Some standard content:
National Standard of the People's Republic of China
Health standard for sumithionin the air for workplace
Subject content and scope of application
This standard specifies the maximum permissible concentration of sumithion in the air for workplace and its monitoring and inspection methods. This standard applies to all types of enterprises that produce and use sumithion. 2 Hygiene requirements
The maximum permissible concentration of sumithion in workplace air is 1mg/m (skin) Monitoring and inspection methods
GB16205-1996
Use gas chromatography, see Appendix A (supplement), or naphthylethylenediamine hydrochloride colorimetric method, see Appendix B (supplement). 4 Supervision and implementation
Health supervision agencies at all levels are responsible for the implementation of this standard. Approved by the State Administration of Technical Supervision on April 3, 1996 442
Implemented on September 1, 1996
A1 Principle
GB16205—1996
Appendix A
Gas chromatography
(Supplement)
Use a silicone tube to collect chlorpyrifos in the air, desorb and inject with acetone, separate with SF-30 and QF-1 mixed columns, and detect with a flame photometric detector. Qualitative analysis is based on retention time and quantitative analysis is based on peak height. The detection limit of this method is 2.5×10-4μg (injection of 1μL liquid sample). A2 Instruments
A2.1 Silicone tube: Use a glass tube with a length of 70mm and an inner diameter of 8mm, which contains two sections of 20-40 mesh silica gel, the front section contains 600mg, the back section contains 200mg, the middle section is separated by 1mm thick glass wool, and the two ends are plugged with 2mm thick glass wool. A2.2 Sampling pump, 01L/min.
A2.3 Micro syringe, lμl., 10ul. A2.4 Stoppered colorimetric tube, 10mL.
A2.5 Gas chromatograph, flame photometric detector. A3 Reagents
A3.1 Silica gel: 20~~40 mesh. Crush the primary silica gel, sieve, select 20~～40 mesh silica gel in a beaker, add 1+1 sulfuric acid and nitric acid mixture to 1~～2cm above the surface of silica gel, boil in a boiling water bath for 4h, discard the acid layer after cooling, wash the acid solution with tap water, and then wash with distilled water several times until there is no sulfate ion, dry the washed silica gel at 110℃, activate at 360℃ for 3h, take out and put it in a dryer for use. A3.2 Acetone
A3.3 Kill pine.
A3.4 SE-30, chromatographic stationary liquid.
A3.5 QF-1, chromatographic stationary liquid.
A3.6 Chromosorb W AW-DMCS support, 80～100 mesh. A4 Sampling
Open the silica gel tube at the sampling site, connect the 200mg end to the sampling pump and place it vertically, and collect 10~～30I of air at a speed of 0.5L/min. 5 Analysis steps
A5.1 Chromatographic conditions
Chromatographic column: 1.5m long, 3mm inner diameter, glass column; SE-30: QF-1: Chromosorb WAW-DMCS=3:2:100; column temperature: 200℃;
vaporization chamber temperature: 250℃;
detection chamber temperature: 250℃;
carrier gas (nitrogen): 1.85kg/cm.
A5.2 Control test: same sampling. Bring the silicone tube to the site, but do not extract air, and analyze the sample. A5.3 Sample processing: Pour the two sections of silica gel collected into stoppered colorimetric tubes, add 4mL acetone, mix on a vortex mixer, and soak for 3h.
GB16205--1996
A5.4 Drawing of standard curve: Accurately weigh a certain amount of chloranil standard, dissolve it with methanol to make 1mL of stock solution equivalent to 1.0mg chloranil, store it in a refrigerator, take the stock solution before use, dilute it with acetone to 0.25, 0.50, 1.0, 2.5, 5.0, 10.0ug/mL standard solution. Use a micro syringe to take 1μL and inject it into the chromatograph, repeat each concentration 3 times, take the average value of the peak height, plot the peak height with the content of chloranil, draw a standard curve, and use the retention time as a qualitative indicator. A5.5 Determination: Take 1μL of acetone desorption solution for injection, and use the retention time for qualitative analysis and the peak height for quantitative analysis. A6 Calculate
X-Ci+c
Where: X
The concentration of chloranil in the air, mg/m;
-is the content of chloranil in the silica gel acetone desorption solution taken from the front section and the back section, μg; CiC2
V. -—-The sample volume under standard conditions, L. A7 Notes
A7.1 When the content of chloranil is 0.25, 0.50, 1.0, 5.0, 10.0ng/uL, the coefficient of variation is 6.9%, 4.4%, 1.1%, 3.6% and 4.4% respectively.
A7.2 The collected samples can be stored at room temperature for 5 days, and the recovery rate is 98.9% to 104.2%. A7.3 With acetone as the desorbent, the desorption efficiency is 96.5%, and the sampling efficiency can reach 100%. A7.4 Neither the intermediates nor the raw materials of sedrin interfere with the determination. Appendix B
Ethylene diamine hydrochloride colorimetric method
(Supplement)
B1 Principle
Use titanium trichloride to reduce sedrin to an amino compound in an acidic solution, and then couple with naphthylethylene diamine hydrochloride to generate a purple-red color. Colorimetric quantification. bzxZ.net
The detection limit of this method is 0.5μg/5mL.
B2 Apparatus
Porous glass plate absorption tube.
B2.2 Vacuum pump.
B2.3 Flow meter, 0～1L/min.
B2.4 Stoppered colorimetric tube, 10mL.
B2.5 Spectrophotometer, 20mm colorimetric cup. B3 Reagents
B3.1 Absorption solution: 40% (V/V) ethanol solution. B3.2
Titanium trichloride, 150g/L.
B3. 3 Hydrochloric acid, c(HCI)=8 mol/L
B3.4 Sodium nitrite solution, 30g/L.
B3.5 Ammonium sulfamate solution, 20g/L.
B3.6 Naphthylethylenediamine hydrochloride solution, 10g/L. GB.16205-1996
B3.7 Standard solution: Weigh an appropriate amount of pure chloranil, dilute it with anhydrous ethanol solution to a 1mL 1mg chloranil stock solution and store it in a refrigerator. Before use, take an appropriate amount of stock solution and dilute it with ethanol (B3.1) to a 1mL = 10μg chloranil standard solution. B4 Sampling
Connect two porous glass plate absorption tubes each containing 5ml of absorption liquid in series, and extract 100L of air at a rate of 0.75L/min. B5 Analysis steps
B5.1 Control test: Same sampling. Take the absorption tubes filled with absorption liquid to the site, but do not extract air, and analyze as the sample. B5.2 Sample treatment: Transfer the absorption liquid in the two absorption tubes to two colorimetric tubes respectively, and wash the absorption tubes with absorption liquid (B3.1) to make the total volume 5mL respectively.
B5.3 Drawing of standard curve:
Prepare standard tubes according to Table B1. Add 0.05mL titanium trichloride (B3.2) and 0.2mL hydrochloric acid (B3.3) to each standard tube, shake vigorously for 5 minutes, add 0.1mL sodium nitrite solution (B3.4), shake until there are no bubbles, let stand for 5 minutes, add 0.5mL ammonium sulfamate solution (B3.5), shake vigorously and let stand for 5 minutes, add 0.5mL naphthylethylenediamine hydrochloride solution (B3.6), and after 30 minutes, use a 20mm colorimetric cup to compare the color at a wavelength of 550nm, and draw a standard curve by plotting the content of sedum chloramphenicol against the absorbance. Table B1 Preparation of sedum chloramphenicol standard tube
Standard solution, mL
Absorbent, mL
Sedum chloramphenicol content·ug
B5.4 Determination: The sample tube operation is the same as the standard tube, and the sedum chloramphenicol content is found from the curve after color comparison. B6 Calculation
X=Ci+C
Where: X is the concentration of chlorpyrifos in the air, mg/m, - is the content of chlorpyrifos in the first and second absorption tubes, μg; CC
V. —The sample volume under standard conditions, L. B7 Notes
B7.1 When the concentration of chlorpyrifos is 2, 6, and 10μg/5mL, the coefficient of variation is 6.0%, 2.2%, and 5.7%, respectively. 5
B7.2 The titanium trichloride solution changes from purple-red to brown and has white precipitation, indicating that it is oxidized and cannot be used. At this time, just add a few zinc particles to the titanium trichloride solution, shake it and leave it for a few minutes. After filtering, it will be purple-red and can be used. B7.3 The first step of this method must be shaken vigorously. If the color is not obvious enough within the specified time, the reaction time of each step needs to be appropriately extended.
B7.4 Nitro compounds below 150μg have no interference with the determination of this method. 445
Additional remarks:
GB16205—1996
This standard is proposed by the Ministry of Health of the People's Republic of China. This standard is drafted by the Institute of Occupational Disease Prevention and Control of Zhejiang Academy of Medical Sciences. The main drafter of this standard is Yu Yongqie.
This standard is interpreted by the Institute of Labor Hygiene and Occupational Diseases of the Chinese Academy of Preventive Medicine, the technical unit entrusted by the Ministry of Health. 116
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