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HJ 711-2014Solid waste-Determination of phenolic compouds. Gas chromatiography (English PDF)

固体废物酚类化合物的测定气相色谱法

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Issued by

Ministry of Ecology and Environment

Level / Type

National · Mandatory

Issue date

November 27, 2014

Implementation date

January 1, 2015

Scope

HJ 711-2014 is the English-translated version of 固体废物酚类化合物的测定气相色谱法.

HJ 711-2014 — Warning. Solvent 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 provides solid waste and solid waste leachate phenolic compounds was measured by gas chromatography. This standard applies to the determination of solid waste leachate phenolic compounds in solid waste and 21 species of other phenolic compounds If the validation is also applicable to this standard.

When the sampling of solid waste was 10.0 g, 21 kinds of phenolic compounds method detection limit of 0.02 ~ 0.33 mg/kg, Detection limit of 0.08 ~ 1.32 mg/kg, see Appendix A. When the sampling of solid waste leachate is 100 ml, 21 kinds of phenolic compounds method detection limit of 0.002 to 0.006 mg/L, detection limit of 0.008 ~ 0.024 mg/L, see Appendix A.

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Document preview — HJ 711-2014

National Standard of the People's Republic of China

Classification: Z 13

Issued by: Ministry of Ecology and Environment

Foreword
1 Gas Chromatography, solid waste phenolic compounds
2 Normative references
3 PRINCIPLE OF THE METHOD
4 Reagents and materials
4.13 Standard solution. rho = 100 mg/L
35 Instruments and equipment
78.2 Calculation Results

Foreword

To implement the "People's Republic of China Environmental Protection Law" and "People's Republic of China Solid Waste Pollution Prevention Law" Protecting the environment, safeguarding human health, standardized monitoring method of solid waste in phenolic compounds, the development of this standard.

This standard provides the solid waste Phenols in Gas Chromatography.

This standard is the first release.

Appendix A of this standard is a normative appendix; Appendix B, Appendix C and 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 November 27, 2014 for approval.

This standard since January 1, 2015 implementation.

The standard explanation by the Ministry of Environmental Protection.

1 Gas Chromatography, solid waste phenolic compounds

Warning. Solvent 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 provides solid waste and solid waste leachate phenolic compounds was measured by gas chromatography.

This standard applies to the determination of solid waste leachate phenolic compounds in solid waste and 21 species of other phenolic compounds If the validation is also applicable to this standard.

When the sampling of solid waste was 10.0 g, 21 kinds of phenolic compounds method detection limit of 0.02 ~ 0.33 mg/kg, Detection limit of 0.08 ~ 1.32 mg/kg, see Appendix A.

When the sampling of solid waste leachate is 100 ml, 21 kinds of phenolic compounds method detection limit of 0.002 to 0.006 mg/L, detection limit of 0.008 ~ 0.024 mg/L, 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.

HJ/T 20 industrial solid waste sampling sample preparation Technical Specifications HJ/T 298 Identification of Hazardous Waste Technical Specifications HJ/T 299 methods for leaching toxicity of solid waste sulfuric acid nitric acid method HJ/T 300 solid waste leaching toxicity Acetic acid buffer solution method HJ 557 solid waste leaching toxicity level oscillation method

3 PRINCIPLE OF THE METHOD

Solid waste or solid waste leachate extraction with a suitable organic solvent, the extract was purified acid distribution, phenolic compounds Substance into the aqueous phase, the aqueous phase was adjusted to acidic phase, extract was dehydrated, concentrated organic solvent extraction with a suitable water volume Backward by gas chromatography, FID measurement, 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 2 prepared by water or water equipment.

4.1 Sodium hydroxide (NaOH).

4.2 hydrochloric acid (HCl). rho = 1.19 g/ml.

4.3 anhydrous sodium sulfate (Na2SO4). baking at 400 °C 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 (NaOH) solution. c (NaOH) = 5 mol/L.

Weigh 20 g of sodium hydroxide (4.1), dissolved in water after cooling 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 ethyl acetate and dichloromethane 4.10. 41.

4.11 methylene chloride mixed solvent of n-hexane. 21.

4.12 Standard stock solution. rho = 1000 mg/L.

It can be purchased directly commercially available certified reference solution, also prepared using standard materials. Include phenol, o - cresol, p - cresol, Room - cresol, 2,4-xylenol, 2-chlorophenol, 2,4-dichlorophenol, 2,6-dichlorophenol, 4-chloro-3-cresol, 2,4,6-tris chlorophenol, 2,4,5 Trichlorophenol, 2,3,4,6-tetra-chlorophenol, chlorophenol 2,3,4,5, 2,3,5,6, pentachlorophenol, 2-nitro-phenol, 4-nitrophenol, 2,4 Dinitrophenol, 2-methyl-4,6-dinitrophenol, 2- (1-methyl - n-propyl) -4,6-dinitrophenol (dinoseb), 2-cyclohexyl 4,6 two Nitrophenol.

4.13 Standard solution. rho = 100 mg/L

With methanol (4.8) diluted stock standard solution (4.12), formulated at a concentration of 100 mg/L of standard solution, 4 °C to Stored in the dark, it can be stored for months.

Quartz sand 4.14 (0.84 ~ 0.297 mm, 20 ~ 50 mesh). Baking 4 h at 400 °C, 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 °C 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.

35 Instruments and equipment

5.1 Gas chromatograph. with a split/splitless inlet, with a hydrogen flame detector (FID).

5.2 Flip oscillating means.

5.3 Column. 30 m × 0.25 mm × 0.25 m, 100% methyl silicone capillary column; or 30 m × 0.25 mm × 0.25 m, 50% 50% phenyl methyl silicone capillary column, capillary column, or other equivalent.

5.4 Extraction equipment. Soxhlet extraction apparatus, the probe can also be used ultrasonic extractor, microwave or pressurized fluid extraction device Extracting means.

5.5 Extraction bottles. 2 L with screw cap and an inner lid of the jar, you can use glass or polytetrafluoroethylene (PTFE) bottle.

5.6 concentration device. a rotary evaporator means or KD concentrators, nitrogen blowing instrument, such as concentrated a considerable performance devices.

5.7 funnel. with polytetrafluoroethylene (PTFE) stoppers.

5.8 micro syringe. 10 µl, 25 µl, 100 µl, 250 µl, 500 µl and 1000 µl.

5.9 mortar. made of glass, agate or other non-interfering substance material.

5.10 General common laboratory instruments and equipment.

6 samples

6.1 Sample Collection and preservation According to HJ/T 20, HJ/T 298 with the relevant provisions of solid waste collected representative 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 14 d. Avoid organic interference. Sample extract dark cold storage, shelf life 40 d.

6.2 Preparation of the sample

6.2.1 Preparation of solid waste leachate sample

6.2.1.1 Leaching

Weigh 100 g samples, as required in accordance with HJ/T 299, HJ/T 300 HJ 557 or leachate sample preparation.

6.2.1.2 Purification Take 6.2.1.1 Solid waste leachate in 100 ml separating funnel (5.6), treated with NaOH solution (4.4) adjusted to pH > 12, was added 30 ml of dichloromethane and a mixed solvent of n-hexane (4.11), thoroughly shaken and allowed to stand, the lower layer was discarded and the organic Phase, 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.

6.2.1.3 extraction and concentration

4 The aqueous phase is adjusted to retain section 6.2.1.2 with hydrochloric acid solution (4.5) to pH 12, thoroughly shaken and allowed to stand, the lower organic phase was discarded, the aqueous phase retained portion.

Note. If the organic phase darker, adding an appropriate amount of methylene chloride and n-hexane solvent mixture (4.11), an increase of 2 to 3 times the number of purification, to the organic phase was substantially colorless.

6.2.2.3.4 extraction and concentration Press 6.2.1.3 steps.

7 Procedure

7.1 GC reference conditions Inlet temperature. 260 °C; injection mode. split or not to split; injection volume. 1.0 ~ 2.0 µl. Oven temperature program.

80 °C held 1.0 min, at a heating rate of 10 °C/min and held raised to 250 °C 4.0 min; FID detector temperature.

280 °C. 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.

62.5 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 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, 18-2-Methyl-4,6-dinitrophenol, pentachlorophenol 19-, 20-2- (1-methyl - n-propyl) -4,6-dinitrophenol (dinoseb), 21-2 - cyclohexyl-4,6 two Nitrophenol

Figure 121 phenols reference chromatogram

7.4 Determination

The prepared sample (6.2) in accordance with the GC reference conditions (7.1) were measured.

7.5 blank test

Solid waste leachate blank. Weigh 100.0 g of quartz sand (4.14), according to the sample preparation step 6.2.1, according to gas GC reference conditions (7.1) were measured.

Solid waste Blank. Weigh 10.0 g of quartz sand (4.14), according to step 6.2.2 A sample was prepared in accordance with the GC reference Test conditions (7.1) were measured.

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 calibration standard flat material retention time I mean, when S is the first calibration standard deviation of each standard retention time. When the sample analysis, the target compound with a retention Room should be retained within the time window. Target compound analysis column retention time (non-polar) on Appendix B.

78.2 Calculation Results

8.2.1 Calculation component concentrations in the leachate of solid wastes the target compound with external standard content (mg/L) of each solid waste leachate phenolic compounds according to formula (1) Calculated.

Where. rhoi-- concentration of target compounds in the sample, mg/L;

rhoi1-- calculate the mass concentration of the resulting target compound, mg/L by the calibration curve;

V1-- constant volume sample volume, ml;

V2-- leachate sample volume, ml.

8.2.2 solid waste component content calculated the target compound with external standard, the content of solid waste each phenolic compounds (mg/kg) according to the formula (2) Calculations.

Wherein. the content of the target compound omegai-- sample, mg/kg;

rhoi-- calculate the mass concentration of the resulting target compound, mg/L by the calibration curve;

V-- constant volume sample volume, ml;

Quality m-- solid waste samples (wet weight), g.

8.3 The results are shown

8.3.1 When the solid waste leachate results than or equal to 1.00 mg/L, the result of three significant figures; less than 1.00 mg/L when the results to two decimal places to retain.

8.3.2 When the content of the solid waste material results than or equal to 1.00 mg/kg, the results of three significant figures; less than 1.00 when mg/kg, the results of reservations to two decimal places.

8.3.3 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 concentrations were 0.05 mg/kg and 3.16 mg/kg ~ 14.5 mg/kg of solid unity

8 Waste samples were measured in the laboratory relative standard deviation range. 3.8% ~ 0.9% ~ 40.7% and 20.2%, inter-laboratory the relative standard deviation. 8.9% ~ 6.2% ~ 30.7% and 29.7%, reproducibility range limit. 0.01 mg/kg ~ 0.05 mg/kg and 1.33 mg/kg ~ 3.34 mg/kg, reproducibility range limit. 0.02 mg/kg ~ 0.08 mg/kg and 2.84 mg/kg ~ 28.5 mg/kg.

Six laboratories of the target compound concentrations were 0.005 mg/L, 0.05 mg/L and 0.20 mg/L of a unified solid waste Leachate samples were measured in the laboratory relative standard deviation of 2.5% ~ 43.3%, 1.1% and 2.4% ~ 25.6% 18.6%; interlaboratory relative standard deviation of 8.0% ~ 38.3%, 44.2% and 6.5% ~ 3.1% ~ 47.5%. Reproducibility limit Range. 0.001 mg/L ~ 0.011 mg/L, 0.009 mg/L ~ 0.024 mg/L and 0.022 mg/L ~ 0.064 mg/L; then Reproducibility range limit. 0.001 mg/L ~ 0.021 mg/L, 0.010 mg/L ~ 0.106 mg/L and 0.033 mg/L ~ 0.293 mg/L.

9.2 Accuracy

Six laboratories for solid waste matrix spiked, amount was 10.0mg/kg, the recoveries of target compounds in the range of 62.3% to 106%.

Six laboratories of solid waste leachate spiked measurement matrix, spiked amount was 0.05 mg/L and 0.20 mg/L, and the recovery range of the target compound was 63.1% ~ 72.0% ~ 101% and 102%.

Specific method precision and accuracy of data 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, 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 at least an analysis of actual samples spiked with a spiked parallel. The actual sample 9 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, then the presence of the sample matrix effects in results Noted.

11 Notes

11.1 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.

11.2 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 m, 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 in Appendix D.

12 waste disposal

Waste generated test reagent containing the central depository shall send qualified unit centralized treatment.

Appendix A

(Normative)

The detection limit and lower limit of determination the detection limit and determination limit of the method in Schedule A no. Ingredient name Solid waste leachate solid waste the detection limit ...

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