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HJ 801-2016

Chinese Standard: 'HJ 801-2016'
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HJ 801-2016English229 Add to Cart Days<=3 Ambient air and waste gas-Determination of amide compounds-Liquid chromatography Valid HJ 801-2016
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BASIC DATA
Standard ID HJ 801-2016 (HJ801-2016)
Description (Translated English) Ambient air and waste gas-Determination of amide compounds-Liquid chromatography
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z15
Word Count Estimation 10,170
Date of Issue 2016-05-13
Date of Implementation 2016-08-01
Quoted Standard GB/T 16157; HJ/T 194
Drafting Organization Dalian Environmental Monitoring Center
Administrative Organization Ministry of Environmental Protection
Regulation (derived from) Ministry of Environmental Protection Announcement No. 39 of 2016

HJ 801-2016
Ambient air and waste gas-Determination of amide compounds-Liquid chromatography
National Environmental Protection Standard of the People 's Republic of China
Ambient air and exhaust
Determination of amide compounds by liquid chromatography
Ambient air and waste gas-Determination of amide compounds
-Liquid chromatography
2016-05-13 release
2016-08-01 implementation
release
Ministry of Environmental Protection
Directory
Preface .ii
1 Scope of application
2 normative reference documents
3 Principle of the method
4 interference and elimination
5 reagents and materials 1
6 instruments and equipment 2
7 Sample 2
8 Analysis steps
The results are calculated and expressed
10 precision and accuracy
Quality assurance and quality control
12 Waste treatment
Appendix A (informative) method of precision and accuracy
Preface
In order 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,
The protection of human health, regulate the ambient air and fixed sources of waste gas amide compounds in the determination of the development of this standard.
This standard specifies liquid chromatography for the determination of amide compounds in ambient air and stationary sources.
This standard is the first release.
Appendix A to this standard is an informative appendix.
This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division.
The main drafting unit of this standard. Dalian Environmental Monitoring Center.
The standard verification unit. Shenyang City Environmental Monitoring Center Station, Shaanxi Province Environmental Monitoring Center Station, Anshan City, environmental monitoring
Heart station, Jinzhou City Environmental Monitoring Center Station, Fushun City Environmental Monitoring Center and Yingkou City Environmental Monitoring Center Station.
The environmental protection department of this standard approved on May 13,.2016.
This standard has been implemented since August 1,.2016.
This standard is explained by the Ministry of Environmental Protection.
Ambient air and waste gas - Determination of amide compounds - Liquid chromatographic method
1 Scope of application
This standard specifies liquid chromatography for the determination of amide compounds in ambient air and stationary sources.
This standard applies to ambient air and fixed sources of waste gas in formamide, N, N-dimethylformamide, N, N-dimethylethyl
Determination of amide and acrylamide.
When the ambient air sampling volume is 30 L (standard state) and the volume of the absorbed liquid is 10 ml, the process formamide, N, N-
The detection limits for dimethylformamide, N, N-dimethylacetamide and acrylamide were 0.03 mg/m3, 0.02 mg/m3, 0.03
Mg/m3 and 0.02 mg/m3, the lower limit of determination was 0.12 mg/m3, 0.08 mg/m3, 0.12 mg/m3 and 0.08 mg/m3, respectively.
When the fixed source of waste gas sampling volume of 30 L (standard state), the absorption volume of 50 ml, the method of formamide, N, N-
The detection limits for dimethylformamide, N, N-dimethylacetamide and acrylamide were 0.2 mg/m3, 0.1 mg/m3, 0.2 mg/m3
And 0.1 mg/m3, the determination of the lower limit of 0.8 mg/m3, 0.4 mg/m3, 0.8 mg/m3 and 0.4 mg/m3.
2 normative reference documents
The contents of this standard refer to the following documents or their terms. Those who do not specify the date of the reference file, the effective version of the appropriate
For this standard.
Determination of particulate matter and sampling method of gaseous pollutants in exhaust gas of fixed pollution sources GB/T 16157
Technical specification for manual monitoring of ambient air quality
3 Principle of the method
Ambient air and fixed sources of amide compounds in the exhaust gas are absorbed by water and then treated with an aqueous solution equipped with an ultraviolet detector
Phase chromatograph separation detection, to retain the time qualitative, external standard method quantitative.
4 interference and elimination
Under the conditions specified in this method, other organic substances may cause interference, can be used under different auxiliary wavelength absorbance
Ratio, UV spectrum or mass spectrometry. According to the nature of the interference, the appropriate method to remove the interference.
5 reagents and materials
Unless otherwise stated, analytical pure chemical reagents are used in accordance with national standards. Experimental water is not prepared for new
Water containing organic matter.
5.1 acetonitrile (CH3CN). HPLC grade.
5.2 Formamide (CH3NO). purity ≥99.0%.
5.3 N, N-Dimethylformamide (C3H7NO). purity ≥99.0%.
5.4 N, N-dimethylacetamide (C4H9NO). purity ≥99.0%.
5.5 Acrylamide (C3H5NO). purity ≥99.0%.
5.6 Amide Compounds Standard stock solution
Accurate weighing 0.100 g (accurate to ± 0.0001 g) Formamide (5.2), 0.050 g (accurate to ± 0.0001 g) N, N-
Dimethylformamide (5.3), 0.100 g (accurate to ± 0.0001 g) N, N-dimethylacetamide (5.4) and 0.050 g (exact
To ± 0.0001 g) acrylamide (5.5), dissolved in water after the full volume into the 100 ml volumetric flask, diluted with water volume to the mark,
Shake well Preparation of Formamide, N, N-Dimethylformamide, N, N-Dimethylacetamide and Acrylamide Concentration of 1000
Mg/L, 500 mg/L, 1000 mg/L and 500 mg/L amide compounds were mixed at 4 ° C,
Dark and sealed can be stored for three months, should be used to restore to room temperature and shake. You can also purchase commercially available certified reference materials
Conditions Refer to the product description.
5.7 Amide Compounds Standard Use Liquid
Accurate removal of 5.00 ml of amide compound standard stock solution (5.6) in a 100 ml volumetric flask, diluted with water to
Marking, shaking. N, N-dimethylformamide, N, N-dimethylacetamide and acrylamide were prepared in the form of formamide, N, N-dimethylformamide
50.0 mg/L, 25.0 mg/L, 50.0 mg/L and 25.0 mg/L amide compounds. Turn into brown glass
Glass reagent bottles, frozen below 4 ℃, dark and sealed can be stored for 6 d. Use should be restored to room temperature, and shake.
6 instruments and equipment
6.1 Liquid Chromatograph. equipped with UV detector or diode array detector.
6.2 Column. The filler is silica gel bonded C18, the side chain is diisobutyl, particle size 5 μm, inner diameter 4.6 mm, column length 150 mm,
Or other equivalent columns.
6.3 Atmospheric Sampler. Flow rate 0.1 L/min ~ 2.0 L/min, accuracy 0.1 L/min.
6.4 Flue gas sampler. flow 0.1 L/min ~ 2.0 L/min, the accuracy of 0.1 L/min. Smoke gun with heating and insulation function.
Thermometer accuracy should not be less than 2.5%, the minimum scale value should not be greater than 2 ℃, sampling gun heating temperature of not less than 120 ℃.
6.5 brown porous glass absorber. meet the requirements of HJ/T 194.
6.6 brown porous glass absorption bottle. in line with GB/T 16157 requirements.
6.7 Balance. Accuracy is 0.0001 g.
6.8 Water phase needle filter. 13 mm × 0.22 μm.
6.9 freezer. easy to transfer, good sealing, can maintain the internal temperature below 4 ℃.
6.10 polytetrafluoroethylene hose or silicone rubber tube with PTFE tape.
6.11 General laboratory equipment and equipment.
7 samples
7.1 Collection of samples
Before sampling, the sampler should be airtight and flow calibrated and open the pump at 1.0 L/min.
Minute, replace the air of the sampling system.
7.1.1 Ambient air samples
The sampling of ambient air shall comply with the relevant provisions in HJ/T 194. At the time of sampling, a porous glass of 10.0 ml of experimental water will be used
(6.5), connected with a polytetrafluoroethylene hose or a silicone rubber tube (6.10) with a Teflon film,
(6.3), the ambient air sample was collected at a flow rate of 0.5 L/min for 60 min, and the temperature and atmospheric pressure of the sampling point were recorded
number.
7.1.2 Fixed sources of waste gas samples
The sampling of the waste gas of the fixed pollution source shall comply with the relevant provisions in GB/T 16157. At the time of sampling, 50.0 ml of the experiment will be performed
(6.6), a polytetrafluoroethylene hose or a silicone rubber tube (6.10) coated with a polytetrafluoroethylene film,
Connect to the flue gas sampler (6.4), heat the sampling gun to above 120 ° C, and collect the fixed source of waste at 1.0 L/min
Gas sample 30 min. According to the actual concentration, appropriate to extend or shorten the sampling time, record the sampling temperature and pressure and other parameters.
Note 1. When the temperature of the sampling gas is high, the perforated glass plate (6.6) can be cooled with an ice water bath.
7.1.3 Full program blank samples
Each sampling should be accompanied by at least one full program blank sample. Will be the same batch of 10.0 ml of experimental water filled with porous glass plate suction
(6.6) or the same batch of 50.0 ml of experimental water with a porous glass plate to absorb the bottle (6.6) to the sampling site, open it
Both ends are not connected to the sampler and closed after 1 minute. Follow the same conditions as the sample transport and storage (7.2)
room.
7.2 Transport and storage of samples
After the sample was collected, the porous glass plate was closed with a Teflon hose or a silicone rubber tube (6.10) filled with polytetrafluoroethylene film
Absorbent tube (6.5) or perforated glass plate (6.6) inlet and outlet ports, placed vertically in the freezer (6.9)
save. If not measured in time, the sample should be refrigerated below 4 ℃, dark and sealed to save, 5 d to complete the analysis and determination.
7.3 Preparation of samples
7.3.1 Ambient air samples
The ambient air sample absorption solution (7.1.1 collected by the absorption solution) into the total volume of 10 ml colorimetric tube, the volume of water to 10 ml
Marking, shaking. Filter with a 0.22 μm aqueous syringe filter (6.8) and discard 2 ml of the initial stock and collect the filtrate to 2 ml of brown
Bottle, to be tested.
7.3.2 Fixed sources of waste gas samples
The fixed source of waste gas sample absorption solution (7.1.2 collected by the absorption solution) into the 50 ml colorimetric tube, with water
Capacity to 50 ml mark, shake. Filter with a 0.22 μm aqueous syringe filter (6.8), discard 2 ml of the initial solution and collect the filtrate to 2 ml
Brown vials, to be tested.
7.3.3 Full program blank samples
The whole program blank sample (7.1.3) is prepared in accordance with the preparation of the sample of the ambient air sample (7.3.1) or the fixed source of waste gas
Preparation of sample sample (7.3.2) The same procedure was used to prepare a full program blank sample.
7.3.4 Laboratory blank samples
Instead of the sample with the same volume and the same volume of experimental water, follow the preparation of the sample with the ambient air sample (7.3.1) or
Preparation of fixed source sample sample (7.3.2) The same procedure was used to prepare a laboratory blank sample.
8 Analysis steps
8.1 Liquid Chromatographic Reference Conditions
Column temperature. 30 ° C;
Mobile phase. water. acetonitrile = 97. 3 (v/v);
Detection wavelength. 198 nm;
Auxiliary wavelength. 195nm, 205nm;
Injection volume. 5.0 μl;
Flow rate. 0.5 ml/min.
8.2 Standard curve drawing
Respectively, 0.50 ml, 5.00 ml, 10.00 ml, 20.00 ml, 50.00 ml of amide compounds standard use of liquid (5.7)
Placed in a group of 50 ml volumetric flask, the water volume to the mark, shake, the standard series of the target compound concentration in Table 1. by
Low concentration to high concentration followed by removal of 5.0 μl into the liquid chromatograph, according to the liquid chromatography reference conditions (8.1) for analysis
set. The concentration of the target compound in the standard series solution (mg/L) was the abscissa, with the peak height or peak area as the ordinate,
Standard curve of amide compounds. The standard chromatograms of amide compounds are shown in the liquid chromatographic conditions specified in this standard
figure 1.
Table 1 Amide Compounds Standard Series Concentration
1-carboxamide; 2-acrylamide; 3-N, N-dimethylformamide; 4-N, N-dimethylacetamide
Figure 1 Standard chromatogram of amide compounds
8.3 Determination of samples
Take a 5.0 μl sample (7.3) into a liquid chromatograph according to the same chromatographic conditions (8.1) and steps as the standard curve
(8.2), and the retention time and peak height (or peak area) of the chromatographic peak were recorded. Standard color of amide compounds
The retention time of the spectra was determined by the external standard method, and the amide compound concentration in the samples was quantitatively calculated.
9 Results calculation and representation
9.1 Results calculation
Standard Series Concentration (mg/L)
Serial number
Formamide N, N-dimethylformamide N, N-dimethylacetamide acrylamide
1 0.50 0.25 0.50 0.25
2 5.00 2.50 5.00 2.50
3 10.0 5.00 10.0 5.00
4 20.0 10.0 20.0 10.0
5 50.0 25.0 50.0 25.0
The concentration of amide compounds in ambient air and exhaust gas (mg/m3) is calculated according to equation (1)
SV
CVC 11 × = (1)
Where. C-ambient air or exhaust gas amide compounds concentration, mg/m3;
C1 - the concentration of the resulting amide compound calculated from the standard curve, mg/L;
V1 - Absorbent liquid volume, ml;
Vs - the sampling volume under the standard state (101.325 kPa, 273.2 K), L.
9.2 The result is shown
For ambient air, when the result is less than 1 mg/m3, the remainder is left after the decimal point; when the result is greater than or equal
At 1 mg/m3, three valid digits are retained.
For fixed sources of waste gas, when the determination results less than 10 mg/m3, retained to the decimal point after a; when the determination of the results
When you are greater than or equal to 10 mg/m3, keep three significant digits.
10 precision and accuracy
10.1 Precision
Six laboratories were treated with formamide (0.50 mg/L, 2.0 mg/L and 10 mg/L), N, N-dimethylformamide (0.50
Mg/L, 2.0 mg/L and 10 mg/L), N, N-dimethylacetamide (0.50 mg/L, 2.0 mg/L and 10 mg/L), acryloyl
Amine (0.25 mg/L, 1.0 mg/L and 5.0 mg/L) of the amide compound mixed standard solution with a uniform blank spiked sample
Six times of repeated determination.
The relative standard deviations (RSDs) of formamides were 3.4% ~ 10%, 2.1% ~ 6.7%, 0.7% ~ 4.9%
The relative standard deviations were 3.1%, 2.4% and 3.0%, respectively, and the repeatability limits were 0.04 mg/m3, 0.09 mg/m3, 0.28 mg/m3,
The reproducibility limits were 0.04 mg/m3, 0.10 mg/m3, and 0.39 mg/m3, respectively.
The relative standard deviations (RSDs) of N, N-dimethylformamide were 3.5% ~ 6.5%, 3.3% ~ 5.7%, 3.2% ~ 5.6%
The relative standard deviations were 4.7%, 4.2%, 3.1%, and the reproducibility limits were 0.03 mg/m3, 0.09 mg/m3,
0.39 mg/m3, and the reproducibility limits were 0.04 mg/m3, 0.11 mg/m3 and 0.46 mg/m3, respectively.
The relative standard deviations (RSDs) of N, N-dimethylacetamide were 4.0% ~ 8.1%, 3.5% ~ 6.3%, 3.4% ~ 6.1%
The relative standard deviations were 4.6%, 4.6% and 2.8%, respectively. The repeatability limits were 0.03 mg/m3, 0.10 mg/m3,
0.43 mg/m3, reproducibility limit was 0.04 mg/m3, 0.13 mg/m3, 0.47 mg/m3, respectively.
The relative standard deviations of acrylamide laboratories were 3.6% ~ 10%, 3.3% ~ 7.0%, 2.7% ~ 4.4%, respectively.
The relative standard deviations were 4.3%, 4.1% and 2.5%, respectively, and the repeatability limits were 0.02 mg/m3, 0.05 mg/m3, 0.16
Mg/m3, reproducibility limit of 0.02 mg/m3, 0.06 mg/m3, 0.19 mg/m3, respectively.
10.2 Accuracy
The six laboratories were treated with formamide (labeled titers of 5.0 μg, 50 μg and 250 μg), N, N-dimethylformamide
50 μg and.200 μg), N, N-dimethylacetamide (plus titer of 5.0 μg, 50 μg and.200 μg) and C
(Labeled with a scalar of 2.5 μg, 25 μg and 100 μg) were subjected to 6 replicates.
The recoveries of formamides were 101% ~ 111%, 97.6% ~ 105%, 98.1% ~ 102%, respectively.
Values were 107% ± 6.4%, 102% ± 5.2%, 100% ± 3.2%.
The recoveries of N, N-dimethylformamide were 94.7% ~ 109%, 95.7% ~ 102%, 97.7% ~ 102%
The final recoveries were 103% ± 9.6%, 97.6% ± 4.6% and 100% ± 4.4%, respectively.
The recoveries of N, N-dimethylacetamide were 94.6% ~ 108%, 94.7% ~ 102%, 97.0% ~ 103%
The final recoveries were 104% ± 9.6%, 97.7% ± 6.0% and 99.0% ± 6.0%, respectively.
The recoveries of acrylamide were 94.4% ~ 107%, 97.3% ~ 103%, 98.5% ~ 103%, respectively.
The final values were 103% ± 9.0%, 101% ± 4.6%, 101% ± 5.0%, respectively.
Details of precision and accuracy are given in Appendix A.
11 quality assurance and quality control
11.1 The correlation coefficient of the standard curve should be ≥0.999.
11.2 Blank analysis
Each analysis is done at least one lab blank and one full program blank to check for possible interference, target combinations
The measured value of the object shall not be higher than the detection limit of the method.
11.3 Calibration
11.3.1 Initial calibration
The initial use of the instrument, or in the instrument repair, replacement column or continuous calibration failed, the need to re-draw the standard curve,
Perform initial calibration.
11.3.2 Continuous calibration
For each 20 samples or each batch (less than 20 samples/batch), a continuous calibration of the standard curve
quasi. The relative error of continuous calibration should be ≤ 20%, otherwise you should find the cause, or re-draw the standard curve. According to formula (2)
Calculate the relative error (D) between cC and calibration point iC.
0 × - =
Ic
CCD (2)
Where.
D - cC relative error with calibration point iC,%;
IC - mass concentration of calibration points;
CC - Determines the mass concentration of the calibration point.
12 Waste treatment
All wastes and wastes produced in the experiment (including the tested residue) should be collected and collected in a closed container
Save, paste the obvious logo, commissioned by the qualified unit disposal.
Appendix A
(Informative)
Method of precision and accuracy of the summary table
Six labs were tested for three different concentrations of uniform blank spiked samples. Precision and accuracy summary
According to Schedule A.1 and Schedule A.2.
Schedule A.1 Summary of the precision of the method
Name CAS number
Amide compounds
Standard solution concentration
(Mg/L)
Equivalent to air
The concentration of the sample
(Mg/m3)
Laboratory relative
standard deviation
(%)
Inter-laboratory
Relative standard
deviation
(%)
Repeatability limit
(Mg/m3)
Reproducibility limit
(Mg/m3)
0.50 0.17 3.4 to 10 3.1 0.04 0.04
2.0 0.67 2.1 to 6.7 2.4 0.09 0.10 Formamide 75-12-7
10 3.33 0.7 to 4.9 3.0 0.28 0.39
0.50 0.17 3.5 to 6.5 4.7 0.03 0.04
2.0 0.67 3.3 to 5.7 4.2 0.09 0.11
N, N-dimethyl
Formylamide
68-12-2
10 3.33 3.2 to 5.6 3.1 0.39 0.46
0.50 0.17 4.0 to 8.1 4.6 0.03 0.04
2.0 0.67 3.5 to 6.3 4.6 0.10 0.13
N, N-dimethyl
Based acetamide
127-19-5
10 3.33 3.4 to 6.1 2.8 0.43 0.47
0.25 0.08 3.6 to 10 4.3 0.02 0.02
1.0 0.33 3.3 to 7.0 4.1 0.05 0.06 Acrylamide 79-06-1
5.0 1.67 2.7 ~ 4.4 2.5 0.16 0.19
Schedule A.2 Summary of the accuracy of the method
Name CAS number
Standard substance spiked
Amount (μg)
Equivalent to the concentration of air samples
(Mg/m3)
Spike recovery (%)
The final value of the recoveries
P 2 PS (%)
5.0 0.17 101 to 111 107 ± 6.4
50 1.67 97.6 ~ 105 102 ± 5.2 Formamide 75-12-7
250 8.33 98.1 to 102 100 ± 3.2
5.0 0.17 94.7 to 109 103 ± 9.6
50 1.67 95.7 to 102 97.6 ± 4.6
N, N-dimethyl-methyl
Amide
68-12-2
200 6.67 97.7 to 102 100 ± 4.4
5.0 0.17 94.6 ~ 108 104 ± 9.6
50 1.67 94.7 to 102 97.7 ± 6.0
N, N-Dimethyl B
Amide
127-19-5
200 6.67 97.0 to 103 99.0 ± 6.0
2.5 0.08 94.4 to 107 103 ± 9.0
25 0.83 97.3 ~ 103 101 ± 4.6 Acrylamide 79-06-1
100 3.33 98.5 to 103 101 ± 5.0
Related standard:   HJ 799-2016  HJ 800-2016
Related PDF sample:   HJ 799-2016  HJ 870-2017
   
 
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