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HJ 676-2013 English PDF

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HJ 676-2013: Water quality. Determination of phenolic compounds. Liquid liquid extraction gas chromatography
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HJ 676-2013	English	419	Add to Cart	3 days [Need to translate]	Water quality. Determination of phenolic compounds. Liquid liquid extraction gas chromatography	Valid	HJ 676-2013

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Basic data

Standard ID	HJ 676-2013 (HJ676-2013)
Description (Translated English)	Water quality. Determination of phenolic compounds. Liquid liquid extraction gas chromatography
Sector / Industry	Environmental Protection Industry Standard
Classification of Chinese Standard	Z16
Classification of International Standard	13.060
Word Count Estimation	16,136
Quoted Standard	GB/T 14581; HJ/T 91; HJ/T 164; HJ/T 493
Regulation (derived from)	Ministry of Environmental Protection Notice No. 70 of 2013
Issuing agency(ies)	Ministry of Ecology and Environment
Summary	This standard specifies the determination of phenolic compounds in water liquid-liquid extraction/gas chromatography. This standard applies to surface water, groundwater, sewage and industrial effluent phenol, 3-cresol, 2, 4-xylenol, 2-chlorophenol, 4-chl

HJ 676-2013: Water quality. Determination of phenolic compounds. Liquid liquid extraction gas chromatography

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Water quality.Determination of phenolic compounds.Liquid liquid extraction gas chromatography National Environmental Protection Standard of the People's Republic Determination of phenolic compounds in water Liquid-liquid extraction/gas chromatography Water quality-Determination of phenolic compounds Liquid liquid extraction gas chromatography Released on.2013-11-21 2014-02-01 implementation release Ministry of Environmental Protection

Content

Preface II 1 Scope 1 2 Normative references 1 3 Principle of the method 1 4 interference and elimination..2 5 reagents and materials..2 6 instruments and equipment..3 7 samples.3 8 Analysis step 4 9 Calculation and representation of results 5 10 precision and accuracy.6 11 Quality Assurance and Quality Control..6 12 Waste treatment.7 Appendix A (informative) The precision and accuracy of the method..8 Appendix B (informative) Auxiliary qualitative column reference conditions..10 Appendix C (informative) Target compound and retention time 11

Foreword

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, to protect the environment, This standard is formulated to ensure human health and to regulate the determination of phenolic compounds in water. This standard specifies liquid-liquid extraction/gas for the determination of phenolic compounds in surface water, groundwater, domestic sewage and industrial wastewater. Phase chromatography. This standard is the first release. Appendix A, Appendix B and Appendix C of this standard are informative annexes. This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection. This standard is mainly drafted by. Ningbo Environmental Monitoring Center. This standard is verified by. Zhoushan Marine Ecological Environment Monitoring Station, Hangzhou Environmental Monitoring Center Station, Taizhou Environment Monitoring Center Station, Jiaxing Environmental Protection Monitoring Station, Huzhou Environmental Protection Monitoring Center Station and Jinhua Environmental Monitoring Center Station. This standard was approved by the Ministry of Environmental Protection on November 21,.2013. This standard has been implemented since February 1,.2014. This standard is explained by the Ministry of Environmental Protection. Water quality - Determination of phenolic compounds - Liquid-liquid extraction/gas chromatography Warning. The solvents and reagents used in the test are all toxic. The sample preparation process should be carried out in a fume hood. In operation, wear protective equipment as required to avoid direct contact between skin and clothing.

1 Scope of application

This standard specifies liquid-liquid extraction/gas chromatography for the determination of phenolic compounds in water. This standard applies to surface water, groundwater, domestic sewage and industrial wastewater in phenol, 3-cresol, 2,4-xylenol, 2- Chlorophenol, 4-chlorophenol, 4-chloro-3-cresol, 2,4-dichlorophenol, 2,4,6-trichlorophenol, pentachlorophenol, 2-nitrophenol, 4-nitrophenol 2,4- Determination of 13 phenolic compounds such as dinitrophenol and 2-methyl-4,6-dinitrophenol. When the sampling volume is 500mL, the method detection limits and lower limit of determination of 13 phenolic compounds are shown in Table 1. Table 1 Method detection limit and lower limit of measurement unit. μg/L Compound name detection limit lower limit compound name detection limit lower limit Phenol 0.5 2.0 2,4,6-trichlorophenol 1.2 4.8 3-cresol 0.5 2.0 pentachlorophenol 1.1 4.4 2,4-xylenol 0.7 2.8 2-nitrophenol 1.1 4.4 2-Chlorophenol 1.1 4.4 4-Nitrophenol 1.2 4.8 4-chlorophenol 1.4 5.6 2,4-dinitrophenol 3.4 13.6 4-chloro-3-cresol 0.7 2.8 2-methyl-4,6-dinitrophenol 3.1 12.4 2,4-dichlorophenol 1.1 4.4

2 Normative references

The contents of this standard refer to the following documents or their terms. For undated references, the valid version is appropriate. Used in this standard. GB/T 14581 Water quality lake and reservoir sampling technical guidance HJ/T 91 Surface Water and Wastewater Monitoring Technical Specifications HJ/T 164 Technical Specifications for Groundwater Environmental Monitoring HJ/T 493 Technical Regulations for Preservation and Management of Water Quality Samples

3 Principle of the method

Under acidic conditions (pH< 2), the phenolic compounds in the water sample were extracted with a mixed solvent of dichloromethane/ethyl acetate. The shrunken extract is separated by gas chromatography capillary column, detected by hydrogen flame detector, and characterized by chromatographic retention time. Quantification by external standard method.

4 interference and elimination

4.1 There may be other organic matter interference measurement in the water sample, which can be purified by alkaline aqueous solution, or by changing color. Spectral conditions, double column characterization or mass spectrometry were further confirmed. 4.2 There may be a memory effect after measuring a high concentration sample, which can be analyzed by blank sample until the target in the blank sample The next sample can only be analyzed if the concentration of the compound is below the lower limit of the assay.

5 reagents and materials

Analytical purification reagents that meet national standards were used for analysis unless otherwise stated. 5.1 Experimental water Secondary distilled water, commercially available purified water or organic-free water prepared by pure water equipment. Should be tested by blank test before use To confirm that there is no interference peak in the retention time interval of the target compound or that the target compound concentration is lower than Method detection limit. 5.2 sodium hydroxide (NaOH). 5.3 Concentrated hydrochloric acid (HCl). ρ (HCl) = 1.19 g/mL. 5.4 Aqueous sodium hydroxide solution. ρ (NaOH) = 0.2 g/mL. Weigh 20g of sodium hydroxide (5.2), dissolve in a small amount of water (5.1), and dilute to 100 mL. 5.5 Hydrochloric acid solution. 1 3 (V/V). Measure 125 mL of concentrated hydrochloric acid (5.3) and dilute to 500 mL with water (5.1). 5.6 Dichloromethane (CH2Cl2). pesticide residue grade. 5.7 Ethyl acetate (CH3COOC2H5). pesticide residue grade. 5.8 n-hexane (C6H14). pesticide residue grade. 5.9 Methanol (CH3OH). pesticide residue grade. 5.10 Mixed solvent of dichloromethane/ethyl acetate. 1 1 (V/V). Mix with dichloromethane (5.6) and ethyl acetate (5.7) in a volume ratio of 1.1. 5.11 Mixed solvent of dichloromethane/n-hexane. 2 1 (V/V). Mix with dichloromethane (5.6) and n-hexane (5.8) in a volume ratio of 2.1. 5.12 Sodium chloride Bake in a muffle furnace at 400 ° C for 4 h, cool to room temperature and store in a desiccator. 5.13 anhydrous sodium sulfate Bake in a muffle furnace at 400 ° C for 4 h, cool to room temperature and store in a desiccator. 5.14 Standard solution of phenolic compound. ρ=500～2500 mg/L A methanol solution containing 13 target phenolic compounds, which can be purchased directly from a certified standard solution or a pure standard material. Ready. The standard solution can be stored for half a year at 4 °C. 5.15 Carrier gas. nitrogen, purity ≥99.999%. 5.16 Combustion gas. hydrogen, purity ≥ 99.99%. 5.17 Gas. Air, which must remove moisture and organic matter.

6 Instruments and equipment

6.1 Gas Chromatograph. With split/splitless inlet, programmable, with a hydrogen flame detector (FID). 6.2 Analytical column. quartz capillary column, 30m × 0.32mm, film thickness 0.25μm, fixed solution 5% phenyl-95% Methyl polysiloxane, or other equivalent column. 6.3 Concentrator. A concentrating device of comparable performance, such as a rotary evaporator, a nitrogen blower, or an organic sample concentrator. 6.4 Balance. Accuracy is 0.1 g. 6.5 muffle furnace. 6.6 Separating funnel. 250 mL and 1000 m L. 6.7 Microinjectors. 10 μL, 50 μL and 100 μL. 6.8 Vial. 1000 mL, brown hard glass bottle. 6.9 Common instruments and equipment used in general laboratories.

7 samples

7.1 Sample Collection and Storage Collection and storage of water samples in accordance with the relevant provisions of GB/T 14581, HJ/T 91, HJ/T 164 and HJ/T 493. Do not pre-wash the sample bottle with water samples when collecting samples. After sampling, adjust the water sample to pH by adding an appropriate amount of hydrochloric acid solution (5.5). < 2, the water sample should be filled with the sample bottle and sealed, and stored at 4 °C in the dark. If the water sample cannot be measured in time, it should be 7 days. Internal extraction. The extract was stored at 4 °C in the dark and analyzed within 20 days. 7.2 Preparation of samples 7.2.1 Extraction of surface water and groundwater samples Shake the water sample, measure 500 mL, pour into a 1000 mL separatory funnel, add 30 g of sodium chloride (5.12), shake and dissolve After solution, add 60 mL of dichloromethane/ethyl acetate mixed solvent (5.10), shake, release gas, and shake extract 5~ 10 min, let stand for more than 10 min, until the organic phase and the aqueous phase are sufficiently separated, and the organic phase is collected. Repeated extraction 1~2 times, combined And organic phase. The organic phase is dehydrated with anhydrous sodium sulfate (5.13) and mixed with a suitable amount of dichloromethane/ethyl acetate (5.10). The anhydrous sodium sulfate was washed, and the organic phase extract was collected. Note 1. Refer to 7.2.2 for surface water and groundwater samples that are contaminated or complex. 7.2.2 Extraction of domestic sewage and industrial wastewater samples Shake the water sample, measure 100 mL, pour into a 250 mL separatory funnel, add 10 g of sodium chloride (5.12), shake to dissolve Then, add 20 mL of dichloromethane/ethyl acetate mixed solvent (5.10), shake, release the gas, and shake and extract for 5-10 min. Allow to stand for more than 10 min until the organic phase is sufficiently separated from the aqueous phase to collect the organic phase. Repeat the extraction 1~2 times and combine the organic phases. The organic phase was dried over anhydrous sodium sulfate (5.13) and washed with an appropriate amount of dichloromethane/ethyl acetate mixed solvent (5.10). The organic phase extract was collected by sodium sulfate. After the water sample is extracted, it needs to be purified. The above extract is concentrated to about 1.0 mL below 45 °C with dichloromethane. /N-hexane mixed solvent (5.11) was diluted to 20 mL, poured into a 250 mL separatory funnel, and added to 50 mL of pre-oxidized The sodium solution (5.4) is adjusted to an aqueous alkaline solution having a pH >12. Shake the separatory funnel for about 3 to 5 minutes, and pay attention to deflation. Rest More than 10 min, the organic phase is sufficiently separated from the aqueous phase. Transfer the aqueous phase to a 250 mL Erlenmeyer flask. Repeated back extraction of organic phase 1 The aqueous phase was combined and the phenolic compound was in the aqueous phase. Transfer the above aqueous phase to another 250 mL separatory funnel, adjust to pH< 2 with hydrochloric acid solution (5.5), add 20 mL of dichloromethane/ethyl acetate mixed solvent (5.10), shake the separatory funnel for about 3 to 5 minutes, and pay attention to deflation. Static Set for more than 10 min until the organic phase is sufficiently separated from the aqueous phase. Transfer the organic phase to another 250 mL Erlenmeyer flask. Repeated extraction The aqueous phase was combined once and the organic phases were combined. The organic phase is dried over anhydrous sodium sulfate (5.13) and mixed with an appropriate amount of dichloromethane/ethyl acetate. The solvent (5.10) was washed with anhydrous sodium sulfate, and the organic phase extract was collected. Note 2. When emulsification occurs during the extraction process, it can be broken by agitating, centrifuging, freezing or filtering with glass wool. Note 3. In order to simplify the extraction and purification process, the water sample can be directly adjusted to pH >12 by using sodium hydroxide solution (5.4), and 10 g of chlorine is added. Sodium (5.12), after shaking and dissolved, add 40 mL of dichloromethane/n-hexane mixed solvent (5.11) to extract twice, collect the aqueous phase, and then take it again. Adjust the aqueous phase to pH< 2 with hydrochloric acid solution (5.5), add 20 mL of dichloromethane/ethyl acetate mixed solvent (5.10) and extract twice, collect The organic phase extracts were combined. 7.2.3 Concentration Transfer the dehydrated extract (7.2.1 or 7.2.2) to a concentrate bottle and concentrate at 45 °C with a concentration unit (6.4) Concentrate to 0.5~1.0 mL, add dichloromethane/ethyl acetate mixed solvent (5.10) 3.0 mL, and concentrate to 1.0 mL. To be tested. Note 4. After high-concentration water sample extraction, it can be injected directly or diluted without concentration. 7.3 Preparation of blank samples The experimental sample was used to replace the actual sample, and a blank sample was prepared in the same manner as in the preparation of the sample (7.2).

8 Analysis steps

8.1 Chromatographic Reference Conditions Different models of gas chromatographs have different working conditions, and should be operated according to the instrument's instruction manual. This standard gives The chromatographic reference conditions are as follows. Temperature programmed. 50 ° C (for 5 min) 6 ° C/min 150 ° C 20 ° C/min 280 ° C 30 ° C/min 300 ° C (guarantee Hold 2min); inlet temperature. 250 °C; FID detector temperature. 300 °C; carrier gas flow rate. 1.5 mL/min; hydrogen flow Amount. 40.0 mL/min; air flow rate. 450.0 mL/min; tail gas flow rate. 30.0 mL/min; injection method. no distinction Flow injection, purge after 1.0 min injection, purge gas flow 30.0 mL/min; injection volume. 1.0 μL. 8.2 Calibration 8.2.1 Drawing of the calibration curve Prepare a certain amount of phenolic compound standard solution (5.14) in dichloromethane/ethyl acetate mixed solvent (5.10) to prepare For the calibration series of 6 concentration points, the calibration series of each target compound is shown in Table 2. According to the chromatographic reference conditions (8.1), respectively Take 1.0 μL of the calibration series solution from the low concentration to the high concentration and analyze the peak area (or peak height) as the ordinate. A calibration curve is drawn with the target compound concentration as the abscissa. Table 2 Preparation of calibration curve. mg/L No. Compound name concentration 1 concentration 2 concentration 3 concentration 4 concentration 5 concentration 6 1 Phenol 1.0 2.5 5.0 12.5 25.0 50.0 2 2-Chlorophenol 2.0 5.0 10.0 25.0 50.0 100 3 3-cresol 1.0 2.5 5.0 12.5 25.0 50.0 4 2-nitrophenol 2.0 5.0 10.0 25.0 50.0 100 5 2,4-xylenol 1.0 2.5 5.0 12.5 25.0 50.0 6 2,4-dichlorophenol 2.0 5.0 10.0 25.0 50.0 100 7 4-Chlorophenol 2.0 5.0 10.0 25.0 50.0 100 8 4-Chloro-3-cresol 1.0 2.5 5.0 12.5 25.0 50.0 9 2,4,6-trichlorophenol 2.0 5.0 10.0 25.0 50.0 100 10 2,4-dinitrophenol 5.0 12.5 25.0 62.5 125 250 11 4-nitrophenol 2.0 5.0 10.0 25.0 50.0 100 12 2-methyl-4,6-dinitrophenol 5.0 12.5 25.0 62.5 125 250 13 Pentachlorophenol 2.0 5.0 10.0 25.0 50.0 100 8.2.2 Reference standard chromatogram Under the chromatographic reference conditions given in this standard, the reference standard chromatogram of each phenolic compound on the analytical column is shown in the figure. 1. 1-phenol, 2-2-chlorophenol, 3-3-cresol, 4-2-nitrophenol, 5-2,4-xylenol, 6-2,4-dichlorophenol, 7-4- Chlorophenol, 8-4- Chloro-3-cresol, 9-2,4,6-trichlorophenol, 10-2,4-dinitrophenol, 11-4-nitrophenol, 12-2-methyl-4,6-di Nitrophenol, 13-pentachlorophenol. Figure 1 Standard chromatogram of phenolic compounds 8.3 Determination Take 1.0 μL of the sample (7.2.3) and inject it into the gas chromatograph to record the retention time and peak area (or peak height) of the chromatographic peak. 8.4 Blank test A blank test was performed during the same batch of samples. A 1.0 μL blank sample (7.3) was taken for measurement.

9 Calculation and representation of results

9.1 Target compound characterization The target compound is characterized according to the chromatogram component retention time (Rt), and if necessary, another polarity difference can be used. The column is aided for qualitative confirmation and can be further confirmed by mass spectrometry. Chromatographic reference conditions and parameters for auxiliary qualitative columns See Appendix B for the standard chromatogram. See Appendix C for retention times for analytical and auxiliary qualitative columns. Min10 12.5 15 17.5 20 22.5 25 27.5 pA 9.2 Calculation of results The concentration of the target compound in the water sample, iρ (μg/L), is calculated according to formula (1). ××= standard ρρ (1) In the formula. Iρ - the concentration of the target compound in the water sample, μg/L; ρ - the concentration of the target compound calculated from the calibration curve, mg/L; 1V - the volume of the volume after concentration of the extract, mL; 2V - sample volume of water sample, mL. 9.3 Result representation When the measurement result is less than 10.0 μg/L, the result is retained to one decimal place; when the measurement result is greater than or equal to 10.0 μg/L The result retains three significant digits. 10 Precision and accuracy 10.1 Precision 6 laboratories have standardized spiked concentrations of 2.0 to 10.0 μg/L, 10.0 to 50.0 μg/L, and 40.0 to.200 μg/L, respectively. The blank spiked samples were measured, and the relative standard deviations in the laboratory were. 5.8 to 19.3%, 2.3 to 16.0%, and 1.0 to 10.9 %; the relative standard deviations between laboratories are. 6.3 to 20.9 %, 9.6 to 19.0 %, 4.8 to 16.4%; reproducibility The limits are. 0.4 to 2.6 μg/L, 1.4 to 10.2 μg/L, and 5.4 to 31.3 μg/L; the reproducibility limits are. 0.4 to 4.8 μg/L, 3.3 to 17.6 μg/L, 9.7 to 47.2 μg/L. Uniform surface water and wastewater from 6 laboratories with spiked concentrations of 10.0-50.0 μg/L and 400-2000 μg/L The spiked samples were measured, and the relative standard deviations in the laboratory were. 1.8 to 15.0%, 2.0 to 19.2%; The relative standard deviations between the chambers were. 5.5 to 13.6% and 7.8 to 18.5%; the repeatability limits were 1.6 to 11.3 μg/L, respectively. 48.8 ~ 349 μg/L; reproducibility limits are. 1.5 ~ 15.1 μg/L, 56.5 ~ 676 μg/L. 10.2 Accuracy 6 laboratories have standardized spiked concentrations of 2.0 to 10.0 μg/L, 10.0 to 50.0 μg/L, and 40.0 to.200 μg/L, respectively. The blank spiked samples were tested for spiked recovery. The average spiked recoveries ranged from 67.2 to 91.9% and 80.8. 94.2%, 79.5~95.1%. The concentration of spiked water in the laboratory was 10.0～50.0 μg/L and 400～2000 μg/L, respectively. The actual spiked samples of water were tested for spiked recovery. The average spiked recoveries ranged from 78.8 to 92.7 % and 64.9 to 84.4%. For specific method precision and accuracy data, see Appendix A. 11 Quality Assurance and Quality Control 11.1 Qualitative analysis A retention time window of t ± 3S should be established prior to sample analysis. t is the retention time of each concentration level of reference material at the initial calibration The average value between the two, S is the standard deviation of the retention time of the standard substance at each concentration level at the initial calibration. When the sample is analyzed, The object to be tested retention time should be within the retention time window. 11.2 Blank test Make at least 1 laboratory blank and full program blank for every 20 samples or batches (less than 20 samples/batch) The concentration of the target compound in the blank sample should be lower than the method detection limit. 11.3 Parallel sample determination For each batch of samples, 10% of parallel samples should be determined, and the relative standard deviation of the results of a single parallel test is within ±25%. 11.4 Sample spike At least 1 blank sample plus standard and actual sample spike should be added for every 20 samples or batches of samples, and the blank sample should be spiked. The concentration is 3 to 10 times the detection limit of the method; the concentration of the actual sample is 1 to 3 times the concentration of the sample, as in the actual sample. The target compound was not detected and its spiked concentration was performed with reference to the blank sample. Blank sample and actual sample spike recovery should be controlled At 60 to 130%. 11.5 Calibration curve A calibration curve should be drawn for each batch of samples. The correlation coefficient of the calibration curve should be ≥0.995, otherwise you should find the reason and redraw Calibration curve. Analyze 1 curve intermediate concentration point standard solution for every 20 samples or batches of samples, and the measured results are compared with the initial curve. The relative deviation of the measured concentration at this point should be ≤ 20%, otherwise the cause should be found and the calibration curve should be redrawn. 12 Waste treatment The waste liquid generated during the experimental operation and the high concentration sample after analysis shall be entrusted to a qualified unit for proper disposal.

Appendix A

(informative appendix) Method precision and accuracy Table A.1 gives the precision and accuracy results of the blank sample method, and Table A.2 gives the actual sample method. Density and accuracy results. Precision and accuracy of the method in Schedule A.1 (blank sample) Compound name Bid concentration (μg/L) average value (μg/L) Laboratory room Relative standard deviation(%) Laboratory room Relative standard deviation(%) Repeatability limit r(μg/L) Reproducibility limit R (μg/L) Spike recovery (%) Plus standard recycling end value(%)

1 phenol

2.0 1.5 8.7~11.5 14.6 0.4 0.6 68.1～96.3 76.7±22.4 10.0 8.5 4.8 to 7.5 14.0 1.4 3.3 74.0 to 107.4 85.4 ± 23.9 40.0 33.3 1.2～10.0 10.4 6.0 9.7 76.3～98.8 83.2±17.3 2 2-chlorophenol 4.0 3.1 7.3~10.8 9.0 0.8 0.8 69.7~84.1 77.3±14.0 20.0 17.0 3.3～8.8 17.4 2.9 8.3 71.9～109.9 85.2±29.7 80.0 67.5 1.4～8.6 10.9 10.1 20.6 74.4～100.3 84.4±18.4 3 3-cresol 2.0 1.5 8.2~11.3 14.4 0.4 0.6 63.8～94.4 76.8±22.0 10.0 8.5 3.2 to 8.8 15.4 1.6 3.7 68.8 to 107.0 84.8 ± 26.2 40.0 34.4 2.4～8.6 10.0 5.9 9.7 75.9～100.1 86.1±17.3 4 2-nitrophenol 4.0 3.2 7.6～10.8 12.9 0.8 1.2 66.6～95.9 79.9±20.5 20.0 16.3 2.9 to 7.8 17.9 2.7 8.2 69.6 to 107.7 81.3±29.1 80.0 67.6 1.5～10.5 11.5 11.4 21.8 72.8～99.3 84.5±19.4 5 2,4-xylenol 2.0 1.3 11.6～19.3 10.9 0.5 0.4 59.4～78.8 67.2±14.6 10.0 8.1 5.2~11.5 14.8 1.8 3.3 62.6～95.8 80.8±23.9 40.0 31.8 2.6 to 8.7 15.8 5.4 14.1 64.2 to 101.0 79.5±25.2 6 2,4-dichlorophenol 4.0 3.1 8.3～14.5 12.6 0.9 1.1 65.9～90.9 77.8±19.6 20.0 16.7 3.1～9.2 19.0 3.2 8.9 71.1～113.3 83.6±31.7 80.0 68.7 1.5～10.6 12.2 10.7 23.5 71.7～101.4 85.8±21.0 7 4-Chlorophenol 4.0 3.2 7.6~13.8 6.9 0.9 0.6 72.5～87.5 81.2±11.2 20.0 17.3 3.1 to 9.3 17.5 3.1 8.5 70.5 to 114.1 86.5 ± 30.2 80.0 70.9 1.0～10.0 10.3 11.4 20.4 78.0～102.2 88.6±18.2 8 4-chloro-3-cresol 2.0 1.6 5.8～18.6 12.7 0.5 0.6 63.8～88.8 79.7±20.2 10.0 9.4 5.9 to 10.3 15.9 2.0 4.2 78.9 to 114.2 93.7±29.7 40.0 36.7 1.2～10.8 16.4 6.6 16.9 77.2～119.3 91.8±30.1 9 2,4,6-trichlorophenol 4.0 3.7 6.6~10.6 12.1 1.0 1.2 72.5～100.9 91.4±22.2 20.0 17.8 2.3~11.2 14.3 3.4 7.1 76.2~112.6 89.1±25.5 80.0 72.2 1.6～10.5 11.0 11.3 22.1 78.6～104.1 90.2±19.8 10 2,4-dinitrophenol 10.0 8.3 7.5 to 15.1 15.0 2.6 3.5 69.9 to 105.1 83.2 ± 24.9 50.0 47.1 2.7～16.0 12.9 10.2 17.0 73.6～105.3 94.2±24.3 200 186 1.3～6.7 9.1 24.4 47.2 80.6～101.5 93.2±16.9 11 4-nitrophenol 4.0 3.5 8.5 to 12.5 9.8 0.9 1.0 80.0 to 100.3 87.6 ± 17.1 20.0 17.1 3.8 to 11.7 16.3 3.4 7.8 71.4 to 110.8 85.4 ± 27.9 80.0 73.5 2.2～10.5 4.8 12.7 9.8 86.6～97.8 91.8±8.7 Continued Compound name Bid concentration (μg/L) average value (μg/L) Laboratory room Relative standard deviation(%) Laboratory room Relative standard deviation(%) Repeatability limit r(μg/L) Reproducibility limit R (μg/L) plus.

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