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HJ 892-2017 English PDF

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HJ 892-2017: Solid waste. Determination of polycyclic aromatic hydocarbons. High performance liquid chromatography
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Basic data

Standard ID HJ 892-2017 (HJ892-2017)
Description (Translated English) Solid waste. Determination of polycyclic aromatic hydocarbons. High performance liquid chromatography
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z13
Classification of International Standard 13.030.10
Word Count Estimation 20,229
Date of Issue 2017-12-17
Date of Implementation 2018-02-01
Quoted Standard HJ 782; HJ/T 20; HJ/T 298; HJ/T 299; HJ/T 300
Regulation (derived from) Ministry of Environmental Protection Bulletin 2017 No. 73
Issuing agency(ies) Ministry of Ecology and Environment
Summary This standard specifies high performance liquid chromatography for the determination of polycyclic aromatic hydrocarbons in solid wastes and their leachates. This standard applies to solid wastes and leachates of naphthalene, pinene, anthraquinone, anthraquinone, phenanthrene, anthraquinone, fluoranthene, anthraquinone, benzo[a]anthraquinone, dibenzothiophene, benzo[b]fungi, benzo[k] Onions, benzo[a, h]anthracene, dibenzo[a, h]anthracene, benzo[g, h, i] oxime, and indole [1, 2, 3-c, dJ flower, etc.] Determination of cyclic aromatics. When the solid waste (ashes) sample volume is 10.0 g and the volume constant volume is 1.0 ml, the detection limit of 16 PAHs with a UV detector is 3 to 5 ��g/kg, and the lower limit of measurement is 12 to 20 ��g/kg. Determination of 15 PAHs (without terpenes) using a fluorescence detector The detection limit is 0

HJ 892-2017: Solid waste. Determination of polycyclic aromatic hydocarbons. High performance liquid chromatography


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(Solid waste - Determination of polycyclic aromatic hydrocarbons - High performance liquid chromatography) People's Republic of China national environmental protection standards Determination of polycyclic aromatic hydrocarbons in solid waste High performance liquid chromatography Solid waste-Determination of polycyclic aromatic hydocarbons -High performance liquid chromatography 2017-12-17 Published 2018-02-01 implementation Ministry of Environmental Protection released i directory Foreword .ii 1 scope of application .1 2 Normative references .1 3 method principle .1 4 Reagents and materials .2 5 instruments and equipment .3 6 samples .3 7 Analysis steps .6 8 Results Calculation and Presentation .8 9 Precision and accuracy .9 10 Quality Assurance and Quality Control ..10 11 Waste treatment .10 Appendix A (Normative) Method detection limit and lower limit of determination Appendix B (informative) method of precision and accuracy 13

Foreword

In order to carry out "Law of the People's Republic of China on Environmental Protection" and "Law of the People's Republic of China on Prevention and Control of Environmental Pollution by Solid Wastes" Protection of the environment, protect human health, standardize the determination of solid waste and polycyclic aromatic hydrocarbons in leachate, the development of this standard. This standard specifies the determination of solid waste and leaching solution of polycyclic aromatic hydrocarbons by high performance liquid chromatography. This standard Appendix A normative appendix, Appendix B is an informative annex. 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. Henan Environmental Monitoring Center. This standard verification unit. Institute of Hydrogeology and Environmental Geology, Chinese Academy of Geological Sciences, Henan Province Environmental Monitoring Center, Zheng State Environmental Protection Monitoring Center Station, Kaifeng City Environmental Monitoring Station, Luoyang City Environmental Monitoring Station and Xinxiang City Environmental Monitoring Station. This standard MEP approved on December 17,.2017. This standard since February 1,.2018 implementation. This standard is interpreted by the MEP. Solid waste - Determination of polycyclic aromatic hydrocarbons - High performance liquid chromatography Warning. Polycyclic aromatic hydrocarbons are carcinogens, standard solution preparation and sample preparation should be carried out in a fume hood; operation Wear protective equipment as required to avoid direct contact with skin and clothing.

1 scope of application

This standard specifies the determination of solid waste and leaching solution of polycyclic aromatic hydrocarbons by high performance liquid chromatography. This standard applies to solid waste and leachate naphthalene, camphene, 苊, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo [a] Anthracene, acenaphthene, benzo [b] fluoranthene, benzo [k] fluoranthene, benzo [a] pyrene, dibenzo [a] anthracene, benzo [g, h, i] [1,2,3-c, d] Pyrene and other 16 kinds of PAHs determination. Solid waste (ash) sampling volume of 10.0 g, the volume of 1.0 ml when measured by UV detector 16 kinds of more The detection limit of the method for the determination of aromatics is from 3 μg/kg to 5 μg/kg, and the lower limit of determination is from 12 μg/kg to 20 μg/kg. The fluorescence detection The detection limit of 15 PAHs (excluding acenaphthylene) is 0.3 μg/kg ~ 0.5 μg/kg, and the lower limit of determination is 1.2 μg/kg ~ 2.0 μg/kg. Solid waste (sludge) sampling volume of 2.00 g, the volume of 1.0 ml, the UV detector measured more than 16 species The detection limit of the method for detecting aromatic hydrocarbons is 0.02 mg/kg and the lower limit of determination is 0.08 mg/kg. Fifteen polycyclics Aromatics (excluding acenaphthylene) method detection limit of 0.002 mg/kg ~ 0.004 mg/kg, the lower limit of determination of 0.008 mg/kg ~ 0.016 mg/kg. Solid waste leachate sampling volume of 100 ml, the volume of 1.0 ml, with UV detector determination of 16 kinds of multi-ring Aromatics detection limit of 0.1 μg/L ~ 2 μg/L, the lower limit of determination of 0.4 μg/L ~ 8 μg/L; with a fluorescence detector The detection limits of 15 polycyclic aromatic hydrocarbons (excluding camphene) were from 0.01 μg/L to 0.1 μg/L with the detection limit of 0.04 μg/L ~ 0.4 μg/L. Methods for detecting solid waste and solid waste leachate detection limits and lower limit see Appendix A.

2 Normative references

This standard references the following documents or the terms. For undated references, the effective version applies to this book standard. HJ 782 Solid waste - Extraction of organic matter - Pressurized fluid extraction HJ/T 20 Industrial solid waste sampling Sampling specifications HJ/T 298 Hazardous Waste Identification Technical Specifications Solid waste extraction toxicity Toxicity method HNO3 method HJ/T 300 solid waste leaching toxic leaching method acetic acid buffer solution method

3 method principle

Polycyclic aromatic hydrocarbons (PAHs) in solid waste or solid waste leachate are extracted with organic solvents and the extract is concentrated and purified to high 2-performance liquid chromatography, UV/fluorescence detector to determine the retention time, external standard method.

4 Reagents and materials

Unless otherwise specified, the analysis of analytical reagents used in line with national standards, experimental water for the new preparation does not contain Machine water. Acetonitrile (CH3CN). Chromatography grade. 4.2 n-Hexane (C6H14). Chromatography grade. 4.3 Dichloromethane (CH2Cl2). Chromatography grade. 4.4 Acetone (CH3COCH3). Chromatography grade. 4.5 acetone - n-hexane mixed solution. 1 1. Mix with acetone (4.4) and n-hexane (4.2) at a volume ratio of 1. 1. 4.6 Dichloromethane - n-hexane mixed solution. 2 3. Mix with methylene chloride (4.3) and n-hexane (4.2) at a volume ratio of 2. 3. 4.7 Dichloromethane - n-hexane mixed solution. 1 1. Mix with methylene chloride (4.3) and n-hexane (4.2) at a volume ratio of 1. 1. 4.8 polycyclic aromatic hydrocarbon standard stock solution. ρ = 100 mg/L ~.2000 mg/L. Buy a commercially available certified standard solution, refrigerated at 4 ° C, protected from light and sealed, or with reference to standard solution certificate requirements save. When used should be returned to room temperature and shake. 4.9 polycyclic aromatic hydrocarbons standard solution. ρ = 10.0 mg/L ~.200 mg/L. Pipette 1.0 ml polycyclic aromatic hydrocarbon standard stock solution (4.8) in 10 ml brown volumetric flask, dilute with acetonitrile (4.1) and set Volume to the mark, shake, transferred to a compact bottle at 4 ℃ refrigerated, protected from light. 4.10 ten fluorine biphenyl (C12F10). 99% purity. Alternatives may also be used. 4.11 decafluorobiphenyl stock solution. ρ = 1000 mg/L. Weigh decafluorobiphenyl (4.10) 0.025 g (accurate to 0.001 g), with acetonitrile (4.1) dissolved and dilute to 25 ml brown Color volumetric flask, shake, transferred to airtight bottles at 4 ℃ refrigerated, protected from light. Or purchase a certified public standard solution. 4.12 Use of decafluorobiphenyl. ρ = 40 μg/ml. Pipette 1.0 ml of decafluorobiphenyl stock solution (4.11) in a 25 ml brown volumetric flask, dilute with acetonitrile (4.1) and allow to volume Graduated, shaken, transferred to a compact bottle at 4 ℃ refrigerated, protected from light. 4.13 Sodium Chloride (NaCl). Bake at 400 ℃ 4 h, cooled and placed in a sealed glass jar sealed. 4.14 desiccant. anhydrous sodium sulfate (Na2SO4) or granular diatomaceous earth. Bake at 400 ℃ 4 h, cooled and placed in a sealed glass jar sealed. 4.15 Silica gel. Chromatographic grade, particle size 75 μm ~ 150 μm (200 mesh ~ 100 mesh). Before use, placed in a flat bottom tray and covered with tin foil, activated at 130 ℃ for at least 16 h. 4.16 glass column. diameter of about 20 mm, length 10 cm ~ 20 cm, with PTFE piston. 4.17 SPE cartridge. silica gel SPE cartridge or magnesium silicate cartridge, 1000 mg/6 ml. 4.18 quartz sand. particle size of 150 μm ~ 830 μm (100 mesh ~ 20 mesh). 3 at 400 ℃ baking 4 h, cooled and placed in a sealed glass jar sealed. 4.19 glass wool or glass fiber filter. before use with methylene chloride (4.3) dip, swing away the solvent, sealed. 4.20 Nitrogen. Purity ≥99.999%.

5 instruments and equipment

5.1 High Performance Liquid Chromatograph. equipped with UV detector or fluorescence detector, with gradient elution function. 5.2 Columns. Reversed-phase columns packed with ODS (octadecylsilane bonded silica) or other similar chromatographic Column; Size. 5 μm × 250 mm × 4.6 mm. 5.3 Extraction device. Soxhlet extractor or other equivalent performance equipment. 5.4 Concentration device. nitrogen blowing concentrator or other equivalent performance equipment. 5.5 solid phase extraction device. 5.6 general laboratory equipment and equipment.

6 samples

6.1 Sample Collection and Storage Solid waste samples were collected and stored in accordance with HJ/T 20 and HJ/T 298. Samples should be clean brown mill Port glass bottle preservation, transportation should be dark, sealed, refrigerated. If not timely analysis, should be below 4 ℃ refrigeration, Dark, sealed, save the time for 7 d. 6.2 Sample Preparation 6.2.1 Preparation of solid waste leachate samples 6.2.1.1 Leaching Prepare solid waste leachate according to HJ/T 299 or HJ/T 300. 6.2.1.2 Extraction Take 100 ml of leachate, put it in a 500 ml separatory funnel and add 50.0 μl of decafluorobiphenyl (4.12) Appropriate amount of sodium chloride (4.13) and 20 ml of dichloromethane (4.3) shake well, after standing layered, the organic phase was loaded with a suitable amount of The water of sodium sulfate (4.14) funnel addition to water, the organic phase was collected in a concentrated flask, according to the above steps repeatedly extracted twice Machine phase, with a small amount of methylene chloride (4.3) repeatedly washed funnel and sodium sulfate layer 2 to 3 times, the combined organic phase to be concentrated. 6.2.1.3 Concentration Place the concentrate bottle containing the extract into a nitrogen purifier, and adjust the nitrogen flow rate to the surface of the solvent at room temperature to have air flow fluctuation (To avoid the formation of vortex), the extract was concentrated to about 1.5 ml ~ 2 ml, with 3 ml ~ 5 ml of n-hexane (4.2) washed nitrogen The process has been exposed concentrator wall, the extract was concentrated to about 1 ml, the concentration was repeated 2 to 3 times, the solvent is finished Fully converted to n-hexane, and then concentrated to about 1 ml, to be purified. If no purification, add about 3 ml of acetonitrile (4.1), and then concentrated Shrink to 1 ml or less, the solvent completely converted to acetonitrile, and accurately set the volume to 1.0 ml, to be measured. Note. Rotary evaporation or other methods of concentration may also be used. 6.2.1.4 Purification 4a) Silica gel column purification Silica gel column preparation. Add glass wool (4.19) to the bottom of glass column (4.16), add 10 mm thick anhydrous Sodium sulfate (4.14) was washed with a small amount of dichloromethane (4.3). Preparation of 10 g of active silica gel (4.15) with methylene chloride (4.3) Suspension, into the column, tap the column with a glass rod to remove air bubbles, silica gel packing. Release methylene chloride, at The column was topped with 10 mm thick anhydrous sodium sulfate (4.14). Column schematic shown in Figure 1. Figure 1 column schematic Purification. The column was rinsed with 40 ml of n-hexane (4.2), the rinse rate was controlled at 2 ml/min, Before sodium is exposed to the air, close the bottom of the column polytetrafluoroethylene piston, discard the effluent. The concentrated about 1 ml mention Take the liquid into the column, with 2 ml of n-hexane (4.2) was washed three times the concentration flask, the lotion all moved to the column, at the top Anhydrous sodium sulfate before exposure to air, add 25 ml of n-hexane (4.2) to rinse, discard the effluent. With 25 ml Methylene chloride - n-hexane mixed solution (4.6), the eluate was collected in a concentration flask, concentrated by nitrogen blowing method (or other concentrated Shrink mode) to concentrate the eluate to about 1 ml, add about 3 ml of acetonitrile (4.1), and then concentrated to 1 ml or less, the solvent is completed All converted to acetonitrile, and accurately set the volume to 1.0 ml, to be measured. b) solid phase extraction column (filler is silica gel or magnesium silicate) purification Use solid-phase extraction column (4.17) as purification column and fix it on solid-phase extraction device (5.5). Use 4 ml of dichloro Methane (4.3) flushing purification column, and then 10 ml n-hexane (4.2) balance column, until the column is full closed flow rate control Valve infiltration 5 min, open the control valve, discard the effluent. About 1 ml of extract will be concentrated before it is exposed to the air Into the column, with 3 ml of n-hexane (4.2) was washed three times the concentration flask, the lotion all moved into the column, discard the effluent. use 10 ml dichloromethane - n-hexane mixed solution (4.7) eluting, receiving eluent until the eluate is full purification column after closing the flow Speed control valve, infiltration 5 min, then open the control valve, to eluate completely out. Concentrate with nitrogen (or other concentrates ) The eluate was concentrated to about 1 ml, about 3 ml of acetonitrile (4.1) was added and concentrated to 1 ml or less to completely turn the solvent 5 for acetonitrile, and accurately set the volume to 1.0 ml, to be measured. Note 1. When the sample concentration is high (the color of the eluent is darker), the volume of the concentrate may be appropriately increased, and the eluent may also be properly diluted with methanol or acetonitrile To be measured after dilution. Note 2. If the purified sample can not be analyzed in time, it should be refrigerated at 4 ℃, protected from light, sealed and stored and analyzed within 30 days. Note 3. This standard is recommended for purification of silica gel column chromatography or solid phase extraction column purification, but also other equivalent purification methods. 6.2.2 Preparation of solid waste samples 6.2.2.1 Aqueous liquid solid waste Weigh 10 g (accurate to 0.01 g) sample, add 90 ml of water, mix thoroughly transferred to a separatory funnel, and the remaining steps Follow steps 6.2.1.2 to 6.2.1.4. 6.2.2.2 Oily liquid solid waste Weigh 10 g (accurate to 0.01 g) sample, add 30 ml of dichloromethane (4.3), after mixing all transferred to liquid separation leak Bucket, add 100 ml of water, the remaining steps in accordance with 6.2.1.2 to 6.2.1.4 steps. 6.2.2.3 Solid and semi-solid solid waste 6.2.2.3.1 Dehydration Weigh 10 g (accurate to 0.01 g) samples, adding an appropriate amount of anhydrous sodium sulfate (4.14), grinding homogenized into sand-like, prepare use. If using pressurized fluid extraction, dehydration is performed according to HJ 782. Note. The composition of solid waste samples is complex, when the sample content of organic matter should be appropriately reduced sample size. 6.2.2.3.2 Extraction The dehydrated samples were all transferred to the glass casing or paper casing, adding 50.0 μl of decafluorobiphenyl liquid (4.12), place the cannula into the Soxhlet extractor. Add 100 ml of acetone-n-hexane mixed solution (4.5) every hour Less than 4 times the reflux rate of extraction 16 h ~ 18 h. Extraction is completed, cooled to room temperature, remove the bottom bottle, wash extraction cup interface, Transfer the cleaning solution to the bottle. Add a small amount of anhydrous sodium sulfate (4.14) to the sodium sulfate particles free-flowing and place 30 min dehydration and drying. Note 1. The extract may also be dehydrated through a funnel containing an appropriate amount of anhydrous sodium sulfate (4.14). Note 2. If you pass the verification and meet the quality control requirements of this standard, you can also use other extraction methods. Note 3. Sleeve specifications based on sample size. 6.2.2.3.3 Concentration The dehydrated extracts were all transferred to the concentration flask, according to 6.2.1.3 steps to concentrate. 6.2.2.3.4 Purification Follow steps 6.2.1.4. 6.3 blank sample preparation 6.3.1 solid waste leachate blank sample preparation With quartz sand (4.18) instead of the sample, a blank sample of solid waste leachate was prepared according to 6.2.1. 6.3.2 Preparation of solid waste blank sample The quartz sand (4.18) instead of the sample, according to 6.2.2 steps to prepare a solid waste blank sample. 67 analysis steps 7.1 Instrument reference conditions Injection volume. 10 μl. Column temperature. 35 ° C. Flow rate. 1.0 ml/min. Mobile phase A. Acetonitrile; Mobile phase B. Water. Gradient elution program in Table 1. Table 1 Gradient elution program Time/min Mobile Phase A /% Mobile Phase B /% Detection wavelength. Based on the peak time of the target, the maximum absorption wavelength or the best excitation/emission wavelength preparation wavelength conversion Procedure, see Table 2. Table 2 target corresponding UV detection wavelength and fluorescence detection wavelength Serial number of the component name UV detector fluorescence detector maximum Absorption wavelength (nm) recommend Absorption wavelength (nm) The best excitation wavelength λex / Emission wavelength λem Recommended excitation wavelength λex / Emission wavelength λem 1 naphthalene 220 220 280/334 280/324 2 Camphene 229 230 - - 3 苊 261 254 268/308 280/324 4 fluorene 229 230 280/324 280/324 5 Philippines 251 254 292/366 254/350 Anthracene 252 254 253/402 254/400 7 fluoranthene 236 230 360/460 290/460 8 Pyrene 240 230 336/376 336/376 9 Benzo [a] anthracene 287 290 288/390 275/385 10 䓛 267 254 268/383 275/385 11 Benzo [b] fluoranthene 256 254 300/436 305/430 12 Benzo [k] fluoranthene 307,240 290 308/414 305/430 13 Benzo [a] pyrene 296 290 296/408 305/430 14 dibenzo [a, h] anthracene 297 290 297/398 305/430 15 Benzo [g, h, i] perylene 210 220 300/410 305/430 16-indeno [1,2,3-c, d] pyrene 250 254 302/506 305/500 17 Decafluorobiphenyl 228 230 - - Note. The fluorescence detector is not suitable for the determination of camphene and decafluorobiphenyl. 77.2 establishment of calibration curve 7.2.1 Calibration curve establishment The appropriate amount of PAHs standard solution (4.9) and 50.0 μl of decafluorobiphenyl solution (4.12) were separately measured with acetonitrile (4.1) diluted to prepare standard series of at least 5 concentration points, the mass concentration of polycyclic aromatic hydrocarbons were 0.05 μg/ml, 0.10 μg/ml, 0.50 μg/ml, 2.00 μg/ml and 5.00 μg/ml (this is the reference concentration), the mass concentration of decafluorobiphenyl 2.00 μg/ml, stored in a brown sample bottle, to be measured. From low to high concentration standard series of solutions were injected into the liquid chromatograph, according to the instrument reference conditions (7.1) points To detect, record the peak time of the peak and peak height or peak area. In a standard series of solutions in the concentration of the target component as abscissa, With its corresponding peak height or peak area for the vertical axis, the establishment of a standard curve. 7.2.2 Standard sample chromatogram Figure 2 and Figure 3, respectively, in this standard recommended instrument conditions, 16 polycyclic aromatic hydrocarbons UV chromatogram and fluorescence chromatography Figure 1-naphthalene; 2-carene; 3-naphthalene; 4-fluorene; a] anthracene; 11-azulene; 12- Benzo [b] fluoranthene; 13-benzo [k] fluoranthene; 14-benzo [a] pyrene; Perylene; 17-indeno [1,2,3-c, d] pyrene. Figure 2 16 kinds of polycyclic aromatic hydrocarbons UV chromatogram Naphthalene; 2-carene (no peak); 3-naphthalene; 4-fluorene; 5- phenanthrene; 6- anthracene; Peak); 10- Benzo [a] pyrene; 15-dibenzo [a, h] fluoranthene; Anthracene; 16-benzo [g, h, i] perylene; 17-indeno [1,2,3-c, d] pyrene. Figure 3 16 kinds of polycyclic aromatic hydrocarbons fluorescence chromatogram 7.3 Determination of the sample The measurement of the sample was carried out according to the same instrument analysis conditions as the establishment of the calibration curve (7.2). 7.4 Blank test The blank sample (6.3) was measured according to the same instrument analysis conditions as the sample measurement (7.3).

8 results calculated and said

8.1 Qualitative analysis of the target compound The retention time of the target compound qualitative, if necessary, can be used standard sample addition method, absorption ratio at different wavelengths, UV spectroscopy scan and other methods to help qualitative. 8.2 Calculation Results 8.2.1 solid waste leachate The content of PAHs in solid waste leachate (μg/L) was calculated according to formula (1). i V   (1) Where. ρ-- solid waste leachate target mass concentration, μg/L; ρi - calculated from the calibration curve of the target mass concentration, μg/ml; V1 - sample volume, ml; V2 - leachate sampling volume, L. 8.2.2 Solid waste PAHs in solid waste (mg/kg), calculated according to equation (2). 9i mw   (2) Where. wi - solid waste sample component i content, mg/kg; ρi - mass concentration of the component i in the sample calculated from the calibration curve, μg/ml; V-- sample volume, ml; m - Weigh the quality of solid waste samples (wet weight), g. 8.3 results indicated Measurement results retained up to three significant figures, the maximum number of digits after the decimal point with the method detection limit consistent.

9 precision and accuracy

9.1 Precision Six laboratories respectively spiked the target concentration of 1.0 μg/kg ~ 20.0 μg/kg, 5.0 μg/kg ~ 100 μg/kg, The blank ash samples from 10.0 μg/kg to.200 μg/kg were subjected to 6 replicate determinations. The relative standard deviations in the laboratory were 3.4% -16%, 2.0% -14% and 3.4% -14%, respectively. The relative standard deviations (RSDs) were 4.1% -9.3% and 3.6% 12% and 3.5% -14% respectively. The range of repeatability was 0.2 μg/kg ~ 4.2 μg/kg, 1.1 μg/kg ~ 24 μg/kg, 2.1 μg/kg ~ 48 μg/kg; reproducibility limits were 0.3 μg/kg ~ 4.8 μg/kg, 1.2 μg/kg ~ 26 μg / 2.6 μg/kg to 59 μg/kg. Six laboratories, respectively, the target spiking levels of 5 μg/kg ~ 100 μg/kg, 25 μg/kg ~ 500 μg/kg, 50 μg/kg ~ 1000 μg/kg spiked samples of spiked samples were repeated 6 times, the relative standard deviation in the laboratory were 3.3% ~ 16%, 3.8% ~ 16%, 3.9% ~ 14%. The relative standard deviations of the laboratories were 3.0% ~ 6.8%, 3.2% The range of repeatability was 1 μg/kg ~ 21 μg/kg, 5 μg/kg ~ 104 μg/kg, 12 μg/kg ~ 215 μg/kg; reproducibility limits were 1 μg/kg ~ 24 μg/kg, 7 μg/kg ~ 110 μg/kg, 13 μg / 225 μg/kg. A laboratory of the target substance concentration of 0.05 μg/L ~ 1.00 μg/L, 0.25 μg/L ~ 5.00 μg/L, 0.50 μg/L ~ 10.0 μg/L waste leachate and ash leachate 6 times repeated determination of relative standard deviation in the laboratory were 4.6% to 12%, 4.8% to 10%, 4.2% to 11% and 4.3% to 11%, 5.3% to 10% and 5.1% to 11% 9.2 Accuracy Six laboratories with ash and sludge as the substrate were spiked recoveries, spiked at a concentration of 10.0 μg/kg ~ 200 μg/kg, the recovery rates of ash and sludge were 53.2% ~ 97.2% and 56.7% ~ 97.9%, respectively. The spiked recoveries were the highest The final values were 67.5% ± 23.2% ~ 88.1% ± 14.4% and 65.4% ± 11.9% ~ 88.8% ± 17.3%, respectively. Alternatives to decafluorobiphenyl The recoveries ranged from 76.8% to 92.6% and 71.1% to 91.7%, respectively. The final recoveries of spiked samples were 88.1% ± 14.4% And 83.6% ± 14.2%. A laboratory of ash residue leachate and waste leachate matrix spike determination, spiking concentration level of 0.50 μg/L ~ 10.0 μg/L, the spiked recoveries were 64.2% -99.3% and 84.5% -98.3%, respectively. See Appendix B for statistics of results of precision and accuracy. 10 Quality Assurance and Quality Control 10.1 Blank test Make at least one lab blank every 20 samples or batches (less than 20 samples/batch). The blank result should be less than Method detection limit. 10.2 Calibration The calibration curve should be established for each batch of samples. The correlation coefficient of the calibration curve should be ≥0.995. Otherwise you should find the re...

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