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Determination of toxic substances in workplace air -- Part 100: Furfural and dimethoxymethane
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Basic data Standard ID | GBZ/T 300.100-2018 (GBZ/T300.100-2018) | Description (Translated English) | Determination of toxic substances in workplace air -- Part 100: Furfural and dimethoxymethane | Sector / Industry | National Standard (Recommended) | Classification of Chinese Standard | C60 | Word Count Estimation | 8,834 | Date of Issue | 2018-07-16 | Date of Implementation | 2019-07-01 | Older Standard (superseded by this standard) | GBZ/T 160.54-2007 | Regulation (derived from) | State-Health-Communication (2018) No.13 | Issuing agency(ies) | National Health and Family Planning Commission |
GBZ/T 300.100-2018: Determination of toxic substances in workplace air -- Part 100: Furfural and dimethoxymethane ---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Determination of toxic substances in workplace air - Part 100. Furfural and dimethoxymethane
ICS 13.100
C 52
National Occupational Health Standards
Partially replace GBZ /T 160.54-2007
Determination of toxic substances in workplace air
Part 100. Furfural and dimethoxymethane
Determination of toxic substances in workplace air-
Part 100. Furfural and dimethoxymethane
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 100th 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 part is divided into GBZ /T 160.54-2007 "Determination of aliphatic aldehydes in workplace air toxic substances", separately
For this part, instead of the aniline spectrophotometric method of furfural in Chapter 7 of GBZ /160.54-2007, the following major modifications were made.
-- modified the standard name;
- Added solvent desorption-gas chromatography of dimethoxymethane;
- Increase the basic information of the object to be tested;
-- Improved air sampling and expression of standard series concentrations;
-- Added sample blank requirements and method performance indicators.
The main drafting unit and main drafters in this section.
-- Solution absorption of furfural - aniline spectrophotometry
The main drafting unit. Shaanxi Provincial Center for Disease Control and Prevention.
Main drafters. Lu Qingsheng, Xu Fangli.
Solvent desorption-gas chromatography of dimethoxymethane
Main drafting units. Longgang District Center for Disease Control and Prevention, Shenzhen, Guangdong Province, Guangdong Provincial Occupational Disease Prevention and Treatment Institute, Shenzhen City, Guangdong Province
Prevention and Control Center, Sichuan Provincial Center for Disease Control and Prevention.
Main drafters. Liu Qu, Cai Zhibin, Zhang Ying, Liu Li, Li Shuiming, Wu Banghua, Chen Wei, Du Hongfeng.
The previous versions of the standards replaced by this section are.
--GBZ /T 160.54-2004;
--GBZ /T 160.54-2007 Chapter 7.
Determination of toxic substances in workplace air
Part 100. Furfural and dimethoxymethane
1 Scope
This part of GBZ /T 300 specifies the solution absorption of furfural in the air of workplaces - aniline spectrophotometry and dimethoxymethane
Solvent desorption-gas chromatography.
This section applies to the detection of concentrations of furfural and dimethoxymethane 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
3 Basic information on furfural and dimethoxymethane
The basic information of furfural and dimethoxymethane is shown in Table 1.
Table 1 Basic information of furfural and dimethoxymethane
Chemical material
Chemical Abstracts
(CAS number)
Molecular formula relative molecular mass
Furfural
(α-furfural, Furfural)
98-01-1 C4H3OCHO 96.09
Dimethoxymethane
(Methylal, Dimethoxymethane)
109-87-5 CH2 (OCH3)2 76.10
4 Solution absorption of furfural - aniline spectrophotometry
4.1 Principle
Vapor state in the air and haze furfural are collected in a porous glass plate absorption tube containing oxalic acid-disodium hydrogen phosphate solution, in the presence of acetic acid,
The red color was generated by the action of aniline, and the absorbance was measured by a spectrophotometer at a wavelength of 530 nm to carry out quantitative analysis.
4.2 Instrument
4.2.1 Porous glass plate absorber tube.
4.2.2 Air sampler, flow range from 0L/min to 1L/min.
4.2.3 with a colorimetric tube, 10mL.
4.2.4 Spectrophotometer with 1 cm cuvette.
4.3 Reagents
4.3.1 The experimental water is distilled water, and the reagent is analytically pure.
4.3.2 Absorbent solution (oxalic acid-disodium hydrogen phosphate solution). 25 g/L oxalic acid solution and 50 g/L disodium hydrogen phosphate solution are mixed in equal volume.
4.3.3 Color developer. Dilute 15.0 mL of aniline (new distillation) to 100.0 mL with glacial acetic acid.
4.3.4 Sodium chloride.
4.3.5 Standard solution. Add the absorption liquid to the volumetric flask. After weighing accurately, add a certain amount of redissolved furfural, and then weigh accurately.
Absorb the liquid to the scale, calculate the concentration of the solution from the difference between the two weighings, which is the standard stock solution. Dilute to 5.0μg/mL with absorbent before use.
Furfural standard solution. 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 a porous glass plate absorption tube containing 10.0 mL of absorption liquid, and collect at a flow rate of 500 mL/min for ≥15 min.
Air sample. Immediately after sampling, the inlet and outlet of the absorption tube are closed and transported and stored in a clean container. The sample should be measured within 24 hours.
4.4.3 Sample blank. At the sampling point, open the inlet and outlet of the absorption tube of the porous glass plate containing 10.0 mL of absorption liquid, and immediately close it.
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. After washing the inner wall of the inlet pipe 3 times with the sample solution in the absorption tube, take 1.0 mL of the sample solution in a plug colorimetric tube.
Add the absorption solution to 5.0 mL for measurement.
4.5.2 Preparation of the standard curve. Take 5 to 8 plug colorimetric tubes, add 0.0mL to 1.0mL standard solution, add the absorption solution to
5.0 mL, formulated into a standard series of furfural in the concentration range of 0.0 μg/mL ~ 1.0 μg/mL. Add 0.3g of sodium chloride to each standard series of tubes and
5.0 mL of the color developing agent, shaken, placed in the dark at 20 ° C for 5 min, and filtered. Using a spectrophotometer at 530 nm, the standard is determined separately.
The absorbance values of the filtrates of each series of the series. Draw a standard curve or calculate the regression for the corresponding furfural concentration (μg/mL) with the measured absorbance value
Cheng, its correlation coefficient should be ≥0.999.
4.5.3 Sample determination. The sample solution and the sample blank solution are determined by the operating conditions of the measurement standard series, and the measured absorbance value is determined by the standard.
The curve or regression equation gives the concentration of furfural (μg/mL) in the sample solution. If the concentration of furfural in the sample solution exceeds the measurement range, use the absorption solution to dilute
After the release measurement, the calculation is 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 furfural in the air according to formula (1).
C ...(1)
In the formula.
C - the concentration of furfural in air, in milligrams per cubic meter (mg/m3);
C0 -- measured concentration of furfural in the sample solution (minus sample blank) in micrograms per milliliter (μg/mL);
10--The volume of the sample solution in milliliters (mL);
5 -- sample dilution factor;
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 lower limit of quantification of this method is 0.24μg/mL, and the quantitative determination range
0.24μg/mL~5.0μg/mL; the lowest quantitative concentration is 1.6mg/m3 based on the sample of 7.5L air; the relative standard deviation is 1.6%~
6.6%.
4.7.2 The concentration of aniline in the reaction solution has a great influence on the color development, and the dosage should be accurate. The reaction temperature should be strictly controlled at 20 ° C, otherwise the solution is sucked
The luminosity value will decrease.
Solvent desorption of 5 dimethoxymethane-gas chromatography
5.1 Principle
Vapor dimethoxymethane in the air is collected by activated carbon tube, desorbed by hexane, injected, separated by gas chromatography column, hydrogen flame ionization
Detector detection, qualitative for retention time, peak height or peak area quantitation.
5.2 Instruments
5.2.1 Activated carbon tube, solvent desorption type, containing.200mg/100mg activated carbon.
5.2.2 Air sampler, flow rate from 0mL/min to 300mL/min.
5.2.3 Solvent desorption bottle, 5mL.
5.2.4 Microinjector, 1L, 10L.
5.2.5 Gas chromatograph with hydrogen flame ionization detector, instrument operation reference conditions.
a) column. 30m × 0.32mm × 0.5m, bonded polyethylene glycol-2M;
b) column temperature. initial temperature 40 ° C, kept for 5 min, heated to 100 ° C at 10 ° C/min, kept for 1 min;
c) gasification chamber temperature..200 ° C;
d) detection chamber temperature. 250 ° C;
e) carrier gas (nitrogen) flow rate. 1.0mL/min;
f) Split ratio. 20.1.
5.3 Reagents
5.3.1 n-hexane, chromatographic identification of interference-free peaks.
5.3.2 Standard solution. Add n-hexane to the volumetric flask. After weighing accurately, add a certain amount of dimethoxymethane, and then accurately weigh it.
The n-hexane was diluted to the mark; the concentration of the solution was calculated from the difference between the two weighings as a standard stock solution. It can be stored for 1 month in a refrigerator at 4 °C. Pro
Before use, it was diluted with n-hexane to a standard solution of 10000.0 g/mL dimethoxymethane. Or formulated with a nationally recognized standard solution.
5.4 Sample collection, transportation and storage
5.4.1 On-site sampling shall be performed in accordance with GBZ 159.
5.4.2 Short-time sampling. At the sampling point, a 15 min air sample was collected with an activated carbon tube at a flow rate of 100 mL/min.
5.4.3 Long-term sampling. At the sampling point, an air sample of 1 h to 2 h is collected with an activated carbon tube at a flow rate of 20 mL/min.
5.4.4 Immediately after sampling, the ends of the activated carbon tube are closed and transported and stored in a clean container. The sample can be stored for 5d at room temperature, 4°C ice
14d can be stored in the box.
5.4.5 Sample blank. At the sampling point, open both ends of the activated carbon tube and immediately close it, then transport, store and measure with the sample.
Not less than 2 sample blanks per batch.
5.5 Analysis steps
5.5.1 Sample treatment. Pour the front and rear activated carbon into two solvent desorption bottles, add 1.0mL of n-hexane each, after blocking, desorb
30min, shaking from time to time. The sample solution is for measurement.
5.5.2 Preparation of standard curve. Take 4 to 7 volumetric flasks, dilute the standard solution with n-hexane to 0.0g/mL~10000.0g/mL.
A range of dimethoxymethane standards. Adjust the gas chromatograph to the best measurement state according to the operating conditions of the instrument, and inject 1.0 L.
The peak height or peak area of each concentration of the standard series was determined separately. The measured peak height or peak area versus the corresponding dimethoxymethane concentration (g/mL)
Draw a standard curve or calculate a regression equation with a correlation coefficient of ≥0.999.
5.5.3 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 measurement standard series.
The concentration of dimethoxymethane in the sample solution (g/mL) was obtained from a standard curve or a regression equation. If the concentration of the analyte in the sample solution exceeds the determination
The range can be determined by diluting with n-hexane and multiplying by the dilution factor.
5.6 Calculation
5.6.1 Convert the sample volume to the standard sample volume according to the method and requirements of GBZ 159.
5.6.2 Calculate the concentration of dimethoxymethane in air according to formula (2).
DV
Vcc
21 )( (2)
In the formula.
C - the concentration of dimethoxymethane in air, in milligrams per cubic meter (mg/m3);
C1, c2-- measured the concentration of dimethoxymethane in the sample solution before and after (minus the sample blank) in micrograms per milliliter
(μg/mL);
v -- the volume of the sample solution in milliliters (mL);
V0 -- standard sampling volume in liters (L);
D -- desorption efficiency, %.
5.6.3 The time-weighted average contact concentration (CTWA) in air is calculated in accordance with GBZ 159.
5.7 Description
5.7.1 This method is developed in accordance with the methods and requirements of GBZ /T 210.4. The detection limit of this method is 0.7g/mL, and the lower limit of quantification is 2.3.
g/mL, the quantitative measurement range is 2.3g/mL~10000g/mL; the minimum detection concentration is 0.5mg/m3 when collecting 1.5L air sample.
The minimum quantitative concentration is 1.5mg/m3; the relative standard deviation is 1.7%~2.9%, the average sampling efficiency is ≥95.7%, and the breakthrough capacity (200mg)
The activated carbon was 17.8 mg and the average desorption efficiency was 96.5%. The desorption efficiency of each batch of activated carbon tubes should be determined.
5.7.2 The sampling time of this method is determined by the concentration of dimethoxymethane in the air of the workplace. The concentration of the analyte in the air exceeds the allowable concentration.
When the concentration is 1 time, the sampling time is not more than 2 hours for a long time, and the sampling time can be appropriately extended when the concentration is low. Can also use 600mg/200mg activated carbon
Pipe sampling, 600mg activated carbon penetration capacity is greater than 58.5mg, sampling efficiency is 100%, can meet 2h ~ 8h long-term sampling.
5.7.3 This method can also be measured using equivalent other GC columns. Constant temperature measurement or temperature programmed measurement can be selected according to the measurement requirements.
5.7.4 See Figure 1 for the chromatographic separation of this method. Methanol, ethanol, acetone, methyl acetate and cyclohexane which may coexist in the field do not interfere with this
law.
4.0 5.0 6.0 7.0 8.0 min
0.00
0.25
0.50
0.75
1.00
uV(x100,000)
Chromatography
Description.
1-cyclohexane;
2-dimethoxymethane;
3--1,1-dimethoxyethane;
4--acetone;
5--methyl acetate;
6--methanol;
7--1,2-dimethoxyethane;
8--ethanol.
Figure 1 Chromatographic separation reference map
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