|
US$559.00 · In stock
Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email.
HJ 810-2016: Water quality - Determination of volatile organic compounds - Headspace / Gas chromatography mass spectrometry
Status: Valid
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| HJ 810-2016 | English | 559 |
Add to Cart
|
4 days [Need to translate]
|
Water quality - Determination of volatile organic compounds - Headspace / Gas chromatography mass spectrometry
| Valid |
HJ 810-2016
|
PDF similar to HJ 810-2016
Basic data | Standard ID | HJ 810-2016 (HJ810-2016) | | Description (Translated English) | Water quality - Determination of volatile organic compounds - Headspace / Gas chromatography mass spectrometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Word Count Estimation | 24,218 | | Date of Issue | 2016-07-26 | | Date of Implementation | 2016-10-01 | | Regulation (derived from) | Ministry of Environmental Protection Notice No.52 of 2016 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 810-2016: Water quality - Determination of volatile organic compounds - Headspace / Gas chromatography mass spectrometry
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
(Water quality - Determination of volatile organic compounds - Headspace/gas chromatography - mass spectrometry)
National Environmental Protection Standard of the People 's Republic of China
Determination of Volatile Organic Compounds in Water
Headspace/gas chromatography - mass spectrometry
Water quality -Determination of volatile organic compounds - Headspace/Gas
Test mass spectrometry
2016-07-26 release
2016-10-01 implementation
Ministry of Environmental Protection
Directory
Preface ii
1 Scope of application 1
2 normative reference document 1
Principle of Method 1
4 reagents and materials
5 instruments and equipment
6 samples
7 Analysis Step 3
Calculation and presentation of results
9 Precision and Accuracy 6
10 Quality assurance and quality control
11 Waste treatment 7
Appendix A (Normative Appendix) Characteristic compounds of the target compound, method detection limit and lower limit of assay 8
Appendix B (informative) Reference chromatogram
Appendix C (informative) Methodological precision and accuracy
Foreword
To implement the "Environmental Protection Law of the People's Republic of China" and "Water Pollution Prevention Law of the People's Republic of China" to protect the environment and protect the human body
Health, regulate the determination of volatile organic compounds in water, the development of this standard.
This standard specifies headspace/gas chromatography for the determination of volatile organic compounds in surface water, groundwater, domestic sewage, industrial waste water and seawater
- mass spectrometry.
This standard is the first release.
Appendix A to this standard is a normative appendix, Appendix B and Appendix C are informative appendices.
This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division.
The main drafting of this standard. Nanjing Environmental Monitoring Center Station.
The standard verification unit. Jiangsu Province Environmental Monitoring Center, Changzhou City Environmental Monitoring Center, Taizhou City Environmental Monitoring Center Station, Zhenjiang City
Environmental Monitoring Center Station, Jiangsu Province Physical and Chemical Testing Center and Nanjing Water Group Co., Ltd. Water Quality Monitoring Center.
The environmental protection department of this standard approved on July 26,.2016.
This standard has been implemented since October 1,.2016.
This standard is explained by the Ministry of Environmental Protection.
Water quality - Determination of volatile organic compounds - Headspace/gas chromatography - mass spectrometry
Warning. The organic solvents and reference materials used in the experiment are toxic and hazardous substances. The preparation and sample preparation process should be carried out in the fume hood.
Line; operation should be required to wear protective equipment, to avoid direct contact with skin and clothing.
1 Scope of application
This standard specifies the headspace/gas chromatography-mass spectrometry for the determination of volatile organic compounds in water.
This standard applies to the determination of 55 volatile organic compounds in surface water, groundwater, domestic sewage, industrial waste water and seawater.
When the sampling volume was 10.0 ml, the detection limit of the method of the target compound was 2 μg/L to 10 μg/L,
The detection limit was 8 μg/L to 40 μg/L. The detection limit of the target compound was 0.4 μg/L ~ 1.7
Μg/L, the lower limit of determination was 1.6 μg/L to 6.8 μg/L. See Appendix A. for details.
2 normative reference documents
The contents of this standard refer to the following documents or their terms. For undated references, the valid version applies to this standard.
Technical specification for surface water and wastewater monitoring
Technical specification for groundwater environmental monitoring
Specification for ocean monitoring - Part 3. Sample collection, storage and transport
3 Principle of the method
Under certain temperature conditions, the volatile components of the sample in the headspace bottle evaporate to the liquid space, resulting in vapor pressure, in the gas-liquid two-phase to
After the dynamic equilibrium of thermodynamics, the volatile organic compounds in the gas phase are separated by gas chromatography and detected by mass spectrometer. By keeping with the reference substance
Time and mass spectrum compared to qualitative, internal standard method quantitative.
4 reagents and materials
Unless otherwise stated, analytical pure chemical reagents are used in accordance with national standards.
4.1 Experimental water. secondary distilled water or water equipment prepared by water.
Before use, subject to a blank test to confirm that there is no interference with the presence or peak of the chromatographic peaks in the retention time interval of the target compound
The concentration of the compound is lower than the method detection limit.
Note 1. If the laboratory has a volatile solvent such as dichloromethane, you need to pay special attention to check the quality of experimental water, you can choose to boil, nitrogen purge or
Use special volatile organic matter to remove the column, etc., until the requirements are met.
4.2 Methanol (CH3OH). Chromatographic Purification. Before use, subject to a blank test to confirm that the target compound or target compound concentration is lower than the method
The detection limit.
4.3 Sodium chloride (NaCl). Before use, in the muffle furnace at 400 ℃ for 4 h, placed in a dryer to cool to room temperature, transferred to the grinding glass
Preserved in a jar.
4.4 ascorbic acid (C6H8O6).
4.5 hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure.
4.6 hydrochloric acid solution. 1 1 (v/v), with hydrochloric acid (4.5) preparation.
4.7 standard stock solution. ρ = 1000 mg/L ~ 5000 mg/L.
Commercially available certified standard solution, according to the instructions required to save.
4.8 standard use of liquid. ρ = 50 mg/L ~.200 mg/L.
The standard stock solution (4.7) was diluted with methanol (4.2). Vinyl chloride standard use of liquid with the current allocation, the remaining standard use of liquid retention period of 30 d.
4.9 internal standard stock solution. ρ = 100 mg/L ~.2000 mg/L.
Should use fluoride benzene, 1,2-dichlorobenzene-d4 as the internal standard, can be directly purchased commercially available standard solution. Meet the requirements of this method and do not work
Other internal standards may also be used under the premise of determining the target compound.
4.10 Internal standard liquid I. ρ =.200 mg/L.
The internal standard stock solution (4.9) was diluted with methanol (4.2).
4.11 Internal standard liquid II. ρ = 20 mg/L.
The internal standard stock solution (4.9) was diluted with methanol (4.2).
4.12 Mass spectrometry Tuning solution. 4-bromofluorobenzene (C6H4BrF, BFB), ρ = 25 mg/L.
Can be directly purchased commercially available standard solution, or with the standard material preparation.
4.13 helium. purity ≥99.999%.
4.14 Nitrogen. Purity ≥99.999%.
Note 2. Unless otherwise stated, the solution (4.7 to 4.12) is stored in methanol (4.2) as a solvent and stored in a brown dense flask at temperatures below -10 ° C.
According to the manufacturer's product description preservation; vinyl chloride stored separately. Before use should be restored to room temperature, mix.
5 instruments and equipment
5.1 Gas Chromatography/Mass Spectrometer. The gas chromatographic section has a split/splitless inlet and can be programmed to warm up. The mass spectrum portion has 70 eV electrons
(EI) ion source with NIST mass spectrometer library with full scan (Scan) and selective ion (SIM) scanning, manual/auto tuning,
Data collection, quantitative analysis and library search and other functions.
5.2 automatic headspace sampler. heating temperature control range between room temperature to 120 ℃; temperature control accuracy of ± 1 ℃.
5.3 Capillary column. 60 m (or 30 m) x 0.25 mm; film thickness 1.4 m (6% nitrile propylphenyl-94% dimethylpolysiloxane
Liquid), or other equivalent capillary column.
5.4 Sampling bottle. 40 ml brown screw glass bottle with silicone rubber - PTFE cover Screw cap, placed in the absence of volatile organic compounds
area.
5.5 Headspace Bottle. 22 ml glass headspace bottle with gasket (polytetrafluoroethylene/silicone rubber or polytetrafluoroethylene/butyl rubber material), sealing cap
(Screw cap or one-time gland), or use a glass headspace bottle with an automatic headspace sampler (5.2).
Note 3. headspace bottle (5.5) before use, must be washed with detergent, tap water, experimental water, clean, and placed in the muffle furnace 300 ℃ bake 30 min,
Ready to be used after cooling; headspace bottle gasket is generally a one-time use, after the closure of the bottle should be kept sealed in clean and non-volatile organic areas.
5.6 glass micro-syringe. 10 μl ~ 100 μl.
5.7 General laboratory equipment and equipment commonly used.
6 samples
6.1 sample collection
The collection of surface water, domestic sewage and industrial waste water samples is carried out in accordance with the relevant provisions of HJ/T 91; groundwater samples are collected in accordance with
HJ/T 164 of the relevant provisions of the implementation of seawater samples collected in accordance with the relevant provisions of GB 17378.3 implementation. When collecting samples, do not use water
Such as dewatering the water sample in the vial and without leaving room, should try to avoid or reduce the sample in the air exposure. all
Samples were collected in parallel.
If the water sample contains residual chlorine, before sampling, should be 40 ml of brown sampling bottle (5.4) plus 25 mg (accurate to 0.001g) ascorbic acid
(4.4). If the water content of residual chlorine in excess of 5 mg/L, should increase the proportion of ascorbic acid added, the remaining chlorine content of each increase of 5 mg/L,
You should add 25 mg (accurate to 0.001g) ascorbic acid.
6.2 Sample storage
After the sample is collected, add appropriate amount of hydrochloric acid solution (4.6), make the sample pH ≤ 2, tighten the stopper, label and put it into
Refrigerated containers in the following 4 ℃ refrigerated transport. Samples shipped back to the laboratory, should be refrigerated below 4 ℃, dark and sealed to save, 14 d to complete
Analysis and determination. The sample storage area should be free of volatile organic matter, the sample should be measured before the water samples to room temperature.
Note 4. If the water sample is added to the hydrochloric acid solution after the bubble generated, to be re-sampling, re-collected samples without hydrochloric acid solution, the sample label should be marked not
Acidification, within 24 h to complete the analysis.
7 Analysis steps
7.1 Instrument reference conditions
Different models of headspace sampler, gas chromatography/mass spectrometer the best working conditions are different, should be set in accordance with the instrument manual.
The standard reference conditions for this standard are as follows.
7.1.1 Headspace sampler reference conditions
Heating equilibrium temperature. 65 ℃; heating equilibrium time. 40 min; sampling needle temperature. 80 ℃; transmission line temperature. 105 ℃;
Product. 1.0 ml.
7.1.2 Gas Chromatographic Reference Conditions (when using a 60 m column)
Inlet flow rate. 250 ° C; carrier gas. helium (4.13); injection mode. split injection (split ratio 5. 1); column flow (constant flow mode
). 1.0 ml/min; heating program. 40 ℃ for 2 min, at 5 ℃/min rate rose to 120 ℃, keep 3 min, then 10 ℃
/ Min to 230 & lt; 0 & gt; C for 5 min.
Scan Mode and SIM Mode Refer to Appendix B for the total ion chromatogram.
7.1.3 Mass Spectral Reference Conditions
Ion source. electron bombardment (EI) ion source. Ion source temperature. 230 ° C. Ionization energy. 70 eV. Interface temperature. 280 ℃.
Quadrupole temperature. 150 ° C. Scan mode. full scan or select ion scan (SIM). Scanning range. 35 amu ~ 300 amu.
When the SIM mode is measured, each target compound should select a quantitation ion and at least one auxiliary ion. The same time window at the same time monitoring
The number of ions should not be measured too much, or may affect the sensitivity, may be appropriate to capture the corresponding time period corresponding to the characteristic ions.
7.2 Calibration
7.2.1 Instrument performance check
Prior to each batch analysis, the GC/MS system requires instrument performance checks. Use a microinjector (5.6) to remove 1 μl to 2 μl of mass spectrometry
(4.12), directly through a gas chromatography inlet, or add 20 μl of the mass spectrometry tuning solution (4.12) to 10.0 ml of the assay
The relative abundance of the 4-bromofluorobenzene bond ions obtained by the quadrupole mass spectrometry in water is measured by the headspace sampler (5.2). Table 1
, Otherwise the parameters of the mass spectrometer are adjusted or cleaned of the ion source.
Note 5. Automatic tuning is required before instrument performance check.
Table 1 BFB ion relative abundance standard
Mass - to - ion ratio abundance standard mass - to - charge ion abundance criterion
95 base peak, 100% relative abundance 175 mass 174% 5% to 9%
96% of the mass of 95% to 9% of the mass of 174 of 95% to 105%
173 Less than 2% of mass 174 177 Mass 176% 5% to 10%
174 is greater than 50% of mass 95
7.2.2 Drawing of calibration curves
7.2.2.1 Scan mode. 4 g (accurate to 0.1 g) sodium chloride (4.3) was added to the headspace flask (5.5) and 10.0 ml
Water, and then use a micro-syringe (5.6) were removed by a certain volume of standard use of liquid (4.8) into which the preparation of the target compound quality
Concentrations of 10.0 μg/L, 40.0 μg/L, 100 μg/L,.200 μg/L and 400 μg/L, respectively,
Approximately 10.0 μl of internal standard was added to each headspace using liquid I (4.10) so that the internal standard concentration in the standard series was.200 μg/L and immediately closed
The top of the bottle, light shake shake, according to the instrument reference conditions (7.1), from low concentration to high concentration followed by injection analysis, record the standard series of target
And the corresponding internal standard retention time, quantitative ion response value. The ratio of the concentration of the target compound to the concentration of the internal standard compound was the abscissa,
The calibration curve was plotted based on the ratio of the quantitative ion response of the target compound to the quantitative ion response value of the internal standard compound as the ordinate.
Equation (1) Calculate the relative response factor (RRF) of the target, calculate the average relative to all standard concentration points of the target according to formula (2)
Response Factor (RRF).
7.2.2.2 SIM mode. 4 g (accurate to 0.1 g) sodium chloride (4.3) was added to the headspace flask (5.5) and 10.0 ml
Water, and then use a micro-syringe (5.6) were removed by a certain volume of standard use of liquid (4.8) into which the preparation of the target compound quality
Concentrations of 2.0 μg/L, 4.0 μg/L, 10.0 μg/L, 20.0 μg/L and 40.0 μg/L, respectively,
Approximately 10.0 μl of internal standard was added to each headspace using liquid II (4.11) so that the internal standard concentration in the standard series was 20.0 μg/L and immediately closed
The top of the bottle, light shake shake, according to the instrument reference conditions (7.1), from low concentration to high concentration followed by injection analysis, record the standard series of target
And the corresponding internal standard retention time, quantitative ion response value. The ratio of the concentration of the target compound to the concentration of the internal standard compound was abscissa.
The calibration curve was plotted based on the ratio of the quantitative ion response of the target compound to the quantitative ion response value of the internal standard compound as the ordinate.
Equation (1) Calculate the relative response factor (RRF) of the target, calculate the average relative to all standard concentration points of the target according to formula (2)
Response Factor (RRF).
Note 6. The total volume of the solution used to add the standard liquid and internal standard solution can not exceed.200 μl.
Note 7. The calibration curve concentration range can be adjusted according to the instrument status and the actual sample concentration. The adjusted calibration curve still needs to meet the requirements of 10.2.
7.2.3 Calculation of average relative response factor (RRF)
The relative response factor (RRFi) of the target compound in the standard series i is calculated according to equation (1).
ISi
ISi
RRF
(1)
Where. RRFi - the relative response of the target compound at point i in the standard series;
Ai - the response value of the quantitation ions 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 - mass concentration of internal standard in standard series, g/L;
Ρi - the mass concentration of the target compound at point i in the standard series, g/L.
The average relative response factor RRF of the target compound in the calibration curve is calculated according to equation (2).
RRF
RRF
1 (2)
Where. RRF - the average relative response of the target compound in the calibration curve;
RRFi - the relative response of the target compound at point i in the standard series;
N - standard series points.
The relative standard deviation (RSD) of RRF is calculated according to equation (3).
0 distance
RRF
SD
RSD (3)
Where. SD - RMHz standard deviation.
7.3 Determination of samples
7.3.1 Scan mode. 4 g (accurate to 0.1 g) sodium chloride (4.3) was added to the headspace flask (5.5), 10.0 ml of water was added,
And then add 10.0 μl of the internal standard using liquid I (4.10), so that the sample within the standard concentration of.200 μg/L, immediately sealed headspace bottle, light shake,
Analyze according to the instrument reference conditions (7.1).
7.3.2 SIM mode. 4 g (accurate to 0.1 g) sodium chloride (4.3) was added to the headspace flask (5.5), 10.0 ml of water was added,
And then add 10.0 μl of the internal standard using liquid II (4.11), so that the sample internal standard concentration of 20.0 μg/L, immediately sealed headspace bottle, light vibration shake,
Analyze according to the instrument reference conditions (7.1).
Note 8. If the sample concentration exceeds the highest concentration point of the calibration curve, the sample should be re-sampled from the unpacked vial. Should reduce the amount of sample, with experimental water
Make up to 10.0 ml, for proper dilution after injection, dilution of the sample response value should be within the calibration curve. After analyzing the high concentration of the sample, it should be done once or more
Sub-laboratory blank test (7.4) until the blank measured value meets the requirements of 10.3.1 to analyze the next sample.
Note 9. The SIM mode is only applicable to samples where the sensitivity of the Scan mode is less than the corresponding standard.
7.4 blank test
The actual water sample was replaced with 10.0 ml of experimental water, and the blank was measured according to the same conditions and procedures for the determination of the sample (7.3).
Calculation and representation of results
8.1 Qualification of the target compound
The target compound was characterized according to the retention time and mass spectrum of the target in the sample and the target in the standard series.
8.1.1 Retention time qualitative
Before the analysis of the sample, the retention time window t ± 3S was established. T is the retention time of the target compound at each concentration level for calibration, and S is the beginning
The standard deviation of the retention time of the target compound at each concentration level at the time of calibration. At the time of sample analysis, the target compound should peak in the retention time window.
8.1.2 Mass spectrometry ion information qualitative
Scan mode, the target compound in the standard mass spectrum of the relative abundance of more than 30% of all ions should be present in the sample mass spectrum;
The relative abundance of the above-mentioned characteristic ions in the sample mass spectrum and the standard mass spectrum should be within ± 30%. For example, an ion is in standard mass spectrometry
The relative abundance of the ions in the sample mass spectrum should be between 20% and 80%. For certain compounds,
Some special ions, such as molecular ion peaks, even if the relative abundance of less than 30%, should also be used as a basis for determining the compound. If practically
There is a significant background disturbance in the sample, and the background effect should be subtracted.
SIM mode, the confirmation of the target compound ions should be present in the sample. For the retention time window within each compound, the sample
The relative abundance of the ions relative to the quantitative ions is compared with the relative abundance obtained by the nearest calibration standard, and the relative deviation should be less than
30%.
8.2 Quantification of the target compound
Quantitative calculations are performed using the average relative response factor or the calibration curve method. When the quantitative ion of the target compound in the sample is interfered with,
Use assisted ion quantification. See Appendix A for specific ions.
8.2.1 Average Relative Response Factor Method
When the average relative response factor method is used to calibrate, the mass concentrati...
Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 810-2016_English be delivered?Answer: Upon your order, we will start to translate HJ 810-2016_English as soon as possible, and keep you informed of the progress. The lead time is typically 2 ~ 4 working days. The lengthier the document the longer the lead time. Question 2: Can I share the purchased PDF of HJ 810-2016_English with my colleagues?Answer: Yes. The purchased PDF of HJ 810-2016_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet. Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. If you need your currency to be printed on the invoice, please write an email to [email protected]. In 2 working-hours, we will create a special link for you to pay in any currencies. Otherwise, follow the normal steps: Add to Cart -- Checkout -- Select your currency to pay.
|