Some standard content:
National Standard of the People's Republic of China
Health standard for acrylic acid in the air of workplace
Subject content and scope of application
This standard specifies the maximum permissible concentration of acrylic acid in the air of workplace and its monitoring and inspection methods. This standard applies to all types of enterprises that produce and use acrylic acid. 2 Hygiene requirements
The maximum permissible concentration of acrylic acid in the air of workplace is 6mg/m (skin). 3 Monitoring and inspection methods
The gas chromatography determination method is shown in Appendix A (Supplement)). GB16213-1996 approved by the State Administration of Technical Supervision on April 3, 1996
Implementation on September 1, 1996
A1 Principle
GB16213--1996
Appendix A
Gas chromatography
(Supplement)
Use a silicone tube to collect acrylic acid in the air, desorb with acetone, separate with a FFAP-HPO.-ChromosorbWAW-DMCS column, detect with a hydrogen flame ionization detector, qualitatively by retention time, quantitatively by height. A2 Instrument
A2.1 Silicone tube, a glass tube with a length of 100mm and an inner diameter of 4mm, 300mg in the front section and 150mg in the back section of 20-40 mesh silica gel, fixed or separated at both ends and in the middle with absorbent cotton, and sealed at both ends with plastic caps. A2.2 Atmospheric sampler, flow rate 0-1L/min. A2.3 Micro syringe, 1μL, 10μL. A2.4 Stoppered colorimetric tube, 10mL.
A2.5 Gas chromatograph, hydrogen flame ionization detector. Chromatographic column: 1.5 m long, 3 mm inner diameter, glass column. FFAP:H,PO,:ChromosorbWAW-DMCS=3:0.5:100 Column temperature: 120℃
Vaporization chamber temperature: 200℃.
Detection chamber temperature: 200℃.
Carrier gas (nitrogen): 15mL/min.
A3 Reagents
A3.1 Silica gel, 20~～40 mesh, microsphere type, coarse pore silica gel is placed in a beaker, and a 1:1 sulfuric acid and nitric acid mixture is added to a height of 1～2cm above the surface of the silica gel. It is placed in a boiling water bath and boiled for 4 hours. After cooling, the acid layer is discarded, and the acid solution is washed with tap water. Then it is washed with distilled water for several times until there is no sulfate ion. The washed silica gel is dried at 110℃, activated at 360℃ for 3 hours, and then taken out and placed in a desiccator for use. A3.2 Acetone.
A3.3 Enoic acid, chromatographic grade.
A3.4 Phosphoric acid.
A3.5 FFAP, chromatographic stationary liquid.
A3.6 Chromosorb W AW-DMCS support, 60~～80 mesh. A4 Sampling
Open the silicone tube at the sampling site, connect the 150mg end to the sampling pump, place it vertically, and extract 20L of air at a rate of 0.5L/min. A5 Analysis Steps
A5.1 Control Test
Sampling is the same as that of the control sample tube. Open the silicone tube at the site, but do not extract air. Store the sample tube and the control sample tube separately, and record the temperature and pressure at the site.
Sample Treatment
Pour the two sections of silicone in the sample tube and the control tube into the stoppered colorimetric tube, add 0.6mL acetone, shake, and soak for 30min. -+66
A5.3 Drawing of standard curve
GB16213--1996
Add 10mL acetone to a 25mL volumetric flask, weigh accurately, add 2 drops of acrylic acid, weigh accurately again, the difference between the two weights is the amount of acrylic acid, add acetone to the scale, mix well, calculate the acrylic acid content in 1mL solution, this solution is the reserve solution, and store in the refrigerator. Before use, take the reserve solution and dilute it with acetone to 1mL standard solution containing 0.25, 0.50, 0.75, 1.0mg acrylic acid. Take 2αL of the above standard solution and inject it respectively, which is equivalent to injecting 0.5, 1.0, 1.5, 2.0μg acrylic acid. Repeat each concentration three times, and draw a standard curve with the average peak height and the corresponding concentration. Retention time is a qualitative indicator. A5.4 Determination
Take 2μL of sample solution for injection, retention time for qualitative analysis, peak height for quantitative analysis, and the chromatogram is shown in the figure below. Acid
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Time, minwww.bzxz.net
Acrylic acid chromatogram
A6 Calculation
X=C× 300
Where: X--acrylic acid concentration in air, mg/m; C, C—respectively, the acrylic acid content in the samples taken from the silica gel desorption solution at the front and back sections, ug, V. ——Sampling volume under standard conditions, L. A7 Explanation
·(A1)
A7. The detection limit of this method is 4.2×10-1μg (injection of 2μL liquid sample). When the acrylic acid concentration is 0.89, 1.79, 2.69μg/2μL, the coefficient of variation is 12.0%, 12.6%, 3.4% respectively. 167
GB16213—1996
2 Acrylic acid is collected by silicone tube and desorbed with acetone. When the acrylic acid content is 0.2~0.8mg, its desorption efficiency is 78.1%~A7.2
101.3%. Its penetration capacity is 39.3mg/300mg silica gel. A7.3 The collected acrylic acid sample can be stored for at least 15 days at room temperature, and its recovery rate is still above 96%. A7.4 Acetone is volatile. When analyzing samples in summer, the desorbed sample tube needs to be placed in an ice bath for low-temperature injection. Additional notes:
This standard was proposed by the Ministry of Health of the People's Republic of China. This standard was drafted by Harbin Medical University. The main drafters of this standard are Zhu Xiuling, Zhao Youye and Liang Lu. This standard is interpreted by the Institute of Labor Hygiene and Occupational Diseases, Chinese Academy of Preventive Medicine, which is the technical management unit entrusted by the Ministry of Health. 168
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