 Instruments and equipment
a. According to the provisions of Article 4.3.2.
4. %. 3 Determination
Into two colorimetric tubes, add 0.1 mL of 3.2/L potassium permanganate solution, 50 mL of water, and 1-2 mL of sulfuric acid respectively. Add 3000mL of oxynitride gas to one of the tubes at a rate of 100mL/min. When the colors of the solutions in the two tubes are the same, the content of easily oxidized substances in the medical nitrous oxide product meets the requirements. 4.8 Determination of hydrogen nitride and phosphine
4.8.1 Reagents
HG 2685—95
Mercury dichloride (HG/T 3—1068), saturated mercuric dinitride test paper: take a filter paper strip and immerse it in a saturated solution of mercuric dinitride. Take it out after it is submerged, and dry it at 60℃ in the dark. Apparatus and equipment
4.8.2 ±
Detection tube: see Appendix B, Figure B3;
b. Gas flow meter.
4. 8.3 Determination
Clamp the mercuric chloride test paper into the upper grinding mouth of the detection tube, and pass 2000mL of nitrous oxide at a speed of 100mL/min. If there is no spot on the mercuric dioxide test paper, it is considered that the content of hydrogen and phosphine in the medical nitrous oxide product meets the requirements. 4.9 Determination of moisture
The determination of moisture in nitrous oxide gas shall be carried out according to the frequency weighing method specified in GB/T5832.1 or GB/T5832.2 or HG/T2537, 4.4:1. The mass weighing method is used as the arbitration method. 5 Inspection rules
5.1 Medical nitrous oxide products shall be inspected and accepted by the quality supervision department of the manufacturer according to this standard. The manufacturer shall ensure that the quality of all products out of the factory meets the requirements of this standard.
5.2 Medical nitrous oxide products shall be inspected bottle by bottle. 5.3 The sampling method of sample gas is to invert the gas cylinder and sample from the liquid phase; the determination of water content is to vertically turn the gas cylinder and take gas phase samples.
When any index of the tested sample does not meet the requirements of this standard, it shall be judged as unqualified product. 5.5 The user has the right to accept in accordance with the provisions of this standard. 5.6
When the supplier and the screening party have objections to the quality of the product: the supplier and the screening party shall jointly accept or submit to arbitration 6 Packaging, marking, storage and transportation
6.1 The principles and general provisions shall comply with the "Gas Cylinder Safety Supervision Regulations", "Dangerous Goods Transportation Regulations" and relevant regulations of the transportation department.
The color marking of gas cylinders for packaging liquid nitrous oxide shall comply with the provisions of GB7144 and have the words *Medical Nitrous Oxide. 6.2
6.3The maximum allowable amount of medical nitrous oxide in gas cylinders shall be calculated as follows: GV·K
Where: G—the amount of nitrous oxide in the gas cylinder, kg; V—the internal volume of the gas cylinder, L
K—the filling coefficient. 0. 62 kg / L.
6.4 The actual amount of bottled medical nitrous oxide shall be measured by direct weighing. The weighing scale shall comply with the provisions of Chapter 7, Article 56 of the "Regulations on Safety Supervision of Gas Cylinders"
6.5 The gas cylinders returned to the manufacturer for refilling with medical nitrous oxide shall be left with pressure, which shall not be less than 0.5MPa. Gas cylinders without residual pressure, new gas cylinders and gas cylinders that have undergone water pressure tests shall be strictly heated before filling: evacuated and fully replaced with nitrous oxide
66 Before leaving the factory, the bottle mouth, bottle valve stem and the connection between the bottle valve and the threaded part of the bottle for medical nitrous oxide shall be checked for leakage and the bottle cap shall be installed.
6.7 Medical nitrous oxide products shall be accompanied by a product quality certificate when leaving the factory. Its contents shall include a. Product name;
Manufacturer name;
Production date and production batch number:
Packing container number:
Mass plate number of nitrous oxide;
Analysis result:
HG 2685-95
HG 2685 --- 95
Appendix A
Determination of purity of medical nitrous chloride
(Supplement)
A.1 The purity of medical nitrous oxide is calculated by the difference method (expressed in volume fraction) by deducting the oxygen and nitrogen contents, according to formula (A1), =100-(0+0
Where: $——purity of medical nitrous chloride, 10-2 (V/V); 91 oxygen content, 10\2 (V/ V);
mono-nitrogen content, 102 (V/V)
A.2 Method Summary
Gas chromatography is used. The sample to be tested is carried into the chromatographic column and separated and then into the thermal conductivity detector for determination. A.3 Instruments and reference conditions for determination
A,3.1 Instrument: gas chromatograph with thermal conductivity detector. Detection limit: 1×10-3 (V/V)A.3.2 Carrier gas: hydrogen, the purity of which should be greater than 99.9×10-2 (V/v). Flow rate: about 45mL/min, (A)
A.3.3 Chromatographic column: stainless steel tube with a length of about 1.5m and an inner diameter of 4mm, filled with 13X molecular sieve, particle size 250~400um. A.3.4 Column temperature: room temperature.
.A.3.5 Injection volume: about 1 mL
A. 3.6 Working current: About 150 mA,
A.4 Determination steps
A.4.1 Calibration
Use a purity greater than 99.9×10-2 (V/V) hydrogen or nitrous oxide is used as the base gas, and 1×10- (V/V) air is added, or air can be directly sampled as the standard mixed gas. The system is fully replaced with the standard gas in an amount of more than ten times the volume of the injection tube and pipeline, and the measurement is carried out. The injection is repeated at least twice, and the retention time and peak area (or peak height) of oxygen and nitrogen are measured and recorded. When the relative average difference is not greater than 5%, the average value is taken as the measurement value. A4.2 Measurement
The system is fully replaced with the sample gas in an amount of more than ten times the volume of the injection tube and pipeline, and the measurement is carried out. The injection is repeated at least twice, and the retention time and peak area (or peak height) of oxygen and nitrogen are measured and recorded. When the relative average deviation is not greater than 5%, take its average value A, (or other) as the measured value,
A, 5 Result processing
A.5.1 The oxygen and nitrogen contents in medical nitrous oxide products are calculated according to formula (A2):,
Wherein:
The content of component i in the sample gas, 102 (V/v); A,—The content of component i in the standard mixed gas, 10 (V/V): A—The peak area of component i in the sample gas: mm\; A,-The peak area of the component in the standard mixed gas, mm; h—The peak height of component i in the sample gas, mm; -The peak height of component i in the standard mixed gas, mm, (A2)
.HG.2685 95
A.5.2 When calibrating with a standard mixed gas using nitrous oxide as the base gas: use the peak area (or peak height) to calculate the oxygen and nitrogen contents. When calibrating with a standard mixed gas using hydrogen as the base gas or pure air, use the peak area to calculate the oxygen and hydrogen contents. Figure B1
Purity tester
HG 2685 — 95
Appendix B
(reference)
Figure B2 Colorimetric tube
Figure B3 Detection tube
Additional note:
HG 2685-95
This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard was approved by the Southwest Research Institute of Chemical Industry of the Ministry of Chemical Industry. This standard was drafted by the Southwest Research Institute of Chemical Industry of the Ministry of Chemical Industry and Guangzhou Gas Plant. The main drafters of this standard are Liu Feng, Duan Shufang, Wang Fulian and Zou Yongzhong. People's Republic of China
Chemical Industry Standard
Medical Substance
HG 2685 --95
Editor Chemical Industry Standard Compilation and Publishing Group
(Standardization Research Institute of Ministry of Chemical Industry)
Postal Code: 100011
Printing Standardization Research Institute of Ministry of Chemical Industry
Copyright reserved. No reprinting allowed
Printing Sheet 1 Words 18000
Format 880 × 1230 1 / 16
First edition in October 1995
First printing in October 1995
Number 1—500
Cost 7.50 Yuan
16-5890
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