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HJ 1010-2018: Specifications and Test Procedures for Ambient Air Quality Continuous Monitoring System with Gas Chromatography for Volatile Organic Compounds
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Specifications and Test Procedures for Ambient Air Quality Continuous Monitoring System with Gas Chromatography for Volatile Organic Compounds
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Basic data | Standard ID | HJ 1010-2018 (HJ1010-2018) | | Description (Translated English) | Specifications and Test Procedures for Ambient Air Quality Continuous Monitoring System with Gas Chromatography for Volatile Organic Compounds | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z15 | | Word Count Estimation | 17,172 | | Date of Issue | 2018-12-29 | | Date of Implementation | 2019-07-01 | | Regulation (derived from) | Ministry of Ecology and Environment Announcement No. 75 of 2018 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 1010-2018: Specifications and Test Procedures for Ambient Air Quality Continuous Monitoring System with Gas Chromatography for Volatile Organic Compounds
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Specifications and Test Procedures for Ambient Air Quality Continuous Monitoring System with Gas Chromatography for Volatile Organic Compounds
National Environmental Protection Standard of the People's Republic
Ambient air volatile organic compounds
Monitoring system technical requirements and testing methods
Specifications and Test Procedures forAmbient Air Quality
Continuous Monitoring System with Gas Chromatography for Volatile
Organic Compounds
Published on.2018-12-29
2019-07-01 Implementation
Department of Ecology and Environment
i directory
Foreword...ii
1 Scope...1
2 Normative references...1
3 Terms and Definitions...1
4 system working principle and composition...1
5 Technical requirements... 2
6 Performance indicators...4
7 Detection method...6
Appendix A (Normative Appendix) Table of 57 Volatile Organic Compounds...11
Appendix B (Normative Appendix) Test Items and Technical Requirements...12
Foreword
To protect the ecological ring for the implementation of the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China
This standard is formulated to ensure human health and to regulate the performance and quality of ambient air volatile organic compounds gas chromatography continuous monitoring system.
This standard specifies the composition, technical requirements, performance indicators and requirements of the ambient air volatile organic compounds gas chromatography continuous monitoring system.
Detection method.
Appendix A to Appendix B of this standard are normative appendices.
This standard is the first release.
This standard is formulated by the Department of Eco-Environmental Monitoring of the Ministry of Ecology and Environment and the Department of Regulations and Standards.
This standard was drafted. Beijing Environmental Protection Monitoring Center, China Environmental Monitoring Center, Peking University, Shanghai Environmental Department
Research Institute, Shanghai Environmental Monitoring Center, Jiangsu Environmental Monitoring Center, Zhejiang Environmental Monitoring Center, Guangzhou Environmental Protection
Science Research Institute, Wuhan Environmental Monitoring Center.
This standard is approved by the Ministry of Ecology and Environment on December 29,.2018.
This standard has been implemented since July 1,.2019.
This standard is explained by the Ministry of Ecology and Environment.
1 Environmental air volatile organic compounds gas chromatography continuous monitoring system technical requirements
And detection method
1 Scope of application
This standard specifies the composition and technical requirements of the continuous monitoring system for volatile organic compounds in ambient air.
Performance indicators and testing methods.
This standard applies to the design, production and inspection of gas chromatography continuous monitoring system for the determination of volatile organic compounds in ambient air.
Measurement.
2 Normative references
This standard refers to the terms of the following documents. For undated references, the valid version applies to this standard.
GB/T 30431 laboratory gas chromatograph
GB/T 33864 mass spectrometer general specification
HJ 212 pollutant online monitoring (monitoring) system data transmission standard
HJ 654 Technical requirements for continuous automatic monitoring system for ambient air gaseous pollutants (SO2, NO2, O3, CO)
Detection method
3 Terms and definitions
3.1 reference state reference state
It refers to the state when the atmospheric temperature is 298.15 K and the atmospheric pressure is 1013.25 hPa.
3.2 valid data rate validated data rate
The percentage of hours that the monitoring data is valid for a period of time as a percentage of the total operating hours.
4 system working principle and composition
4.1 Working principle
Ambient air or standard gas enters the sampling system at a constant flow rate, and the volatile organic compounds are passed through low temperature or traps.
Enrichment, separation by gas chromatography, etc., and detection by hydrogen flame ionization detector (FID) or mass spectrometry
The detector (MSD) was tested to obtain the concentration of each component of the volatile organic compounds.
4.2 System components
The monitoring system consists of a sample collection unit, a quality control unit, a gas source unit, an analysis unit, a data acquisition and transmission unit, and
It consists of other auxiliary equipment.
24.2.1 Sample Collection Unit
The sample collection unit is mainly composed of sampling pipeline, sampling pump and flow control unit for environmental air volatile organic
Continuous automatic sampling of objects. The specific requirements of the sample collection unit are given in 5.4.1.
4.2.2 Quality Control Unit
The quality control unit is mainly composed of zero gas, standard gas and dilution system, and is used for calibration and daily verification of analytical instruments.
The specific requirements of the quality control unit are given in 5.4.2.
4.2.3 Air source unit
The air source unit is mainly composed of a gas source and a pipeline, and is used for providing carrier gas, gas, and combustion gas required for system operation.
See 5.4.3 for specific requirements for the air supply unit.
4.2.4 Analysis unit
The analysis unit is mainly composed of an enrichment module, a column oven, a column, a detector, etc., and is used for collecting ambient air.
The volatile organic components are enriched and separated, and the volatile organic components are quasi-deterministic and quantified. Analysis sheet
See Section 5.4.4 for specific requirements.
4.2.5 Data Acquisition and Transmission Unit
The data acquisition and transmission unit is used to collect, process and store monitoring data, and can transmit monitoring data and instruments according to instructions.
Device working status information. The specific requirements for the data acquisition and transmission unit are given in 5.4.5.
5 Technical requirements
5.1 Appearance requirements
5.1.1 The appearance is neat and tidy, the surface coating and plating layer are not obviously peeled off, scratched, exposed and dirt, and the surface of the parts is free from rust;
5.1.2 should have a product nameplate, which should be marked with the instrument name, model specifications, production unit, factory number, date of manufacture,
Information such as rated voltage and power;
5.1.3 The display of the host panel is clear, and the characters and logos are easy to identify;
5.1.4 All fasteners are not loose, each operation button and button are flexible and function properly;
5.1.5 The detachable part should be dismantled and disassembled.
5.2 Working conditions
The monitoring system should function properly in the following environmental conditions.
Ambient temperature. (20 ~ 30) ° C;
Relative humidity. ≤85%;
Atmospheric pressure. (800 ~ 1060) hPa;
Supply voltage. AC (220 ± 22) V or (380 ± 38) V, (50 ± 1) Hz.
35.3 Safety requirements
5.3.1 Insulation resistance
In the case of ambient temperature (20 ~ 30) ° C, relative humidity ≤ 85%, monitoring the system power terminal to the ground or the chassis
The edge resistance is not less than 20 MΩ.
5.3.2 Insulation strength
The monitoring system is at 1500 V (rms), 50 Hz at an ambient temperature of (20 to 30) ° C and a relative humidity of ≤ 85%.
Under the sine wave test voltage for 1 min, there should be no breakdown or arcing.
5.3.3 Power Requirements
The monitoring system should be equipped with a regulated power supply to ensure that the power supply meets AC (220 ± 22) V or (380 ± 38) V, (50 ± 1)
Hz requirements.
5.3.4 Other requirements
The airtightness of units and pipelines with flammable gases and toxic gases shall meet the requirements of GB/T 30431, ie 0.3 MPa.
Next, the pressure drop of 30 min is not more than 0.01 MPa to ensure that it will not leak.
The high temperature heating zone of the instrument shall be provided with an anti-scald mark.
5.4 Functional requirements
5.4.1 Sample Collection Unit
5.4.1.1 The sample collection unit can adopt the sampling manifold that meets the requirements of HJ 654, or directly adopt the independent requirements.
Pipeline. When using a multi-branch sampling manifold, the sampling branch of volatile organic compounds should be located at the forefront of the sampling manifold. Sampling tube
The route should be as short as possible to reduce the adsorption of the target compound.
5.4.1.2 The materials for the sampling pipelines, valves and connecting parts shall be selected so as not to release interfering substances and not with the target compound.
A chemical reaction material such as polytetrafluoroethylene, borosilicate glass or stainless steel. If you use stainless steel, you need to enter
Inertialization.
5.4.1.3 The sampling pipeline should be equipped with a heating device. The heating temperature is generally controlled at (30 ° C ~ 50 ° C) to avoid the inner wall of the sampling pipeline.
Condensation.
5.4.1.4 A PTFE membrane with a pore size of ≤ 5 μm should be installed to remove particulate matter from the air.
5.4.1.5 Sampling shall be carried out at a steady flow rate, and the cumulative sampling time per hour shall be not less than 30 min.
5.4.2 Quality Control Unit
The quality control unit of the monitoring system is used for periodic verification and calibration. Should have an automatic verification function to achieve volatile organic compounds
Periodic automatic verification of components, and frequency can be set. With manual and/or automatic calibration function, flame ionization detector should
Calibration by external standard method, mass spectrometer should be calibrated by internal standard method.
45.4.3 Air source unit
According to the needs of the monitoring system, it is equipped with high-purity nitrogen, helium, hydrogen, air and other gas sources. Gas source into the analysis unit
A hydrocarbon removal unit is required before. The air tightness requirement is 5.3.4.
5.4.4 Analysis unit
5.4.4.1 Enrichment module Enrichment and concentration of volatile organic compounds to be measured, and simultaneous removal of water, CO2 and other interferences,
And can achieve rapid thermal analysis.
5.4.4.2 Gas chromatography enables efficient separation of target compounds.
5.4.4.3 The detector responds well and stably to the target compound and meets the requirements of GB/T 30431 and GB/T 33864. Such as
The hydrogen-containing flame ionization detector should be able to judge the working state of the detector and have a flameout auto-ignition function. Such as equipped with mass spectrometry
The detector should have full scan/select ion scan, automatic/manual tuning, library search and other functions.
5.4.4.4 has a reference analysis method and can be edited.
5.4.4.5 It has the function of recording the flow, temperature, pressure, chromatogram and measurement concentration during the working process, which can automatically
Identify chromatographic peaks, peak heights and peak areas can be automatically calculated in batches.
5.4.5 Data Acquisition and Transmission Unit
5.4.5.1 Software with Chinese interface data acquisition and transmission.
5.4.5.2 Real-time acquisition, storage and calculation of monitoring data, which can output data with 1 h time resolution. The output should be able to
Set to the concentration in the standard state or the concentration in the reference state and enable switching between the two states; with mass concentration and
Volume concentration unit switching function, the mass concentration unit is μg/m3, and the volume concentration unit is nmol/mol. Minimum display unit 0.01
Gg/m3 or 0.01 nmol/mol.
5.4.5.3 With network access function, it can transmit data and charts at regular intervals. The transmission protocol shall comply with the requirements of HJ 212.
5.4.5.4 It is possible to display the monitoring data and working status parameters of each target compound in real time, and set conditional query and display history.
Historical data.
5.4.5.5 It is able to record and store data for more than half a year, with historical data query and export functions. Automatically protect after power failure
Save data.
5.4.6 Other requirements
5.4.6.1 has the function of displaying and setting the system time.
5.4.6.2 The monitoring system restarts after being stopped under normal conditions, and the time required to meet the technical requirements is less than 6 hours.
6 Performance indicators
6.1 Measurement range
The determination component should include at least 57 volatile organic compounds, and 57 components are listed in Appendix A. The highest concentration of each component is not low
At 50 nmol/mol.
56.2 Standard curve
The standard curve correlation coefficient of the target compound is ≥ 0.98.
The lowest point concentration was calculated using a standard curve, and the relative error between the measured average value and the standard value was ≤ 15%.
6.3 Zero noise
The zero noise of each component instrument is ≤0.05 nmol/mol.
6.4 Method detection limit
The detection limit of 90% of the components (including at least ethane and ethylene) is ≤0.1 nmol/mol.
6.5 Accuracy
Accuracy of each component. ±10%.
6.6 Precision
The precision of each component is ≤10%.
6.7 Resolution
Resolution of cyclopentane and isopentane, resolution of 2,3-dimethylpentane and 2-methylhexane, and o-xylene and styrene
The resolution is above 1.0.
6.8 24 h concentration drift
The 24 h concentration drift of 10 nmol/mol does not exceed ±1 nmol/mol.
6.9 Long-term concentration drift, retention time drift
Continuous operation for 30 d, the concentration drift of the component detected by the hydrogen flame ion detector is ≤15%; the mass spectrometer detects the concentration of the component
Degree drift ≤ 30%; retention time drift ≤ 0.5 min.
6.10 Effective data rate
The monitoring instrument was continuously operated for 30 days, and the effective data rate was ≥80%.
6.11 Instrument Parallelism
The instrument parallelism of each component is ≤ 20%.
6.12 Clock error
The instrument is tested for 6 h under normal working conditions with a clock error of ±20 s.
The instrument industrial machine is powered off for a total of 3 times (the duration of each power failure is 20 s, 2 min and 20 min, respectively, and each time
The power supply should be guaranteed for not less than 10 min between power failures, and tested for 6 h with a clock error of less than 2 min.
66.13 System residue
The system residual concentration of 90% component is ≤0.1 nmol/mol.
7 Detection methods
7.1 General requirements
7.1.1 Extract at least 2 sets of instruments of the same type to be tested simultaneously at the designated laboratory site, and test the knot of each instrument.
For evaluation.
7.1.2 The default operating method is selected for each type of instrument test. This method meets the requirements of 5.4.1.5 and 5.4.5.2.
7.1.3 If the test is interrupted due to power supply problems, after the power supply returns to normal, continue to test, the completed test
Indicators and data are valid.
7.1.4 If the test is interrupted due to instrument failure, restart the test after the instrument returns to normal; during the test, each set
The number of instrument failures is ≤2 times.
7.1.5 The test data of each technical indicator is the final result stored by the instrument data acquisition and processing unit.
7.2 Standard substance requirements
7.2.1 Standard gas. contains 57 volatile organic compounds. Standard gas produced for certified standard gases or qualified units.
In this standard, the target compounds are evaluated as 57 volatile organic compounds, unless otherwise stated.
7.2.2 Internal standard gas. The components are monobromochloromethane, 1,4-difluorobenzene, chlorobenzene-d5, 1-bromo-4fluorobenzene. For use
Monitoring system for mass spectrometry detectors.
7.3 standard curve
Under the normal working condition of the instrument, the labels of 0.5, 2, 4, 6, 8, 10 nmol/mol are sequentially introduced from low concentration to high concentration.
Quasi-gas injection analysis, each concentration is analyzed at least 3 times. Flame ionization detector adopts external standard method, target compound concentration
For the abscissa, the peak area (or peak height) of the target compound is plotted on the ordinate, and the standard curve is drawn by least squares; mass spectrometry
The internal standard method is adopted, the concentration ratio of the target compound and the internal standard is the abscissa, and the response ratio of the target compound to the internal standard is vertical.
Coordinates, the standard curve is drawn by least squares method. Calculate the standard curve correlation coefficient of the target compound using a standard curve
Calculate the lowest point concentration, calculate the relative error between the measured average value and the standard value according to formula (1), and should meet the requirements of 6.2.
0×
Ltest
CC
(1)
Where. d--the relative error between the mean value of the lowest concentration point and the standard value, %;
Test
- the lowest concentration point to measure the concentration average, nmol/mol;
- the lowest concentration point standard concentration value, nmol/mol.
7.4 Zero noise
Under normal working conditions of the instrument, pass high-purity nitrogen or air for analysis, at least 7 consecutive measurements, calculate the test
Concentration value measured by the instrument
, where i is the number of measurements (i = 1, 2..., n), and the standard deviation of the obtained data is calculated according to formula (2)
7S
, that is, the zero noise of the instrument, should meet the requirements of 6.3.
( )
0 −
Rr
(2)
Where. S
-- zero noise, nmol/mol;
-- the i-th measurement concentration value, nmol/mol;
R--n measured concentration average, nmol/mol;
I--the serial number of the recorded data (i=1~n);
n--The total number of recorded data.
7.5 Method Detection Limit
Under the normal working condition of the instrument, the standard gas with the concentration close to the detection limit is passed for analysis (MDL< standard gas concentration)
< 10×MDL, recommended not to be higher than 0.5 nmol/mol), at least 7 consecutive measurements, calculate the concentration value X of the instrument to be tested
,its
The middle i is the number of measurements (i = 1, 2..., n), and the standard deviation S of the obtained data is calculated according to the formula (3).
( )
XX
(3)
Where. S--standard deviation, nmol/mol;
-- the i-th measurement concentration value, nmol/mol;
--n measured concentration average, nmol/mol;
I--the serial number of the recorded data (i=1~n);
n--The total number of recorded data.
Then calculate the method detection limit MDL according to formula (4), which should meet the requirements of 6.4.
MDL=t
N-1, 0.99×S (4)
7.6 Accuracy and precision
Under normal working conditions of the instrument, a standard gas of 5 nmol/mol is passed for analysis to calculate the components in the instrument to be tested.
Monitoring concentration Y
Repeat the test at least 7 times for each concentration. Calculate the average measured concentration and known standard gas according to formula (5)
The relative error of the concentration, that is, the accuracy, should meet the requirements of 6.5; calculate the relative standard of the measured concentration according to formula (6)
The quasi-deviation RSD, which is precision, should meet the requirements of 6.6.
0×
YY
(5)
In the 8th formula. δ--the accuracy of the instrument to be tested, %;
Y -- multiple measurements of the average concentration, nmol/mol;
- Standard gas concentration, nmol/mol.
( )
×−
YY
RSD
(6)
Where. RSD - precision of the instrument to be tested, %;
-- the i-th measurement concentration value, nmol/mol;
Y -- multiple measurements of the average concentration, nmol/mol;
n--The total number of recorded data.
7.7 resolution
Under normal working conditions of the instrument, pass 1~5 nmol/mol of volatile organic standard gas. After the reading is stable, record
Peak width and retention time were recorded to assess the degree of separation between adjacent components. Calculate the resolution of cyclopentane and isopentane, 2,3-dimethyl
The resolution of pentane and 2-methylhexane, the separation of o-xylene and styrene should meet the requirements of 6.7.
Jj 1
2(t -t )
RR
Jj
WW
(7)
Where. R
- the degree of separation of adjacent components;
Rj
- retention time of the latter component of the two adjacent components, min;
Rj-1
- retention time of the former component of the two adjacent components, min;
- the peak width of the latter component of the two adjacent components, min;
J-1
- the peak width of the former component of the two adjacent components, min.
7.8 24 h concentration drift
Under the normal working condition of the instrument, 10 nmol/mol of standard gas is introduced, and the average value of the measured instrument is measured for 3 consecutive times.
After the end of the ventilation, the analytical instrument to be tested is continuously operated for 24 h (no maintenance or calibration is allowed during the period), and the above operation is repeated.
The average value of the measured concentrations was calculated three times after 24 hours. Calculate the 24 h concentration drift according to formula (8), which should meet the requirements of 6.8.
(8)
Where. - the concentration drift of the analyzer to be tested 24 h, nmol/mol;
- average concentration of the first three measurements of 24 h, nmol/mol;
- The average concentration of 3 measurements after 24 h, nmol/mol.
7.9 Long-term concentration drift, retention time drift
After the instrument under test is commissioned, it starts running for 30 consecutive days, without instrument adjustment, and once every day, 2 nmol/mol
Standard gas test. Calculate the concentration drift of the measured concentration and the standard value per day according to formulas (9) and (10).
And retaining each component
The drift of time DTn should meet the requirements of 6.9.
9 0×=
Sn
CC
(9)
Where. D
-- concentration drift on day n, %;
- the measured concentration of the instrument on the nth day, nmol/mol;
- The concentration of the standard gas, nmol/mol.
0×=
0n
RT
RT-RT
DT
(10)
Where. DTn--the retention time drift of the nth day, %;
RTn--the retention time of a component on the nth day, min;
RT0--Day 1 test the retention time of a component, min.
7.10 Effective data rate
After the instrument under test passes the commissioning, it starts running for 30 consecutive days and tests the effective data rate. During each maintenance period and
The content is recorded in detail and a daily check of 2 nmol/mol of standard gas is performed once a day. Statistics missing within 30 days and
The number of hours of abnormal data, data missing refers to the lack of data caused by normal maintenance and instrument failure. The day's verification data is not satisfied
When the long-term concentration drift is required, the data of 24 h before and after is recorded as abnormal data. Calculate the effective number according to formula (11)
According to the rate, it should meet the requirements of 6.10.
0)
1 ( ×
−=
(11)
Where. D--30 d effective data rate, %;
T--30 d Loss of instrument data and hours of significant abnormalities, h.
7.11 Instrument Parallelism
Under the same test environment conditions, adjust the sample inlets of at least two instruments to the same height, and the sampling port of the instrument
The distance between them is about 1 m, or sampling from the same sampling manifold. Choose high, medium and low, different pollution concentrations for 3 days, at least every day.
20 hours sample, record the hourly sample concentration value measured by each instrument C
Ij
, i is the instrument number (i=1, 2..., n), j is per
Sample number of the sampling period (j=1, 2..., m). Calculate the component whose average concentration is higher than the method limit of quantitation according to formula (12)
Relative standard deviation of concentration as instrumental parallelism result for each sample P
. Calculate the parallelism of the instrument according to formula (13).
Meet the requirements of 6.11.
( )
Jij
CC
(12)
Where. P
-- the parallelism of the jth sample measurement of n instruments;
Ij
- the concentration value measured by the jth sample of the i-th instrument, nmol/mol;
The average value of the concentration measured by the jth sample of n instruments, nmol...
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