This standard specifies the maximum permissible concentration of hydrazine in the atmosphere of residential areas and its monitoring and testing methods. This standard is applicable to the monitoring and evaluation of the atmospheric environment in residential areas. GB 18060-2000 Hydrazine ...

GB18060-2000
All technical contents of this standard are mandatory.
In order to implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on the Prevention and Control of Air Pollution, prevent and control the pollution of the residential environment by the waste gas generated by the aerospace industry enterprises, and protect the health of the general public. This standard is formulated in accordance with the principles of formulating residential air hygiene standards, with reference to foreign research results, and based on the actual situation in my country. This standard shall be implemented on January 1, 2001. Appendix A and Appendix B of this standard are both appendices to the standard. This standard was proposed by the Ministry of Health of the People's Republic of China and the Ministry of Aerospace Industry. The responsible drafting unit of this standard is the Seventh Design Institute of the Ministry of Aerospace Industry; participating drafting units are the Academy of Military Medical Sciences of the Chinese People's Liberation Army and the 101st Institute of the Ministry of Aerospace Industry. The main drafters of this standard are Wang Xinchao, Xia Yadong, and Zhu Mingsheng. This standard is entrusted by the Ministry of Health to the Institute of Environmental Health Monitoring of the Chinese Academy of Preventive Medicine for interpretation. 60
National Standard of the People's Republic of China
Hygienic standard for hydrazine in air of residential area
Hygienic standard for hydrazine in air of residential area This standard specifies the maximum permissible concentration of hydrazine in air of residential area and its monitoring and inspection methods. This standard is applicable to the monitoring and evaluation of the atmospheric environment in residential areas. 2 Standard Content
2.1 The hygienic standard value of hydrazine in air of residential area is stipulated as follows: daily average maximum permissible concentration: 0.02mg/m2; one-time maximum permissible concentration: 0.05tmg/m2. 2.2 Monitoring and Inspection Methods
The monitoring and inspection methods of this standard are exempted from Appendix A and Appendix B. Approved by the State Administration of Quality and Technical Supervision on April 10, 2000, GB 18060--2000
Implementation on January 1, 2001
A1 Principle
GB 18060--2000
Appendix A
(Appendix to the standard)
Monitoring and testing methods for hydrazine in air Solid adsorption/spectrophotometric method Trace amounts of hydrazine in the air are concentrated by solid adsorbents coated with sulfuric acid, react with sulfuric acid to form hydrazine sulfate, and react with p-dimethylaminobenzaldehyde after desorption to form yellow azine compounds. When measured at a wavelength of 460nm, it complies with the Lambert-Beer law when 0~11.25μg hydrazine is contained in 25mL solution. The molar absorption coefficient is 6.5×10*L/mol·cm. Determination range: 0.007141.00mg/m.
At a flow rate of 1L/min, the minimum detection concentration of 60L of air collected is 0.0012mg/m2. This method is interfered by the oxidation products of chlorine, monomethylhydrazine, and unsymmetrical dimethylhydrazine. Ammonia, unsymmetrical dimethylhydrazine, nitrogen dioxide, sulfur dioxide, hydrogen sulfide, etc. in the air do not interfere with the determination of hydrazine. 2 Reagents or materials
A2.1 Sulfuric acid: high-grade pure. bzxz.net
A2.2 Methanol: high-grade pure.
A2.3 Ethanol: analytical grade.
Hydrazine sulfate: analytical grade.
A2.5 p-Dimethylaminobenzaldehyde: analytical grade. 101 White support: 40-60 mesh.
A2.7 0.05mol/L sulfuric acid: Use a graduated pipette to draw 7mL of concentrated sulfuric acid, slowly add it into a reagent bottle containing 2500mL of distilled water, and shake well.
A2.86mol/L sulfuric acid: slowly inject 33.3mL concentrated sulfuric acid into 50mL distilled water, then dilute accurately to 100mL with distilled water, and shake well.
A2.9 Sulfuric acid-methanol solution: add 200mL methanol into a 250mL volumetric flask, slowly inject 36mL sulfuric acid (A2.8), dilute to scale with methanol, and shake well.
A2.102% p-dimethylaminobenzaldehyde solution: weigh 10.0g p-dimethylaminobenzaldehyde, dissolve it in a reagent bottle containing 500mL ethanol, add 20mL sulfuric acid (A2.1), and shake well. It can be stored at room temperature for two weeks. A3 Instruments or equipment
Graduated tubes with stoppers: 25mL, 10 pcs.
Graduated pipettes: 5mL, 2 pcs; 10mL, 2 pcs. Spectrophotometer.
A3.4 Atmospheric sampler.
A3.5 Barometer with empty box.
A3.6 Sampling sieve.
A3.7 Sampling tube: Process according to Figure A1.
A4 Sampling
Choose the sampling point, install the sampler, and adjust the height so that it is about 1.5m from the ground. Connect the sampling tube, make the tube mouth downward, adjust the timer, and sample at a flow rate of 1I./min. Sample 60L in the living area and 30L in the factory area. At the same time, record the ambient temperature, atmospheric pressure, wind direction, wind speed, etc. When sampling 62
GB 18060--2000
parallel samples, tie the two sampling tubes together. After sampling, remove the sampling tube, seal the two ends of the tube with polyethylene caps, put them in a plastic bag, and send them to the laboratory for analysis. The sampling tube can be stored for half a year at room temperature. A5 Analysis steps
A5.1 Preparation of solid adsorbent and sampling tube Weigh 8.0g of 101 white support, boil in 80ml distilled water for 3min, pour off the upper turbid liquid, rinse repeatedly with distilled water until the rinse liquid is clear and transparent (do not stir with a glass rod). Take the upper clear liquid and use distilled water as a blank, measure the absorbance at 460nm with a 2cm colorimeter, and it is qualified if it is not greater than 0.02.
The washed support is drained with a Buchner funnel, transferred to a table blood, dried at 70C for 40min, moved to a dryer, and cooled to room temperature. Weigh 4.0g of the clean support, spread it flat on table III, and add 11.00ml of sulfuric acid-methanol solution to make it evenly soaked. Place it in a fume hood to air dry, and then dry it at 60C±1C for 40~50min until it is loose and not lumpy, move it to a dryer, and cool to room temperature. Weigh 0.30g of sulfuric acid-coated support and inject it into a special glass sampling tube (Figure A1). Fix the two ends of the support with clean stainless steel mesh (60 mesh) and seal the two ends of the tube with polyethylene caps.
1—Stainless steel mesh; 2-sulfuric acid-coated support
Figure A1 Glass sampling tube
A5.2 Preparation of standard solution
Weigh 0.4066g of hydrazine sulfate and place it in a 1000mL volumetric flask, dilute it to the mark with sulfuric acid (A2.7), and shake it. Take 5.0mL of this solution in a 500ml volumetric flask, dilute it to the mark with sulfuric acid (A2.7), and shake it well. The concentration of hydrazine in this standard solution is 1μg/mL. A5.3 Drawing of standard curve
Take 7 stoppered graduated tubes, add 0.30g of solid adsorbent to each, 2 tubes as blank, and add 1.0, 2.0, 3.0, 4.0.5.0mL of 1ug/mL standard solution to the remaining 5 tubes, respectively. Wash the tube mouth with 0.05mol/L sulfuric acid for 3 times, add 10ml of 2% p-dimethylaminobenzaldehyde solution to each tube, make up to volume with 0.05mol/L sulfuric acid, shake well, and let stand for 30min. Take 0.05mol/L sulfuric acid as reference, measure absorbance at 460nm with 2cm colorimetric III, subtract the blank average absorbance, and get the net absorbance value of each solution. Draw the mass (μg) of hydrazine contained in the solution and the absorbance curve.
A5.4 Colorimetry
The solid adsorbent and stainless steel mesh after sampling are transferred into a stoppered graduated tube. Rinse the sampling tube 4~~5 times and the graduated tube wall 3 times with 0.05mol/L sulfuric acid to make the solution in the tube about 10mL. Shake it intermittently within 10min to promote desorption. The blank tube is operated in the same steps. After 10min, add 10mL of 2% p-dimethylaminobenzaldehyde solution to each graduated tube, dilute it to the scale with 0.05mol/l. sulfuric acid, shake it, let it stand for 30min, and determine its absorbance according to the conditions and steps for making the standard curve. Deduct the blank average absorbance to obtain the mass (μg) of hydrazine contained in the solution.
Result calculation
Calculate the concentration of hydrazine in the atmosphere according to formula (A1). =n×W×1:013X10° X(273 ±T)Q ×tX P × 273
W--the mass of hydrazine contained in the measured solution, μg;...(Al)
Q--sampling flow rate, L/min;
t--sampling time, min;
Pt--atmospheric pressure at sampling, Pa;
T---ambient temperature at sampling, C.
A7 Precision or allowable error
GB 18060-2000
The average coefficient of variation of hydrazine concentration in the range of 0.00714~～1.00mg/m is 0.074. Appendix B
(Standard Appendix)
Methods for monitoring and testing hydrazine in the atmosphere Solid adsorption/gas chromatography B1 Principle
Use a solid adsorbent coated with sulfuric acid to capture hydrazine in the air, then elute with water, add furfural derivatization reagent to generate hydrazine derivatives. Extract with ethyl acetate, and inject the extract into the chromatograph for analysis. Check the standard curve according to the peak height and calculate the hydrazine content. This method can simultaneously determine unsymmetrical dimethyl hydrazine.
Determination range: hydrazine 0.00714~1.00mg/m; unsymmetrical dimethyl hydrazine 0.026~6.7mg/m. The upper limit of determination can be expanded. The minimum detection concentration of the method: hydrazine - 0.0072mg/m2 when sampling 60L; unsymmetrical dimethyl hydrazine - 0. 020 8 mg/m* when sampling 120L.
B2 Reagents or materials
B2.1 Furfural: analytical grade.
B2.2 Ethyl acetate: analytical grade.
B2.3 Sodium acetate: analytical grade.
B2.4 Partial dimethyl: purity above 98%.
B2.5 Hydrazine, sulfuric acid, methanol, 6201 carrier, 0.05mol/L sulfuric acid, 6mol/L sulfuric acid, sulfuric acid-methanol solution are the same as Appendix A. B3 Instruments or equipment
B3.1 Gas chromatograph: with hydrogen flame ionization detector. B3.2 Stoppered test tube: 5mL, 10 pieces.
B3.3 Micro syringe: 10μL, 2 pieces
B3.4 Atmospheric sampler, empty box barometer, sampling tube are the same as Appendix A. B4 Sampling
The sampling operation steps and requirements are the same as Appendix A. B5 Analysis steps
B5.1 Preparation
B5.1.1 Preparation of aldehyde derivatization reagent: Pipette 2mL of freshly distilled aldehyde into a 50mL volumetric flask, dilute to the mark with 0.5mol/L sodium acetate solution, and shake well. B5.1.2 Preparation of solid adsorbent and sampling tube: Prepare solid adsorbent with 6201 support. The steps of boiling, rinsing, acid coating, and drying are the same as those in Appendix A.
GB18060—2000
Weigh 0.20g of sulfuric acid-coated support and inject it into a special glass sampling tube. The two ends of the support are fixed with clean stainless steel mesh. The two ends of the tube are sealed with polyethylene caps.
B5.1.3 Preparation of standard solution:
Take unsymmetrical dimethylhydrazine Wi with a purity of ct and inject it into 0.4mol/L sulfuric acid with a volume of V, (mL) to prepare a standard solution of unsymmetrical dimethylhydrazine. The concentration of unsymmetrical dimethyl (A) is shown in formula (B1). ASXW
Bake hydrazine sulfate at 100℃ for 2h, weigh Wz (mg), dissolve it in 0.4mol/L sulfuric acid V (mL) to prepare a standard solution of hydrazine. The concentration of hydrazine (B) is shown in formula (B2).
Wherein: 0.246
B5.2 Derivatization
Conversion coefficient of hydrazine sulfate and hydrazine;
Purity of hydrazine sulfate.
0. 246c: X Wz
.....( B2 )
After sampling, transfer the solid adsorbent into a stoppered test tube, elute with 2mL of distilled water, add 2mL of aldehyde derivatization reagent, react at room temperature for 60 min, and extract with 1 ml. ethyl acetate for 20 min. B5.3. Chromatographic conditions
Chromatographic column: 10% OV-7/supelcoport, 80~100 mesh; 4m×3mm glass column. Flow rate: carrier gas (N2), 50mL/min; fuel gas (H2), 70mL/min; auxiliary gas (air), 500mL/min. The above values ​​are all indicated by the rotor flowmeter.
Temperature: column temperature 205℃, vaporization chamber and detection chamber 315℃. Injection volume: 10μL.
Typical chromatographic peak diagram is shown in Figure B1.
Figure B1 Chromatographic peak diagram under selected conditions
B5.4 Drawing of standard curve
GB18060--2000
Take 6 test tubes, add 0.20g of solid adsorbent and 2mL of distilled water respectively, add a series of standard solutions of unsymmetrical dimethylhydrazine or hydrazine in turn, and then add 2ml of furfural derivatization reagent respectively, react at room temperature for 60min, extract with 1mL of ethyl acetate for 20min, and inject 10ul of extract into the chromatograph for analysis. Draw the standard curve with the peak height as the ordinate and the sample mass contained in the solution as the abscissa. B5.5 Sample determination
Take 10uL of the extract of the sample to be tested, inject it into the chromatograph for analysis, measure the peak height of unsymmetrical dimethylhydrazine and hydrazine, and find the mass (ug) of unsymmetrical dimethylhydrazine and hydrazine contained in the solution from the standard curve. Mixed samples of unsymmetrical dimethylhydrazine and hydrazine should be analyzed on the same day after sampling. B6 Result calculation
Calculate the concentration of unsymmetrical dimethylhydrazine and hydrazine in the atmosphere according to formula (B3) and (B4). c
Wherein: ct—unsymmetrical dimethylhydrazine concentration, mg/; C2-hydrazine concentration, mg/m*;
α—mass of unsymmetrical dimethylhydrazine contained in the sample solution, μg; b——mass of hydrazine contained in the sample solution, ug; V. —Flow rate corrected to standard state, L/min; Sampling time, min.
Precision or allowable error
The average relative error of unsymmetrical dimethylhydrazine is 9.3%; the average relative error of hydrazine is 3.7%. 66
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·(B3 )
......( BA )80~100 mesh; 4m×3mm glass column. Flow rate: carrier gas (N2), 50mL/min; fuel gas (H2), 70mL/min; auxiliary gas (air), 500mL/min. The above values ​​are all indicated by the rotor flowmeter.
Temperature: column temperature 205℃, vaporization chamber and detection chamber 315℃. Injection volume: 10μL.
Typical chromatographic peak diagram is shown in Figure B1.
Figure B1 Chromatographic peak diagram under selected conditions
B5.4 Drawing of standard curve
GB18060--2000
Take 6 test tubes, add 0.20g of solid adsorbent and 2mL of distilled water respectively, add a series of standard solutions of unsymmetrical dimethylhydrazine or hydrazine in turn, and then add 2ml of furfural derivatization reagent respectively, react at room temperature for 60min, extract with 1mL of ethyl acetate for 20min, and inject 10ul of extract into the chromatograph for analysis. Draw the standard curve with the peak height as the ordinate and the sample mass contained in the solution as the abscissa. B5.5 Sample determination
Take 10uL of the extract of the sample to be tested, inject it into the chromatograph for analysis, measure the peak height of unsymmetrical dimethylhydrazine and hydrazine, and find the mass (ug) of unsymmetrical dimethylhydrazine and hydrazine contained in the solution from the standard curve. Mixed samples of unsymmetrical dimethylhydrazine and hydrazine should be analyzed on the same day after sampling. B6 Result calculation
Calculate the concentration of unsymmetrical dimethylhydrazine and hydrazine in the atmosphere according to formula (B3) and (B4). c
Wherein: ct—unsymmetrical dimethylhydrazine concentration, mg/; C2-hydrazine concentration, mg/m*;
α—mass of unsymmetrical dimethylhydrazine contained in the sample solution, μg; b——mass of hydrazine contained in the sample solution, ug; V. —Flow rate corrected to standard state, L/min; Sampling time, min.
Precision or allowable error
The average relative error of unsymmetrical dimethylhydrazine is 9.3%; the average relative error of hydrazine is 3.7%. 66
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·(B3 )
......( BA )80~100 mesh; 4m×3mm glass column. Flow rate: carrier gas (N2), 50mL/min; fuel gas (H2), 70mL/min; auxiliary gas (air), 500mL/min. The above values ​​are all indicated by the rotor flowmeter.
Temperature: column temperature 205℃, vaporization chamber and detection chamber 315℃. Injection volume: 10μL.
Typical chromatographic peak diagram is shown in Figure B1.
Figure B1 Chromatographic peak diagram under selected conditions
B5.4 Drawing of standard curve
GB18060--2000
Take 6 test tubes, add 0.20g of solid adsorbent and 2mL of distilled water respectively, add a series of standard solutions of unsymmetrical dimethylhydrazine or hydrazine in turn, and then add 2ml of furfural derivatization reagent respectively, react at room temperature for 60min, extract with 1mL of ethyl acetate for 20min, and inject 10ul of extract into the chromatograph for analysis. Draw the standard curve with the peak height as the ordinate and the sample mass contained in the solution as the abscissa. B5.5 Sample determination
Take 10uL of the extract of the sample to be tested, inject it into the chromatograph for analysis, measure the peak height of unsymmetrical dimethylhydrazine and hydrazine, and find the mass (ug) of unsymmetrical dimethylhydrazine and hydrazine contained in the solution from the standard curve. Mixed samples of unsymmetrical dimethylhydrazine and hydrazine should be analyzed on the same day after sampling. B6 Result calculation
Calculate the concentration of unsymmetrical dimethylhydrazine and hydrazine in the atmosphere according to formula (B3) and (B4). c
Wherein: ct—unsymmetrical dimethylhydrazine concentration, mg/; C2-hydrazine concentration, mg/m*;
α—mass of unsymmetrical dimethylhydrazine contained in the sample solution, μg; b——mass of hydrazine contained in the sample solution, ug; V. —Flow rate corrected to standard state, L/min; Sampling time, min.
Precision or allowable error
The average relative error of unsymmetrical dimethylhydrazine is 9.3%; the average relative error of hydrazine is 3.7%. 66
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·(B3 )
......( BA )
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