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HJ 959-2018 English PDF

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HJ 959-2018: Water quality-Determination of tetraethyl lead - Headspace/gas chromatography-mass spectrometry
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Standard ID	Contents [version]	USD	STEP2	[PDF] delivered in	Standard Title (Description)	Status	PDF
HJ 959-2018	English	269	Add to Cart	3 days [Need to translate]	Water quality-Determination of tetraethyl lead - Headspace/gas chromatography-mass spectrometry	Valid	HJ 959-2018

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Basic data

Standard ID	HJ 959-2018 (HJ959-2018)
Description (Translated English)	Water quality-Determination of tetraethyl lead - Headspace/gas chromatography-mass spectrometry
Sector / Industry	Environmental Protection Industry Standard
Classification of Chinese Standard	Z16
Word Count Estimation	11,197
Date of Issue	2018-07-29
Date of Implementation	2019-01-01
Regulation (derived from)	Ministry of Ecology and Environment Announcement No. 23 of 2018
Issuing agency(ies)	Ministry of Ecology and Environment

HJ 959-2018: Water quality-Determination of tetraethyl lead - Headspace/gas chromatography-mass spectrometry

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Water quality-Determination of tetraethyl lead - Headspace/gas chromatography-mass spectrometry National Environmental Protection Standard of the People's Republic Determination of tetraethyl lead in water quality Headspace/gas chromatography-mass spectrometry Water quality-Determination of tetraethyl lead -Headspace/gas chromatography-mass spectrometry Published on.2018-07-29 2019-01-01 Implementation Ministry of Ecology and Environment released i directory 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 samples..2 7 Analysis step 2 8 Results calculation and representation 4 9 Precision and accuracy 5 10 Quality Assurance and Quality Control..6 11 Waste treatment.7

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 Water Pollution Prevention and Control, to protect the environment, This standard is formulated to ensure human health and to regulate the determination method of tetraethyl lead in water. This standard specifies the headspace/gas chromatography for the determination of tetraethyl lead in surface water, groundwater, domestic sewage and industrial wastewater. Mass spectrometry. This standard is the first release. This standard is formulated by the Environmental Monitoring Department and the Science and Technology Standards Department. This standard was drafted. China Environmental Monitoring Station, Luoyang City Environmental Monitoring Station. The standard verification unit. Beijing Environmental Protection Monitoring Center, Tianjin Environmental Monitoring Center, Jiangsu Province Environmental Monitoring Heart, Zhejiang Environmental Monitoring Center, Guangxi Zhuang Autonomous Region Environmental Monitoring Center Station, Ningbo Environmental Monitoring Center and Xuzhou City Environmental Monitoring Center Station. This standard is approved by the Ministry of Ecology and Environment on July 29,.2018. This standard has been implemented since January 1,.2019. This standard is explained by the Ministry of Ecology and Environment. 1 Determination of tetraethyl lead in water quality by headspace/gas chromatography-mass spectrometry Warning. The reagents and standard solutions used in this method are volatile toxic compounds. The preparation process should be in the fume hood. In the middle; protective equipment should be worn as required to avoid contact with skin and clothing.

1 Scope of application

This standard specifies the headspace/gas chromatography-mass spectrometry for the determination of tetraethyl lead in water. This standard applies to the determination of tetraethyl lead in surface water, groundwater, domestic sewage and industrial wastewater. When the water sample volume is 10.0 ml and the headspace injection volume is 1.0 ml, the detection limit of tetraethyl lead is 0.02 μg/L. The lower limit of determination is 0.08 μg/L.

2 Normative references

This standard refers to the following documents or their terms. For undated references, the valid version applies to this standard. HJ/T 91 Surface Water and Wastewater Monitoring Technical Specifications HJ/T 164 Technical Specifications for Groundwater Environmental Monitoring

3 Principle of the method

Under certain temperature conditions, the tetraethyl lead in the water sample in the headspace bottle volatilizes into the liquid space and reaches the heat in the gas-liquid two phase. After the mechanical dynamic equilibrium, the tetraethyl lead in the gas phase was separated by gas chromatography and detected by a mass spectrometer. Pass and standard The material retention time was compared with the relative abundance of key ions, and the internal standard method was used for quantification.

4 reagents and materials

Analytically pure reagents in accordance with national standards were used for analysis, unless otherwise stated. Pure water. 4.1 Methanol (CH3OH). chromatographically pure. 4.2 Tetraethyl lead ((CH3CH2)4Pb) standard stock solution. ρ =.200 mg/L, the solvent is methanol. Commercially available certified standard solutions are stored in accordance with the instructions. 4.3 Tetraethyl lead standard use solution I. ρ = 2.00 mg/L. Prepare with tetraethyl lead standard stock solution (4.2) diluted with methanol (4.1) and transfer to a spiral bottle with Teflon liner In the brown reagent bottle, it can be stored in 0~4C for one month after being stored in the dark. 4.4 Tetraethyl lead standard use solution II. ρ = 0.20 mg/L. Prepared by diluting tetraethyl lead intermediate solution (4.3) with methanol (4.1) and transferring to a screw cap with a Teflon liner. Store in brown reagent bottles at 0~4C for one month. 4.5 Internal standard stock solution. ρ=2000 mg/L, the solvent is methanol. 2 1,2-dichlorobenzene-d4 should be selected as the internal standard, and the commercially available certified standard solution can be directly purchased. 4.6 Internal standard use solution. ρ=2.00 mg/L. Prepare by diluting the internal standard stock solution (4.5) with methanol (4.1). 4.7 Helium, purity ≥ 99.999%.

5 Instruments and equipment

5.1 Gas Chromatography-Mass Spectrometer. The chromatographic section has a split/splitless inlet for temperature programming. Mass spectrometry with electron bombardment (EI) ionization source with manual/automatic tuning, data acquisition, quantitative analysis and library search. 5.2 Automatic Headspace Sampler. The temperature control range is adjustable from room temperature to 100 °C. 5.3 Column. quartz capillary column, 30 m × 0.25 mm, film thickness 0.25  m, stationary phase 5% phenyl 95% A Polysiloxane; or other equivalent capillary column. 5.4 Sampling bottle. 40 ml brown screw glass bottle, silicone rubber pad lined with PTFE, or other similar Sampling bottle. 5.5 Headspace vial. 22 ml screw or jaw headspace bottle with Teflon silicone rubber gasket. 5.6 Microinjectors. 5 μl, 10 μl, 50 μl, 100 μl and 250 μl. 5.7 Common instruments and equipment used in general laboratories.

6 samples

6.1 Sample Collection Add 800 μl of methanol (4.1) preservative to the 40 ml vial (add.200 μl of methanol per 10 ml of water (4.1) Preservative), then collect samples according to the relevant regulations for volatile organic compounds in HJ/T 91 and HJ/T 164, and follow the samples along the bottle The wall is slowly introduced into the sampling bottle (5.4) until the full bottle is used. The tetraethyl lead escape due to agitation should be minimized and avoided. Air bubbles are introduced into the sampling bottle. On-site collection of parallel double samples, one for laboratory measurements, one for backup. 6.2 Sample storage After the sample is collected, it is stored in the dark at around 4 °C, and sent to the laboratory as soon as possible. The analysis is completed within 24 hours. Note. Tetraethyl lead in water is unstable, easy to decompose, difficult to store, and should be analyzed as soon as possible.

7 Analysis steps

7.1 Instrument Reference Conditions 7.1.1 Headspace Autosampler Heating equilibrium temperature. 60  C; heating equilibrium time. 10 min; shaking; injection amount. 1.0 ml. 7.1.2 Gas Chromatography Inlet temperature. 250 C; carrier gas. helium (4.7); injection mode. split injection (split ratio 5.1); column flow (constant current mode). 1.0 ml/min; 3 heating program. 40  C (for 1 min) 15 C/min ..200 C (for 1 min). 7.1.3 Mass spectrometry Ion source. EI source; ion source temperature. 230  C; ionization energy. 70 eV; interface temperature. 280  C; quadrupole Temperature. 150  C; scanning method. Select ion scanning (SIM). Target scanning ions. 208, 237, 295; quantitative ions. 237. Internal standard scanning ions. 150, 152, 78; quantitative ions. 150. Note. For more deterministic, high-concentration samples are available in full scan mode. 7.2 Establishment of the working curve 7.2.1 Instrument performance check Before the sample is analyzed, it should be tuned and inspected according to the calibration compounds and procedures specified in the instrument manual. If it does not meet the requirements, The parameters of the mass spectrometer need to be adjusted or the ion source cleaned. 7.2.2 Establishment of the working curve In 5 headspace bottles (5.5) containing 10 ml of experimental water, rapidly add.200 μl of methanol (4.1), respectively. Seal the cap and inject 5.0 μl of the standard solution into the headspace bottle (5.5) with a micro syringe (5.6) from the septum. II (4.4), 2.5 μl, 5.0 μl, 10.0 μl, 25.0 μl of standard use solution I (4.3) at a concentration of 0.10 μg/L, 0.50 μg/L, Standard series of 1.00 μg/L, 2.00 μg/L, 5.00 μg/L, then add 10.0 μl to the septum with a micro syringe (5.6) Internal standard (4.6). Then according to the instrument reference conditions (7.1), measure from low concentration to high concentration, record the calibration series. The retention time of the target compound, the internal standard, and the response value of the quantitative ion. Note 1. In order to avoid the influence of the amount of methanol added on the analysis results, attention should be paid to the standard use solution when preparing the calibration curve or performing the matrix spike analysis. The volume should not exceed 50 μl. Note 2. The appropriate working curve concentration range can be selected according to the concentration level of the target in the sample. The total ion chromatogram of tetraethyl lead is shown in Figure 1 under the chromatographic conditions specified in this standard. 1- 1,2-dichlorobenzene-d4 (internal standard); 2-tetraethyl lead Figure 1 Total ion chromatogram of tetraethyl lead Taking the ratio of the concentration of tetraethyl lead to the concentration of the internal standard compound as the abscissa, quantifying the ion response value with tetraethyl lead The ratio of the quantitative ion response value of the standard compound is the ordinate, and the working curve is established; the average relative response factor method can also be used. Line calculation. The relative correction factor (iRRF) of the tetraethyl lead at the i-th point in the calibration series is calculated according to formula (1). IS IS RRF   (1) Where. iRRF -- the relative correction factor for point i in the calibration series; iA - the response value of the tetraethyl lead quantitative ion at the i-th point in the calibration series; iIS A -- the response value of the quantitation ion of the internal standard at the i-th point in the calibration series; IS - mass concentration of internal standard, μg/L; I -- The mass concentration of tetraethyl lead at the i-th point in the calibration series, μg/L. The average relative response factor RRF of tetraethyl lead is calculated according to formula (2). RRF RRF I  1 (2) Where. RRF - the average relative response factor of tetraethyl lead; iRRF - the relative response factor of the tetraethyl lead at the i-th point in the calibration series; n -- Calibrate the series of points. The relative standard deviation of RRF is calculated according to formula (3). 0 RRF SD RSD (3) Where. SD -- standard deviation of iRRF. 7.3 Specimen determination Take 10.0 ml of water in the headspace bottle (5.5), immediately seal the headspace bottle, and add 10.0 μl with a micro-syringe (5.6) Internal standard (4.6). The measurement was carried out according to the instrument reference conditions (7.1). Note. After the sample is analyzed, if there is a need for retesting, an unopened spare sample should be used. 7.4 Blank test Take 10.0 ml of experimental water in a headspace vial (5.5) and quickly add.200 μl of methanol (4.1) according to step (7.3) and The instrument is determined by reference conditions (7.1).

8 Calculation and representation of results

8.1 Qualitative analysis According to the retention time of tetraethyl lead, the relative abundance of key ions of the sample and the relative abundance of key ions of the working curve Qualitative. The calibration solution was analyzed several times to obtain the mean retention time of tetraethyl lead, with a standard deviation of ±3 times of the average retention time. 5 Retain the time window, the retention time of the target in the sample should be within its range. The relative abundance deviation of characteristic ions in the sample mass spectrum and the standard mass spectrum should be within ±30%. 8.2 Quantitative analysis 8.2.1 Calibration curve method The mass concentration of tetraethyl lead is directly obtained from the calibration curve, and the concentration of tetraethyl lead in the sample x is performed according to formula (4). Calculation. Fx  1 (4) Where. x - the mass concentration of tetraethyl lead in the sample, μg/L; 1 - concentration of tetraethyl lead obtained from the calibration curve, μg/L; f -- sample dilution factor. 8.2.2 Average relative response factor method When calculated by the average relative response factor method, the mass concentration of tetraethyl lead in the sample x  is calculated according to formula (5). RRFA fA IS ISx x    (5) Where. x - the mass concentration of tetraethyl lead in the sample, μg/L; xA - the response of tetraethyl lead quantitative ions; ISA - internal standard quantitation ion response value; IS - mass concentration of internal standard, μg/L; RRF - the average relative response factor of tetraethyl lead; f -- sample dilution factor. 8.3 result representation When the measurement result is < 1 μg/L, it is retained to 2 decimal places; when the measurement result is ≥1 μg/L, 3 bits are retained. Effective figures.

9 Precision and accuracy

9.1 precision 7 validation laboratories performed 6 samples of pure water with spiked concentrations of 0.10 μg/L, 1.00 μg/L, and 5.00 μg/L, respectively. For the repeated measurements, the relative standard deviations in the laboratory were. 4.5% to 7.8%, 3.1% to 8.3%, and 1.8% to 8.7%. experiment The relative standard deviations between the chambers were 7.3%, 8.0%, and 4.3%, respectively; the repeatability limits were 0.02 μg/L, 0.17 μg/L, and 0.71, respectively. Μg/L; reproducibility limits were 0.03 μg/L, 0.27 μg/L, and 0.89 μg/L, respectively. Seven replicates were performed on 7 surface water samples spiked at concentrations of 0.10 μg/L and 1.00 μg/L, respectively. The relative standard deviations in the experimental room were. 2.0%~13% and 1.5%~8.2%, respectively. The relative standard deviation between laboratories is 11% And 11%; the repeatability limits were 0.02 μg/L and 0.19 μg/L, respectively; the reproducibility limits were 0.04 μg/L and 0.35 μg/L, respectively. Seven replicates were performed on groundwater samples spiked at concentrations of 0.10 μg/L and 1.00 μg/L, respectively. 6 The relative standard deviations in the laboratory were. 2.6%~10% and 2.1%~11%, respectively. The relative standard deviation between laboratories is 13% And 8.5%; the repeatability limits were 0.02 μg/L and 0.18 μg/L, respectively; the reproducibility limits were 0.04 μg/L and 0.29 μg/L, respectively. 7 laboratories performed 6 samples of domestic sewage with concentration of 0.10 μg/L, 1.00 μg/L and 5.00 μg/L, respectively. For the repeated measurements, the relative standard deviations in the laboratory were. 3.5% to 11%, 3.7% to 16%, and 1.7% to 6.9%. laboratory The relative standard deviations were 3.0%, 8.6%, and 6.9%, respectively; the repeatability limits were 0.02 μg/L, 0.24 μg/L, and 0.55 μg/L, respectively; Reproducibility limits were 0.02 μg/L, 0.32 μg/L, and 1.1 μg/L, respectively. 7 laboratories carried out industrial wastewater samples with spiked concentrations of 0.10 μg/L, 1.00 μg/L and 5.00 μg/L, respectively. For the repeated measurements, the relative standard deviations in the laboratory were. 4.7% to 11%, 4.3% to 11%, and 2.1% to 6.1%, respectively. laboratory The relative standard deviations were 12%, 10%, and 8.4%, respectively; the repeatability limits were 0.02 μg/L, 0.19 μg/L, and 0.55 μg/L, respectively; The reproducibility limits were 0.04 μg/L, 0.32 μg/L, and 1.2 μg/L, respectively. 9.2 Accuracy Seven replicates were performed on 7 surface water samples spiked at concentrations of 0.10 μg/L and 1.00 μg/L, respectively. The average spike recovery rates ranged from 84.0% to 117% and 81.3% to 115%, respectively. The final values of the spiked recovery were 97.6% ± 22% and 98.7% ± 22%. Seven replicates were performed on groundwater samples spiked at concentrations of 0.10 μg/L and 1.00 μg/L, respectively. The average spike recovery rates ranged from 83.0% to 120% and 86.1% to 112%, respectively. The final values of the spiked recovery were 94.8% ± 26% and 99.0% ± 8.4%. 7 laboratories performed 6 samples of domestic sewage with concentration of 0.10 μg/L, 1.00 μg/L and 5.00 μg/L, respectively. For the repeated measurement, the average spike recovery range was 89.5%~97.0%, 81.9%~102% and 82.6%~103%, respectively. The final recoveries were 93.5%±5.6%, 93.7%±17%, and 96.7%±14%, respectively. 7 laboratories carried out industrial wastewater samples with spiked concentrations of 0.10 μg/L, 1.00 μg/L and 5.00 μg/L, respectively. For the repeated measurement, the average spike recovery range was 80.0%~114%, 76.0%~105% and 81.2%~99.0%, respectively. The final recoveries were 92.6% ± 24%, 95.0% ± 20%, and 91.8% ± 17%, respectively. 10 Quality Assurance and Quality Control 10.1 Calibration The working curve requires at least 5 concentration points (excluding 0 points), the curve correlation coefficient should be ≥0.995, or the relative response factor The relative standard deviation should be ≤ 20%. Analyze the intermediate concentration point of the curve every 24 h, and the relative error between the measured result and the standard value should be within ±20%, no You should find the cause or redraw the calibration curve. 10.2 Blank determination At least one blank sample should be analyzed for every 20 samples or batches (less than 20 samples/batch). The determination of ethyl lead should be below the method detection limit. 10.3 Determination of parallel samples A parallel sample should be analyzed for every 20 samples or batches (less than 20 samples/batch) and targeted for parallel sample analysis The relative deviation of the 7 complex should be less than 30%. 10.4 Determination of standard samples For every 20 samples or batches (less than 20 samples/batch), the substrate should be spiked and the matrix spiked recovery should be Between 60% and 125%. 11 Waste treatment Wastes containing organic reagents in the laboratory should be collected and stored in a closed container, marked, and funded. The quality unit is handled uniformly.

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