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GBZT300.62-2017: Determination of toxic substances in workplace air -- Part 62: Solvent gasoline, liquified petroleum gas, raffinate and turpentine
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Determination of toxic substances in workplace air -- Part 62: Solvent gasoline, liquified petroleum gas, raffinate and turpentine
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GBZ/T 300.62-2017
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Basic data | Standard ID | GBZ/T 300.62-2017 (GBZ/T300.62-2017) | | Description (Translated English) | Determination of toxic substances in workplace air -- Part 62: Solvent gasoline, liquified petroleum gas, raffinate and turpentine | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | C52 | | Word Count Estimation | 10,125 | | Date of Issue | 2017-11-09 | | Date of Implementation | 2018-05-01 | | Older Standard (superseded by this standard) | GBZ/T 160.40-2004 | | Regulation (derived from) | State-Health-Communication (2017) 24 | | Issuing agency(ies) | National Health and Family Planning Commission | GBZ/T 300.62-2017: Determination of toxic substances in workplace air -- Part 62: Solvent gasoline, liquified petroleum gas, raffinate and turpentine
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GBZ /T 300.62-2017
Determination of toxic substances in workplace air - Part 62.Solvent gasoline, liquified petroleum gas, raffinate and turpentine
ICS 13.100
C 52
National Occupational Health Standards of the People's Republic of China
Replace GBZ /T 160.40-2004
Determination of Toxic Substances in Workplace Air
Part 62.Solvent gasoline, liquefied petroleum gas, raffinate
Oil and turpentine
Determination of toxic substances in workplace air-
Part 62.Solvent gasoline, liquified petroleum gas, raffinate and
turpentine
2017-11-09 released.2018-05-01 implemented
Determination of Toxic Substances in Workplace Air
Part 62.Solvent gasoline, liquefied petroleum gas, raffinate oil and turpentine
1 Scope
This part of GBZ /T 300 specifies the direct injection of liquefied petroleum gas in the air of the workplace-gas chromatography, solvent gasoline and raffinate oil
Thermal desorption-gas chromatography of turpentine, solvent desorption-gas chromatography of turpentine.
This section applies to the detection of the concentration of vaporous liquefied petroleum gas, solvent gasoline, raffinate oil and turpentine in the air of the workplace.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this document.
For undated reference documents, the latest version (including all amendments) is applicable to this document.
GBZ 159 Sampling Specification for Monitoring of Hazardous Substances in the Air of Workplaces
GBZ /T 210.4 Guidelines for the Establishment of Occupational Hygiene Standards Part 4.Determination Methods of Chemical Substances in the Air of Workplaces
3 Basic information of liquefied petroleum gas, solvent gasoline, raffinate oil and turpentine
The basic information of liquefied petroleum gas, solvent gasoline, raffinate oil and turpentine is shown in Table 1
4 Thermal desorption of solvent gasoline-gas chromatography
4.1 Principle
The vaporous solvent gasoline in the air is collected with activated carbon, injected after thermal desorption, separated by a gas chromatographic column, and detected by a hydrogen flame ionization detector.
Measured by retention time qualitatively, peak height or peak area quantified.
4.2 Apparatus
4.2.1 Activated carbon tube, thermal desorption type, with 100 mg activated carbon inside.
4.2.2 Air sampler, the flow range is 0 mL/min～500 mL/min.
4.2.3 Airtight syringes, 1 mL and 100 mL.
4.2.4 Thermal desorber.
4.2.5 Gas chromatograph with hydrogen flame ionization detector.
4.2.5.1 Reference conditions for operation of packed column instrument.
a) Chromatographic column. 2 m×4 mm, with 28 g 80 mesh ~ 100 mesh glass microspheres, 3 g 100 mesh ~ 140 mesh glass microspheres and 2.5
g Tetrakis (2-cyanoethoxymethyl) methane. 202 red support = 25.100;
b) Column temperature. 110℃;
c) The temperature of the gasification chamber. 150℃;
d) Testing room temperature. 150℃;
e) Carrier gas (nitrogen) flow rate. 46 mL/min.
4.2.5.2 Reference conditions for capillary column instrument operation.
a) Chromatographic column. 30 m×0.53 mm×1.20 m, PEG 20M;
b) Column temperature. 110℃;
c) The temperature of the gasification chamber. 150℃;
d) Testing room temperature. 150℃;
e) Carrier gas (nitrogen) flow rate. 6 mL/min.
4.3 Reagents
4.3.1 Tetrakis (2-cyanoethoxymethyl) methane, chromatographic stationary liquid.
4.3.2 202 red carrier. 60 mesh to 80 mesh.
4.3.3 Glass microspheres, 80 mesh to 100 mesh and 100 mesh to 140 mesh.
4.3.4 n-hexane, at 20℃, the mass of 1 L liquid is 0.6603 mg.
4.3.5 Standard gas. before use, use a micro syringe to accurately extract a certain amount of n-hexane and inject it into a 100 mL airtight glass syringe.
Dilute it to 100.0 mL with clean air, prepare a standard gas, and calculate its concentration.
4.4 Collection, transportation and storage of samples
4.4.1 On-site sampling shall be carried out in accordance with GBZ 159.
4.4.2 Short-term sampling. At the sampling point, use an activated carbon tube to collect air samples for 15 minutes at a flow rate of 100 mL/min.
4.4.3 Long-term sampling. At the sampling point, use an activated carbon tube to collect air samples for 2 h to 8 h at a flow rate of 50 mL/min.
4.4.4 After sampling, immediately seal both ends of the activated carbon tube and place it in a clean container for transportation and storage. The sample can be stored for 7 days at room temperature.
4.4.5 Sample blank. At the sampling point, open both ends of the activated carbon tube and close it immediately, and then transport, store and measure the same product together.
There are no less than 2 blank samples for each batch of samples.
4.5 Analysis steps
4.5.1 Sample processing. Put the sampled activated carbon tube into the thermal desorber, and connect its inlet end to a 100 mL airtight syringe, and the other
The end is connected to the carrier gas (nitrogen), the flow rate is 50 mL/min, and it is desorbed to 100.0 mL at 230°C. Sample gas supply for measurement.
4.5.2 Preparation of the standard curve. Take 4~7 100mL airtight glass syringes and dilute the standard gas with clean air to 0.0 g/mL~
10.0 g/mL concentration range of solvent gasoline standard series. According to the operating conditions of the instrument, adjust the gas chromatograph to the best measurement state,
Inject 1.0 mL, and measure the peak height or peak area of each concentration of the standard series. Concentrate the corresponding solvent gasoline with the measured peak height or peak area
Degree (g/mL) draw a standard curve or calculate a regression equation, the correlation coefficient should be ≥0.999.
4.5.3 Sample measurement. use the operating conditions of the standard series to determine the sample gas and sample blank gas, and the measured peak height or peak area value is determined by the standard
The standard curve or regression equation is used to obtain the concentration of solvent gasoline in the sample gas (g/mL). If the concentration of solvent gasoline in the sample gas exceeds the measurement range,
Measure after being diluted by clean air, and multiply by the dilution factor when calculating.
4.6 Calculation
4.6.1 Convert the sampling volume to the standard sampling volume according to the method and requirements of GBZ 159.
4.6.2 Calculate the concentration of solvent gasoline in the air according to formula (1).
DV
C (1)
Where.
C-The concentration of solvent gasoline in the air, in milligrams per cubic meter (mg/m3);
C0-Measure the concentration of solvent gasoline in the sample gas (minus the sample blank), the unit is micrograms per milliliter (g/mL);
V0-standard sampling volume, the unit is liter (L);
D --Desorption efficiency, %;
100--The volume of the sample gas, in milliliters (mL).
4.6.3 The time-weighted average exposure concentration (CTWA) in the air is calculated according to GBZ 159.
4.7 Description
4.7.1 This law is developed in accordance with the methods and requirements of GBZ /T 210.4.The detection limit of this method is 0.002 g/mL, and the lower limit of quantification is 0.007
g/mL, the quantitative determination range is 0.007 g/mL～1 g/mL; based on the collection of 1.5 L air samples, the lowest detected concentration is 0.13 mg/m3,
The lowest quantitative concentration is 0.44 mg/m3; the average relative standard deviation is about 4%, the penetration capacity (100 mg activated carbon) is 14 mg, and the average
The desorption efficiency is 96.5% (solvent gasoline with low boiling point). The desorption efficiency of each batch of activated carbon tubes should be determined.
4.7.2 The main components of solvent gasoline are C4-C12 aliphatic hydrocarbons and alicyclic hydrocarbons. This method is suitable for solvent gasoline with a boiling point of 60℃～70℃.
The chromatographic peak is the same as that of n-hexane. Solvent gasoline with a higher boiling point has lower desorption efficiency and is unstable, so this method is not suitable for determination.
4.7.3 This method can also be determined by other equivalent gas chromatographic columns.
5 Direct injection of liquefied petroleum gas-gas chromatography
5.1 Principle
The vaporous liquefied petroleum gas in the air is collected by a gas bag, directly injected, separated by a gas chromatographic column, and detected by a hydrogen flame ionization detector.
Qualitatively by retention time, and quantified by peak height or peak area.
5.2 Apparatus
5.2.1 Gas bag, the volume is 1L～10L.
5.2.2 Air sampler, the flow range is 0 mL/min～500mL/min, or double ball.
5.2.3 Airtight syringes, 1 mL and 100 mL.
5.2.4 Gas chromatograph with hydrogen flame ionization detector. Reference conditions for instrument operation.
a) Chromatographic column. 2 m×4 mm, glass microspheres;
b) Column temperature. 70℃;
c) The temperature of the gasification chamber. 150℃;
d) Testing room temperature. 150℃;
e) Carrier gas (nitrogen) flow rate. 40 mL/min.
5.3 Reagents
5.3.1 Glass microspheres, 80 mesh to 100 mesh.
5.3.2 For n-pentane, the mass of 1 μL of gas at 20°C is 0.6253 mg.
5.3.3 Standard gas. before use, use a micro syringe to accurately extract a certain amount of n-pentane and inject it into a 100 mL airtight glass syringe.
Dilute it to 100.0 mL with clean air and prepare it as a standard gas.
5.4 Collection, transportation and storage of samples
5.4.1 On-site sampling shall be performed in accordance with GBZ 159.
5.4.2 Sample collection. At the sampling point, after cleaning the air bag 3 to 5 times with an air sample, collect an air sample. After sampling, immediately seal
Close the intake valve of the gas bag and place it in a clean container for transportation and storage. The sample should be measured within 24 hours.
5.4.3 Sample blank. Bring the air bag to the workplace, and after collecting clean air, the same product should be transported, stored and measured together. Each batch
The sample is not less than 2 sample blanks.
5.5 Analysis steps
5.5.1 Sample processing. Put the sampled gas bag in the laboratory of the measurement standard series for measurement.
5.5.2 Preparation of the standard curve. Take 4~7 100mL airtight glass syringes and dilute the standard gas with clean air to 0.0 μg/mL~
The standard series of liquefied petroleum gas in the concentration range of 1.0 μg/mL. According to the operating conditions of the instrument, adjust the gas chromatograph to the best measurement state,
Inject 1.0 mL, and measure the peak height or peak area of each concentration of the standard series. Use the measured peak height or peak area to compare the corresponding liquefied petroleum gas
Draw a standard curve or calculate a regression equation for the concentration (μg/mL), and the correlation coefficient should be ≥0.999.
5.5.3 Sample measurement. Use the operating conditions of the standard series to determine the sample gas and sample blank gas, and the measured peak height or peak area value is determined by the standard
The quasi-curve or regression equation obtains the concentration of liquefied petroleum gas in the sample gas (μg/mL). If the concentration of liquefied petroleum gas in the sample gas exceeds the measurement range,
Measure after dilution with clean air, and multiply by the dilution factor when calculating.
5.6 Calculation
5.6.1 Calculate the concentration of liquefied petroleum gas in the air according to formula (2).
10000 CC (2)
Where.
C--The concentration of liquefied petroleum gas in the air, in milligrams per cubic meter (mg/m3);
C0--The measured concentration of liquefied petroleum gas in the sample gas (minus the sample blank), in micrograms per milliliter (g/mL).
5.6.2 The time-weighted average exposure concentration (CTWA) in the air is calculated according to GBZ 159.
5.7 Description
5.7.1 This law is developed in accordance with the methods and requirements of GBZ /T 210.4.The lowest detectable concentration of this method is 2.4 mg/m3, and the lowest quantitative concentration
The concentration is 8 mg/m3, the quantitative determination range is 8 mg/m3～1000 mg/m3, and the relative standard deviation is 1.2%～6.3%.
5.7.2 Liquefied petroleum gas is a mixture of alkanes and olefins. Under the chromatographic conditions of this method, a chromatographic peak of liquefied petroleum gas will be retained.
The time and response value are the same as those of n-pentane.
5.7.3 Aromatic hydrocarbons, alcohols, esters, ketones, etc. that may coexist in the air of the workplace do not interfere with the determination.
5.7.4 This method can also be determined by other equivalent gas chromatography columns.
5.7.5 This method can also be used for sampling with a 100 mL syringe.
6 Thermal desorption of raffinate oil-gas chromatography
6.1 Principle
The vaporized raffinate oil in the air is collected with activated carbon, injected after thermal desorption, separated by a gas chromatographic column, and detected by a hydrogen flame ionization detector.
Qualitatively by retention time, and quantified by peak height or peak area.
6.2 Apparatus
6.2.1 Activated carbon tube, thermal desorption type, with 100 mg activated carbon inside.
6.2.2 Air sampler, the flow range is 0 mL/min～500 mL/min.
6.2.3 Syringe, 1 mL, 100 mL.
6.2.4 Thermal desorber.
6.2.5 Micro sampler, 10 µL.
6.2.6 Gas chromatograph with hydrogen flame ionization detector. Reference conditions for instrument operation.
a) Chromatographic column. 1.5 m×4 mm, polyethylene glycol 6000.6201 red support=10.100;
b) Column temperature. 120℃;
c) The temperature of the gasification chamber. 150℃;
d) Testing room temperature. 150℃;
e) Carrier gas (nitrogen) flow rate. 40 mL/min.
6.3 Reagents
6.3.1 Polyethylene glycol 6000, chromatographic stationary phase.
6.3.2 6201 red support, 60 mesh to 80 mesh.
6.3.3 For n-hexane, the mass of 1.0 µL of liquid at 20°C is 0.6603 mg. Chromatographic identification of no interference peaks.
6.3.4 Standard gas. Before use, use a micro syringe to measure a certain amount of n-hexane and inject it into a 100 mL airtight glass syringe.
The clean air is diluted to 100.0 mL, which is the standard gas. Or use nationally recognized standard gas to prepare.
6.4 Collection, transportation and storage of samples
6.4.1 On-site sampling shall be carried out in accordance with GBZ 159.
6.4.2 Short-term sampling. At the sampling point, use an activated carbon tube to collect air samples for 15 minutes at a flow rate of.200 mL/min.
6.4.3 Long-term sampling. At the sampling point, use an activated carbon tube to collect air samples for 2 h to 8 h at a flow rate of 50 mL/min.
6.4.4 After sampling, immediately seal both ends of the activated carbon tube and place it in a clean container for transportation and storage. The sample can be stored in the refrigerator for 7 days.
6.4.5 Sample blank. At the sampling point, open both ends of the activated carbon tube and close it immediately, and then transport, store and measure the same product together.
There are no less than 2 blank samples for each batch of samples.
6.5 Analysis steps
6.5.1 Sample processing. Put the sampled activated carbon tube into the thermal desorber, connect one end of the air inlet to a 100 mL syringe, and the other end
Connected to carrier gas (nitrogen), with a flow rate of 30 mL/min, desorb to 100.0 mL at 300°C. Sample gas supply for measurement.
6.5.2 Preparation of the standard curve. Take 4 to 7 100 mL airtight glass syringes and dilute the standard gas with clean air to 0.0 g/mL～
The standard series of raffinate oil in the concentration range of 0.70 g/mL. Refer to the operating conditions of the instrument, adjust the gas chromatograph to the best measurement state, and then
Sample 1.0 mL, and measure the peak height or peak area of each concentration of the standard series. Use the measured peak height or peak area to compare the corresponding raffinate concentration
(Μg/mL) Draw a standard curve or calculate a regression equation, and the correlation coefficient should be ≥0.999.
6.5.3 Sample measurement. Use the operating conditions of the standard series to determine the sample gas and sample blank gas, and the measured peak height or peak area value is determined by the standard
The standard curve or regression equation is used to obtain the concentration of raffinate oil in the sample gas (µg/mL). If the concentration of the raffinate oil in the sample gas exceeds the measurement range, use a clean
Measure after air dilution, and multiply by the dilution factor when calculating.
6.6 Calculation
6.6.1 Convert the sampling volume to the standard sampling volume according to the method and requirements of GBZ 159.
6.6.2 Calculate the concentration of raffinate oil in the air according to formula (3).
C...(3)
Where.
C-the concentration of the raffinate oil in the air, in milligrams per cubic meter (mg/m3);
C0-the measured concentration of the raffinate in the sample gas (minus the sample blank), the unit is micrograms per milliliter (g/mL);
V0-standard sampling volume, the unit is liter (L);
100--The volume of the sample gas, in milliliters (mL).
6.6.3 The time-weighted average exposure concentration (CTWA) in the air is calculated according to GBZ 159.
6.7 Description
6.7.1 This law is developed in accordance with the methods and requirements of GBZ /T 210.4.The detection limit of this method is 0.006 µg/mL, and the lower limit of quantification is 0.02
µg/mL, the quantitative determination range is 0.02 µg/mL～0.7 µg/mL; based on the collection of 3 L air samples, the lowest detectable concentration is 0.2 mg/m3,
The minimum quantitative concentration is 0.7 mg/m3; the relative standard deviation is 1.9% to 4.4%, the sampling efficiency is 100%, and the desorption efficiency is 94.6% to 98.4%.
The desorption efficiency of each batch of activated carbon tubes should be determined.
6.7.2 The raffinate is a mixture of alkanes and alkenes with a boiling point of 60℃～150℃.
Keep a peak meter with consistent time.
6.7.3 This method can also be determined by other equivalent gas chromatographic columns.
6.7.4 Benzene, toluene, xylene, etc. that may coexist on site do not interfere with the determination of this method.
7 Solvent desorption of turpentine-gas chromatography
7.1 Principle
The vaporous turpentine in the air is collected with activated carbon, carbon disulfide is desorbed and then injected, separated by a gas chromatographic column, and detected by hydrogen flame ionization
It can be qualitatively determined by retention time, peak height or peak area is quantified.
7.2 Apparatus
7.2.1 Activated carbon tube, solvent desorption type, 100 mg/50 mg activated carbon.
7.2.2 Air sampler, the flow range is 0 mL/min～500 mL/min.
7.2.3 Solvent desorption bottle, 5 mL.
7.2.4 Micro syringe.
7.2.5 Gas chromatograph with hydrogen flame ionization detector, reference conditions for instrument operation.
a) Chromatographic column. 30 m×0.32 mm×0.5 m, FFAP;
b) Column temperature. 60℃;
c) The temperature of the gasification chamber. 140℃;
d) Testing room temperature. 180℃;
e) Carrier gas (nitrogen) flow rate. 1 mL/min;
f) Split ratio. 10.1.
7.3 Reagents
7.3.1 Carbon disulfide, chromatographic identification without interference peaks.
7.3.2 Standard solution. add carbon disulfide to the volumetric flask, add a certain amount of turpentine after accurate weighing, and then accurately weigh it with disulfide
Chemical carbon constant volume. Calculate the concentration of the solution from the difference between the two weighings, which is the turpentine standard stock solution. Before use, dilute to 1000.0 with carbon disulfide
g/mL standard solution. Or use a nationally recognized standard solution to prepare.
7.4 Collection, transportation and storage of samples
7.4.1 On-site sampling shall be carried out in accordance with GBZ 159.
7.4.2 Short-time sampling. At the sampling point, use an activated carbon tube to collect air samples for 15 minutes at a flow rate of 100 mL/min.
7.4.3 Long-term sampling. At the sampling point, use an activated carbon tube to collect air samples for 2 h to 8 h at a flow rate of 50 mL/min.
7.4.4 After sampling, immediately seal both ends of the activated carbon tube and place it in a clean container for transportation and storage. The sample can be stored for 8 days at room temperature.
7.4.5 Sample blank. At the sampling point, open both ends of the activated carbon tube and close it immediately, and then transport, store and measure the same product together.
There are no less than 2 blank samples for each batch of samples.
7.5 Analysis steps
7.5.1 Sample processing. Pour the sampled active carbon before and after the sample into two solvent desorption bottles, add 1.0 mL carbon disulfide to each, and seal
After closing, desorb for 30 min, shaking from time to time. The sample solution is available for determination.
7.5.2 Preparation of standard curve. take 4 to 7 volumetric flasks, dilute the standard solution with carbon disulfide to 0.0 g/mL～500.0 g/mL
Turpentine standard series of concentration range. Refer to the operating conditions of the instrument, adjust the gas chromatograph to the best measurement state, and inject 1.0 L,
Determine the peak height or peak area of each concentration of the standard series. Use the measured peak height or peak area to plot the corresponding turpentine concentration (g/mL)
For quasi-curve or calculated regression equation, the correlation coefficient should be ≥0.999.
7.5.3 Sample measurement. use the operating conditions of the standard series to determine the sample solution and sample blank solution, and the measured peak height or peak area value
The concentration of turpentine in the sample solution (g/mL) is obtained from the standard curve or regression equation. If the concentration of turpentine in the sample solution exceeds the measurement range,
Measure after diluting with carbon disulfide, and multiply by the dilution factor when calculating.
7.6 Calculation
7.6.1 Convert the sampling volume to the standard sampling volume according to the method and requirements of GBZ 159.
7.6.2 Calculate the concentration of turpentine in the air according to formula (4).
DV
vcc
21)(...(4)
Where.
C-Concentration of turpentine in the air, in milligrams per cubic meter (mg/m3);
c1, c2-the measured concentration of turpentine in the sample solution before and after (minus the sample blank), the unit is micrograms per milliliter (g/mL);
v --The volume of the sample solution, in milliliters (mL);
V0-standard sampling volume, the unit is liter (L)
D --Desorption efficiency, %.
7.6.3 The time-weighted average exposure concentration (CTWA) in the air is calculated according to GBZ 159.
7.7 Description
7.7.1 This law is developed in accordance with the methods and requirements of GBZ /T 210.4.The detection limit of this method is 7 g/mL, and the lower limit of quantification is 23 g/mL,
The quantitative determination range is 23 g/mL～500 g/mL; based on the collection of 1.5 L air samples, the lowest detectable concentration is 5 mg/m3, and the lowest
The concentration is 16 mg/m3; the relative standard deviation is 2.5%～3.1%, the penetration capacity (100 mg activated carbon) is ≥11 mg, and the average desorption efficiency
It is 100.4%. The desorption efficiency of each batch of activated carbon tubes should be determined.
7.7.2 This method can also be determined by other equivalent gas chromatographic columns.
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