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HJ 822-2017: Water quality -- Determination of aniline compounds -- Gas chromatography mass spectrometry
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Water quality -- Determination of aniline compounds -- Gas chromatography mass spectrometry
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HJ 822-2017
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Basic data | Standard ID | HJ 822-2017 (HJ822-2017) | | Description (Translated English) | Water quality -- Determination of aniline compounds -- Gas chromatography mass spectrometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Word Count Estimation | 20,219 | | Date of Issue | 3/30/2017 | | Date of Implementation | 5/1/2017 | | Regulation (derived from) | Ministry of Environment Protection Announcement 2017 [16] | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 822-2017: Water quality -- Determination of aniline compounds -- Gas chromatography mass spectrometry
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Water quality-Determination of aniline compounds - Gas chromatography mass spectrometry
National Environmental Protection Standard of the People 's Republic of China
Determination of Aniline Compounds in Water
Gas chromatography - mass spectrometry
2017-03-30 released
2017-05-01 Implementation
Ministry of Environmental Protection released
Directory
Preface ..ii
1 Scope of application
2 normative reference documents
3 Principle of the method
4 reagents and materials
5 instruments and equipment
6 samples .3
7 Analysis steps
8 results calculated
9 results show
10 precision and accuracy
11 Quality assurance and quality control
12 Waste treatment .9
Appendix A (normative) The quantitation of the target compound, the auxiliary ion, the detection limit of the method, and the lower limit of determination.
Appendix B (informative) method of precision and accuracy
Foreword
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 Water Pollution,
The protection of human health, regulate the determination of aniline compounds in water, the development of this standard.
This standard specifies the gas of 19 kinds of aniline compounds in surface water, groundwater, seawater, domestic sewage and industrial waste water.
Determination of Chromatography - Mass Spectrometry.
This standard is the first release.
Appendix A of this standard is a normative appendix, Appendix B is an informative appendix.
This standard is formulated by the Environmental Monitoring Division of the Ministry of Environmental Protection and the Standards Division of Science and Technology.
The main drafting of this standard. Shanghai Pudong New Area Environmental Monitoring Station.
The standard verification unit. Shanghai Environmental Monitoring Center, Suzhou City Environmental Monitoring Center Station, Shanghai Entry-Exit Inspection and Quarantine
Bureau, Shanghai Chemical Environmental Protection Monitoring Station, Shanghai Jiading District Center for Disease Control and Prevention.
The environmental protection department of this standard approved on March 30,.2017.
This standard has been implemented since May 1,.2017.
This standard is explained by the Ministry of Environmental Protection.
Water quality - Determination of aniline compounds - Gas chromatography - mass spectrometry
Warning. Dichloromethane, aniline compounds and other reagents and solutions are volatile or semi-volatile toxic substances, the solution
Preparation should be carried out in the fume hood, the operation should be required to wear protective equipment, to avoid inhalation or contact with skin and clothing.
1 Scope of application
This standard specifies the determination of 19 aniline compounds in water by gas chromatography-mass spectrometry.
This standard is applicable to the determination of aniline compounds in surface water, groundwater, seawater, domestic sewage and industrial waste water.
19 aniline compounds include aniline, 2-chloroaniline, 3-chloroaniline, 4-chloroaniline, 4-bromoaniline, 2-nitroaniline,
2,4,6-trichloroaniline, 3,4-dichloroaniline, 3-nitroaniline, 2,4,5-trichloroaniline, 4-chloro-2-nitroaniline, 4-
Nitroaniline, 2-chloro-4-nitroaniline, 2,6-dichloro-4-nitroaniline, 2-bromo-6-chloro-4-nitroaniline, 2-chloro-
Nitroaniline, 2,6-dibromo-4-nitroaniline, 2,4-dinitroaniline, 2-bromo-4,6-dinitroaniline. After verification,
Other methods can also be used for other aniline compounds.
When the sampling volume is 1000ml and the concentrated volume is 1.0ml, the detection limit is 0.05μg/L ~ 0.09μg/L,
Limited to 0.20μg/L ~ 0.36μg/L, see Appendix A.
2 normative reference documents
The contents of this standard refer to the following documents or their terms. For undated references, the valid version is applicable
In this standard.
Specification for ocean monitoring
Technical specification for surface water and wastewater monitoring
Technical specification for groundwater environmental monitoring
3 Principle of the method
The aniline compounds in the water sample were extracted with dichloromethane under the condition of pH≥11. The extract was dehydrated, concentrated and purified,
Measured by gas chromatography/mass spectrometry. Depending on the retention time of the target compound and the standard mass spectrum or characteristic ion characterization,
Quantitative method.
4 reagents and materials
Unless otherwise stated, analytical analytical reagents and distilled water in accordance with national standards are used for analysis.
4.1 dichloromethane (CH2Cl2). pesticide residues.
4.2 isopropyl alcohol (C3H8O). pesticide residues.
4.3 n-Hexane (C6H14). Pesticide level.
4.4 Methanol (CH3OH). Pesticide level.
4.5 Sodium thiosulfate (Na2S2O3).
4.6 sodium chloride (NaCl). 400 ℃ baking 4h, slightly cold after the sealed glass bottle, cold to room temperature stand-by.
4.7 anhydrous sodium sulfate (Na2SO4). 400 ℃ baking 4h, slightly cold after the sealed glass bottle, cold to room temperature stand-by.
4.8 Sodium hydroxide solution. c (NaOH) = 10 mol/L.
Take 40 g of sodium hydroxide in a small amount of water and dilute to 100 ml.
4.9 Sulfuric acid solution. 1 1.
4.10 aniline compounds standard stock solution. ρ = 1000μg/ml, containing 19 kinds of target compounds.
4.11 Substitutes (aniline-d5) Standard stock solution. ρ =.2000 μg/ml.
4.12 internal standard (1,2-dichlorobenzene-d4, phenanthrene-d10) stock solution. ρ =.2000μg/ml.
4.13 aniline compounds standard intermediate. ρ = 100μg/ml.
Take 1.00 ml of aniline compound standard stock solution (4.10) into a 10 ml volumetric flask and use methylene chloride (4.1)
The volume is transferred to the reagent bottle (5.9) of the attached polytetrafluoroethylene spin cover.
4.14 Substituted (aniline-d5) Intermediate. ρ = 100 μg/ml.
Absorb 0.50 ml of the standard stock solution (4.11) to 10 ml volumetric flask, with methylene chloride (4.1) volume,
Transfer to the reagent bottle (5.9) of the attached polytetrafluoroethylene spin cover.
4.15 Internal standard 1 (1,2-dichlorobenzene-d4) Intermediate. ρ = 400μg/ml.
Take 2.0ml of 1,2-dichlorobenzene-d4 stock solution (4.12) into a 10ml volumetric flask, mix with methylene chloride (4.1)
Transfer to the reagent bottle (5.9) of the attached polytetrafluoroethylene spin cover.
4.16 Internal standard 2 (phenanthrene-d10) Intermediate. ρ = 40 μg/ml.
Take.200 μl of phenanthrene-d10 stock solution (4.12) into a 10 ml volumetric flask and equilibrate with dichloromethane (4.1)
Attached to the reagent bottle (5.9) of the attached tetrafluoroethylene rotary cover.
4.17 aniline compounds standard use of liquid (including substitutes). ρ = 10.0μg/ml.
Respectively, 1.00 ml of aniline compounds standard intermediate (4.13) and 1.00 ml of the intermediate (4.14)
To a 10 ml volumetric flask, transferred to methylene chloride (4.1), transferred to an agglutinated tetrafluoroethylene rotary cap reagent bottle (5.9)
In the preservation.
4.18 internal standard liquid. internal standard 1. ρ = 80.0μg/ml, internal standard 2. ρ = 4.0μg/ml.
(4.15) and 1.0 ml internal standard 2 intermediate liquid (4.16) to 10 ml volumetric flask, respectively,
With methylene chloride (4.1) constant volume, mix.
4.19 Substitute for the use of liquid. ρ = 10 .0μg/ml.
Take the 1.00 ml of the standard standard intermediate (4.14) to 10 ml volumetric flask and mix with methylene chloride (4.1)
Transferred to the reagent bottle (5.9) of the attached polytetrafluoroethylene rotary cap.
4.20 decafluorotriphenylphosphine (DFTPP) solution. ρ = 1000 μg/ml.
4.21 decafluorotriphenylphosphine (DFTPP) using the liquid. ρ = 5.0μg/ml.
50 μl of decafluorotriphenylphosphine (DFTPP) solution (4.20) was added to a 10 ml volumetric flask and treated with dichloromethane (4.1)
The volume is transferred to the reagent bottle (5.9) of the attached polytetrafluoroethylene spin cover.
4.22 helium. purity ≥99.999%.
5 instruments and equipment
5.1 Gas Chromatography/Mass Spectrometer. EI source with split/splitless inlet, scanning range of at least 35 ~ 500amu.
5.2 Column. column length 30m, inner diameter 0.32mm or 0.25mm, liquid film thickness 0.25μm 5% diphenyl-95% dimethyl
Polysiloxane quartz capillary column or a similar performance column.
5.3 Concentrator and supporting concentrator.
5.4 solid phase extraction device. through the vacuum pump to adjust the flow rate, flow rate range of 1 ~ 20ml/min.
5.5 Florisil column. 1000 mg/6 ml, commercially available. You can also buy diatomaceous earth made of silica column, but must pass
Experimental verification, to meet the characteristics of the method requirements.
5.6 microinjector. 10 μl, 50 μl, 100 μl, 1000 μl.
5.7 separatory funnel. 1L or 2L, with tetrafluoroethylene plug.
5.8 capacity bottle. A grade, 10ml, 25ml.
5.9 Reagent Bottle. 50ml, attached Teflon Rotary Cover.
5.10 Vial. 1000ml brown glass bottle with PTFE inner liner.
5.11 General laboratory equipment and equipment commonly used.
6 samples
6.1 Collection of samples
According to GB 17378, HJ/T 91, HJ/T 164 of the relevant provisions of the water sample collection. Samples were collected in vials
(5.10), the water sample is filled with vials, leaving no gaps.
6.2 Storage of samples
Samples were collected immediately after the addition of sodium hydroxide (4.8) or sulfuric acid solution (4.9), adjust the pH value in the 6 ~ 8,4 ℃
save. If there is residual chlorine in the water sample, add 80 mg of sodium thiosulfate (4.5) to each 1000ml sample. Samples must be collected
After extraction within 7 days, the extract was analyzed within 40 days.
6.3 Preparation of the sample
6.3.1 Extraction
Accurately measure 1000 ml of water in a separatory funnel (5.7), add 30 g of sodium chloride (4.6), gently shake to chlorine
Sodium chloride solution, sodium hydroxide solution (4.8) to adjust the pH value greater than 11, add 100.0 μl of the substitute using the liquid (4.19),
Mixed with 60ml of dichloromethane (4.1), shake extraction for 10min, standing for 5min, two-phase stratification, collecting organic
Phase to the Erlenmeyer flask. Water phase continued to add 60ml dichloromethane (4.1), repeated extraction 2 times, the organic phase combined to the triangular burning
Bottle.
Note 1. the extraction process occurs when the emulsification phenomenon, can be used to stir, ultrasonic and other methods to break the milk. Ultrasonic conditions. power 250W, water temperature 25 ℃,
Ultrasonic extraction time 10min (emulsification serious, can continue to ultrasonic extraction 10min).
6.3.2 Dehydration
Triangle funnel by adding appropriate (greater than 3g) of anhydrous sodium sulfate (4.7), the entire organic phase over anhydrous sodium sulfate dry
Dry, standing until the organic extract is completely filtered into the concentrated tube. Heat the sample at about 35 ° C in a water bath and blow the sample with high purity nitrogen
Concentrated to 1ml.
6.3.3 Purification
The Florisil silica column (5.5) was fixed on a solid phase extraction (5.4) with 10 ml of n-hexane (4.3)
The column was equilibrated and the concentrated sample extract was transferred to a column before the solvent was dried, washed with 3 to 4 ml of n-hexane
(50/50, v/v) eluting the column with 50 ml of dichloromethane/n-hexane (50/50, v/v)
The eluent was eluted with 50 ml of isopropanol/n-hexane (5/95, v/v) and the eluate 2 was collected. Finally,
50 ml of methanol/n-hexane (5/95, v/v) for the third elution column.
Note 2. The elution rate should be controlled at about 5 ml/min; for more clean surface water, groundwater, seawater, domestic sewage, and
Background interference Low industrial waste water can omit the purification steps.
6.3.4 constant capacity
The eluate was concentrated to 0.5 to 1.0 ml, 20.0 μl of the internal standard was added to the solution (4.18), washed with dichloromethane (4.1)
To 1.0ml, mix, into the automatic sampling vial, to be measured.
6.4 blank sample preparation
Take 1L reagent water instead of water sample, according to the steps of 6.3 prepared into a blank sample.
7 Analysis steps
7.1 Instrument reference conditions
7.1.1 Gas Chromatographic Reference Conditions
Inlet temperature. 260 ℃; injection method. no split injection; injection volume of 1.0μl.
Process temperature. 40 ° C (5 min) - 5 ° C/m --in - 100 ° C - 1 ° 0 ° C/- min -.200 ° C (8 min) - 3 - 0 ° C/m -
Carrier gas. helium (4.22), flow rate. 1.00ml/min.
The total ion chromatogram of the target compound is shown in Fig.
1, aniline-d5 2, aniline 3,1,2-dichlorobenzene-d4 4,2-chloroaniline 5,3-chloroaniline 6,4-chloroaniline 7,4-bromoaniline
8,2-nitroaniline 9,2,4,6-trichloroaniline 10,3,4-dichloroaniline 11,3-nitroaniline 12,2,4,5-trichloroaniline
13,4-chloro-2-nitroaniline 14,4-nitroaniline 15,2-chloro-4-nitroaniline 16,2,6-Dichloro-4-nitroaniline 17, phenanthrene-d10
18,2-bromo-6-chloro-4-nitroaniline 19,2-chloro-4,6-dinitroaniline 20,2,6-dibromo-4-nitroaniline 21,2,4-bis Nitro
Aniline 22,2-bromo-4,6-dinitroaniline
Figure 1 Total ion chromatogram of the target compound
7.1.2 Mass Spectral Reference Conditions
Ion source. EI source; ion source temperature. 230 ° C; ionization energy. 70 eV. Scan mode. full scan; scan mode
Wai. m/z 35 ~ 500amu; scan time. 1s/scan. Interface temperature. 260 ℃. The remaining parameters refer to the instrument instructions
Book to set.
7.2 Calibration
7.2.1 Instrument performance check
Before the day of analysis, the GC/MS system must perform instrument performance checks. Use DFTPP to use liquid (4.21) for injection, GC/MS
analysis. The critical ion abundance of DFTPP obtained by GC/MS system should meet the criteria specified in Table 1. Otherwise,
Instrument some parameters to adjust or clean the ion source.
Table 1 DFTPP Critical Ion Abundance Standard
Mass number ion abundance standard mass number ion abundance standard
51 198 30% to 60% of mass.199 198 5% to 9% of mass
68 is less than 69% of mass 2% 275 198% of mass 10% to 30%
70 Less than 69 Mass 2% 365 More than 198 Mass 1%
127 198% of the mass number of 40% to 60% 441 appear, but less than 443 mass abundance
197 Less than 198 Mass 1% 442 Greater than 198 Mass 40%
198 base, the relative abundance of 100% 443 442 mass of 17% to 23%
7.2.2 Drawing of calibration curves
(4.17) 50.0 μl, 100 μl,.200 μl, 300 μl, 500 μl, 5 μl
The flask was charged with 20.0 μl of internal standard (4.18), and the volume was adjusted to 1.0 ml with methylene chloride. Preparation of aniline compounds
And the concentration of the substitutes were 0.50μg/ml, 1.00μg/ml, 2.00μg/ml, 3.00μg/ml, 5.00μg/ml,
Concentration of 1.60μg/ml, internal standard 2 concentration of 0.08μg/ml calibration curve.
According to the instrument reference conditions (7.1), from low to high concentration in accordance with the determination of the concentration of each target compound and
Chromatographic peak area or peak height to draw the calibration curve. The linear range of this method is 0 ~ 5.00μg/ml, which can be used in the pretreatment of the sample
To appropriately reduce or increase the sample size so that the concentration of the concentrated sample is near the middle of the linear range in order to be quantified.
7.3 Sample determination
Take the test sample (6.3) and measure it according to the instrument reference condition (7.1).
7.4 Determination of blank sample
In the analysis of the sample at the same time, should do blank test. Take 1.0 μl of the blank sample (6.4) into the gas chromatograph and press
The same procedure as 7.3 was used for analysis.
8 results calculated
8.1 Qualitative analysis
Depending on the retention time of the target compound and the mass spectrum of the sample after subtracting the background from the mass spectrum in the standard mass spectrum
More sure.
8.2 Quantitative analysis
According to the quantitative ion peak area or peak height, with the internal standard method. When the target compound quantifies the amount of ions in the sample,
Allows the use of auxiliary ion quantification. Quantitative ions, auxiliary ions see Appendix A.
8.2.1 Quantification with the average response factor
8.2.1.1 When the target compound is quantified with the average response factor, the mass concentration ρx of the target compound in the sample is expressed by equation (1)
Line calculation.
Where. ρx - mass concentration of the target compound in the sample, μg/L;
X A - the target compound quantifies the ion response value;
Is A - the response value of the quantified ion of the internal standard substance corresponding to the target compound;
Ρis - mass concentration of internal standard substance, μg/ml;
I RF - the average response of the target compound;
Vex - the volume of the sample extract, ml;
V0 - sample volume of water sample, L;
DF - dilution factor.
8.2.1.2 Calculation method of average response factor
The response factor (RFi) of the target compound in the standard series i is calculated according to equation (2).
Where. RFi - response factor for the target compound at point i in the standard series;
The quantification of the ion response value of the target compound in the standard series;
AIsi - the standard series of i point with the target compound corresponding to the internal standard quantitative ion response value;
ΡIsi - the mass concentration of the internal standard in the standard series, μg/ml;
Ρi - the mass concentration of the target compound in the standard series, μg/ml.
The average response factor i RF of the target compound is calculated according to equation (3).
Where i RF - the average response of the target compound;
I RF - Response factor for the target compound at point i in the standard series;
N - standard series points.
8.2.2 Quantify with calibration curve
When the target compound is quantified by a linear calibration curve, the target compound mass concentration ρx is determined by the corresponding calibration curve
Process to calculate.
9 results show
When the sample content is less than 1.00μg/L, the results remain the second after the decimal point; when the sample content is greater than or equal to 1.00
Μg/L, the result retains three significant digits.
10 precision and accuracy
10.1 Precision
In the six laboratories, the samples were collected at the concentration of 0.30μg/L, 2.50μg/L and 4.50μg/L respectively.
The relative standard deviations in the laboratory were 0.70% ~ 24%, 0.29% -16%, 0.30% ~ 14%, respectively. The laboratory
The relative standard deviations were 3.0% ~ 23%, 2.7% ~ 18%, 2.0% ~ 28%, respectively. The repeatability limits were 0.01μg/L ~
0.10μg/L, 0.04μg/L ~ 0.61μg/L, 0.05μg/L ~ 0.64μg/L, the reproducibility limit was 0.03μg/L ~ 0.23μg/L,
0.18μg/L ~ 1.02μg/L, 0.29μg/L ~ 3.29μg/L.
10.2 Accuracy
Six laboratories carried out the actual samples (including surface water, domestic sewage and two industrial wastewater) and the actual sample
analysis. The standard concentration is. surface water 1.0μg/L, domestic sewage 0.5μg/L, industrial wastewater 0.5μg/L. Spike recovery rate
Do not for the surface water 64% ~ 79%; domestic sewage 45% ~ 105%; industrial wastewater 1. 47% ~ 94%; industrial wastewater 2. 52%
(54 ± 16)% (79 ± 12)%; (45 ± 18)% ~ (105 ± 36)%, respectively (47 ± 12)%
(94 ± 46)%; (52 ± 28)% ~ (97 ± 22)%.
Details of precision and accuracy are given in Appendix B.
11 quality assurance and quality control
11.1 Instrument performance check
Each batch of samples before or every 24 hours, the need for instrument performance checks, get DFTPP spectrum ion abundance must
Shall meet all the standards of Table 1.
11.2 Initial calibration
Calibration curve at least 5 concentration series, the majority of the target compound response factor RSD should be less than or equal to 20%, table
A.1 The last four target compounds (2-chloro-4,6-dinitroaniline, 2,6-dibromo-4-nitroaniline, 2,4-dinitrobenzene
Amine, 2-bromo-4,6-dinitroaniline) should be less than or equal to 30%; the correlation coefficient is greater than or equal to 0.990,
Find the cause or re-establish the calibration curve.
Note. Generally in the instrument maintenance, column or continuous calibration failure when the need for initial calibration, routine measurement, can be used to continuously calibrate
method.
11.3 Continuous calibration
Every 12 hours to analyze the calibration curve at the middle of the concentration point, the measured results and the actual concentration value of the relative deviation should be less than
At 20%, otherwise you should find the cause or re-establish the calibration curve.
11.4 internal standard
Continuous calibration, the internal standard and calibration curve of the middle point of the retention time changes of not more than 10s, quantitative ion peak area changes
Between -50% and 100%.
11.5 Recovery of substitutes
All samples and blanks need to be added substitutes, according to the same steps with the sample analysis, the recovery rate of substitutes 50% ~
150%.
Standard sample
Quality control of the accuracy of the analytical results was carried out using a certified standard sample.
11.7 samples
11.7.1 Each analysis of a batch of samples has at least one reagent blank and blank spikes. The recoveries of the target compounds in the blank spiked
50% to 150%.
11.7.2 Each sample must be 10% parallel to each sample, less than 5 samples, 100% parallel,
Relative deviation of less than 20%.
11.7.3 Each sample of a sample must be labeled with no more than 5% of the sample size, and the target compound
Yield of surface water in 50% to 150%; sewage and wastewater in 40% to 150%.
12 Waste treatment
All waste and waste (including the treated residue) produced during the course of the test shall be collected in a closed container and
Custody, mark, paste the label, commissioned by qualified units to deal with.
Appendix A
(Normative appendix)
The quantification of the target compound, the auxiliary ion, the detection limit of the method, and the lower limit of the assay
Table A.1 shows the quantification of the target compound, internal standard and substitutes in the order of the peak, the auxiliary ions, the method of detection
Limit and lower limit.
Table A.1 Retention Time, Quantum Ion, Auxiliary Ion, Method Detection Limit and Lower Limit of Aniline Compounds
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