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HJ 644-2013

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HJ 644-2013English449 Add to Cart Days<=3 Ambient air. Determination of volatile organic compounds. Sorbent adsorption and thermal desorption/gas chromatography mass spectrometry method Valid HJ 644-2013
HJ 644-2013Chinese17 Add to Cart <=1-day [PDF from Chinese Authority, or Standard Committee, or Publishing House]

   
Detail Information of HJ 644-2013; HJ644-2013
Description (Translated English): Ambient air. Determination of volatile organic compounds. Sorbent adsorption and thermal desorption/gas chromatography mass spectrometry method
Sector / Industry: Environmental Protection Industry Standard
Word Count Estimation: 17,188
Quoted Standard: HJ/T 194
Drafting Organization: Dalian Municipal Environmental Monitoring Center
Regulation (derived from): Department of Environmental Protection Notice No. 12 of 2013
Summary: This standard specifies the determination of volatile organic compounds in ambient air (VOCs) adsorption tube sampling thermal desorption/gas chromatography mass spectrometry. This standard applies to the ambient air 35 kinds of volatile organic compounds

HJ 644-2013
Ambient air.Determination of volatile organic compounds.Sorbent adsorption and thermal desorption/gas chromatography mass spectrometry method
National Environmental Protection Standard of the People's Republic
Determination of volatile organic compounds in ambient air
Adsorption tube sampling-thermal desorption/gas chromatography-mass spectrometry
Ambient air - Determination of volatile organic compounds -
Sorbent adsorption and thermal desorption/ gas chromatography mass
Spectrometry method
2 0 1 3 - 2 - 1 7 released
2 0 1 3 - 7 - 1 Implementation
Ministry of Environmental Protection released
Content
Foreword. II
1 Scope.1
2 Normative references.1
3 principle of the method.1
4 reagents and materials 1
5 Instruments and equipment 2
6 sample 2
7 Analysis steps.3
8 Calculation and representation of results. 5
9 precision and accuracy.6
10 Quality Assurance and Quality Control 7
11 Notes..7
Appendix A (Normative Appendix) Detection limit and lower limit of determination of target 8
Appendix B (informative) Reference information for target determination..9
Appendix C (Informative) Precision and Accuracy 10
Foreword
To implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on the Prevention and Control of Atmospheric Pollution
This standard is formulated to ensure human health and to regulate the determination of volatile organic compounds in ambient air.
This standard specifies the adsorption tube sampling-thermal desorption/gas chromatography-mass spectrometry for the determination of volatile organic compounds in ambient air.
This standard is the first release.
Appendix A of this standard is a normative appendix, and Appendix B and Appendix C are informative appendices.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard is mainly drafted by. Dalian Environmental Monitoring Center and Environmental Standards Research Institute of the Ministry of Environmental Protection.
This standard is verified by. Jiangsu Environmental Monitoring Center, Anshan Environmental Monitoring Center Station, Shenyang Environmental Monitoring Center
Station, Harbin Environmental Monitoring Center Station, Fushun Environmental Monitoring Center Station and Changchun Environmental Monitoring Center Station.
This standard was approved by the Ministry of Environmental Protection on February 17,.2013.
This standard has been implemented since July 1,.2013.
This standard is explained by the Ministry of Environmental Protection.
Determination of volatile organic compounds in ambient air
Adsorption tube sampling-thermal desorption/gas chromatography-mass spectrometry
Warning. The standard solution used in the experiment is a volatile toxic chemical. The solution preparation process should be in a fume hood.
When operating, the operator should wear protective gear.
1 Scope of application
This standard specifies the adsorption tube sampling-thermal desorption/gas chromatography-mass spectrometry for the determination of volatile organic compounds (VOCs) in ambient air.
Spectral method.
This standard applies to the determination of 35 volatile organic compounds in ambient air. If it is verified, this standard can also be applied to other
Determination of non-polar or weakly polar volatile organic compounds.
When the sampling volume is 2L, the detection limit of this standard is 0.3-1.0 μg/m3, and the lower limit of measurement is 1.2-4.0 μg/m3.
See Appendix A for details.
2 Normative references
The contents of this standard refer to the following documents or their terms. For undated references, the valid version applies.
In this standard.
HJ/T 194 Technical Specifications for Manual Air Quality Monitoring
3 Principle of the method
Enriching volatile organic compounds in ambient air with a solid adsorbent, placing the adsorption tube in a thermal desorber, by gas chromatography
After separation, detection was carried out by mass spectrometry. Qualitative by comparing with the standard mass spectrum of the target to be tested and retention time, external standard
Method or internal standard method for quantification.
4 reagents and materials
4.1 Methanol (CH3OH). Analytical grade of pesticide residues.
4.2 Standard stock solution. ρ =.2000 mg/L, commercially available certified standard solution.
4.3 4-bromofluorobenzene (BFB) solution. ρ = 25 mg/L, commercially available certified standard solution, or prepared with a high concentration of standard solution.
4.4 Adsorbent. Carbopack C (specific surface area 10 m2/g), 40/60 mesh; Carbopack B (specific surface area 100 m2/g),
40/60 mesh; Carboxen 1000 (specific surface area 800 m2/g), 45/60 mesh or other equivalent adsorbent.
4.5 Adsorption tube. stainless steel or glass, inner diameter 6mm, filled with Carbopack C, CarbopackB, Carboxen 1000,
The lengths are 13, 25, and 13 mm, respectively. Or use other products with the same features.
4.6 Focus tube. stainless steel or glass material, the inner diameter is not more than 0.9mm, and the type and length of the adsorbent are filled with the adsorption tube.
with. Or use other products with the same features.
4.7 Aging and storage of the adsorption tube.
The newly purchased adsorption tube or the adsorption tube after collecting a high concentration sample needs to be aged.
The aging temperature is 350 °C, the aging flow rate is 40 ml/min, and the aging time is 10-15 minutes.
Immediately after aging of the adsorption tube, seal both ends or put them into a special sleeve and wrap a layer of aluminum foil on the outside. Wrapped suck
The attached tube is placed in a desiccator containing a mixture of activated carbon or activated carbon silica gel, and the desiccator is placed in a refrigerator free of organic reagents.
Store at 4 ° C for 7 days.
Note 1. Focus tube aging and preservation methods are the same as adsorption tubes.
4.8 Carrier gas. helium, purity 99.999%.
5 Instruments and equipment
5.1 Gas Chromatograph. With capillary column split/splitless inlet, it can control the electronic pressure of the carrier gas and can be programmed.
Note 2. The gas chromatograph is equipped with an oven cooling device to improve the peak shape of highly volatile targets and improve sensitivity.
5.2 Mass Spectrometer. Electron Impact (EI) ionization source, capable of scanning from 35 amu to 270 amu in one second with NIST mass spectrum
Library, manual/automatic tuning, data acquisition, quantitative analysis, and library search.
5.3 Capillary column. 30 m × 0.25 mm, 1.4 μm film thickness (6% nitrile propylbenzene, 94% dimethylpolysiloxane fixative),
Other equivalent capillary columns can also be used.
5.4 Thermal desorption device
The thermal desorption device should have a secondary desorption function and the focusing tube portion should be heated rapidly (at least 40 ° C/sec). Thermal desorption
The silanized stainless steel tube should be used in the gas chromatographic connection and the gas pipeline in the instrument, and it can be at least 50-150 °C.
Heat evenly between.
Note 3. The use of a thermal desorption device with a cold focus function can reduce the loss of highly volatile targets and improve sensitivity.
5.5 aging device
The maximum temperature of the aging device should reach above 400 °C, the maximum carrier gas flow rate can reach at least 100 ml/min, and the flow rate can be adjusted.
5.6 sampler
Dual-channel oil-free sampling pump, dual channel can independently regulate flow and accurately maintain flow in 10~500 ml/min
The amount error should be within ±5%.
5.7 Calibration flowmeter. The flow rate can be accurately measured within 10~500 ml/min, and the flow accuracy is 2%. Electronic mass flow
meter.
5.8 Microinjectors. 5.0, 25.0, 50.0, 100, 250 and 500 μl.
5.9 Common instruments and equipment used in general laboratories.
6 samples
6.1. Sampling flow and sampling volume
Sampling flow. 10 ~.200 ml/min; sampling volume. 2 L. When the relative humidity is greater than 90%, the sampling volume should be reduced.
But at least it should not be less than 300 ml.
6.2 Sample collection and preservation
6.2.1 Air tightness check. A sorbent pipe (same as the sorbent pipe used for sampling, this sorbent pipe is only used for air tightness inspection)
Connect to the sampling pump (5.6) with the preset flow rate, open the sampling pump, block the intake end of the adsorption tube, and if the flow rate is zero,
The sampling device air connection is airtight, otherwise the air circuit should be checked for air tightness.
6.2.2 Preset sampling flow. Adjust the flow to the set value.
6.2.3 Remove the adsorption tube from 6.2.1 and connect a new adsorption tube to the sampling pump. Press the direction of the air flow indicated on the adsorption tube.
Sampling. The collection of ambient air samples is performed in accordance with the relevant provisions of HJ/T 194. Pay attention to the process of collecting samples.
Check to adjust the sampling flow to keep the flow constant. After sampling, record the sampling point, time, ambient temperature, atmosphere
Information such as pressure, flow and adsorption tube number.
6.2.4 After the sample collection is completed, the adsorption tube should be quickly removed, and the ends of the adsorption tube should be sealed or placed in a special casing.
Wrap a layer of aluminum foil and transport it to the laboratory for analysis. Samples that cannot be analyzed immediately are stored in step 4.7 and analyzed within 7 days.
6.2.5 Collection of candidate adsorption tubes. Connect an aging adsorption tube in series after the adsorption tube. At least one sample should be collected for each batch of samples.
A candidate adsorption tube is used to monitor whether the sample is penetrated.
6.2.6 Collection of blank samples on site. transport the adsorption tube to the sampling site, open the sealing cap or remove it from the special casing.
Immediately seal the ends of the tube or put it into a special sleeve and wrap a layer of aluminum foil on the outside. Same as the adsorption tube of the sample already collected
Store and bring back to the laboratory for analysis. At least one field blank sample should be taken each time the sample is taken.
Note 4. Temperature and wind speed have an effect on sample collection. When sampling, the ambient temperature should be less than 40 °C; when the wind speed is greater than 5.6 m/s, sampling
The sorbent tube should be placed perpendicular to the wind direction and the bunker placed in the upwind direction.
7 Analysis steps
7.1 Instrument Reference Conditions
7.1.1 Thermal Desorber Reference Conditions
Transmission line temperature. 130 ° C; adsorption tube initial temperature. 35 ° C; focus tube initial temperature. 35 ° C; adsorption tube desorption temperature.
325 ° C; adsorption tube desorption time. 3 min; focus tube desorption temperature. 325 ° C; focus tube desorption time. 5 min;
With flow. 40 ml/min; focusing tube aging temperature. 350 ° C; dry blowing flow. 40 ml/min; dry blowing time. 2 min.
7.1.2 Gas Chromatograph Reference Conditions
Inlet temperature..200 ° C; carrier gas. helium; split ratio. 5.1; column flow (constant current mode). 1.2 ml/min;
Temperature program. initial temperature 30 °C, hold 3.2 min, heat up to.200 °C at 11 °C/min for 3 min.
Note 5. In order to eliminate the interference of moisture and the overload of the detector, the split ratio can be set according to the situation. Some thermal desorbers have sample shunting capabilities.
It can be set according to the manufacturer's recommendations or specific conditions.
7.1.3 Mass Spectrometry Reference Conditions
Scanning mode. full scan; scanning range. 35 ~ 270 amu; ionization energy. 70 eV; interface temperature. 280 °C.
The rest of the parameters are set according to the instruction manual of the instrument.
Note 6. In order to improve the sensitivity, the selective ion scanning method can also be used for analysis. The characteristic ion selection is referred to Appendix B.
7.2 Instrument performance check
Pipette 1.0 μl of BFB solution (4.3) with a micro-syringe and directly inject it into the gas chromatograph for analysis.
The BFB key ion abundance obtained by the spectrum should meet the standards specified in Table 1, otherwise the parameters of the mass spectrometer should be adjusted or
Consider cleaning the ion source.
Table 1 BFB key ion abundance standards
Mass ion abundance standard mass ion abundance standard
50% 95% of 5% to 40% 174 is greater than 50% of mass 95
75 quality 95% to 80% 175 quality 174 5% to 9%
95 base peak, 100% relative abundance 176 quality 174 93% ~ 101%
96% 95% 5% to 9% 177 Quality 5% 5% to 9%
173 is less than 2% of mass 174 - -
7.3 Calibration
7.3.1 Drawing of the calibration curve
Pipette 25.0, 50.0, 125, 250, and 500 μl of standard stock solution (4.2) to 10 ml using a microsyringe
In a volumetric flask, the volume was adjusted to a concentration of 5.00, 10.0, 25.0, 50.0, and 100 mg/L with methanol (4.1).
Standard series. Use a micro-syringe to remove 1.0 μl of the standard series solution into the thermal desorber, according to the instrument reference conditions,
The measurement was performed from a low concentration to a high concentration, and a calibration curve was drawn.
Note 7. If the thermal desorber used does not have the function of “Liquid Injection Preparation Standard Series”, it can be prepared as follows. Connect the aged adsorption tube to
Gas chromatograph packed in the column inlet, set the inlet temperature to 50 ° C, use a micro-syringe to remove 1.0 μl standard series solution and inject into the gas color
Spectrometer inlet, using carrier gas of 100 ml/min for 5 min, quickly remove the adsorption tube, and prepare the target content to be 5.00, 10.0, 25.0, respectively.
50.0 and 100 ng standard series tubes.
Note 8. The calibration curve can also be prepared by purchasing a commercial standard sample tube directly.
7.3.1.1 Draw a calibration curve using least squares
The calibration curve is drawn by taking the target mass (ng) as the abscissa and the corresponding response value as the ordinate. Phase of the calibration curve
The number of relationships should be greater than or equal to 0.99.
7.3.1.2 Draw a calibration curve with an average relative response factor
The relative response factor (RRFi) of the target in point i of the standard series is calculated according to formula (1).
ISi
ISi
i Am
mA
RRF ×
×= (1)
In the formula.
RRFi--the relative response factor of the i-th target in the standard series;
Ai--the response value of the target ion of the i-th target in the standard series;
Mi--the mass of the i-th target in the standard series, ng;
AIS--the internal standard quantitation ion response value;
mIS--the quality of the internal standard, ng.
The average relative response factor RRF of the target is calculated according to formula (2).
RRF
RRF
I∑
== 1
(2)
In the formula.
RRF - the average relative response factor of the target;
RRFi--the relative response factor of the i-th target in the standard series;
n--Standard series points.
The standard deviation (SD) of RRF is calculated according to formula (3).
)( 2
RRFRRF
SD
(3)
The relative standard deviation (RSD) of RRF is calculated according to formula (4).
0×=
RRF
SDRSD
(4)
The relative standard deviation (RSD) of the standard series of target relative response factors (RRF) should be less than or equal to 20%.
Note 9. When quantifying by internal standard method, internal standard should be added to standard series tube and sample tube. Recommended internal standard materials are fluorobenzene, chlorobenzene-d5 and 1,4-two.
Chlorobenzene-d4, the internal standard concentration was 25 mg/L, and the addition amount was 1.0 μl.
Note 10. If the relative standard deviation (RSD) of a target relative to the response factor (RRF) in the standard series is greater than 20%, then the target
Calibration is required using a least squares calibration curve.
7.3.2 Standard chromatogram
The target reference chromatogram is shown in Figure 1.
1-1,1-dichloroethylene; 2-1,1,2-trichloro-1,2,2-trifluoroethane; 3-chloropropene; 4-dichloromethane; 5-1, 1-di Ethyl chloride; 6-trans
-1,2-dichloroethylene; 7-trichloromethane; 8-1,2-dichloroethane; 9-1,1,1-trichloroethane; 10-tetrachloromethane; 11-benzene; - trichloroethylene;
13-1,2-dichloropropane; 14-trans-1,3-dichloropropene; 15-toluene; 16-cis-1,3-dichloropropene; 17-1,1,2-trichloro Ethane; 18-
Tetrachloroethylene; 19-1,2-dibromoethane; 20-chlorobenzene; 21-ethylbenzene; 22-m-, p-xylene; 23-o-xylene; 24-styrene; 1,2,2-
Tetrachloroethane; 26-4-ethyltoluene; 27-1,3,5-trimethyl; 28-1,2,4-trimethylbenzene; 29-1,3-dichlorobenzene; 30- 1,4-dichlorobenzene; 31-
Benzyl chloride; 32-1,2-dichlorobenzene; 33-1,2,4-trichlorobenzene; 34-hexachlorobutadiene.
Figure 1 Total ion chromatogram of the target
7.4 Determination
7.4.1 Determination of samples
The collected adsorption tube is quickly placed in the thermal desorber, and the thermal desorption is carried out according to the instrument reference condition (7.1).
The direction of the adsorption tube should be opposite to the direction in which the gas enters the adsorption tube during sampling. The target in the sample enters the column with desorbed gas
The measurement was carried out. After the analysis is completed, remove the adsorption tube and aging and store according to step 4.7. If the sample concentration is low, the adsorption tube may not be needed.
Ageing.
7.4.2 Blank test
The blank sample was analyzed in the same procedure as the sample determination.
8 Calculation and representation of results
8.1 Qualitative analysis
Characterize by retention time and mass spectrum comparison.
8.2 Quantitative analysis
The calculation is performed according to the response value of the first characteristic ion of the target. When the first characteristic ion of the target in the sample interferes,
A second characteristic ion quantification can be used, as detailed in Appendix B.
8.2.1 Calculation of the mass of the target in the adsorption tube
8.2.1.1 External standard method
When the calibration curve is drawn by the least squares method, the target mass m (ng) in the sample is calculated by the corresponding calibration curve.
8.2.1.2 Internal standard method
When calibrating with the average relative response factor, the mass m(ng) of the target in the sample is calculated according to formula (5).
Count.
RRFA
mAm
IS
ISx
×= (5)
In the formula.
M--the mass of the target in the sample, ng;
Ax--the target quantitation ion response value;
AIS--the response value of the internal standard quantitative ion corresponding to the target;
mIS--the quality of the internal standard, ng;
RRF - The average relative response factor of the target.
8.2.2 The mass concentration of the target to be tested in the ambient air shall be calculated according to formula (6).
ndV
m=ρ (6)
In the formula.
Ρ--the mass concentration of the target in ambient air, μg/m3;
M--the mass of the target in the sample, ng;
Vnd - the sampling volume in the standard state (101.325 kPa, 273.15K), L.
8.3 result representation
When the measurement result is less than 100 μg/m3, it is retained to 1 decimal place; when the measurement result is greater than or equal to 100 μg/m3,
Keep three significant digits.
When the capillary column specified in this standard is used, the target of peak number 22 is metaxylene and p-dimethylene.
The sum of both benzene.
9 Precision and accuracy
9.1 precision
Six laboratories performed blank spiked samples equivalent to 5.0 μg/m3, 12.5 μg/m3, and 35.0 μg/m3.
The relative standard deviations in the laboratory were 1.1% to 24.9%, 2.4% to 21.1%, and 2.0% to 18.7%, respectively.
The relative standard deviations between the chambers were 0.7% to 11.5%, 0.7% to 10.0%, and 0.44% to 6.38%, respectively. The repeatability limits were
0.4~3.2μg/m3, 2.2~10.8 μg/m3, 3.3~14.6μg/m3; the reproducibility limits are 0.9~3.3 μg/m3, 2.3~10.0 μg/m3, respectively.
3.1~15.2 μg/m3.
9.2 Accuracy
Six laboratory laboratories added standard amounts of ambient air equivalent to 5.0μg/m3, 12.5μg/m3 and 35.0μg/m3
The measurement was carried out, and the recoveries were 56.4% to 122%, 53.4% to 126%, and 76.1% to 132%, respectively.
The results of precision and accuracy are detailed in Appendix C.
10 Quality Assurance and Quality Control
10.1 Before collecting samples, 20% of the adsorption tube should be taken for blank inspection. When the number of samples is less than 10, it should be pumped at least.
Take 2 roots. The concentration of the target equivalent to 2 L of sample in the blank tube should be less than the detection limit, otherwise it should be re-aged.
10.2 Apply a blank adsorption tube instead of the sample adsorption tube before each sample analysis to measure the system blank and the system blank is small.
Samples can only be analyzed after the detection limit.
10.3 A calibration curve intermediate concentration check point should be made every 12h. The intermediate concentration check point measurement value is corresponding to the calibration curve.
The relative error of degrees should not exceed 30%.
10.4 The amount of the single target in the blank sample should be less than 10% of the corresponding detected amount in the sample or with the blank adsorption tube.
The amount of detection is equivalent.
11 Precautions
11.1 The residual VOCs in the adsorption tube interfere with the measurement, and the aging and preservation procedures (4.7) can be strictly performed to make this dry.
The disturbance is reduced to a minimum.
11.2 Newly purchased sorbent tubes shall be marked with a unique code and an arrow indicating the direction of the sample gas flow, and a sorbent tube information card shall be established.
Records include information such as the fill or purchase date of the sorbent tube, the maximum allowable temperature, and the number of uses.
Appendix A
(normative appendix)
Target detection limit and lower limit of measurement
When the sampling volume is 2L, the method detection limit and lower limit of measurement for 35 targets are shown in Appendix A.1.
Schedule A.1 Target detection limit and lower limit of measurement
No. Compound Chinese name Compound English name detection limit (μg/m3) Lower limit of determination (μg/m3)
1, 1,1-dichloroethylene 1,1-Dichloroethene 0.3 1.2
2 1,1,2-trichloro-1,2,2-trifluoroethane 1,1,2-Trichloro-1,2,2-trifluormethane 0.5 2.0
3 Chloropropene Allyl chloride 0.3 1.2
4 dichloromethane Methylene chloride 1.0 4.0
5 1,1-Dichloroethane 1,1-Dichloroethane 0.4 1.6
6 cis-1,2-dichloroethylene cis-1,2-Dichloroethene 0.5 2.0
7 Trichloromethane 0.4 1.6
8 1,1,1-trichloroethane 1,1,1-Trichloroethane 0.4 1.6
9 Carbon tetrachloride Carbon tetrachloride 0.6 2.4
10 1,2-Dichloroethane 1,2-Dichloroethane 0.8 3.2
11 Benzene Benene 0.4 1.6
12 Trichloroethylene 0.5 2.0
13 1,2-dichloropropane 1,2-Dichloropropane 0.4 1.6
14 cis-1,3-dichloropropene cis-1,3-Dichloropropene 0.5 2.0
15 toluene Toluene 0.4 1.6
16 trans-1,3-dichloropropene trans-1,3-Dichloropropene 0.5 2.0
17 1,1,2-trichloroethane 1,1,2-Trichloroethane 0.4 1.6
18 Tetrachloroethylene 0.4 1.6
19 1,2-Dibromoethane 1,2-Dibromoethane 0.4 1.6
20 chlorobenzene Chlorobenzene 0.3 1.2
21 ethylbenzene Ethylbenzene 0.3 1.2
22, p-xylene m, p-Xylene 0.6 2.4
23 o-xylene o-Xylene 0.6 2.4
24 Styrene Styrene 0.6 2.4
25 1,1,2,2-tetrachloroethane 1,1,2,2-Tetrachloroethane 0.4 1.6
26 4-ethyltoluene 4-Ethyltoluene 0.8 3.2
27 1,3,5-trimethylbenzene 1,3,5-Trimethylbenzene 0.7 2.8
28 1,2,4-trimethylbenzene 1,2,4-Trimethylbenzene 0.8 3.2
29 1,3-dichlorobenzene 1,3-Dichlorobenzene 0.6 2.4
30 1,4-dichlorobenzene 1,4-Dichlorobenzene 0.7 2.8
31 benzyl chloride Benzyl chloride 0.7 2.8
32 1,2-dichlorobenzene 1,2-Dichlorobenzene 0.7 2.8
33 1,2,4-trichlorobenzene 1,2,4-Trichlorobenzene 0.7 2.8
34 Hexachlorobutadiene 0.6 2.4 Hexachlorobutadiene
Appendix B
(informative appendix)
Target reference measurement information
The peak sequence, quantitative ion and auxiliary ion information of 35 targets are shown in Appendix B.1.
Schedule B.1 Determination of target information
No. Compound Chinese name compound English name CAS No. Quantitative ion assisted ion
1, 1,1-dichloroethylene 1,1-Dichloroethene 75-35-4 61 96,63
2 1,1,2-trichloro-1,2,2-trifluoroethane 1,1,2-Trichloro-1,2,2-trifluormethane 76-13-1 151 101,103
3 Chloropropene Allyl chloride 107-05-1 41 39,76
4 Methylene chloride 75-09-2 49 84,86
5 1,1-Dichloroethane 1,1-Dichloroethane 75-34-3 63 65
6 cis-1,2-dichloroethylene cis-1,2-Dichloroethene 156-59-2 61 96,98
7 Trichloromethane 67-66-3 83 85,47
8 1,1,1-trichloroethane 1,1,1-Trichloroethane 71-55-6 97 99,61
9 Carbon tetrachloride Carbon tetrachloride 56-23-5 117 119
10 1,2-dichloroethane 1,2-Dichloroethane 107-06-2 62 64
11 Benzene Benene 71-43-2 78 77,50
12 Trichloroethylene 79-01-6 130 132,95
13 1,2-dichloropropane 1,2-Dichloropropane 78-87-5 63 41,62
14 cis-1,3-dichloropropene cis-1,3-Dichloropropene 542-75-6 75 39,77
15 Toluene Toluene 108-88-3 91 92
16 trans-1,3-dichloropropene trans-1,3-Dichloropropene 542-75-6 75 39,77
17 1,1,2-trichloroethane 1,1,2-Trichloroethane 79-00-5 97 83,61
18 Tetrachloroethylene 127-18-4 166 164,131
19 1,2-Dibromoethane 1,2-Dibromoethane 106-93-4 107 109
20 Chlorobenzene Chlorobenzene 108-90-7 112 77,114
21 ethylbenzene Ethylbenzene 100-41-4 91 106
22, p-xylene m, p-Xylene
108-38-3/1
06-42-3
23 o-xylene o-Xylene 95-47-6 91 106
24 Styrene Styrene 100-42-5 104 78,103
25 1,1,2,2-tetrachloroethane 1,1,2,2-Tetrachloroethane 630-20-6 83 85
26 4-ethyltoluene 4-Ethyltoluene 622-96-8 105 120
27 1,3,5-trimethylbenzene 1,3,5-Trimethylbenzene 108-67-8 105 120
28 1,2,4-trimethylbenzene 1,2,4-Trimethylbenzene 95-63-6 105 120
29 1,3-dichlorobenzene 1,3-Dichlorobenzene 541-73-1 146 148,111
30 1,4-dichlorobenzene 1,4-Dichlorobenzene 106-46-7 146 148,111
31 Benzyl chloride Benzyl chloride 100-44-7 91 126
32 1,2-dichlorobenzene 1,2-Dichlorobenzene 95-50-1 146 148,111
33 1,2,4-trichlorobenzene 1,2,4-Trichlorobenzene 120-82-1 180 182,184
34 Hexachlorobutadiene Hexachlorobutadiene 87-68-3 225 227,223
Appendix C
(informative appendix)
Precision and accuracy
Precision and accuracy indicators such as method repeatability, reproducibility, and spike recovery are given in Table C.1.
Schedule C.1 Precision and Accuracy
No. Compound name plus scalar quantity (μg/m3)
Total mean
(μg/m3)
Relative standard in the experimental room
Quasi-bias (%)
Interlaboratory
standard deviation(%)
Repeatability limit r
(μg/m3)
Reproducibility limit R
(μg/m3)
_2 pSP ±
(%)
1 1,1-dichloroethylene
5.0 6.1 2.9~10.1 2.7 1.2 1.3 121±9.8
12.5 14.3 8.4~12.2 1.7 4.3 4.1 114±5.6
35.0 34.9 4.1~6.6 1.1 5.5 5.0 99.6±1.8
2 dichloromethane
5.0 6.1 4.4~15.2 3.0 1.7 1.9 122±14.4
12.5 14.6 4.6~15.7 4.1 5.3 5.5 116±16.0
35.0 35.8 4.2~7.0 1.1 6.3 5.9 102±2.4
1,1,2-trichloro-1,2,2-three
Fluoroethane
5.0 6.0 5.2~10.3 2.1 1.3 1.4 120±10.6
12.5 10.6 12.7~16.7 1.7 4.4 4.3 84.6±8.4
35.0 36.5 2.2~4.3 0.8 3.6 3.4 104±2.0
4 chloropropene
5.0 5.8 6.1~8.9 1.0 1.2 1.3 114±15.8
12.5 9.4 9.2~21.1 10.0 10.8 10.0 75.2±8.6
35.0 40.4 4.0~16.1 4.2 9.0 9.0 115±7.4
5 1,1-dichloroethane
5.0 6.1 4.3~7.0 1.1 1.0 1.0 121±6.2
12.5 14.1 4.8~8.9 1.6 2.7 2.7 112±5.8
35.0 37.0 4.6~9.4 1.6 6.3 6.4 106±6.2
6 trans-1,2-dichloroethylene
5.0 6.0 5.5~8.4 1.0 1.2 1.2 120±6.4
12.5 13.1 4.9~8.8 1.1 2.5 2.5 105±5.2
35.0 36.8 5.4~7.6 0.8 6.2 5.7 105±1.6
7 chloroform
5.0 5.8 3.5~8.6 0.7 3.3 3.1 116±9.6
12.5 12.5 8.4~10.5 0.7 3.3 3.1 99.8±5.6
35.0 36.2 4.5~6.0 0.5 5.5 5.1 103±2.4
8 1,2-dichloroethane
5.0 5.9 3.6~8.2 1.6 0.9 1.0 118±8.2
12.5 13.7 3.9~9.4 2.1 2.8 2.6 109±5.0
35.0 36.2 4.3~5.9 0.6 5.3 4.9 103±2.4
9 1,1,1-trichloroethane
5.0 5.8 4.1~8.2 1.7 1.0 1.1 117±9.4
12.5 10.4 7.9~11.1 1.2 2.7 2.7 82.9±6.0
35.0 37.8 3.9~5.0 0.5 4.9 4.7 108±2.8
10 carbon tetrachloride
5.0 5.3 4.8~9.9 1.6 1.1 1.4 105±12.8
12.5 12.8 13.9~28.8 4.6 6.9 6.6 102±10.4
35.0 37.1 3.7~6.1 0.9 4.7 4.5 106±3.0
11 benzene
5.0 5.6 6.1~15.8 4.0 1.7 1.7 112±10.4
12.5 11.9 6.3~13.1 2.2 3.5 3.4 95.5±6.4
35.0 36.5 4.7~6.6 0.7 5.6 5.2 104±2.0
12 trichloroethylene
5.0 5.7 5.4~15.7 3.0 1.5 1.7 114±14.2
12.5 14.1 2.4~9.1 2.4 2.3 2.3 113±5.6
35.0 33.6 5.1~7.5 0.8 5.8 5.7 96.1±4.2
13 1,2-dichloropropane
5.0 5.9 6.4~11.9 2.3 1.6 1.5 118±7.0
12.5 13.5 7.0~10.9 1.6 3.5 3.3 108±4.6
35.0 35.7 5.7~6.9 0.5 6.4 6.0 102±2.6
14 trans-1,3-dichloropropene
5.0 4.8 3.4~5.3 0.8 0.6 0.9 96.3±10.4
12.5 13.8 3.7~7.3 1.3 2.2 2.3 111±5.2
35.0 37.8 6.7~9.3 1.1 8.7 8.1 108±3.6
15 toluene
5.0 5.5 10.5~18.5 3.2 2.2 2.3 110±13.6
12.5 14.0 11.1~16.1 1.8 5.2 5.5 111±17.4
35.0 38.1 8.5~14.0 2.0 11.0 10.3 109±4.6
16 cis-1,3-dichloropropene
5.0 4.9 1.1~4.0 1.1 0.4 0.9 97.0±12.4
12.5 14.8 6.2~8.6 0.9 3.3 3.1 118±3.8
35.0 41.5 5.7~7.1 0.7 7.4 6.8 119±2.0
17 1,1,2-trichloroethane
5.0 5.5 8.5~19.9 11.5 3.2 3.3 115±9.8
12.5 14.4 11.8~17.4 2.6 5.8 5.7 116±11.0
35.0 37.4 4.2~6.6 1.0 5.2 4.8 107±1.2
18 tetrachloroethylene
5.0 5.4 4.9~16.8 4.8 1.8 2.1 109±15.0
12.5 14.9 12.0~14.7 1.0 5.6 5.2 119±3.8
35.0 38.0 5.0~6.5 0.7 6.2 5.7 108±1.0
19 1,2-dibromoethane
5.0 5.7 3.8~5.8 1.1 0.8 1.3 113±15.4
12.5 15.8 6.5~9.6 1.2 3.7 3.4 126±3.8
35.0 40.3 6.2~7.4 0.4 7.8 7.2 115±2.0
20 chlorobenzene
5.0 5.8 2.1~5.9 1.5 0.7 1.2 117±14.4
12.5 13.8 5.4~9.0 1.6 2.7 2.8 110±7.0
35.0 41.0 5.4~11.0 2.4 8.8 9.0 117±7.8
21 ethylbenzene
5.0 5.7 1.6~8.9 2.8 1.2 1.3 115±10.0
12.5 13.3 8.6~20.7 4.4 5.5 5.1 106±4.6
35.0 42.9 2.6~6.6 1.8 5.1 5.9 123±7.6
22, p-xylene
5.0 5.8 6.6~12.1 2.3 1.6 1.6 116±9.2
12.5 14.2 13.0~19.9 2.4 6.9 6.5 112±13.4
35.0 41.5 6.7~18.7 6.4 14.6 15.2 118±15.0
23 styrene
5.0 5.7 4.7~6.5 0.7 0.9 1.2 114±12.8
12.5 12.9 6.7~12.3 1.8 3.1 3.9 103±16.8
35.0 41.6 3.8~6.0 0.9 5.4 5.0 119±2.4
24 o-xylene
5.0 5.5 5.1~11.0 2.2 1.3 1.5 110±13.0
12.5 13.2 11.5~18.8 2.8 5.7 5.3 105±5.8
35.0 40.2 5.0~7.3 0.8 6.7 6.5 115±4.0
25 1,1,2,2-tetrachloroethane
5.0 5.4 3.0~10.7 3.2 1.1 1.8 108±21.4
12.5 12.8 6.7~9.5 1.4 2.9 3.1 102±9.0
35.0 41.7 5.2~7.8 1.1 7.0 6.9 119±5.0
26 4-ethyltoluene
5.0 4.7 3.6~10.1 3.1 1.1 1.3 95.6±11.2
12.5 12.5 11.8~16.5 3.0 4.8 5.5 99.7±19.2
35.0 38.2 8.6~14.7 2.4 12.4 11.4 109±3.6
27 1,3,5-trimethylbenzene
5.0 5.9 3.2~5.4 0.9 0.7 1.2 118±14.4
12.5 13.3 6.9~11.1 1.7 3.3 3.3 106±7.0
35.0 43.2 4.1~7.0 1.3 7.3 7.6 123±7.8
28 1,2,4-trimethylbenzene 5.0 5.3 8.3~14.8 1.9 1.7 1.8 107±14.0
12.5 13.2 5.8~22.4 6.8 5.2 5.3 106±13.8
35.0 39.7 8.6~10.9 1.0 10.7 9.8 113±2.0
29 1,3-dichlorobenzene
5.0 5.8 2.6~6.8 1.6 0.7 1.1 116±13.2
12.5 13.7 11.1~15.6 1.5 4.9 4.6 110±5.8
35.0 42.8 5.2~9.2 1.5 8.3 7.7 122±3.4
30 1,4-dichlorobenzene
5.0 5.7 1.8~5.2 1.0 0.6 1.1 114±13.4
12.5 13.8 11.3~18.9 2.4 5.8 5.6 110±10.2
35.0 41.3 6.5~13.1 3.8 11.5 13.3 118±16.2
31 benzyl chloride
5.0 5.0 3.9~5.4 0.9 0.7 1.4 99.3±17.4
12.5 11.6 8.1~15.7 3.2 3.6 3.4 92.1±4.0
35.0 41.7 8.7~14.2 2.8 12.7 11.9 119±5.8
32 1,2-dichlorobenzene
5.0 5.5 4.1~8.0 1.8 0.9 1.2 109±13.8
12.5 12.7 8.7~13.3 1.9 3.9 3.7 102±3.8
35.0 40.5 5.4~6.8 0.5 7.2 6.7 115±3.0
33 1,2,4-trichlorobenzene
5.0 5.8 5.3~14.6 4.3 1.8 1.8 115±11.2
12.5 13.9 8.4~13.9 2.0 4.7 4.4 111±6.0
35.0 46.3 2.0~7.3 2.1 6.4 8.0 132±11.4
34 Hexachloro-1,3-butadiene
5.0 4.8 2.0~5.2 1.2 0.5 0.9 95.5±12.2
12.5 13.0 10.6~16.6 2.2 5.2 5.0 104±9.0
35.0 42.5 5.5-7.7 0.9 7.9 7.4 121±3.4
Related standard:   HJ 645-2013  HJ 646-2013
   
 
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