HJ 591-2010 (HJ591-2010) & related versions
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Water quality. Determination of pentachlorophenol by gas chromatography
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HJ 591-2010
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HJ 591-2010
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HJ 591-2010: PDF in English
HJ 591-2010
Water quality.Determination of pentachlorophenol by gas chromatography
National Environmental Protection Standard of the People's Republic
Replace GB 8972-88
Water quality - Determination of pentachlorophenol - Gas chromatography
Released on.2010-10-21
2011-01-01 Implementation
Ministry of Environmental Protection released
Ministry of Environmental Protection
announcement
No. 77 of.2010
In order to implement the "Environmental Protection Law of the People's Republic of China", protect the environment, and protect human health, we now approve the measurement of ambient air ozone.
Six standards, such as the fixed ultraviolet photometry, are national environmental protection standards and are released.
The standard name and number are as follows.
1. Determination of ambient air ozone by ultraviolet photometry (HJ 590-2010);
3. Determination of water quality nitrobenzene compounds by gas chromatography (HJ 592-2010);
4. Determination of water quality, elemental phosphorus, phosphorus molybdenum blue spectrophotometry (provisional) (HJ 593-2010);
5. Determination of the total amount of water-based developer and its oxides - Iodine-starch spectrophotometry (interim) (HJ 594-2010);
6. Determination of the total amount of water color developing agent 169 Coupler spectrophotometry (provisional) (HJ 595-2010).
The above standards have been implemented since January 1,.2011 and published by the China Environmental Science Press. The standard content can be found on the website of the Ministry of Environmental Protection.
From the date of implementation of the above standards, the following three national environmental protection standards approved and issued by the former National Environmental Protection Agency shall be abolished.
The name and number are as follows.
1. Determination of ambient air ozone by ultraviolet spectrophotometry (GB/T 15438-1995);
2. Determination of water quality pentachlorophenols by gas chromatography (GB 8972-88);
3. Determination of Total Nitro Compounds in Industrial Wastewater Gas Chromatography (GB 4919-85).
Special announcement.
October 21,.2010
Content
Foreword..iv
1 Scope..1
2 Method principle..1
3 reagents and materials.1
4 instruments and equipment. 2
5 samples. 2
6 Analysis steps..2
7 Calculation and representation of results..4
8 precision and accuracy..4
9 Quality Assurance and Quality Control 5
Appendix A (informative) Filling method of packed column..6
Iv
Foreword
To protect the environment and protect the human body 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 Water Pollution Prevention and Control
This standard is established for the determination of health and standardization of pentachlorophenol in water.
This standard specifies the gas chromatographic method for the determination of pentachlorophenol and pentachlorophenolate in water.
This standard is a revision of the "Gas Chromatography for the Determination of Pentachlorophenol in Water" (GB 8972-88).
This standard was first published in 1988. The original standard was drafted by the Ministry of Railways Labor Health Research Institute. This is the first revision. Revision
The main contents are as follows.
-- Expanded the scope of application;
-- Added capillary column analysis method;
-- modified the quantitative method;
-- Added provisions for quality control and quality assurance.
From the date of implementation of this standard, the national environmental protection standard “Water quality approved and issued by the former National Environmental Protection Agency on March 26, 1988.
Determination of pentachlorophenol gas chromatography (GB 8972-88) is abolished.
Appendix A of this standard is an informative annex.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard is mainly drafted by. Qingdao Environmental Monitoring Center Station.
This standard is verified by. Jinan Environmental Protection Monitoring Station, Zibo Environmental Monitoring Station, Weifang Environmental Monitoring Center Station, Qingdao Institute of Technology
College of Environmental and Municipal Engineering, Agricultural Products Supervision and Inspection Center of the Ministry of Agriculture (Qingdao).
This standard was approved by the Ministry of Environmental Protection on October 21,.2010.
This standard has been implemented since January 1,.2011.
This standard is explained by the Ministry of Environmental Protection.
Water quality - Determination of pentachlorophenol - Gas chromatography
1 Scope of application
This standard specifies the gas chromatographic method for the determination of pentachlorophenol and pentachlorophenolate in water.
This standard applies to the determination of pentachlorophenol and pentachlorophenolate in surface water, groundwater, seawater, domestic sewage and industrial wastewater.
When the sample volume is 100 ml, the detection limit of capillary column gas chromatography is 0.01 μg/L, and the lower limit of determination is 0.04 μg/L.
The limit is 5.00 μg/L; the detection limit of packed column gas chromatography is 0.02 μg/L, and the lower limit of determination is 0.08 μg/L.
2 Principle of the method
The pentachlorophenolate in the sample is converted to pentachlorophenol under acidic conditions, extracted with n-hexane, and then back extracted with potassium carbonate solution to give
The pentachlorophenol in the organic phase is converted to pentachlorophenolate into an alkaline aqueous solution. Adding acetic anhydride and pentachlorophenolate to an alkaline aqueous solution for derivatization
Should produce pentachlorophenyl acetate. After extraction with n-hexane, the measurement was carried out using a gas chromatograph with an electron capture detector.
3 reagents and materials
Analytical purification reagents conforming to national standards were used for the analysis, and the experimental water was freshly prepared distilled water unless otherwise stated.
3.1 n-hexane (C6H14). pesticide residue level.
3.2 Acetic anhydride [(CH3CO)2O].
3.3 Methanol (CH3OH). pesticide residue grade.
3.4 Copper sulfate (CuSO4).
3.5 sodium thiosulfate (Na2S2O3 · 5H2O).
3.6 Sulfuric acid (H2SO4). ρ = 1.84 g/ml.
3.7 Sulfuric acid solution. 19.
3.8 Potassium carbonate solution (K2CO3). c = 0.1 mol/L.
Weigh 13.8 g of anhydrous potassium carbonate and dissolve it in 1 000 ml of water.
3.9 anhydrous sodium sulfate (Na2SO4).
After burning at 400 ° C for 2 h in a muffle furnace, after cooling, it was stored in a ground glass bottle and sealed.
3.10 Pentachlorophenol standard stock solution. ρ=1.00 mg/ml.
Store at 4 ° C in cold storage. Commercially available certified standards can be used.
3.11 Pentachlorophenol standard intermediate solution. ρ=100.0 μg/ml.
Accurately transfer 100.0 μl of pentachlorophenol standard stock solution (3.10) to 1 ml with methanol.
3.12 Pentachlorophenol standard use solution. ρ = 1.00 μg/ml.
Accurately remove 10.00 μl of pentachlorophenol standard intermediate (3.11) and dilute to 1 ml with methanol.
3.13 Carrier gas. High purity nitrogen [purity ≥ 99.99% (volume fraction)].
4 Instruments and equipment
4.1 Gas Chromatograph. with an electron capture detector.
4.2 Column
Packed column. made of hard glass or stainless steel, 1.5 to 2.5 m long, 3 to 4 mm in inner diameter, 1.5% phenyl-containing poly-coated
Chromsorb W (80-100 mesh) of methyl siloxane (OV-17) and 2% polyfluoroalkylsiloxane (QF-1). Packed column preparation
See Appendix A for the method.
Capillary column. The stationary phase was 5% phenyl-95% methylpolysiloxane, 30 m × 0.32 mm (inside diameter) × 0.25 μm (film thickness). Or
He is equivalent to a capillary column.
4.3 Microinjectors. 10 μl, 50 μl and 500 μl.
4.4 Separating funnel. 125 ml and 250 ml with Teflon stopper.
4.5 Common instruments and equipment used in general laboratories.
5 samples
5.1 Sample collection and preservation
A brown glass bottle should be used for sampling. Add 1 ml of sulfuric acid solution (3.7) and 0.5 g of copper sulfate (3.4) per 100 ml of water sample at 4 °C.
Save in the dark. If residual chlorine is present during sampling, add approximately 80 mg of sodium thiosulfate (3.5) to each 100 ml of water and shake well. sample
Avoid direct sunlight.
All samples must be extracted within 7 days, and the extract is stored at 4 ° C in the dark and analyzed within 30 days.
5.2 Preparation of samples
5.2.1 Extraction
Take 100 ml of water sample in a 250 ml separatory funnel, add 1 ml of concentrated sulfuric acid (3.6), and extract with 10 ml of n-hexane (3.1).
The water sample was taken twice, and the hexane phase was combined and the aqueous phase was discarded. Then extract the n-hexane phase twice with 0.1 mol/L potassium carbonate solution (3.8) 10 ml, respectively.
The aqueous phase was combined and the n-hexane phase was discarded.
5.2.2 Derivatization
Add 1 ml of acetic anhydride (3.2) to the aqueous phase, shake for 5 min, add 5 ml of n-hexane (3.1), shake for 5 min, and let stand for stratification.
The aqueous phase was discarded and the n-hexane phase was collected. The n-hexane phase was dehydrated with anhydrous sodium sulfate (3.9) and then nitrogen-blown to a volume of 1 ml to be tested.
Note. For high concentration sewage and wastewater samples, appropriate amount of water should be added to the separatory funnel according to the concentration of the sample, and water should be added to 100 ml.
6 Analysis steps
6.1 Chromatographic conditions
6.1.1 Filled Column Gas Chromatography Reference Conditions
Inlet temperature. 220 ° C; detector temperature. 220 ° C; column temperature. 180 ° C; carrier gas flow. 40 ~ 60 ml/min.
6.1.2 Capillary column gas chromatography reference conditions
Inlet temperature. 250 ° C; detector temperature. 300 ° C; column temperature. 60 ° C for 2 min, from 20/min ° C to 220 ° C,
Increased from 10/min °C to 250 °C for 3 min; carrier gas flow rate. 1.5 ml/min; tail gas flow rate. 60 ml/min; injection volume. 1.0 μl;
Injection method. no split injection, 0.75 min split after injection, split ratio 40.1.
6.2 Drawing of the working curve
Add 0, 5, 10, 50, 100, 250 to 7 125 ml separatory funnels containing 20 ml of K2CO3 solution (3.8).
500 μl of pentachlorophenol standard use solution (3.12), mix, according to the same procedure of derivatization (5.2.2) to get the concentration of pentachlorophenol is 0, 5,
Standard series solutions of 10, 50, 100, 250, 500 ng/ml. 1.0 μl of the standard series solution was injected into the gas phase with a micro-syringe
In the spectrometer, the peak area (peak height) of the chromatographic peak corresponding to the solution of different mass concentrations was recorded. Taking the concentration of pentachlorophenol standard series solution as the abscissa,
The corresponding peak area (peak height) is the ordinate and the working curve is drawn.
6.3 Chromatogram of standard solution
When using a capillary column and a packed column, respectively, the pentachlorophenyl acetate reference chromatogram is shown in Fig. 1 and Fig. 2.
Hz
2 4 6 8 10 12 t/min
1--n-hexane; 2-pentachlorophenyl acetate.
Figure 1 Chromatogram of pentachlorophenyl acetate in a capillary column
Hz
2 3 4 5 t/min
1--n-hexane; 2-pentachlorophenyl acetate.
Figure 2 Chromatogram of pentachlorophenyl acetate in packed column
6.4 Determination
1.0 μl of the sample (5.2.2) was injected into the gas chromatograph and measured under the same chromatographic conditions as the working curve. Recording peak
Retention time and peak area (peak height).
6.5 Blank test
While the sample is being analyzed, a blank test should be performed. That is, the test water was used instead of the water sample, and the analysis was carried out in the same manner as in the measurement (6.4).
7 Calculation and representation of results
7.1 Calculation of results
The mass concentration (ρ) of pentachlorophenol in the sample was calculated according to the formula (1).
1V
Ρρ ×= standard (1)
Where. ρ--the concentration of pentachlorophenol in the water sample, μg/L;
ρ standard--the concentration of pentachlorophenol calculated from the working curve, μg/L;
1V - the volume of the volume after concentration of the extract, ml;
V -- water sample volume, ml.
7.2 Results representation
When the result is less than 1 μg/L, it is retained to two decimal places; when the result is greater than or equal to 1 μg/L, three significant digits are retained.
8 precision and accuracy
8.1 Precision
8.1.1 Capillary column precision
Uniform samples containing 0.05 μg/L, 1.00 μg/L, and 2.50 μg/L of pentachlorophenol were measured in five laboratories.
The relative standard deviations in the experimental room were. 6.0% to 9.7%, 4.4% to 8.0%, and 3.4% to 8.0%;
The relative standard deviations between laboratories were. 7.1%, 6.0%, 1.9%;
The repeatability limits r are. 0.01 μg/L, 0.17 μg/L, 0.38 μg/L;
The reproducibility limits R were. 0.01 μg/L, 0.20 μg/L, and 0.40 μg/L, respectively.
8.1.2 Filled column precision
When the concentration of pentachlorophenol in the sample is less than 2 μg/L, the reproducibility coefficient of variation is less than 9%, and the repeatability coefficient of variation is less than 6%.
8.2 Accuracy
8.2.1 Capillary column accuracy
Five laboratories tested the standard substance containing pentachlorophenol at 102 μg/L. The relative error is −1.9% to 2.2%, and the relative error is finally
Value. 0.22% ± 3.94%.
Five laboratories added standard samples of surface water and sewage containing less than 0.01 μg/L and 0.27 μg/L of pentachlorophenol.
The recoveries were 81.8%~96.6% and 89.9%~104%. The final recoveries were 90.1%±10.8% and 97.0%±12.0%, respectively.
8.2.2 Filled column accuracy
When the concentration of pentachlorophenol in the sample is less than 2 μg/L, the recovery rate is greater than 90%, and the coefficient of variation of accuracy is less than 12%.
9 Quality Assurance and Quality Control
9.1 Qualitative analysis
A retention time window of t ± 3S should be established prior to sample analysis. t is the average value of the retention time of each concentration level of the reference material at the initial calibration,
S is the standard deviation of each standard analysis at the initial calibration. When the sample is analyzed, the sample retention time should be within the retention time window.
9.2 Blank test
Make at least one blank sample and blank spiked sample for each batch of samples. Blank samples are compared with actual samples using the same method, blank
The concentration of pentachlorophenol in the sample should be below the detection limit. The recovery rate of the blank sample should be controlled at 80% to 120%.
9.3 The correlation coefficient of the working curve should be greater than or equal to 0.995, otherwise the working curve should be redrawn.
9.4 Intermediate mass concentration test
The intermediate mass concentration test shall be carried out during sample analysis. The relative deviation between the measured value of the intermediate mass concentration and the value of the curve shall be less than or equal to
15%, otherwise a new work curve should be established.
9.5 Matrix addition
At least one matrix spiked sample shall be prepared for each batch of samples. The matrix spiked sample and the actual sample shall be analyzed and determined by the same method.
The recovery rate should be controlled at 70% to 130%.
Appendix A
(informative appendix)
Filling method of packed column
Weigh 5% of the weight of the coated OV-17 (polymethylsiloxane containing phenyl) on a thousandth of a balance and take up the load.
2% by weight of QF-1 was placed in a small beaker and dissolved in methylene chloride in an amount sufficient to submerge the support. Transfer the solution to 250 ml
In the round bottom flask, a weighing carrier to be coated was added, and the condenser was attached, and the mixture was heated under reflux for 2 hours. Then, place the flask in the warm
On the water bath, depressurize with a water pump to slowly evaporate the solvent. Finally, the support is placed in a petri dish and baked with an infrared lamp for later use.
The end of the column (connected to the detector end) is plugged with quartz wool, connected to a vacuum pump, and the other end of the column is connected to a funnel through a hose.
After the vacuum pump, the stationary phase is slowly loaded into the column through the funnel, and the column is tapped while packing to make the filling uniform. After filling, use quartz
Cotton is plugged into the other end of the column.
The filled column is connected to the inlet of the instrument, and the detector is not connected at one end. The carrier gas is supplied at a flow rate of 20-30 ml/min. The column oven is maintained.
Continuous aging for 48 h at 240 °C. Check before use, straighten to the baseline.
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| Standard ID | HJ 591-2010 (HJ591-2010) | | Description (Translated English) | Water quality. Determination of pentachlorophenol by gas chromatography | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Classification of International Standard | 13.060 | | Word Count Estimation | 11,127 | | Date of Issue | 2010-10-21 | | Date of Implementation | 2011-01-01 | | Older Standard (superseded by this standard) | GB/T 8972-1988 | | Drafting Organization | Qingdao Municipal Environmental Monitoring Center Station | | Administrative Organization | Ministry of Environment Protection | | Regulation (derived from) | Department of Environmental Protection Notice No. 77 of 2010 | | Summary | This standard specifies the water PCP and PCP salts gas chromatographic method. This standard applies to surface water, groundwater, water, sewage and industrial wastewater PCP and PCP salts determination. |
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