HJ 1051-2019 English PDF

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HJ 1051-2019: Soil - Determination of petroleum oil - Infrared spectrophotometry
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Basic data

Standard ID: HJ 1051-2019 (HJ1051-2019)
Description (Translated English): Soil - Determination of petroleum oil - Infrared spectrophotometry
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z18
Classification of International Standard: 13.080
Word Count Estimation: 11,184
Date of Issue: 2019
Date of Implementation: 2020-04-24
Issuing agency(ies): Ministry of Ecology and Environment

HJ 1051-2019: Soil - Determination of petroleum oil - Infrared spectrophotometry

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Soil-Determination of petroleum oil-Infrared spectrophotometry National Environmental Protection Standard of the People's Republic of China Determination of soil petroleum Infrared spectrophotometry Soil-Determination of petroleum oil -Infrared spectrophotometry 2019-10-24 released 2020-04-24 Implementation Released by the Ministry of Ecology and Environment

Contents

Foreword ... ii 1 Scope ... 1 2 Normative references ... 1 3 Terms and definitions ... 1 4 Methodology ... 1 5 Reagents and materials ... 1 6 Instruments and equipment ... 3 7 Sample ... 3 8 Analysis steps ... 4 9 Results calculation and representation ... 5 10 Precision and accuracy ... 5 11 Quality Assurance and Quality Control ... 6 12 Waste disposal ... 6 13 Notes ... 7

Foreword

In order to implement the "Environmental Protection Law of the People's Republic of China" Environment, protect human health, standardize the determination method of petroleum in soil, and formulate this standard. This standard specifies infrared spectrophotometry for the determination of petroleum in soil. This standard is issued for the first time. This standard is formulated by the Department of Eco-Environmental Monitoring, Laws and Standards Department of the Ministry of Ecology and Environment. This standard was drafted. Liaoning Anshan Ecological Environment Monitoring Center. Verification units of this standard. Liaoning Province Ecological Environment Monitoring Center, Liaoning Province Shenyang Ecological Environment Monitoring Center, Changchun City Environmental Monitoring Center Station, Dalian Ecological Environment Monitoring Center in Liaoning Province, Liaoyang Ecological Environment Monitoring Center in Liaoning Province, and Panjin, Liaoning Province Ecological Environment Monitoring Center. This standard was approved by the Ministry of Ecology and Environment on October 24,.2019. This standard will be implemented from April 24, 2020. This standard is explained by the Ministry of Ecology and Environment. Determination of petroleum in soils-Infrared spectrophotometry Warning. The tetrachloroethylene used in the experiment is harmful to human health. Standard solution preparation, sample preparation, and determination The process should be performed in a fume hood, and protective equipment should be worn during operation to avoid contact with skin and clothing.

1 Scope

This standard specifies infrared spectrophotometry for the determination of petroleum in soil. This standard applies to the determination of petroleum in soil. When the sample size is 10 g, the volume of the extraction solution is 50 ml, and the 40 mm quartz cuvette is used, the detection limit of the method is 4 mg/kg, the lower limit of determination is 16 mg/kg.

2 Normative references

This standard refers to the following documents or clauses therein. For undated references, the valid version applies to this standard. HJ 613 Soil dry matter and moisture determination by gravimetric method HJ/T 166 Technical Specifications for Soil Environmental Monitoring

3 terms and definitions

The following terms and definitions apply to this standard. 3.1 Petroleum petroleum It means that under the conditions specified in this standard, it can be extracted by tetrachloroethylene and not adsorbed by magnesium silicate. The wave number is 2930. cm -1, 2960 cm-1, 3030 cm-1 Substances with characteristic absorption at all or part of the band.

4 Method principle

The soil was extracted with tetrachloroethylene, and the extract was adsorbed by magnesium silicate. After removing polar materials such as animal and vegetable oils, the petroleum was measured. The content of petroleum is determined by the wave numbers of 2930 cm-1 (the stretching vibration of the CH bond in the CH2 group) and 2960 cm -1 (CH3 Stretching vibration of the CH bond in the group) and absorbance A3030 at 3030 cm-1 (stretching vibration of the CH bond in the aromatic ring), A2960 and A3030 are calculated based on the correction factor.

5 Reagents and materials

Unless otherwise specified, analytical reagents that comply with national standards are used in the analysis. The experimental water is distilled water or equivalent. Degrees of water. 5.1 Tetrachloroethylene (C2Cl4). Using a dry 40 mm empty quartz cuvette as a reference, at a wavenumber of 2930 cm -1, 2960 cm-1 And 3030 cm-1 should not exceed 0.34, 0.07 and 0, respectively. 5.2 n-hexadecane (C16H34). chromatographically pure. 5.3 Isooctane (C8H18). chromatographically pure. 5.4 Benzene (C6H6). chromatographically pure. 5.5 Anhydrous sodium sulfate (Na2SO4). It was placed in a muffle furnace at 450 ° C for 4 h, cooled slightly, placed in a ground glass bottle, and stored in a desiccator. 5.6 Magnesium silicate (MgSiO3). 150 μm to 250 μm (100 mesh to 60 mesh). Take the magnesium silicate in a porcelain evaporating dish, place it in a muffle furnace at 450 ° C for 4 h, cool it a little, then transfer it to a desiccator to cool to room Warm, store in ground glass bottle. During use, weigh an appropriate amount of magnesium silicate into a ground glass bottle. Amount, add an appropriate amount of distilled water in accordance with the ratio of 6% (m/m), seal and fully shake, and use after 12 hours. 5.7 Quartz sand. 270 μm to 830 μm (50 mesh to 20 mesh). Bake in a muffle furnace at 450 ° C for 4 h, cool slightly, place in a ground glass bottle, and store in a desiccator. 5.8 Glass fiber filter. 60 mm diameter. Bake in a muffle furnace at 450 ° C for 4 h, cool a bit and store in a desiccator. 5.9 Standard stock solution of n-hexadecane. ρ≈10000 mg/L. Weigh 1.0 g (accurate to 0.1 mg) of n-hexadecane (5.2) in a 100 ml volumetric flask, dilute with tetrachloroethylene (5.1) Release the volume to the mark and shake well. It can be stored in the refrigerator at 0 ℃ ～ 4 ℃ for one year in the dark. Or purchase a commercially available certified reference material. 5.10 Standard solution of n-hexadecane. ρ = 1000 mg/L. Dilute the n-hexadecane standard stock solution (5.9) with tetrachloroethylene (5.1) and make up to a 100 ml volumetric flask. Temporary use Match. 5.11 Isooctane standard stock solution. ρ≈10000 mg/L. Weigh 1.0 g (accurate to 0.1 mg) of isooctane (5.3) into a 100 ml volumetric flask and make up to volume with tetrachloroethylene (5.1). Shake well. It can be stored in the refrigerator at 0 ℃ ～ 4 ℃ for one year in the dark. Or purchase a commercially available certified reference material. 5.12 Isooctane standard solution. ρ = 1000 mg/L. Dilute the isooctane standard stock solution (5.11) with tetrachloroethylene (5.1) and make up to a 100 ml volumetric flask. Temporary use Match. 5.13 Benzene standard stock solution. ρ≈10000 mg/L. Weigh 1.0 g (accurate to 0.1 mg) benzene (5.4) into a 100 ml volumetric flask, make up to volume with tetrachloroethylene (5.1), shake uniform. It can be stored in the refrigerator at 0 ℃ ～ 4 ℃ for one year in the dark. Or purchase a commercially available certified reference material. 5.14 Standard benzene solution. ρ = 1000 mg/L. Dilute the benzene standard stock solution (5.13) with tetrachloroethylene (5.1) and make up to a 100 ml volumetric flask. Provisional use. 5.15 Petroleum standard stock solution. ρ≈10000 mg/L. According to the ratio of 65.25.10 (V/V), measure the amount of n-hexadecane (5.2), isooctane (5.3) and benzene (5.4). mixture. Weigh 1.0 g (accurate to 0.1 mg) of the mixture into a 100 ml volumetric flask and make up to volume with tetrachloroethylene (5.1). Shake well. It can be stored in the refrigerator at 0 ℃ ～ 4 ℃ for one year in the dark. Or purchase a commercially available certified reference material. 5.16 Standard petroleum liquid. ρ = 1000 mg/L. Dilute the petroleum standard stock solution (5.15) with tetrachloroethylene (5.1) and make it into a 100 ml volumetric flask. Temporary use Match. 5.17 Glass wool. Before use, the glass wool is soaked and washed with tetrachloroethylene (5.1), and dried for use. 5.18 Adsorption column. Pack a small amount of glass wool (5.17) at the exit of a glass column with an inner diameter of 10 mm and a length of about.200 mm, and replace the magnesium silicate (5.6) Slowly pour into the glass column and tap lightly while inverting, the filling height is about 80 mm.

6 Instruments and equipment

6.1 Infrared oil gauge or infrared spectrophotometer. can measure absorbance at 2930 cm-1, 2960 cm-1, 3030 cm-1, And comes with a 40 mm quartz cuvette with lid. 6.2 Horizontal oscillator. The oscillation frequency is (150 ～ 250) times/min. 6.3 Muffle furnace. 6.4 Balance. Sensitivity is 0.01 g and 0.0001 g. 6.5 Erlenmeyer flask with stopper. 100 ml. 6.6 Glass funnel. 60 mm diameter. 6.7 Sampling bottle. 500 ml, wide mouth brown glass bottle with Teflon liner. 6.8 General laboratory utensils and equipment.

7 samples

7.1 Sample collection and storage Collect and store samples in accordance with the relevant requirements of HJ/T 166. The sample is filled with the filled sampling bottle (6.7) and sealed Store in the refrigerator and return to the laboratory for analysis as soon as possible. If it is not analyzed temporarily, it should be stored refrigerated below 4 ℃ for a storage time of 7 d. 7.2 Sample preparation Remove foreign materials (stones, leaves, etc.) from the sample and mix well. Weigh a 10 g (accurate to 0.01 g) sample and add Measure the amount of anhydrous sodium sulfate (5.5), grind and homogenize into a quicksand shape, and transfer to a stoppered conical flask (6.5). 7.3 Determination of dry matter content While weighing the sample, take another sample and determine the dry matter content of the soil sample according to HJ 613. 7.4 Preparation of test specimens Add 20.0 ml of tetrachloroethylene (5.1) to the Erlenmeyer flask (7.2), seal, place in a shaker (6.2), and add.200 Extraction frequency of 30 times per minute. After standing for 10 minutes, use a glass funnel (6.6) with a glass fiber filter (5.8) Filter the extract into a 50 ml cuvette. Repeat the extraction with 20.0 ml of tetrachloroethylene (5.1). All samples were transferred and filtered. Wash the conical flask, filter, glass funnel, and soil with 10.0 ml of tetrachloroethylene (5.1) Samples and combined extracts. Pour the extract into the adsorption column (5.18), discard the first 5 ml of the effluent, and retain the remaining effluent. To be tested. Note. If the oil content in the soil sample is too high, the number of repeated extractions can be appropriately increased. 7.5 Preparation of blank sample Weigh 10 g (accurate to 0.01 g) quartz sand (5.7) in place of the soil sample, as per the sample preparation (7.4) The procedure is to prepare a blank sample.

8 Analysis steps

8.1 Calibration Pipette 2.00 ml of standard use solution of n-hexadecane (5.10), 2.00 ml of standard use solution of isooctane (5.12), and 10.00 ml of benzene standard use solution (5.14) in three 100 ml volumetric flasks, make up to the mark with tetrachloroethylene (5.1), Shake well. The concentrations of n-hexadecane, isooctane and benzene standard solutions were 20.0 mg/L, 20.0 mg/L and 100 mg/L, respectively. Using a 40 mm quartz cuvette with tetrachloroethylene (5.1) as a reference, measure n-hexadecane, isooctane and benzene standards The absorbances of the quasi-solutions at 2930 cm-1, 2960 cm-1, and 3030 cm-1 were A 2930, A 2960, and A3030. N-hexadecane, The absorbances of the isooctane and benzene standard solutions at the above-mentioned wavenumbers are simultaneous equations according to formula (1). Corresponding correction coefficients X, Y, Z and F.  AZAYAX 29303030296029301 (1) Where. ρ1-concentration of petroleum standard solution, mg/L; A2930, A 2960, A3030--absorbance measured at each corresponding wave number; X--the coefficient corresponding to the absorbance of the CH bond in the CH2 group, mg/L/absorbance; Y--the coefficient corresponding to the absorbance of the CH bond in the CH3 group, mg/L/absorbance; Z--coefficient corresponding to the absorbance of the CH bond in the aromatic ring, mg/L/absorbance; F--The correction factor for the effect of aliphatic hydrocarbons on aromatic hydrocarbons, that is, the absorption of n-hexadecane at 2930 cm-1 and 3030 cm-1 Photometric ratio. For n-hexadecane and isooctane, due to their zero aromatic content, 029303030  A, then. ) ( ) ( HA HA F  (2) ) () () (29602930 HAYHAXH  (3) ) () () (29602930 IAYIAXI  (4) The F value can be obtained from formula (2), and the X and Y values can be obtained from formulas (3) and (4). For benzene.  BA BAZBAYBAXB ) ( ) () () () (2930303029602930 (5) The Z value can be obtained from formula (5). Where. ρ (H)-the concentration of n-hexadecane standard solution, mg/L; ρ (I)-concentration of isooctane standard solution, mg/L; ρ (B)-the concentration of benzene standard solution, mg/L; A2930 (H), A2960 (H), A3030 (H)-Measure the absorbance of n-hexadecane standard solution at each corresponding wave number A2930 (I), A2960 (I), A3030 (I)-the absorbance of the isooctane standard solution measured at each corresponding wavenumber; A2930 (B), A2960 (B), A3030 (B)-Measure the absorbance of benzene standard solution at each corresponding wavenumber Note. If the calibration coefficient is set when the infrared oil meter or infrared spectrophotometer is shipped from the factory, you can directly check the calibration coefficient according to 11.3.1. Check. 8.2 Determination of sample Transfer the remaining effluent after adsorption with magnesium silicate (7.4) to a 40 mm quartz cuvette and use tetrachloroethylene (5.1) For reference, the absorbances A 2930, A2960, and A3030 were measured at the wave numbers of 2930 cm-1, 2960 cm-1, and 3030 cm-1. according to Equation (1) calculates the petroleum concentration. 8.3 Blank test Follow the same procedure as for the measurement of the sample (8.2), and perform the measurement of the blank sample (7.5).

9 Calculation and representation of results

9.1 Calculation of results The content of petroleum in the soil w (mg/kg) is calculated according to formula (6). dmWm  2 (6) Where. w- petroleum content in soil, mg/kg; ρ2--Petroleum concentration in the extract, mg/L; V--extract volume, ml; m--mass of soil sample, g; Wdm--dry matter content of soil,%. 9.2 Representation of results The number of digits after the decimal point in the measurement result is the same as the detection limit of the method. A maximum of 3 significant digits are retained. 10 Precision and accuracy 10.1 Precision Six laboratories have uniformly collected garden soil samples with a petroleum concentration of about 30 mg/kg and 70 mg/kg sewage irrigation areas The soil uniform sample and the 150 mg/kg iron smelter soil uniform sample were subjected to 6 repeated determinations. The relative standard deviation in the laboratory The differences were 5.0% to 7.4%, 3.9% to 5.9%, and 1.9% to 4.0%; the relative standard deviations between laboratories were 3.9%, 2.7% and 2.4%; repeatability limits are 5 mg/kg, 9 mg/kg, and 11 mg/kg, respectively; reproducibility limits are 6 mg/kg, 10 mg/kg and 14 mg/kg. 10.2 Accuracy Six laboratories have uniformly collected garden soil samples with a petroleum concentration of about 30 mg/kg and 70 mg/kg sewage irrigation areas A unified sample of soil and a uniform sample of 150 mg/kg of iron from the ironworks were used for analysis and determination. The spiked amounts were 300 μg, 700 μg and 1500 μg, with spiked recoveries ranging from 83.6% to 88.9%, 84.9% to 91.7%, and 84.4% to 90.3%; The final recoveries were (86.5 ± 4.2)%, (88.0 ± 5.0)%, and (87.1 ± 4.8)%. 11 Quality Assurance and Quality Control 11.1 Tetrachloroethylene quality inspection Tetrachloroethylene shall be stored protected from light. Before use, the quality inspection and judgment of tetrachloroethylene must be carried out in accordance with (5.1) to confirm compliance. Can only be used after required. 11.2 Blank test Do at least two laboratory blank tests for every 20 samples or batches (≤20 samples/batch). The blank test results should be Below method detection limit. 11.3 Calibration coefficient test Each batch of samples should be tested for the correction coefficient. When using, according to the required concentration, take an appropriate amount of petroleum standard use solution. (5.16), using tetrachloroethylene as a solvent to prepare a petroleum standard solution of appropriate concentration, the same step as the sample measurement (8.2) Carry out the measurement immediately, and calculate the concentration of petroleum standard solution according to formula (1). If the relative error between the measured value and the standard value Within ± 10%, the correction factor can be used, otherwise the correction factor is re-measured and checked until it meets the conditions. Testing can also be performed using certified reference materials/samples. 11.4 Parallel samples Every 20 samples or each batch (≤20 samples/batch) samples should be measured in a parallel sample, the relative deviation of parallel samples Should be ≤30%. 11.5 Matrix Spiking Every 20 samples or each batch (≤20 samples/batch) samples should be measured for a matrix spiked sample, and the spiked recovery rate should be Controlled between 70% and 110%. 12 Waste treatment The waste generated in the experiment should be collected separately, and properly identified, and entrusted to a qualified unit for processing. 13 Notes 13.1 The tetrachloroethylene used for the determination of the same batch of samples should come from the same bottle. If there are a large number of samples, multiple bottles of tetrachloroethylene can be used. Use after mixing. 13.2 The sample preparation room should be clean and free from contamination. The sample preparation process should be kept away from organic gases. All tools used should be Perform thorough cleaning to prevent cross-contamination. ......

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