GBZT300.163-2018 English PDF

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GBZT300.163-2018: Determination of toxic substances in workplace air -- Part 163: Toluene diisocyanate
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Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GBZ/T 300.163-2018	139	Add to Cart	3 days	Determination of toxic substances in workplace air -- Part 163: Toluene diisocyanate	Valid

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GBZ 20   GBZ 57   GBZ 49   GBZ/T 300.165   GBZ/T 300.162   GBZ/T 300.164   

Basic data

Standard ID: GBZ/T 300.163-2018 (GBZ/T300.163-2018)
Description (Translated English): Determination of toxic substances in workplace air -- Part 163: Toluene diisocyanate
Sector / Industry: National Standard (Recommended)
Classification of Chinese Standard: C60
Word Count Estimation: 7,755
Date of Issue: 2018-07-16
Date of Implementation: 2019-07-01
Regulation (derived from): State-Health-Communication (2018) No.13
Issuing agency(ies): National Health and Family Planning Commission

GBZ/T 300.163-2018: Determination of toxic substances in workplace air -- Part 163: Toluene diisocyanate

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Determination of toxic substances in workplace air - Part 163. Toluene diisocyanate ICS 13.100 C 52 National Occupational Health Standards Determination of toxic substances in workplace air Part 163. Toluene diisocyanate Determination of toxic substances in workplace air- Part 163. Toluene diisocyanate Published on.2018 - 07 - 16 2019 - 07 - 01 implementation National Health and Wellness Committee of the People's Republic of China

Foreword

This part is the 163th part of GBZ /T 300 "Measurement of Toxic Substances in Workplace Air". This part is drafted in accordance with the rules given in GB/T 1.1-2009. This section is mainly drafted by. Shanghai Chemical Occupational Disease Prevention and Control Institute, Zhejiang Provincial Center for Disease Control and Prevention, Shanghai Disease Prevention and Control center. The main drafters of this section. Wang Zubing, Wang Xiang, Yuan Weiming, Zhu Yiping, Lin Yuanjie. Determination of toxic substances in workplace air Part 163. Toluene diisocyanate

1 Scope

This part of GBZ /T 300 specifies the measurement of impregnated filter paper for the determination of toluene diisocyanate (TDI) in the workplace air - high performance liquid phase Chromatography. This section applies to the detection of toluene diisocyanate concentration in the workplace air.

2 Normative references

The following documents are indispensable for the application of this document. For dated references, only the dated version applies to this document. For undated references, the latest edition (including all amendments) applies to this document. GB/T 6682 Analytical laboratory water specifications and test methods GBZ 159 Sampling specification for monitoring of hazardous substances in the workplace air Basic information on 3 toluene diisocyanate The basic information of toluene diisocyanate is shown in Table 1. Table 1 Basic information of toluene diisocyanate Chemical material Chemical Abstracts (CAS number) Molecular formula relative molecular mass Toluene-2,4-diisocyanate (Toluene-2,4-diisocyanate, 2,4-TDI) 584-84-9 C9H6N2O2 174.15 Toluene-2,6-diisocyanate (Toluene-2,6-diisocyanate, 2,6-TDI) 91-08-7 4 Impregnated filter paper collection of toluene diisocyanate - high performance liquid chromatography 4.1 Principle Reaction of toluene diisocyanate (TDI) in air with 1-(2-pyridyl)piperazine (1-2PP) on impregnated filter paper to form TDI-urea derivatives It is adsorbed on the filter paper, and after elution and filtration, it is determined by high performance liquid chromatography, and the retention time is qualitative, and the peak height or the peak area is quantified. 4.2 Instrument 4.2.1 Glass fiber filter paper with a pore size of 0.8 μm and a diameter of 37 mm or 40 mm. 4.2.2 Impregnated filter paper. In the fume hood, spread the glass fiber filter paper on a clean flat carrier and add 0.50 mL to the center of the filter paper. 1-2PP solution A, the solution should be saturated with the entire filter paper. After being placed for 30 minutes, it should be stored in a sealed dark container and stored in an environment of 2 ° C to 8 ° C. One month. 4.2.3 Sampling clamp, filter material diameter is 37 mm or 40 mm. 4.2.4 Air sampler, flow rate 0.1 L/min ~ 5.0 L/min. 4.2.5 Plug-in test tube, 5 mL or 10 mL. 4.2.6 Microinjector, 10 μL or 100 μL. 4.2.7 Organic phase needle filter with a pore size of 0.45 μm. 4.2.8 Analytical balance with an accuracy of 0.00001 g and 0.001 g. 4.2.9 High performance liquid chromatograph equipped with UV detector or diode array detector, instrument operation reference conditions. a) Column. C18 column, 250 mm × 4.6 mm × 5 μm, or other LC column with similar separation performance; b) mobile phase. acetonitrile. ammonium acetate solution = 40.60 (volume ratio); c) Measurement wavelength. 254 nm; d) Flow rate. 1.0 mL/min; e) Column temperature. 30 °C; f) Injection volume. 20 μL. 4.3 Reagent materials 4.3.1 Unless otherwise specified, the reagents used were of analytical grade. The water is the first grade water specified in GB/T 6682. 4.3.2 Acetonitrile. chromatographically pure. 4.3.3 Dichloromethane. 4.3.4 Dimethyl sulfoxide. 4.3.5 Ammonium acetate. 4.3.6 1-(2-Pyridyl)piperazine (1-2PP). purity ≥ 98%. 4.3.7 Eluent. Measure 10 mL of dimethyl sulfoxide and pour into 90 mL of acetonitrile and mix. 4.3.8 Ammonium acetate solution (0.02 mol/L). Weigh 1.540 g of ammonium acetate, dissolve in water, and dilute to 1000 mL, and mix. 4.3.9 1-2PP solution A (2.0 mg/mL). Weigh 0.200 g of 1-2PP and dissolve it in 100 mL of dichloromethane. 4.3.10 1-2PP solution B (10.0 mg/mL). Weigh 0.100 g of 1-2PP and dissolve it in 10 mL of acetonitrile. 4.3.11 Toluene-2,4-diisocyanate (2,4-TDI). purity ≥98%. 4.3.12 Toluene-2,6-diisocyanate (2,6-TDI). purity ≥98%. 4.3.13 Standard solution. accurately weigh the appropriate amount of 2,4-TDI or 2,6-TDI into a brown volumetric flask, dissolve it with acetonitrile and prepare a concentration of about 2.0. The mg/mL 2,4-TDI or 2,6-TDI standard stock solution can be stored for one week in the dark at 2 °C ~ 8 °C. Dilute with acetonitrile before use The standard solution was mixed with 250 μg 2,4-TDI and 250 μg 2,6-TDI per ml. Or formulated with a nationally recognized standard solution. 4.4 Sample collection, transportation and storage 4.4.1 On-site sampling shall be performed in accordance with GBZ 159. 4.4.2 Short-time sampling. At the sampling point, use the sampling clamp with the impregnated filter paper to collect the sample at a fixed point sampling rate of 1 L/min for 15 min. Air sample. 4.4.3 Long-time sampling. At the sampling point, use the sampling clamp with the impregnated filter paper, and use the fixed point or individual sampling method, 1 L/min flow rate. Set ≤ 1 h air sample. 4.4.4 After sampling, open the sampling clamp, take out the filter paper, fold the dust face inward and fold it twice, and put it into the stopper with 4 mL of eluent. In a test tube, transport and store after sealing. The sample can be stored for 14 days in the dark at 2 ° C ~ 8 ° C. 4.4.5 Sample blank. At the sampling point, open the sampling clamp with the impregnated filter paper, immediately remove the filter paper, and pre-load the 4 mL eluent. In a stoppered test tube, then transported, stored and measured with the sample. Not less than 2 sample blanks per batch. 4.5 Analysis steps 4.5.1 Sample processing. The sample in the plugged test tube is vortexed and eluted for 10 min at room temperature, filtered through a needle filter, and the filtrate is tested. set. 4.5.2 Preparation and determination of the standard series. Take at least 6 volumetric flasks, add 0.10 mL each of 1-2PP solution B, add with a micro syringe Mix 0 μL～100 μL of the mixed standard solution, shake for 30 s, and dilute to 5 mL with eluent to prepare 0.00 μg/mL～5.00 μg/mL. A mixed standard solution of 2,4-TDI and 2,6-TDI. Adjust the HPLC to the best measurement state according to the operating conditions of the instrument. The peak height or peak area of each concentration of the mixed standard series was determined separately. Measure the peak height or peak area to the corresponding 2,4-TDI or 2,6-TDI Degree (μg/mL) is used to draw a standard curve or to calculate a regression equation with a correlation coefficient of ≥0.999. 4.5.3 Sample determination. The sample and sample blank filtrates are determined using the operating conditions of the assay standard series. The measured peak height or peak area value is determined by The standard curve or regression equation gives the concentration of 2,4-TDI or 2,6-TDI in the sample filtrate (μg/mL). If the concentration of the analyte in the filtrate exceeds the test The range is determined by diluting with the eluent and multiplying by the dilution factor. 4.6 Calculation 4.6.1 Convert the sample volume to the standard sample volume according to the method and requirements of GBZ 159. 4.6.2 Calculate the concentration of TDI in air according to equation (1). DV Cc 21)(4  (1) In the formula. c ── the concentration of TDI in the air in milligrams per cubic meter (mg/m3); C1 ─ Measure the concentration of 2,4-TDI in the sample filtrate (minus the sample blank) in micrograms per milliliter (g/mL); C2 ─ Measure the concentration of 2,6-TDI in the sample filtrate (minus the sample blank) in micrograms per milliliter (g/mL); 4 ─ the volume of the eluent in milliliters (mL); V0 —— standard sampling volume in liters (L); D ─ elution efficiency, %. 4.6.3 The time-weighted average contact concentration (CTWA) of TDI in air is calculated in accordance with GBZ 159. 4.7 Description 4.7.1 The detection limits of 2,4-TDI and 2,6-TDI in this method are both 0.003 μg/mL, and the lower limit of quantification is 0.01 μg/mL. From 0.01 μg/mL to 5.00 μg/mL; the lowest detectable concentration is 0.0008 mg/m3 based on the collection of 15 L air sample. The lowest quantitative concentration is 0.0027 mg/m 3. The relative standard deviation is 1.22% to 4.10%. 4.7.2 This method has a high collection efficiency (>90%) for vapor state and particle size < 2 μm aerosol state TDI. In this case, it can be sampled for a long time. 1 h ~ 4 h; for particle size > 2 μm aerosol TDI in some cases, the collection efficiency is low, such as particle size > 10 μm TDI aerosol and impregnation The filter paper is trapped after impact, and the TDI wrapped in it may not fully react with 1-2PP, due to falling off or in the air during long sampling. Other substances are lost due to reaction. In this case, the sampling time for long-term sampling should be ≤1 h. If you cannot judge the existence status of TDI, long time The sampling time of the sample should also be ≤1 h. 4.7.3 The adsorption capacity of the impregnated glass fiber filter paper used in this method is 45 μg TDI. If the TDI adsorbed on the membrane exceeds this limit, it can pass. The sampling time is adjusted to reduce the amount of adsorption. 4.7.4 The elution efficiency of this method is greater than 90%. Different batches of impregnated glass fiber filter paper should be tested for their elution efficiency. 4.7.5 The standard curve in 4.5.2 of this method can also be prepared by chromatographically pure TDI-urea derivatives. The basic information of TDI-urea derivatives is shown in Table 2. TDI-urea derivatives have two characteristic absorption peaks in the ultraviolet spectrum. 254 nm and 313 nm, when 254 nm is used as the measurement wavelength. When interfering, you can choose 313 nm. Table 2 Basic information of TDI-urea derivatives Chemical material Chemical Abstracts (CAS number) Molecular formula Relative molecular mass Conversion factor (TDI/T DI-urea derivative) 2,4-TDI-urea derivative (2,4-Bis(4-(2-pyridyl)-1 -piperazinylcarbamyl) toluene) 72375-21-4 C27H32N8O2 500.61 0.3479 2,6-TDI-urea derivative (2,6-Bis(4-(2-pyridyl)-1 -piperazinylcarbamyl) toluene) ......

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