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GBZT300.116-2018 English PDF

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GBZT300.116-2018: Determination of toxic substances in workplace air -- Part 116: P-toluene sulfonic acid
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PDF similar to GBZT300.116-2018


Standard similar to GBZT300.116-2018

GBZ 20   GBZ 57   GBZ 49   GBZ/T 300.114   GBZ/T 300.115   GBZ/T 300.112   

Basic data

Standard ID GBZ/T 300.116-2018 (GBZ/T300.116-2018)
Description (Translated English) Determination of toxic substances in workplace air -- Part 116: P-toluene sulfonic acid
Sector / Industry National Standard (Recommended)
Classification of Chinese Standard C60
Word Count Estimation 7,765
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 300.116-2018: Determination of toxic substances in workplace air -- Part 116: P-toluene sulfonic acid


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Determination of toxic substances in workplace air - Part 116. p-Toluenesulfonic acid ICS 13.100 C 52 National Occupational Health Standards Determination of toxic substances in workplace air Part 116. p-toluenesulfonic acid Determination of toxic substances in workplace air- Part 116. p-Toluenesulfonic acid 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 116th 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. Sichuan Provincial Center for Disease Control and Prevention, Shandong Institute of Occupational Health and Occupational Disease Prevention, Sichuan University Huaxi Fourth Hospital, Chengdu Municipal Center for Disease Control and Prevention. The main drafters of this section. Du Hongfeng, You Vana, Hu Bin, Shen Yuehua, Wang Xiaoyun, Bie Mingjiang, Yu Huiju, Song Liqun, Wang Yongwei, Sorghum. Determination of toxic substances in workplace air Part 116. p-toluenesulfonic acid

1 Scope

This part of GBZ /T 300 specifies solvent elution-high performance liquid chromatography for the determination of p-toluenesulfonic acid in the workplace air. This section applies to the detection of the concentration of p-toluenesulfonic acid in the aerosol state and vapor state 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. GBZ 159 Sampling specification for monitoring of hazardous substances in the workplace air GBZ /T 210.4 Guide to the development of occupational health standards - Part 4. Methods for the determination of chemical substances in the workplace air Basic information on 3 p-toluenesulfonic acid See Table 1 for basic information on p-toluenesulfonic acid. Table 1 Basic information of p-toluenesulfonic acid Chemical material Chemical Abstracts (CAS number) Molecular formula relative molecular mass p-Toluenesulfonic acid (p-Toluene sulfonic acid) 104-15-4 CH3C6H4SO3H 172.2 Solvent elution of 4-p-toluenesulfonic acid-high performance liquid chromatography 4.1 Principle The aerosol state and vapor state of p-toluenesulfonic acid in air are collected by impregnated ultrafine glass fiber filter paper, eluted with isopropanol solution, and then passed through C18. Liquid chromatography column separation, UV detector detection, qualitative retention time, peak height or peak area quantification. 4.2 Instrument 4.2.1 Impregnated filter paper. The ultrafine glass fiber filter paper is immersed in the immersion liquid (4.3.2) for 10 min, taken out and drained, and baked at 60 ° C ~ 80 ° C Dry, sealed and stored. 4.2.2 Large sampling clamp, the filter material diameter is 37mm or 40mm. 4.2.3 Small sampling clamp, the filter material diameter is 25mm. 4.2.4 Air sampler, flow rate range is 0L/min ~ 2L/min and 0L/min ~ 5L/min. 4.2.5 Solvent desorption bottle, 10 mL. 4.2.6 Needle filter, organic phase, 0.45 μm. 4.2.7 High performance liquid chromatograph with UV detector or diode array detector, measuring wavelength 222nm; instrument operation reference conditions. a) Column. 250mm × 4.6mm × 5μm, C18; b) Column temperature. 30 ° C; c) mobile phase. acetonitrile. tetrabutylammonium hydrogen sulfate solution (4.3.6) = 20.80 (volume ratio); d) Mobile phase flow. 1.0 mL/min. 4.3 Reagents 4.3.1 The experimental water is ultrapure water, and the reagents are analytically pure except those indicated. 4.3.2 Impregnation solution. 0.8 g of sodium hydroxide is dissolved in water, 1 mL of glycerol is added, and water is added to 100 mL. 4.3.3 Desorbent, 2% (volume fraction) isopropanol (premium pure) solution. 4.3.4 Ammonia solution, 0.5 mol/L. 4.3.5 Acetonitrile, chromatographically pure. 4.3.6 tetrabutylammonium hydrogen sulfate solution, 0.005mol/L. 1.70g of tetrabutylammonium hydrogen sulfate dissolved in about 900mL of water, adjusted with ammonia solution After the pH is about 4.5 (indicated by the acidity meter), dilute to 1000 mL. 4.3.7 Standard solution. accurately weigh a certain amount of p-toluenesulfonic acid, dissolve it in the desorption solution, quantitatively transfer it into a volumetric flask, and make up the volume. It is a standard stock solution. Dilute to 1000.0 μg/mL p-toluenesulfonic acid standard solution with desorbent and store at room temperature for 2 months. Or use the country to recognize Formulated in a 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, a large sampling clamp containing impregnated filter paper was used to collect a 15 minute air sample at a flow rate of 2.0 L/min. 4.4.3 Long-term sampling. At the sampling point, use a small sampling clamp with impregnated filter paper to collect air samples from 2h to 8h at a flow rate of 1.0L/min. 4.4.4 After sampling, open the sampling clamp, take out the immersion filter paper, fold the dust face inward, put it into the solvent desorption bottle, and put it in the clean container. Lose and save. The sample can be stored for 7 days at room temperature. 4.4.5 Sample blank. At the sampling point, open the sampling clamp with the impregnated filter paper, immediately remove the impregnated filter paper and put it into the solvent desorption bottle. It is then transported, stored and measured with the sample. Not less than 2 sample blanks per batch. 4.5 Analysis steps 4.5.1 Sample treatment. Add 5.0 mL of desorbed solution to the solvent desorption bottle containing the impregnated filter paper, and ultrasonically elute for 10 min. Sample solution The needle filter is filtered for measurement. 4.5.2 Preparation of standard curve. Take 4 to 7 volumetric flasks and dilute the standard solution with desorbent solution to a concentration of 0.0μg/mL to 1000.0μg/mL. Range of p-toluenesulfonic acid standard series; adjust the HPLC to the best measurement state according to the operating conditions of the instrument, and inject the sample 10.0 μL, respectively, to determine the peak height or peak area of each concentration of the standard series. Measure the peak height or peak area to the corresponding concentration of p-toluenesulfonic acid (μg/mL) Draw a standard curve or calculate a regression equation with a correlation coefficient of ≥0.999. 4.5.3 Sample determination. The peak height or peak area value measured by measuring the sample solution and the sample blank solution using the operating conditions of the standard series. The concentration (μg/mL) of p-toluenesulfonic acid in the sample solution was obtained from a standard curve or a regression equation. If the concentration of p-toluenesulfonic acid in the sample solution exceeds the test The range is determined by diluting with a desorbent and multiplied 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 p-toluenesulfonic acid in air according to formula (1). C  ...(1) In the formula. C - the concentration of p-toluenesulfonic acid in air, in milligrams per cubic meter (mg/m3); 5 -- the volume of the sample solution in milliliters (mL); C0 -- measured concentration of p-toluenesulfonic acid in the sample solution (minus sample blank) in micrograms per milliliter (μg/mL); V0 - the standard sampling volume in liters (L). 4.6.3 The time-weighted average contact concentration (CTWA) in air is calculated in accordance with the provisions of GBZ 159. 4.7 Description 4.7.1 This method is developed in accordance with the methods and requirements of GBZ /T 210.4. The detection limit of this method is 1.0μg/mL, and the lower limit of quantification is 3.3. Gg/mL, the quantitative determination range is from 3.3μg/mL to 1000μg/mL; the minimum detection concentration is 0.2mg/m3 based on the collection of 30L air sample. The minimum quantitative concentration is 0.6mg/m3; the relative standard deviation is 1.7%~4.0%, the standard recovery is 94.7%~99.4%, and the sampling efficiency is 92.9%~ 98.9%, average elution efficiency > 96%. 4.7.2 If only the aerosol state p-toluenesulfonic acid is present at the sampling site, it can be collected on ultra-fine glass fiber filter paper. 4.7.3 Tetrabutylammonium hydrogen sulfate in the mobile phase of this method is an ion pair reagent. The mobile phase ratio and flow rate should be adapted to the instrument and column used. When adjusted to achieve proper retention time and good separation. 4.7.4 When there are more coexisting sites in the field, the sample may be separated by gradient elution. Common benzenesulfonic acids in workplace air and Phenylsulfonate (such as p-aminobenzenesulfonic acid, m-aminobenzenesulfonic acid, anthranilic acid, benzenesulfonic acid, p-toluenesulfinic acid, m-nitrobenzene) Sulfonic acid, 2,4-dinitrobenzenesulfonic acid, methyl p-toluenesulfonate and ethyl p-toluenesulfonate, etc., can be separated by gradient elution without affecting the para Determination of benzenesulfonic acid. See Table 2 for the reference gradient procedure. Table 2 Mobile phase gradient program time Min Tetrabutylammonium hydrogen sulfate solution Acetonitrile 0 to 4 79 21 4~22 70 30 22~27 10 90 30~40 79 21 4.7.5 Refer to Figure 1 for the reference chromatographic separation of this method. Description. 1--p-aminobenzenesulfonic acid; 2--m-aminobenzenesulfonic acid; 3--o-aminobenzenesulfonic acid; 4--benzenesulfonic acid; 5--p-toluenesulfinic acid; 6--p-toluenesulfonic acid; 7--m-nitrobenzenesulfonic acid; 8--2,4-dinitrobenzenesulfonic acid; 9--p-toluenesulfonic acid methyl ester; Ethyl 10--p-toluenesulfonate. Figure 1 Reference chromatogram

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