Home Cart Quotation About-Us
www.ChineseStandard.net
SEARCH

HJ 922-2017 English PDF

US$489.00 · In stock
Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email.
HJ 922-2017: Soil and sediment--Determination of polychlorinated biphenyls--Gas chromatography
Status: Valid
Standard IDUSDBUY PDFLead-DaysStandard Title (Description)Status
HJ 922-2017489 Add to Cart 4 days Soil and sediment--Determination of polychlorinated biphenyls--Gas chromatography Valid

Similar standards

HJ 803   GB/T 17139   GB/T 17136   HJ 491   HJ 923   HJ 921   

Basic data

Standard ID: HJ 922-2017 (HJ922-2017)
Description (Translated English): Soil and sediment--Determination of polychlorinated biphenyls--Gas chromatography
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z18
Word Count Estimation: 20,224
Date of Issue: 2017-12-28
Date of Implementation: 2018-04-01
Regulation (derived from): Ministry of Environmental Protection Bulletin 2017 No. 85
Issuing agency(ies): Ministry of Ecology and Environment

HJ 922-2017: Soil and sediment--Determination of polychlorinated biphenyls--Gas chromatography


---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.
People's Republic of China national environmental protection standards Soil and sediment-Determination of polychlorinated biphenyls -Gas chromatography 2017-12-28 Published 2018-04-01 implementation Directory Foreword .ii 1 Scope 1 2 Normative references 1

3 Terms and definitions

4 method principle 2 5 Interference and elimination .2 6 Reagents and materials .2

7 instruments and equipment

8 samples .3 9 Analysis Step 5 10 Results Calculation and Presentation 6 11 Precision and accuracy .8 12 Quality Assurance and Quality Control .8 13 Waste treatment .9 Appendix A (Normative) Methods of detection limit and lower limit of determination Appendix B (informative) precision and accuracy of the method Appendix C (informative) sample purification method 16

Foreword

In order to carry out "Environmental Protection Law of the People's Republic of China", protect the environment, protect human health, standardize the soil and sediments Determination of PCBs, the development of this standard. This standard specifies the gas chromatography determination of 18 kinds of PCBs in soil and sediment. Appendix A of this standard is a normative appendix, Appendix B and Appendix C are informative appendices. This standard is released for the first time. This standard by the Environmental Protection Department of Environmental Monitoring Division and Science and Technology Standards Division to develop. This standard was drafted. Jiangsu Provincial Environmental Monitoring Center. This standard verification unit. Taizhou Environmental Monitoring Center Station, Henan Province Environmental Monitoring Center, Nanjing Environmental Monitoring Center Station, Dalian City Environmental Monitoring Center, Nanjing Environmental Protection Research Institute and the Nanjing Entry-Exit Inspection and Quarantine Electronic and Electrical Products Laboratory. This standard MEP approved on December 28, This standard since April 1,.2018 come into operation. This standard is interpreted by the MEP. Soil and sediment - Determination of PCBs - Gas chromatography Warning. The solvents and reagents used in the experiment have some toxicity, some PCBs are carcinogenic, the standard Solution preparation and sample preparation process should be carried out in a fume hood; operation should be worn protective equipment, avoid direct contact with the skin and clothing.

1 scope of application

This standard specifies the determination of PCBs in soil and sediment by gas chromatography. This standard applies to the determination of 7 indicative PCBs and 12 coplanar polychlorinated biphenyls in soils and sediments. other PCBs, if verified, can also be measured using this standard. When the sample volume is 10.0 g, the detection limit of PCBs is 0.03 μg/kg ~ 0.07 μg/kg, and the lower limit of determination 0.12 μg/kg to 0.28 μg/kg. See Appendix A for details.

2 Normative references

This standard references the following documents or the terms of them. For undated references, the effective version applies to this standard. GB 17378.3 Marine monitoring code - Part 3. Sample collection, storage and transport GB 17378.5 Marine monitoring code - Part 5. Sediment analysis HJ 494 water sampling technical guidance HJ 613 Determination of soil dry matter and moisture Gravimetric method HJ 783 Extraction of organic matter from soils and sediments by pressurized fluid extraction HJ/T 91 Technical Specifications for Surface Water and Sewerage Monitoring HJ/T 166 Soil Environmental Monitoring Technical Specifications

3 Terms and definitions

3.1 Indicative PCBs PCBs Refers to PCBs that are used as alternative monitors for the contamination of PCBs, including 2,4,4'-trichlorobiphenyl (PCB28), 2,2 ', 5,5'-tetrachlorobiphenyl (PCB52), 2,2', 4,5,5'-pentachlorobiphenyl (PCB101), 2,3 ', 4,4 ', 5-pentachlorophenol (PCB118), 2,2 ', 3,4,4', 5'-hexachlorobiphenyl (PCB138), 2,2 ', 4,4', 5,5'-hexachlorobiphenyl (PCB153) , 2,2 ', 3,4,4', 5,5'-heptachlor biphenyl (PCB180) and other seven compounds. Co-planar PCBs coplanar PCBs Refers to polychlorinated biphenyls that are not ortho or ortho-ortho substituted in PCBs and are similar in their toxicity to dioxins, including 3,3 ', 4,4'-tetrachlorobiphenyl (PCB77), 3,4,4', 5-tetrachlorobiphenyl (PCB81), 2,3,3 ', 4,4'- Benzene (PCB105), 2,3,4,4 ', 5-Pentachlorobenzene (PCB114), 2,3', 4,4 ', 5-Pentachlorobenzene (PCB118), 2', 3,4,4 ', 5 - Pentachlorobenzene (PCB123), 3,3 ', 4,4', 5-Pentachlorobenzene (PCB126), 2,3,3 ', 4,4', 5-Hexachlorobiphenyl (PCB156), 2,3,3 ', 4 , 4 ', 5'-hexachlorobiphenyl (PCB 157), 2,3 ', 4,4', 5,5'-hexachlorobiphenyl (PCB 167), 3,3 ', 4,4', 5,5'-hexachlorobiphenyl 2,3,3 ', 4,4', 5,5'-heptachlorobiphenyl (PCB189) and other 12 kinds of compounds. Among them 2,3 ', 4,4', 5-Pentachlorobenzene (PCB118) also Is indicative of PCBs.

4 method principle

PCBs in soils or sediments are extracted, purified, concentrated and fixed. Electron capture detectors Gas chromatography. According to the retention time of qualitative, external standard method.

5 Interference and elimination

Other organic impurities in the sample, interference PCBs determination, the choice of sulfuric acid, magnesium silicate column, such as appropriate net Method to remove. After purification, there will still be other compounds and the target compound at the same time peak, interference determination, through another Different polarity of the column auxiliary qualitative. If required, confirm that the sensitivity meets the requirements by gas chromatography-mass spectrometry.

6 Reagents and materials

Unless otherwise stated, analytical grade reagents that meet national standards are used. Experimental water for the new preparation of pure water or distilled water. 6.1 n-Hexane (C6H14). Chromatographic purity. 6.2 Acetone (CH3COCH3). Chromatography pure. 6.3 anhydrous sodium sulfate (Na2SO4). excellent grade pure. Baking in a muffle furnace at 450 ° C for 4 h, cooling and placing in a glass jar with a grit stopper and holding in a desiccator. 6.4 Potassium carbonate (K2CO3). excellent grade pure. 6.5 Sulfuric acid. ρ (H2SO4) = 1.84 g/ml. 6.6 acetone - n-hexane mixed solvent I. 1 1. Mix with acetone (6.2) and n-hexane (6.1) at a volume ratio of 1.1. 6.7 acetone - n-hexane mixed solvent Ⅱ. 1 9. Mix 1.9 volumes with acetone (6.2) and n-hexane (6.1). 6.8 Potassium carbonate solution. p = 0.1 g/ml. Weigh 100 g of potassium carbonate (6.4) dissolved in water, set to 1000 ml. 6.9 Polychlorinated biphenyls standard stock solution. ρ = 10.0 mg/L to 100 mg/L. Buy a commercially available certified standard solution, store at 4 ° C in a dark, airtight refrigerator or with reference to a standard solution certificate. Make Use should be returned to room temperature and shake. 6.10 PCB standard solution. ρ = 1.0 mg/L (reference concentration). Dilute PCB stock standard solution with n-hexane (6.1) (6.9). Avoid light at 4 ℃ closed refrigeration, storage period of six months. 6.11 Magnesium silicate solid phase extraction column. commercially available, 1000 mg/6 ml. Or according to the impurity content to choose other capacity of magnesium silicate SPE column. 6.12 quartz sand. 270 μm ~ 830 μm (50 mesh ~ 20 mesh). Baking in a muffle furnace at 450 ° C for 4 h, cooling and placing in a glass jar with a grit stopper and holding in a desiccator. 6.13 Diatomaceous earth. 37 μm to 150 μm (400 mesh to 100 mesh). Baking in a muffle furnace at 450 ° C for 4 h, cooling and placing in a glass jar with a grit stopper and holding in a desiccator. 6.14 glass wool or glass fiber filter. 400 ° C in a muffle furnace baking 1 h, cooled and placed in a sealed glass jar sealed. 6.15 high purity nitrogen. purity ≥ 99.999%.

7 instruments and equipment

7.1 Gas Chromatograph with Electronic Capture Detector (ECD) with Split/Splitless Inlet for Programmable Temperature. 7.2 Column 7.2.1 Column 1. Column length 30 m, inner diameter 0.32 mm, film thickness 0.25 μm, stationary phase 5% polydiphenylsiloxane and 95% polydimethylsiloxane, or other equivalent column. 7.2.2 Column 2. Column length 30 m, inner diameter 0.32 mm, film thickness 0.25 μm, stationary phase 14% Polynyl cyanopropyl silicone Alkane and 86% polydimethylsiloxane, or other equivalent column. 7.3 Extraction device. microwave extraction device, Soxhlet extraction device, pressurized fluid extraction device or a device with a considerable function, No grease lubricant is allowed on all interfaces. 7.4 Concentration device. Nitrogen blowing instrument, rotary evaporator, KD concentrator or equipment with a considerable function. 7.5 Sampling Bottles. Wide-mouth brown glass bottles or Teflon-lined screw-on glass bottles. 7.6 General laboratory commonly used instruments and equipment.

8 samples

8.1 Sample Collection and Storage Soil samples were collected and stored according to the relevant requirements of HJ/T 166, and samples of marine sediments were related according to GB 17378.3 Requirements for collection and preservation, surface water sediment samples collected according to HJ/T 91 and HJ 494 requirements. Samples are saved in advance Clean the clean bottle (7.5), back to the laboratory analysis as soon as possible, the process of transportation should be sealed dark. If temporarily unable to analyze, It should be refrigerated at below 4 ℃ for 14 days. Sample extract (8.4.1) 4 ℃ below the dark storage, preservation The time is 40 days. 8.2 Preparation of samples Remove foreign matter (stones, leaves, etc.) from the sample and weigh two portions of sample at about 10 g (to the nearest 0.01 g). Soil samples One for the determination of dry matter content; the other by adding an appropriate amount of anhydrous sodium sulfate (6.3), grinding into stream sand dehydration; such as If the fruit is extracted by pressurized fluid extraction, it is dehydrated with celite (6.13). One sample of sediment is used to determine the moisture content and the other A reference soil sample is dehydrated. 8.3 Determination of moisture Determination of dry matter content of soil samples performed according to HJ 613, Determination of moisture content of sediment samples in accordance with GB 17378.5 implementation. 8.4 Preparation of test specimens 8.4.1 Extraction 8.4.1.1 Microwave extraction Sample (8.2) was transferred to the extraction tank, and 30 ml acetone-n-hexane mixed solvent I (6.6) was added. Set extraction The temperature was 110 ℃, microwave extraction 10 min. The extract is collected after centrifugation or filtration. 8.4.1.2 Soxhlet extraction The sample (8.2) was transferred to the Soxhlet extractor paper sleeve, 100 ml acetone-n-hexane mixed solvent (I 6.6) Extraction 16 h ~ 18 h, reflux rate of about 3 times/h ~ 4 times/h. The extract is collected after centrifugation or filtration. 8.4.1.3 Pressurized fluid extraction HJ 783 in accordance with the requirements of the extraction. Note. Other equivalent extraction methods may be used if verified. 8.4.2 Dehydration Apply a glass wool or glass fiber filter (6.14) to the glass funnel and apply about 5 g of anhydrous sodium sulfate (6.3), then The extract (8.4.1) was filtered through a funnel directly to the concentration device (7.4), then 5 ml ~ 10 ml of acetone - n-hexane mixed Solvent I (6.6) The container containing the extract was thoroughly washed and filtered through a funnel to the above concentrator. 8.4.3 Concentration After the dehydration at 45 ℃ below the extract (8.4.2) concentrated to 1 ml, to be purified. To replace the solvent system, the extract was concentrated to 1.5 ml ~ 2.0 ml, with 5 ml ~ 10 ml of n-hexane (6.1) Replacement, and then concentrated extract to 1 ml, to be purified. 8.4.4 Purification 8.4.4.1 Sulfuric acid purification If the extract color darker, you can first use sulfuric acid purification to remove most of the oxygenated organic compounds and some organochlorine medicine. The displacement solvent n-hexane extract (8.4.3) was transferred to 150 ml separatory funnel, slowly added 5 ml ~ 10 ml Sulfuric acid (6.5), mix gently and shake for 1 min. Stand aside stratification, discard the sulfuric acid layer. Repeat the above steps several times to sulfur Acid layer colorless. An appropriate volume of potassium carbonate solution (6.8) was added to the n-hexane extract, and after shaking, the layers were allowed to stand and the aqueous phase discarded. This procedure is repeated until the aqueous phase is neutral. Dehydration of the n-hexane extracts is carried out according to the same procedure as in 8.4.2. Note. In the sulfuric acid purification process, to prevent the heat explosion, add sulfuric acid and gently mix, continue to deflate, then slightly violent shake. 8.4.4.2 Magnesium silicate solid phase extraction column purification The magnesium silicate solid phase extraction column (6.11) was washed with about 8 ml of n-hexane (6.1), and the magnesium silicate solid phase extraction column adsorbent Surface infiltration. The concentrated extract (8.4.3) was transferred to a magnesium silicate solid phase extraction column with a straw for 1 min and then discarded Effluent. Add 2 ml acetone-n-hexane mixed solvent Ⅱ (6.7) and stay for 1 min, with 10 ml small concentrated tube to receive wash After degreasing, continue to wash the cartridge with acetone-n-hexane mixed solvent II (6.7) until the volume of the eluate received is 10 ml. Note. If verified, other equivalent methods can also be used to purify. See Appendix C for details. 8.4.5 concentrated volume The purified eluate (8.4.4) according to the 8.4.3 step concentration and volume to 1.0 ml, then transferred to 2 ml sample vial, To be analyzed. 8.5 blank sample preparation A blank sample was prepared according to the same procedure as Sample Preparation (8.4), replacing the actual sample with quartz sand (6.12).

9 Analysis steps

9.1 GC reference instrument conditions Inlet temperature. 250 ℃; Injection mode. splitless injection to 0.75min after opening shunt, split outlet flow of 60ml/min; Carrier gas flow. high purity nitrogen (6.15), 2.0 ml/min, constant current; Makeup gas. high purity nitrogen (6.15), 20 ml/min; Column temperature program. The initial temperature of 100 ℃, 15 ℃/min heating to 220 ℃, hold 5 min, with 15 ℃/min liter Temperature to 260 ℃, hold 20 min; Detector temperature. 280 ℃; Injection volume. 1.0 μl. 9.2 Calibration 9.2.1 The establishment of calibration curve Were appropriate amount of PCB standard solution (6.10), diluted with n-hexane (6.1), the preparation of the standard series, and more The mass concentrations of PCBs were 5.0 μg/L, 10.0 μg/L, 20.0 μg/L, 50.0 μg/L, 100 μg/L,.200 μg/L and 500 μg/L (this is the reference concentration). According to the instrument conditions (9.1) from low concentration to high concentration in order to standard series of solution injection, detection, record the target Retention time, peak height or peak area. The concentration of the target in a standard series of solutions is taken as abscissa, with its corresponding peak height or peak Area for the vertical axis, the establishment of a standard curve. 9.2.2 Standard sample chromatogram Under the recommended instrument reference conditions, the chromatograms for target 1 and 2 are shown in Figure 1 and Figure 2, respectively. 17.5 20 22.5 25 27.5 30 32.5 35 min Hz ECD1 A, (DXN2010 \\ 101117000010.D) 1.PCB28; 2.PCB52; 3.PCB101; 4.PCB81; 5.PCB77; 6.PCB123; 7.PCB118; 8.PCB114; 9.PCB153; PCB105; PCB138; PCB126; PCB1367; PCB146; PCB157; PCB141; PCB169; Figure 1 Reference GC chromatogram of 18 PCB standards (column 1, ρ = 100 μg/L) 1.PCB28; 2.PCB52; 3.PCB101; 4.PCB81; 5PCB777; 6, PCB123; 7.PCB118; 8.PCB114; 9.PCB153; PCB105; PCB138; PCB126; PCB137; PCB167; PCB146; PCB157; PCB141; PCB169; PCB1818. Figure 2 Reference Gas Chromatogram of 18 PCB Standards (Column 2, ρ = 100 μg/L) 9.3 Sample Determination The determination of sample (8.4) is carried out according to the same instrument analysis conditions as established in the standard curve (9.2.1). 9.3.2 Blank test The blank sample (8.5) was measured according to the same instrument analysis conditions as the sample measurement (9.3). 10 Results Calculation and Presentation 10.1 Qualitative analysis According to the retention time of the target qualitative. Before sample analysis, you should establish a retention time window t3S, t for the standard series of solutions 12 14 16 18 20 22 min Hz ECD2 B, (DXN2010 \\ 101220000017.D) In a target within 72 h retention time average, S standard solution of a target in an average retention time standard deviation. When analyzing samples, the target retention time should be within the retention window. When the analysis of the target on the column is detected, it is necessary to use a different polarity of the column to help qualitative. The target is double When the column is detected, as detected, otherwise not detected. 10.2 Quantitative analysis According to the established standard curve (9.2.1), according to the target peak area or peak height, the use of external standard method. 10.3 Results Calculation 10.3.1 Calculation of soil sample results The target soil content ω1 (μg/kg), calculated according to equation (1).  dm mw (1) Where. ω1 - soil samples in the target content, μg/kg; ρ - calculated from the standard curve of the sample mass concentration of the target, μg/L; V-- sample volume, ml; m - Weigh the quality of the sample, g; wdm - dry matter content of the sample,%. 10.3.2 Calculation of results in sediment samples Target sediment content ω2 (μg/kg), calculated according to equation (2).   2   H 2O mw (2) Where. ω2 - sediment sample target content, μg/kg; ρ - calculated from the standard curve of the sample mass concentration of the target, μg/L; V-- sample volume, ml; m - Weigh the quality of the sample, g; wH2O - moisture content of the sample,%. 10.4 results show When the determination result is less than 1.00 μg/kg, the result will remain two digits after the decimal point. When the measurement result is greater than or equal to 1.00 μg/kg, The result retained three significant figures. 11 precision and accuracy 11.1 precision Six laboratories performed a series of six samples of quartz sand spiked at concentrations of 2.00 μg/kg, 20.0 μg/kg and 80.0 μg/kg, respectively The relative standard deviations in the laboratory ranged from 2.1% to 11%, from 1.5% to 7.8% and from 0.49% to 6.2%, respectively Laboratory relative standard deviation ranged from 2.3% to 14%, 1.3% to 8.5% and 1.0% to 3.6%, respectively; the repeatability limits were 0.26 μg/kg ~ 0.44 μg/kg, 1.8 μg/kg ~ 2.8 μg/kg and 3.7 μg/kg ~ 8.7 μg/kg respectively.The reproducibility limits were 0.29 μg/kg ~ 0.78 μg/kg, 2.0 μg/kg to 4.1 μg/kg, 4.0 μg/kg to 9.5 μg/kg. See Appendix B. 11.2 Accuracy Six laboratories tested spiked quartz sand samples spiked at concentrations of 2.00 μg/kg, 20.0 μg/kg and 80.0 μg/kg, respectively The recoveries ranged from 77.0% to 115%, from 73.6% to 104% and from 98.1% to 102%, respectively. The spiked recoveries were the highest The final values were 86.9% ± 15.2% ~ 105% ± 15.2%, 77.5% ± 13.1% ~ 96.4% ± 11.1%, 93.6% ± 1.8% ~ 100% ± 2.5%. Sandy soil spiked at a concentration of 20.0 μg/kg, sediment samples from Taihu Lake at a spiking concentration of......
Image     

Tips & Frequently Asked Questions:

Question 1: How long will the true-PDF of HJ 922-2017_English be delivered?

Answer: Upon your order, we will start to translate HJ 922-2017_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 922-2017_English with my colleagues?

Answer: Yes. The purchased PDF of HJ 922-2017_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+ countries

Question 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 Sales@ChineseStandard.net. 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.