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HJ 703-2014 English PDF

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HJ 703-2014: Soil and sediment-Determination of phenolic compounds.
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Basic data

Standard ID HJ 703-2014 (HJ703-2014)
Description (Translated English) Soil and sediment-Determination of phenolic compounds.
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z18
Word Count Estimation 15,123
Date of Issue 9/15/2014
Date of Implementation 12/1/2014
Quoted Standard GB 17378.3; GB 17378.5; HJ/T 166; HJ 613
Regulation (derived from) Ministry of Environmental Protection Notice 2014 No. 60
Issuing agency(ies) Ministry of Ecology and Environment
Summary This Standard specifies the determination by gas chromatography on soil and sediments phenolic compounds. This Standard applies to the determination of soil and sediment of 21 kinds of phenolic compounds, other phenolic compounds may also be applied if ve

HJ 703-2014: Soil and sediment-Determination of phenolic compounds.

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Soil and sediment-Determination of phenolic compounds. People's Republic of China National Environmental Protection Standards Determination of phenolic compounds in soil and sediment Gas chromatography -Gas Chromatography (release draft) Issued on.2014-09-15 2014-12-01 implementation Ministry of Environmental Protection released

Table of Contents

Preface .ii 1. Scope ..1 2 Normative references ..1 3 principle of the method ..1 4 Reagents and materials .1 5. Apparatus .2 6 .3 Sample 8 represents the results of calculation and ..5 9 precision and accuracy ..6 10 Quality Assurance and Quality Control .7 11 waste treatment 7 12 Note 7 Appendix A (normative) Determination of the detection limit and a lower limit ..9 Annex B (informative) of the title compound with a retention time and reference .10 Annex C (informative) method precision and accuracy .11 Annex D (normative) assisted qualitative reference chromatogram .12

Foreword

To implement the "People's Republic of China Environmental Protection Law", protecting the environment, safeguarding human health, regulate soil and sediment Determination of phenolic compounds, the development of this standard. This standard specifies the gas chromatographic determination of soil and sediment phenolic compounds. This standard is the first release. The Standard Appendix A normative annex, appendix B ~ Appendix D is an informative annex. This standard is developed by the Ministry of Environmental Protection Science, Technology organization. This standard is mainly drafted by. Nanjing Environmental Monitoring Center. The standard verification. Jiangsu Provincial Environmental Monitoring Center, Changzhou Municipal Environmental Monitoring Center, Taizhou City Environment Monitoring Central station, Zhenjiang Municipal Environmental Monitoring Center, Ningbo Municipal Environmental Monitoring Center Station and the physical and chemical testing center in Jiangsu Province. This standard MEP September 15, 2014 for approval. This standard shall be December 1, 2014 implementation. The standard explanation by the Ministry of Environmental Protection. Gas chromatography of phenolic compounds in soil and sediment Warning. Reagents and standard solutions used in the experiment on human health hazards, the operation should be carried out in a hood, Prescribed wear protective equipment to avoid skin contact.

1 Scope

This standard specifies the gas chromatographic determination of soil and sediment phenolic compounds. This standard applies to the determination of phenolic compounds in soil sediments and 21 species of other phenolic compounds if verified Also apply to this standard. When the sample volume is 10.0 g, 21 kinds of phenolic compounds method detection limit of 0.02 ~ 0.08 mg/kg, detection limit is 0.08 ~ 0.32 mg/kg. See Appendix A.

2 Normative references

This standard refers to the contents of the following documents or the terms. For undated references, the effective version suitable For this standard. GB 17378.3 specification for marine monitoring Part 3 sample collection, storage and transport GB 17378.5 specification for marine monitoring Part 5 Analysis of Sediments HJ/T 166 soil environmental monitoring technical specifications HJ 613 Determination of dry matter and soil moisture weight method

3 PRINCIPLE OF THE METHOD

Soil or sediment with a suitable organic solvent extraction, the extract was purified acid distribution, phenolic compounds into the aqueous phase, The aqueous phase was adjusted to acidic water and extracted with a suitable organic solvent phase, the extract was dehydrated, concentrated, backward constant volume Gas Chromatography Separation, hydrogen flame detector. Retention time qualitative, external standard.

4 Reagents and materials

Unless otherwise indicated, the use of chemical reagents analytical line with national standards of analysis, the experiment doubly distilled water Or prepared by pure water equipment. 4.1 Sodium hydroxide (NaOH). 4.2 hydrochloric acid (HCl). ρ = 1.19 g/ml. 4.3 anhydrous sodium sulfate (Na2SO4). baking at 400 ℃ for 4 h, cooled to room temperature and placed in a desiccator, was transferred to a glass grinding mouth Glass bottle and stored in a desiccator. 4.4 Sodium hydroxide solution. c (NaOH) = 5 mol/L. The solid weighed 20 g NaOH (4.1), cooled with water to dissolve and dilute to 100 ml. 4.5 hydrochloric acid solution. c (HCl) = 3 mol/L. Measure 125 ml of hydrochloric acid (4.2), diluted to 500 ml. 4.6 dichloromethane (CH2Cl2). chromatography. 4.7 ethyl acetate (CH3COOC2H5). chromatography. 4.8 methanol (CH3OH). chromatography. 4.9 n-hexane (C6H14). chromatography. A mixed solvent of dichloromethane and 4.10 ethyl acetate. 4 1 (V/V). A mixed solvent of dichloromethane and 4.11 hexane. 2 1 (V/V). 4.12 Standard stock solution. ρ = 1000 mg/L. Can be purchased directly certified standard solution including all relevant analytes can also be used pure reference material prepared. Include phenol, O - cresol, p - cresol, m - cresol, 2,4-xylenol, 2-chlorophenol, 2,4-dichlorophenol, 2,6-dichlorophenol, 4-chloro-3- cresol, 2,4,6-trichlorophenol, 2,4,5-trichlorophenol, 2,3,4,6-tetra-chlorophenol, 2,3,4,5-chlorophenol, 2,3,5, 6-tetrafluoro, pentachlorophenol, 2- Nitrophenol, 4-nitrophenol, 2,4-dinitrophenol, 2-methyl-4,6-dinitrophenol, 2- (1-methyl - n-propyl) -4,6 dinitrophenol (ground Dinoseb), 2-cyclohexyl-4,6-dinitrophenol. 4.13 standard solution. ρ = 100 mg/L. With methanol (4.8) diluted stock standard solution (4.12), formulated at a concentration of 100 mg/L of standard solution at 4 ℃ Refrigerator away from light, sealed save one month. Quartz sand 4.14 (0.84 ~ 0.297 mm, 20 ~ 50 mesh). Baking 4 h at 400 ℃, placed in a desiccator to cool to room Temperature, transferred to a grinding mouth glass bottles, stored in a desiccator. Celite 4.15 (0.15 ~ 0.038 mm, 100 ~ 400 mesh). baking at 400 ℃ for 4 h, placed in a desiccator and cooled to Room temperature, transferred to a grinding mouth glass bottles, stored in a desiccator. 4.16 Nitrogen (N2). purity ≥ 99.999%. 4.17 Hydrogen (H2). purity ≥ 99.999%. 4.18 paper sleeve with Soxhlet apparatus supporting. Before use, check the residual amount of phenolic compounds, to avoid interference. 5. Apparatus 5.1 Gas chromatograph. with a split/splitless inlet, with a hydrogen flame detector (FID). 5.2 Column. 30 m × 0.25 mm × 0.25 μm, 100% methyl silicone capillary column; or 30 m × 0.25 mm × 0.25 μm, 50% 50% phenyl methyl silicone capillary column, capillary column, or other equivalent. 5.3 Extraction equipment. Soxhlet extraction apparatus, the probe can also be used ultrasonic extractor, microwave or pressurized fluid extraction device Extracting means. 5.4 funnel. with polytetrafluoroethylene (PTFE) stoppers. 5.5 concentration device. a rotary evaporator means or KD concentrators, nitrogen blowing instrument, such as concentrated a considerable performance devices. 5.6 mortar. made of glass, agate or other non-interfering substance material. 5.7 micro syringe. 10 μl, 25 μl, 100 μl, 250 μl, 500 μl and 1000 μl. 5.8 General Commonly used laboratory instruments and equipment.

6 samples

6.1 Sample Collection and preservation Soil samples were collected in accordance with HJ/T relevant provisions of 166. According to GB 17378.3 and GB 17378.5 relevant Provisions collect sediment samples. In brown glass bottles, should be analyzed as soon as possible after sample collection enclosed storage. If not timely analysis should be refrigerated from light, Retention period of 10 d. Avoid organic interference. Sample extract dark cold storage, shelf life 40 d. 6.2 Preparation of the sample 6.2.1 Dehydration Removal of a sample of foreign objects (stones, blades, etc.), weigh about 10 g (accurate to 0.01 g) in duplicate samples, soil samples A product according to HJ 613 Determination of dry matter content, another adding an appropriate amount of anhydrous sodium sulfate (4.3), are milled into quicksand Like, such as using pressurized fluid extraction, then dehydrated with diatomaceous earth (4.15). A sediment sample measured in accordance with GB 17378.5 Fixed moisture content, another reference soil samples dehydration. 6.2.2 Extraction Alternatively Soxhlet extraction, pressurized fluid extraction, ultrasonic extraction and microwave extraction any way desired compound extract. 6.2.2.1 Soxhlet 6.2.1 The sample was fully transferred to the paper sleeve (4.18), add 100 ml of methylene chloride and n-hexane mixed Co-solvent (4.11) and extracted 16 ~ 18 h, the reflux rate controlled at 10 times/h or so, after cooling to collect all extracts prepared Net Of use. 6.2.2.2 pressurized fluid extraction According to a sample obtained 6.2.1 Volume Select the appropriate extraction cell, sample loading, methylene chloride and n-hexane mixed solvent Agent (4.11) as the extraction solvent, the following reference conditions for extraction. extraction temperature of 100 ℃, extraction pressure of 1500 psi, Static extraction time 5 min, elution volumes of 60% of the cell volume, nitrogen purge time 60 s, extraction cycles twice. and also You can refer to the instrument manufacturers instructions set conditions. The extract was collected, to be purified. 6.2.2.3 ultrasonic extraction 6.2.1 sample volume obtained according to choose the right Erlenmeyer flask, add the amount of methylene chloride and n-hexane mixed solvent (4.11), making up at least a solid surface 2 cm, the ultrasound probe is placed below the liquid surface, the ultrasonic extraction 3 times 3 min, Control the extraction temperature does not exceed 40 ℃ (can be conical flask in an ice-water bath), the combined extracts were to be purified. 6.2.2.4 microwave extraction The sample was transferred to a microwave extraction 6.2.1 was special container, adding an appropriate amount of a mixed solvent of dichloromethane and hexane (4.11), the liquid level must not over-sample and less than 2/3 of the depth of the container (sample can be divided into multiple separate excessive extraction, and finally close And extract). Microwave extraction reference conditions. power 800 W, within 5 min to warm to 75 ℃, maintained 10 min. Be extracted After cooling liquid filtration, mixed with the amount of solvent (4.11) and wash the container wall sample collected extract, to be purified. 6.2.3 Purification 6.2.2 The extract was transferred to a separatory funnel (5.4), and twice the volume of the aqueous extract with NaOH Solution (4.4) was adjusted to pH > 12, thoroughly shaken and allowed to stand, the lower organic phase was discarded, the aqueous phase retained portion. NOTE. If the darker the organic phase may be appropriate to increase the number of times to purify the 2 or 3 times. 6.3 extraction and concentration 6.2.3 The obtained portion was washed with aqueous hydrochloric acid solution (4.5) adjusted pH < 2, plus 50 ml of methylene chloride and ethyl acetate A mixed solvent of an ester (4.10), thoroughly shaken and allowed to stand, the aqueous phase was discarded, the organic phases were provided with an appropriate amount of anhydrous sodium sulfate (4.3) The addition funnel a mixture of water (4.10) and ethyl acetate rinse well with dichloromethane sodium sulfate, all organic phases were combined, Volume was concentrated to 1.0 ml, to be measured.

7 Procedure

7.1 GC reference conditions Inlet temperature. 260 ℃; injection mode. split or not to split; injection volume. 1.0 μl. Oven temperature program. 80 ℃ held 1.0 min, at a heating rate of 10 ℃/min and held raised to 250 ℃ 4.0 min; FID detector temperature. 280 ℃. Within the column carrier gas flow rate. 1.0 ml/min; makeup. nitrogen, flow rate. 30 ml/min; flow rate of hydrogen. 35 ml/min; Air flow rate. 300 ml/min. 7.2 Calibration Exact Pipette stock standard solution (4.12) 5.0μl, 25.0μl, 100μl, 250μl and 500μl in 5 ml flask, Mixed with methylene chloride and ethyl acetate solvent (4.10) diluted to the mark, the preparation of the calibration series, the concentration of the target compound, respectively Of 1.00 mg/L, 5.00 mg/L, 20.0 mg/L, 50.0 mg/L and 100 mg/L. Instrument under recommended conditions (7.1) into Line measurements to the concentration of each component as abscissa, to the component peak area (or height) as ordinate plotted calibration curve. 7.3 reference chromatogram According to gas chromatography reference conditions (7.1) analysis, 21 kinds of phenolic compounds in 100% methyl polysiloxane (non-polar) Reference chromatogram column on Figure 1. Elution order. 1 - Phenol, 2- 2-chlorophenol, 3-o - cresol, 4/5-p/m - cresol, 6-2- nitrophenol, 7-2,4-di-p-cresol , 8- 2,4-dichlorophenol, 2,6-dichlorophenol 9-, 10- 4-chloro-m-cresol, 11-2,4,6- trichlorophenol, 12-2,4,5 - trichlorophenol, 13-2,4- Dinitrophenol, 14-4- nitrophenol, 15-2,3,4,6- tetrachlorophenol, 16/17- 2,3,4,5-chlorophenol/2,3,5,6 - four chlorophenol, methyl-4,6-18-2- Dinitrophenol, 19- pentachlorophenol, 20-2- (1-methyl - n-propyl) -4,6-dinitrophenol (dinoseb), 21-2- cyclohexyl-4,6 dinitrophenol Figure 121 phenols reference chromatogram 7.4 Determination The prepared sample (6.3) in accordance with the GC reference conditions (7.1) were measured. 7.5 blank test Weigh 10.0 g of quartz sand (4.14), according to the sample preparation step from 6.2 to 6.3, according to gas chromatography reference conditions (7.1) Determination.

8 represents the results of calculation and

8.1 Qualitative target compound Sample analysis should be established retention time windows t ± 3S. t when the initial concentration of each standard calibration material retention time Average initial calibration when S is the standard deviation of each standard retention time. When the sample analysis, the target compound with a retention Retention time should be within the time window. Target compound analysis column retention time (non-polar) on Appendix B. 8.2 Calculation Results The target compound with external standard, the content of phenolic compounds in soil (mg/kg) according to formula (1) is calculated, 2.5 5.0 7.5 10.0 12.5 15.0 17.5 min 0.00 0.25 0.50 0.75 1.00 1.25 twenty one Sediment content of phenolic compounds (mg/kg) according to the formula (2) is calculated. dm i wm × = ρω (1) Wherein. the content of the target compound ωi-- sample, mg/kg; ρi-- calculate the mass concentration of the resulting target compound, mg/L by the calibration curve; V-- constant volume sample volume, ml; Quality m-- soil sample (wet weight), g; Soil samples wdm-- dry matter content,%. ) 1 (wm Vi i - × = ρω (2) Wherein. the content of the target compound ωi-- sample, mg/kg; ρi-- calculate the mass concentration of the resulting target compound, mg/L by the calibration curve; V-- constant volume sample volume, ml; Quality m-- sediment sample (wet weight), g; w-- sediment sample moisture content,%. 8.3 The results are shown 8.3.1 When the result is greater than equal to 1.00 mg/kg, the result of three significant figures; less than 1.00 mg/kg, the result Reserved to two decimal places. 8.3.2 Inter - cresol and p - cresol, 2,3,4,5-chlorophenol and 2,3,5,6-chlorophenol difficult separation of substances on the measurement results difficult Separation of substances and for the two.

9 precision and accuracy

9.1 Precision Six laboratories of the target compound concentration of about 0.05 mg/kg, 0.65 mg/kg ~ 3.63 mg/kg and 2.58 mg/kg ~ 6.46 mg/kg of unified samples were measured in the laboratory relative standard deviation of 3.8% ~ 40.7%, 24.4% and 1.6% 2.1% 20.4%; interlaboratory relative standard deviation of 8.9% ~ 30.7%, 56.0% and 13.3% ~ 22.2% ~ 41.6%; Reproducible range limit. 0.01 mg/kg ~ 0.05 mg/kg, 0.14 mg/kg ~ 1.03mg/kg and 0.48 mg/kg ~ 1.40 mg/kg; reproducibility range limit. 0.02 mg/kg ~ 0.08 mg/kg, 0.42 mg/kg ~ 5.72 mg/kg and 1.81 mg/kg ~ 7.58 mg/kg. 9.2 Accuracy Six laboratories actual sediment samples of two different concentrations of matrix spiked sample measured, the amount of matrix spiked 1.00 mg/kg and 4.00 mg/kg, the recoveries range of the target compound. 59.1% ~ 89.2% and 61.8% ~ 95.9%. Specific method precision and accuracy of the data provided in Appendix C. 10 Quality Assurance and Quality Control 10.1 calibration curve Linear calibration curve fitting, and the correlation coefficient should be greater than or equal 0.995, or need to re-draw the calibration curve. 10.2 Calibration Verification Each analysis should select the calibration curve calibration curve for an intermediate concentration of the sample prior to verification, the measurement results relative deviation should ≤30%, otherwise it should be re-calibration curve. 10.3 Blank Each batch of samples to be simultaneously a blank test. Blank results should be less than the target compound concentration detection limit. Parallel sample measured 10.4 Each batch of samples (up to 20 samples) shall be measured at least once parallel, parallel twin-like measurement results relative deviation should Less than 30%. 10.5 actual spiked and spiked parallel Each batch of samples (up to 20 samples) should be analyzed at least one actual samples spiked with a spiked parallel. The actual sample Product recoveries should be between 50% to 140% and the parallel sample measurement results relative deviation should be less than 30%. If the recovery rate below standard, and spiked in parallel to meet the requirements, indicating the presence of the sample matrix effects, note in results Bright. 11 waste disposal Waste generated test reagent containing the central depository shall send qualified unit centralized treatment. 12 Notes 12.1 calibration curve range Calibration curve concentration range may be suitably adjusted according to the actual sample concentration. Low concentration profile available standard solution (4.13) Formulated. 12.2 actual samples For samples exceeding the upper limit of the target compound of the calibration curve can be diluted or reduce the amount of re-sampling analysis. The instrument will sample containing a high concentration of phenolic compounds memory effect, should then analyze one or more blank Product until after the results of blank test meet the quality control requirements in order to analyze the next sample. When necessary, can be 30 m × 0.25 mm × 0.25 μm, 50% to 50% phenyl methyl polysiloxane (medium polarity) capillary Do the qualitative secondary confirmation column, mass spectrometry can also be used for further confirmation. Qualitative auxiliary column chromatography reference conditions see 7.1, color Spectrum See Appendix D.

Appendix A

(Normative) The detection limit and lower limit of determination Table A detection limit and lower limit of determination No. Ingredient name detection limit (mg/kg) detection limit (mg/kg) 1 phenol 0.04 0.16 22- chlorophenol 0.04 0.16 3 o - cresol 0.02 0.08 4/5 p/m - cresol 0.02 0.08 62- nitrophenol 0.02 0.08 7 2,4-cresol 0.02 0.08 8 0.03 0.12 2,4-dichlorophenol 2,6-dichlorophenol 0.03 9 0.12 104--chloro-3-cresol 0.02 0.08 11 2,4,6-trichlorophenol 0.03 0.12 12 2,4,5-trichlorophenol 0.03 0.12 13 2,4-dinitrophenol 0.08 0.32 144- nitrophenol 0.04 0.16 15 0.02 0.08 2,3,4,6-tetra-chlorophenol 16/17 2,3,4,5-chlorophenol/2,3,5,6-chlorophenol 0.03 0.12 182- methyl-4,6-dinitrophenol 0.03 0.12 PCP 19 0.07 0.28 2- (1-methyl - n-propyl) -4,6-dinitrophenol (Dinoseb) 0.02 0.08 212- cyclohexane-4,6-dinitrophenol 0.02 0.08

Appendix B

(Informative) Retention time of the target compound and reference Table B phenolic compounds on a non-polar column reference retention time No. Ingredient name English name keep time* (Min) 1 Phenol Phenol 4.76 22- Chlorophenol 2-Chlorophenol 5.05 3 o - cresol 2-Methylphenol 5.70 4/5 p/m - cresol 4-Methylphenol/3-Methylphenol 6.05 62- nitrophenol 2-Nitrophenol 6.80 7 2,4-cresol 2,4-Dimethylphenol 6.99 8 2,4-dichlorophenol 2,4-Dichlorophenol 7.38 9 2,6-dichlorophenol 2,6-Dichlorophenol 7.82 104--chloro-3-cresol 4-Chloro-3-methylphenol 8.89 11 2,4,6-trichlorophenol 2,4,6-Trichlorophenol 9.89 12 2,4,5-trichlorophenol 2,4,5-Trichlorophenol 9.98 13 2,4-dinitrophenol 2,4-Dinitrophenol 11.43 144- Nitrophenol 4-Nitrophenol 11.82 15 2,3,4,6-tetra-chlorophenol 2,3,4,6-Tetrachlorophenol 12.05 16/17 2,3,4,5-chlorophenol/2,3,5,6-chlorophenol 2,3,4,5-Tetrachlorophenol/2,3,5,6-Tetra 12.52 182- methyl-4,6-dinitrophenol, 2-Methyl-4,6-dinitrophenol 13.03 19 PCP Pentachlorophenol 14.95 2- (1-methyl - n-propyl) -4,6-dinitrophenol (Dinoseb) 2-sec-butyl-4,6-dinitrophenol 15.49 212- cyclohexane-4,6-dinitrophenol, 2-Cyclohexyl-4,6-dinitrophenol 19.18 * Note. The table in accordance with a retention time of 7.1 under the recommended conditions obtain.

Appendix C

(Informative) The precision and accuracy Table C method precision and accuracy Compound name Spiking levels (Mg/kg) average value (Mg/kg) Laboratory phase Standard deviation (%) Laboratory phase Standard deviation (%) Repeatability Limit r (Mg/kg) Reproducibility Limit R (Mg/kg) PSP 2 ± (%) 1.00 0.84 3.5 ~ 24.4 27.4 0.21 0.67 80.9 ± 21.7 phenol 4.00 3.04 2.0 ~ 19.0 27.9 0.48 2.42 72.1 ± 18.1 1.00 0.84 2.2 ~ 20.6 26.7 0.18 0.65 80.3 ± 19.4 2- chlorophenol 4.00 3.61 2.1 ~ 15.3 31.2 0.55 3.19 87.1 ± 32.3 1.00 0.82 2.0 ~ 9.4 31.8 0.14 0.74 78.6 ± 30.2 o - cresol 4.00 3.52 3.8 ~ 17.5 36.7 0.56 3.65 86.7 ± 45.6 2.00 1.77 1.8 ~ 13.5 35.7 0.32 1.79 82.0 ± 44.6 p/m - cresol 8.00 7.25 2.1 ~ 11.9 33.7 0.93 6.90 86.2 ± 38.1 1.00 0.95 2.9 ~ 17.1 33.7 0.16 0.91 89.2 ± 32.9 2- nitrophenol 4.00 3.94 2.1 ~ 19.0 36.1 0.67 4.03 95.9 ± 47.2 1.00 0.74 1.8 ~ 21.4 31.8 0.13 0.67 72.8 ± 25.9 2, 4- xylenol 4.00 3.32 3.7 ~ 20.4 31.7 0.56 2.99 81.0 ± 29.1 1.00 0.83 4.2 ~ 15.1 28.7 0.19 0.69 79.6 ± 24.1 2, 4- dichl...

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