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HJ 804-2016: (Determination of Available Soil eight kinds of elements diethylenetriamine pentaacetic acid extraction - inductively coupled plasma emission spectrometry)
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Basic data

Standard ID HJ 804-2016 (HJ804-2016)
Description (Translated English) (Determination of Available Soil eight kinds of elements diethylenetriamine pentaacetic acid extraction - inductively coupled plasma emission spectrometry)
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z18
Word Count Estimation 11,167
Date of Issue 2016-06-24
Date of Implementation 2016-08-01
Regulation (derived from) Ministry of Environmental Protection Announcement No.47, 2016
Issuing agency(ies) Ministry of Ecology and Environment

HJ 804-2016: (Determination of Available Soil eight kinds of elements diethylenetriamine pentaacetic acid extraction - inductively coupled plasma emission spectrometry)


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(Determination of available soil eight kinds of elements diethylenetriamine pentaacetic acid extraction - inductively coupled plasma emission spectrometry) National Environmental Protection Standard of the People 's Republic of China Determination of 8 Effective Elements in Soil Extraction of diethylene triamine pentaacetic acid - inductively coupled plasma Body emission spectroscopy Soil - Determination of bioavailable form of eight elements - Extraction with Buffered DTPA solution/Inductively coupled plasma optical emission spectrometry 2016-06-24 released 2016-08-01 implementation Ministry of Environmental Protection I directory Preface ii 1 Scope of application 1 2 normative reference document 1

3 Terms and Definitions

Principle of Method 1

5 interference and elimination

6 reagents and materials

7 Instruments and equipment

8 samples

9 Analysis Step 4 Results and Expressions 11 Precision and Accuracy 6 12 Quality assurance and quality control 13 Waste treatment 6 14 Precautions 6 Appendix A (informative) method of precision and accuracy of summary data 7

Foreword

To implement the "People's Republic of China Environmental Protection Law" to protect the environment, protect human health, regulate the soil in the effective state The determination of the method, the development of this standard. This standard specifies the extraction of copper, iron, manganese, zinc, cadmium, cobalt, nickel and lead in soil by extraction with diethylenetriaminepentaacetic acid. Inductively Coupled Plasma Atomic Emission Spectrometry. This standard is the first release. Appendix A of this standard is an informative appendix. This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division. The main drafting unit of this standard. Yunnan Province Environmental Monitoring Center Station. This standard is verified by. Institute of Biogeochemistry, Xishuangbanna Tropical Botanical Garden, Chinese Academy of Sciences, Shanghai Environmental Monitoring Measuring center, Sichuan Province Environmental Monitoring Station, Jiangsu Province Environmental Monitoring Center, Yuxi City Environmental Monitoring Station and Taizhou Environmental Monitoring Center station. The Environmental Protection Department of this standard was issued on June 24,.2016. This standard has been implemented since August 1,.2016. This standard is explained by the Ministry of Environmental Protection. Determination of 8 active elements in soil Extraction of diethylene triamine pentaacetic acid - inductively coupled plasma - atomic emission spectrometry

1 Scope of application

This standard specifies the use of diethylenetriaminepentaacetic acid (DTPA) extraction of soil in the determination of the effective elements of the inductance coupling Son emission spectroscopy. This standard is applicable to the effects of copper (Cu), iron (Fe), manganese (Mn), zinc (Zn), cadmium (Cd), cobalt (Co) (Ni) and lead (Pb) were measured. When the sampling volume is 10.0 g and the volume of the extract is 20 ml, the detection limit and the determination limit of this method are shown in Table 1. Table 1 Method Detection limit and lower limit of determination (mg/kg) Elemental copper, iron, manganese, zinc, cadmium and cobalt Method Detection limit 0.005 0.04 0.02 0.04 0.007 0.02 0.03 0.05 Determination of the lower limit of 0.02 0.16 0.08 0.16 0.028 0.08 0.12 0.2

2 normative reference documents

The contents of this standard refer to the following documents or their terms. Those who do not specify the date of the reference file, the effective version of the appropriate For this standard. Technical specification for soil environmental monitoring Determination of Dry Matter and Moisture in Soil

3 terms and definitions

The following terms and definitions apply to this standard. 3.1 Soil active elements The elements that can be absorbed by the plant roots during the growing period of the plant, that is, under the conditions specified in this standard can be DTPA buffer solution is extracted from the soil.

4 principle of the method

(DTPA-CaCl2-TEA) buffer solution was extracted with diethylene triamine pentaacetic acid-calcium chloride-triethanolamine (DTPA-CaCl2-TEA) The element was determined by inductively coupled plasma emission spectrometry. The sample is atomized by the carrier gas into the atomization system, enters the plasma in the form of aerosols, and the target element is in the plasma The torch is vaporized, ionized, excited and radiated to the characteristic line. In a certain concentration range, the characteristic line intensity and the element The concentration of the ingredients is proportional.

5 interference and elimination

5.1 spectral interference 2 spectral interference, including spectral overlap interference and continuous background interference. Select the appropriate analysis line to avoid the overlap of spectral lines Interference, Table 2 for the measured elements in the proposed analysis of the wavelength of the main spectral interference. Use the instrument's own calibration software or interference Coefficient method to correct the spectral interference, when there is a single element of interference, according to formula (1) obtained interference coefficient. T Q Qq ) '(  (1) Where. tK - interference coefficient; 'Q - content measured at the wavelength of the element, μg/L; Q - Analysis of elemental content, μg/L; TQ - the content of interfering elements, μg/L. By preparing a series of known interfering element content solutions, the 'Q is determined at the position of the elemental wavelengths, (1) to find tK, and then artificial deduction or computer automatic deduction. Continuous background interference is usually deducted by the instrument Background method to eliminate. Note that the interferometric coefficients for different instruments are different. Table 2 The main spectral interference of the element to be measured Measured element wavelength/nm interference element element to be measured wavelength/nm interference element Cu 324.754 327.396 Fe, Al, Ti, Mo Cd 214.438 Fe Fe 239.924 Cr, W 226.502 Fe, Ni, Ti, Ce, K, Co 240.488 Mo, Co, Ni 228.806 As, Co, Sc 259.940 Mo, W Co 228.616 Ti, Ba, Cd, Ni, Cr, Mo, Ce 261.762 Mg, Ca, Be, Mn 230.768 Fe, Ni Mn 257.610 Fe, Mg, Al, Ce 238.892 Al, Fe, V, Pb 293.306 Al, Fe Ni 231.604 Fe, Co Zn 202.548 Co, Mg 221.647 W 206.200 Ni, La, Bi Pb 220.353 283.306 Fe, Al, Ti, Co, Ce, Sn, Bi 213.856 Ni, Cu, Fe, Ti 5.2 Non-spectral interference Non-spectral interference mainly includes chemical interference, ionization interference, physical interference and solvent interference. In the actual analysis process , All kinds of interference is difficult to separate. Whether it is compensated and corrected, and the concentration of interfering elements in the sample. In addition, Physical interference is generally caused by the viscosity of the sample and the surface tension changes, especially the sample contains a large number of soluble salts or Acid is too high, will interfere with the determination. An effective way to eliminate or reduce such interference is dilution or matrix matching (That is, the components of the standard solution used in addition to the target substance are consistent with the sample solution). 36 reagents and materials Unless otherwise stated, analytical reagents conforming to national standards are used for analysis. Experimental water is a newly prepared deionized Water or water of the same purity. 6.1 Triethanolamine (C6H15NO3). TEA. 6.2 Diethylenetriaminepentaacetic acid (C14H23N3O10). DTPA. 6.3 Calcium chloride dihydrate (CaCl2 · 2H2O) .. 6.4 hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure. 6.5 nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure. 6.6 Hydrochloric acid solution. 1 1, prepared with hydrochloric acid (6.4). 6.7 nitric acid solution. 2 98, with nitric acid (6.5) preparation. 6.8 Nitric acid solution. 1 1, with nitric acid (6.5) preparation. 6.9 leaching solution. c (TEA) = 0.1 mol/L, c (CaCl2) = 0.01 mol/L, c (DTPA) = 0.005 mol/L; Is 7.3. 14.92 g (accurate to 0.0001 g) triethanolamine (6.1), 1.967 g (accurate to 0.0001 g) were added sequentially to the beaker, (6.3), 1.470 g (0.0001 g) of calcium chloride dihydrate (6.3), water was added and stirred to give The solution was completely dissolved and the water was diluted to about 800 ml. The pH was adjusted to 7.3 ± 0.2 with hydrochloric acid solution (6.6) Measured), transferred to 1000 ml volumetric flask to constant volume, shake. 6.10 standard solution 6.10.1 Elemental standard stock solution. available high purity metal (purity greater than 99.99%) or metal salts (reference or high purity Reagent) formulated as a standard stock solution of 1000 mg/L or 500 mg/L hydrochloric acid solution (6.6) with a hydrochloric acid content of 1% (V/v) or more. You can also purchase commercially available certified materials. 6.10.2 single element standard use of liquid. respectively, remove the single element standard stock solution (6.10.1) dilution preparation. When diluted, add one Quantitative hydrochloric acid solution (6.6), so that the standard use of hydrochloric acid content of 1% (v/v) above. 6.10.3 multi-element standard solution. ρ =.200 mg/L, dilutable single element standard stock solution (6.10.1) preparation, dilution Add a certain amount of hydrochloric acid solution (6.6), so that the standard use of hydrochloric acid content of 1% (v/v) or more. You can also purchase commercially available certificates standard material. Note 1. All elements of the standard solution after preparation, should be sealed in polyethylene or polypropylene bottles. 6.11 Carrier gas. argon (purity ≥99.99%).

7 instruments and equipment

7.1 Inductively Coupled Plasma Atomic Emission Spectrometer. Computer Control System with Background Correction Emission Spectroscopy. 7.2 Oscillator. The frequency can be controlled at 160 r/min ~.200 r/min. 7.3 pH meter. The index is 0.1 pH. 7.4 Analysis of balance. accuracy of 0.0001 g and 0.01 g. 7.5 Centrifuge. 3000 r/min ~ 5000 r/min. 7.6 Centrifuge tube. 50 ml. 7.7 with a triangular bottle. 100 ml. 7.8 medium speed quantitative filter paper. 47.9 nylon screen. pore size 2.0 mm (10 mesh). 7.10 General laboratory equipment and equipment commonly used.

8 samples

8.1 Sample collection and storage Collect and preserve soil samples in accordance with the relevant provisions of HJ/T 166. Sampling, transport and preservation should avoid contamination And the element to be measured. 8.2 Determination of dry matter content The dry matter content of soil samples was measured in accordance with HJ 613. 8.3 Sample preparation Remove the sample of sticks, leaves, stones and other foreign matter, in accordance with the requirements of HJ/T 166, the collected samples in the laboratory Dry air, coarse grinding, fine grinding to through diameter 2.0 mm (10 mesh) nylon sieve (7.9). The preparation of the sample should avoid contamination And the element to be measured. 8.4 Preparation of sample Weigh the sample with 10.0 g (accurate to 0.01 g) and place it in a 100 ml Erlenmeyer flask (7.7). Add 20.0 ml of the extract (6.9), Tighten the stopper. And oscillated at an oscillation frequency of 160 r/min ~.200 r/min for 2 h at 20 ° C ± 2 ° C. The extract is slow (7.6) centrifuged in the centrifuge (7.5) for 10 min, the supernatant was quantified by medium speed quantitative filter paper (7.8) After filtration, the assay was carried out within 48 h. If the amount of leaching solution required is large, the amount of sample can be increased appropriately, but the ratio of sample to extract is 1. 2 (m/v) At the same time should be used with the volume of the extraction of the container to ensure the full oscillation of the sample. 8.5 Preparation of laboratory blank samples A laboratory blank sample was prepared without the same procedure as in the preparation of the sample (8.4).

9 Analysis steps

9.1 Instrument reference measurement conditions Different models of the best test conditions of different instruments should be in accordance with the instrument manual to optimize the RF power, atomizer pressure, Carrier gas flow rate, cooling air flow rate and other working parameters. Instrument reference measurement conditions in Table 3. Table 3 Instrument determination reference conditions element Detection wavelength (Nm) Secondary detection wavelength (Nm) RF power nebulizer pressure carrier gas flow rate cooling air flow rate determination times Copper 324.754 327.396 1100 W 55 psi 1.4 L/min 19 L/min 3 times Iron 259.940 239.924 Manganese 257.610 293.306 Zinc 213.856 202.548 Cadmium 214.438 226.502 Cobalt 228.616 238.892 Nickel 231.604 221.647 Lead 220.353 217.000 59.2 Drawing of standard curves Ignite the plasma, according to the manufacturers to provide the operating parameters set, until the instrument preheat to the indicators after the stability of the open Start the measurement. Respectively, to remove a volume of multi-element standard solution (6.10.3) placed in a group of 100 ml volumetric flask, with a dip Extract (6.9) diluted to constant volume, mix. The lowest concentration point of the leaching solution (6.9) as the standard series was prepared at the same time 5 standard concentration of the standard series, the standard series of solution concentrations in Table 4. According to the optimized instrument reference conditions (9.1), the standard system Columns are sequentially analyzed from low concentration to high concentration into the atomizer. The mass concentration of the target element is the abscissa, corresponding to it The emission intensity is the ordinate and the standard curve is established. The concentration range of the standard curve can be determined according to the concentration of the element to be measured in the actual sample To adjust the situation. Table 4 Standard Series Solution Concentration Elemental C0 (mg/L) C1 (mg/L) C2 (mg/L) C3 (mg/L) C4 (mg/L) C5 (mg/L) Copper 0.00 0.25 0.50 1.00 2.00 4.00 Iron 0.00 5.00 10.0 20.0 40.0 80.0 Manganese 0.00 2.00 5.00 10.0 20.0 30.0 Zinc 0.00 0.20 0.50 1.00 2.00 4.00 Cadmium 0.00 0.01 0.02 0.04 0.08 0.12 Cobalt 0.00 0.10 0.20 0.30 0.40 0.50 Nickel 0.00 0.05 0.25 0.50 0.75 1.00 Lead 0.00 0.50 1.00 1.50 2.00 5.00 9.3 Determination 9.3.1 Determination of sample Before measuring the sample, rinse the system with nitric acid solution (6.7) until the instrument signal is minimized and the signal to be stabilized Can begin to measure. The determination of the sample was carried out according to the same conditions and procedures as for the establishment of the standard curve (9.2). If the sample is to be tested The concentration of the element is outside the standard curve, and the sample must be re-measured after dilution. The diluent is extracted with the extract (6.9), diluted Multiple f 9.3.2 Determination of laboratory blank samples The laboratory blank samples were determined according to the same conditions and procedures as the test (9.3.1) of the sample. 10 results are calculated and expressed 10.1 Result calculation The content of the active elements in the soil sample  (mg/kg) is calculated according to the formula (2)   Dm FV W    (2) Where.  - the content of the active element in the soil sample, mg/kg; Ρ - by the standard curve to determine the determination of the effective concentration of the sample element concentration, mg/L; 6ρ0 - mass concentration of active elements in laboratory blank samples, mg/L; V - the volume of the extract added when the sample is prepared, ml; F - the dilution factor of the sample; M - the quality of the sample after sieving, g; Wdm - dry matter content of soil samples,%. 10.2 results are shown The number of decimal places for the determination is consistent with the method detection limit, and a maximum of three significant digits are retained. 11 precision and accuracy 11.1 precision Six laboratory samples were used for three different levels of uniform soil standard samples and two different concentrations of actual soil samples Six parallel determinations were performed. The precision of the results is shown in Table A.1 in Appendix A. 11.2 Accuracy Six laboratories carried out six parallel tests on soil samples of three different levels of soil, respectively. With the concentration of the actual soil samples were 6 times the standard recovery rate determination. The accuracy of the results is given in Table A.2 in Appendix A. 12 quality assurance and quality control 12.1 each batch of samples to do at least two laboratory blank samples, the determination of the results should be lower than the lower limit of determination. 12.2 Each test shall establish a standard curve with a correlation coefficient ≥0.999. Every 20 samples or per batch (less than 20 samples) Product/batch) sample, should be analyzed a standard curve of the middle concentration point, the measured results and the actual concentration of the relative deviation of ≤ 10% Otherwise, you should find the cause or reestablish the standard curve. 12.3 Each batch of samples shall be tested in parallel at least 10% of the proportions. If the number of samples is less than 10, at least one The relative deviation of the results of parallel parallel samples should be less than 20%. 12.4 Each batch of samples shall be analyzed for at least one valid soil reference material. The results shall be determined in the range of uncertainty given Inside. 13 Waste treatment Waste and waste generated in the experiment should be collected and stored in a sorted manner. 14 Precautions 14.1 The glassware used in the experiment shall be soaked in nitric acid solution (6.8) for 24 h, washed with tap water and experimental water, Placed in a clean environment to dry. Newly used or suspected contaminated container, applied with hot hydrochloric acid solution (6.6) soaked (temperature Higher than 80 ℃, below the boiling temperature) 2 h or more, and hot nitric acid solution (6.8) soaking more than 2 h, followed by tap water And the experimental water rinse, placed in a clean environment to dry. 14.2 After the instrument is ignited, it should be preheated for more than 30 min to prevent wavelength drift. 14.3 When preparing standard solutions and preparing samples, use the same batch of formulated extracts.

7 Appendix A

(Informative) Method of precision and accuracy summary data Table A.1 gives the method for determining the precision of the eight active elements of this standard. Table A.2 shows the eight elements Effective method of accuracy. Table A.1 Summary of the precision of the method Name Sample number average value (Mg/kg) Laboratory relative standard deviation(%) Inter-laboratory relative standard deviation(%) Repetitive limit r (Mg/kg) Reproducibility R (Mg/kg) Standard Sample 1 1.18 0.91 to 2.7 3.7 0.072 0.138 Standard sample 2 1.84 0.47 to 5.8 6.5 0.138 0.360 Standard sample 3 0.238 2.1 to 11 9.5 0.050 0.078 Actual sample 1 1.24 0.42 to 2.4 6.3 0.093 0.234 Actual sample 2 0.283 0.67 to 6.0 10 0.028 0.083 Standard sample 1 53.3 0.45 to 5.1 7.4 3.50 11.4 Standard sample 2 38.8 0.36 to 2.8 7.3 1.64 8.05 Standard sample 3 22.5 0.28 to 5.7 15 1.73 9.38 Actual sample 1 26.9 0.52 to 2.4 6.8 0.99 5.22 Actual sample 2 79.6 0.67 to 3.2 3.0 4.39 7.73 Standard sample 1 16.7 0.36 to 4.8 6.9 1.17 3.39 Standard sample 2 22.3 0.57 ~ 2.9 5.7 1.01 3.70 Standard sample 3 5.71 0.43 to 8.0 9.4 0.62 1.60 Actual sample 1 16.9 0.48 to 5.3 14 1.61 6.76 Actual sample 2 7.92 0.52 ~ 2.3 1.8 0.31 0.48 Standard sample 1 1.04 1.7 to 4.6 3.0 0.09 0.12 Standard sample 2 2.24 0.24 to 6.0 6.3 0.17 0.43 Standard sample 3 0.54 0.51 to 5.8 8.6 0.05 0.14 Actual sample 1 1.14 0.72 to 5.7 13 0.11 0.42 Actual sample 2 0.67 1.0 to 3.7 12 0.05 0.22 Standard sample 1 0.040 1.0 to 4.2 2.1 0.005 0.005 Standard sample 2 0.116 0.92 to 5.8 2.6 0.012 0.014 Standard sample 3 0.016 3.3 ~ 6.8 10 0.003 0.005 Actual sample 1 0.021 2.8 ~ 8.7 12 0.004 0.008 Actual sample 2 0.020 2.2 ~ 12 17 0.004 0.010 Standard sample 1 0.13 1.9 to 6.4 12 0.02 0.05 Standard sample 2 0.10 1.8 to 7.3 7.3 0.01 0.02 Standard sample 3 0.08 1.0 to 8.8 12.2 0.01 0.03 Actual sample 1 0.13 1.4 to 4.4 15 0.01 0.06 Actual sample 2 0.02 9.1 to 15 14 0.01 0.01 Standard sample 1 0.27 1.5 to 16 7.4 0.06 0.08 Standard sample 2 0.42 0.36 to 6.3 3.4 0.04 0.05 Standard sample 3 0.07 1.8 to 11 8.8 0.01 0.02 Actual sample 1 0.23 1.2 to 5.2 6.7 0.02 0.05 Actual sample 2 0.06 2.9 to 6.9 14 0.01 0.03 Standard sample 1 1.62 0.94 to 6.2 3.9 0.16 0.23 Standard sample 2 1.57 1.6 ~ 7.5 5.9 0.20 0.32 Standard sample 3 1.52 1.7 ~ 14.7 18 0.29 0.79 Actual sample 1 1.18 0.70 to 4.6 8.8 0.11 0.31 Actual sample 2 5.25 1.0 to 5.7 6.7 0.46 1.07 8 Table A.2 Summary of the accuracy of the method Name Sample number Recognized and incorrect (Mg/kg) Determine the mean (Mg/kg) Relative error (%) Relative error Final value (%) Spiked recovery rate range(%) Spiked recovery rate Final value (%) Standard sample 1 1.17 ± 0.07 1.18 -3.4 ~ 7.7 0.93 ± 7.5 // Standard Sample 2 1.85 ± 0.17 1.84 -9.2 ~ 9.2 -0.33 ± 13 // Standard sample 3 0.24 ± 0.04 0.238 -15 ~ 13 -0.70 ± 19 // Actual sample 1/1.24 // 86.7 to 113 99.7 ± 21.0 Actual sample 2/0.283 // 85.9 ~ 97.9 92.1 ± 8.8 Standard sample 1 55 ± 7 53.3 -12 ~ 6.6 -3.1 ± 14 // Standard sample 2 38 ± 5 38.8 -9.7 ~ 13 2.1 ± 15 // Standard sample 3 23 ± 5 22.5 -18 to 16 -2.0 ± 29 // Actual sample 1/26.9 // 90.8 ~ 114 102 ± 18.0 Actual sample 2/79.6 // 93.9 to 106 99.9 ± 10.2 Standard sample 1 17.3 ± 2.5 16.7 -11 to 4.1 -3.4 ± 13 // Standard sample 2 23 ± 3 22.3 -12 ~ 1.7 -2.9 ± 11 // Standard sample 3 5.7 ± 0.7 5.71 -12 ~ 13 0.12 ± 19 // Actual sample 1/16.9 // 90.0 to 139 106 ± 35.4 Actual sample 2/7.92 // 89.9 ~ 105 95.8 ± 10.2 Standard sample 1 1.08 ± 0.09 1.04 -6.5 ~ 0.93 -3.6 ± 5.6 Standard sample 2 2.4 ± 0.3 2.24 -14 ~ 3.3 -6.5 ± 12 Standard sample 3 0.53 ± 0.08 0.54 -14 ~ 8.3 1.7 ± 18 Actual sample 1/1.14 // 81.2 ~ 112 93.8 ± 21.4 Actual sample 2/0.67 // 83.2 ~ 102 94.0 ± 12.8 Standard sample 1 0.040 ± 0.003 0.040 -2.8 ~ 2.5 -0.74 ± 4.0 // Standard sample 2 0.12 ± 0.01 0.116 -6.7 ~ 0.0 -3.4 ± 5.0 // Standard sample 3 0.016 ± 0.004 0.016 -19 ~ 12 0.10 ± 21 // Actual sample 1/0.021 // 87.4 ~ 102 94.7 ± 11.3 Actual sample 2/0.020 // 92.0 ~ 114 99.5 ± 18.0 Standard sample 1 0.13 ± 0.04 0.13 -18 ~ 15 1.3 ± 24 // Standard sample 2 0.10 ± 0.03 0.10 -11 to 10 0.62 ± 15 // Standard sample 3 0.083 ± 0.018 0.08 -20 ~ 15 -1.9 ± 24 // Actual sample 1/0.13 // 83.6 ~ 104.8 95.9 ± 15.7 Actual sample 2/0.02 // 85.6 ~ 110.8 98.4 ± 18.6 Standard sample 1 0.27 ± 0.03 0.27 -11 to 7.8 0.98 ± 15 // Standard sample 2 0.43 ± 0.04 0.42 -7.7 ~ 0.27 -3.4 ± 6.7 // Standard sample 3 0.072 ± 0.012 0.07 -11 to 11 1.0 ± 18 // Actual sample 1/0.23 // 91.3 ~ 105 95.5 ± 10.0 Actual sample 2/0.06 // 89.7 to 104 95.0 ± 12.9 Standard sample 1 1.7 ± 0.2 1.62 -12 ~ -1.2 -4.9 ± 7.5 // Standard sample 2 1.6 ± 0.2 1.57 -12 ~ 2.5 -2.0 ± 12 // Standard sample 3 1.5 ± 0.4 1.52 -25 ~ 21 1.5 ± 36 // Actual sample 1/1.18 // 88.8 ~ 110 97.1 ± 15.0 Actual sample 2/5.25 // 90.7 to 104 95.7 ± 9.54

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