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HJ 813-2016: Analysis of Polonium-210 in water
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Basic data

Standard ID: HJ 813-2016 (HJ813-2016)
Description (Translated English): Analysis of Polonium-210 in water
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z33
Word Count Estimation: 11,165
Date of Issue: 2016-10-12
Date of Implementation: 2016-11-01
Older Standard (superseded by this standard): GB/T 12376-1990
Regulation (derived from): Ministry of Environmental Protection Notice No.62 of 2016
Issuing agency(ies): Ministry of Ecology and Environment

HJ 813-2016: Analysis of Polonium-210 in water

---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
(Analysis of polonium - 210 in water) National Environmental Protection Standard of the People 's Republic of China Replacing GB 12376-90 Analysis of polonium - 210 in water Analysis of Polonium-210 in water 2016-10-12 released 2016-11-01 implementation Issued by the Ministry of Environmental Protection Directory Preface ..II 1 Scope of application 1 2 normative reference document 1 Principle of Method 1

4 reagents and materials

5 instruments and equipment

6 the scale of the instrument

7 sample collection 2 8 Analysis Procedure 2 9 blank experiment 3 10 results calculated 3 Quality control 4 12 Uncertainty Assessment .4 Appendix A..8

Foreword

In order to implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on the Prevention and Control of Radioactive Pollution, Protect the human health, regulate the environmental monitoring methods, the development of this standard. This standard specifies the method of analysis of polonium-210 in water. This standard is the "water polonium -210 analysis method electroplating sample preparation method" (GB 12376-90) revision, the use of the analysis side Principle and the original standard is basically the same, the main technical content has updated changes. "Determination of polonium-210 in the electroplating method" (GB 12376-90) was first released in.1990, the original standard draft Unit for the Nuclear Industry Corporation Beijing Institute of uranium mining and smelting. The main technical contents of this standard are as follows. - delete the "plating sample preparation method" and other non-standard text expression; - revised methodological principles; - introduced polonium -209 tracer; - Partial revision of the analytical procedures; - self-deposition material replaced by silver by the original standard copper; - the measuring instrument is replaced by the alpha energy spectrometer with the original standard low background α, β proportional counter; - revised the results of the calculation formula; - Increased assessment of the uncertainty of the results; - Blank experiment and quality control made clear requirements; Since the implementation of this standard, the former State Environmental Protection Bureau on June 9,.1990 approved and issued the People's Republic of China national standard Quasi "water polonium -210 analysis method electroplating method" (GB 12376-90) abolished. The appendix to this standard is an informative appendix. This standard is organized by the Ministry of Environmental Protection Nuclear Safety Management Division, Science and Technology Standards Division. The main drafting of this standard. Ministry of Environmental Protection Radiation Environmental Monitoring Technology Center (Zhejiang Province, radiation environmental monitoring station). The environmental protection department of this standard approved on October 12,.2016. This standard has been implemented since November 1,.2016. This standard is explained by the Ministry of Environmental Protection. Analysis of polonium - 210 in water

1 Scope of application

This standard specifies the determination of polonium-210 in water. This standard applies to surface water, seawater, groundwater and nuclear industry wastewater discharge. The measurement range of this method is. the activity concentration is greater than 1 × 10-3Bq/L.

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. GB 12997 water quality sampling program design technical specifications Technical Guidance for Water Quality Sampling Technical specification for preservation and management of samples for water quality sampling Technical specification for radiation environmental monitoring of HJ/T 61

3 Principle of the method

Water samples were added to the known 209Po tracer, with iron hydroxide as carrier, adsorbed in water carrying 210Po and 209Po. Hydrochloric acid dissolved After precipitation, add ascorbic acid and hydroxylamine hydrochloride to restore ferric iron. In the hydrochloric acid system, 210Po and 209Po were self-deposited to pure silver on. Measured in the alpha spectrometer, according to 210Po and 209Po count, calculate the concentration of 210Po activity in water. When each sample contains 25 μg of gold, 25 μg of platinum, 25 μg of tellurium, 50 μg of mercury and 100 μg of vanadium, the 210Po results are low.

4 reagents and materials

Unless otherwise stated, analytical pure chemical reagents conforming to national standards are used in the analysis, and the test water is freshly prepared. Ionized water or distilled water. 4.1 ascorbic acid (C6H8O6). 4.2 potassium permanganate solution (KMnO4) solution. 2% (m/V). 4.3 concentrated hydrochloric acid (HCl). mass concentration of 36.0% ~ 38.0% (m/m). The 4.4 Hydrochloric acid. 1 mol/L. 4.5 hydrochloric acid. 0.5mol/L. 4.6 Hydrochloric acid. 0.1 mol/L. 4.7 ferric chloride (FeCl3) solution. 20mgFe/mL, 0.1mol/L hydrochloric acid system. 4.8 ammonia (NH3 · H2O). mass concentration of 25% to 28% (m/m). 4.9 Hydrogen Peroxide (H2O2). Concentration Concentration 30% (m/m). 4.10 Hydroxylamine hydrochloride (NH2HClOH). mass concentration 25% (m/m) 4.11 anhydrous ethanol (C2H5OH). content of not less than 99.5% (m/m). 4.12 polonium -209 standard solution. 0.1 Bq/mL, 1 mol/L hydrochloric acid system. 4.13 pH test paper. pH = 0.5 ~ 5.5 and pH = 5.5 ~ 9.0. 4.14 silver. thickness 0.5mm, diameter 21mm. Before use, the silver side should be coated with paint, the other side with water sandpaper throwing Light, clean water after drying dry.

5 instruments and equipment

5.1 α spectrometer, the background is less than 1 cph. 5.2 Analysis of balance, the amount of 0.1 mg. 5.3 Magnetic heating electric stirrer. 5.4 hot plate. 5.5 Oven.

6 the scale of the instrument

6.1 Energy scale The energy scale is used to store the energy of the energy spectrum with mixed plating. The result is preserved. 6.2 Efficiency scale Use the mixed plating α surface source to perform the efficiency scale on the energy spectrum, and take the average value as the instrument efficiency value.

7 sample collection

7.1 Acquisition and storage Samples were collected and stored in accordance with the relevant provisions in GB 12997, GB 12998 and HJ 493. 7.2 Pretreatment of the sample After the sample collection, add concentrated hydrochloric acid acidification, pH < 2, standing, filtering, stand-by.

8 analysis procedures

8.1 Accurately measure 5L of filtered water, add 1 mL of 209Po standard solution (4.12), add 2 to 3 drops Potassium permanganate solution (4.2) until the water samples were stable lavender, allowed to stand for 30 min. 8.2 Add 5.0 mL of ferric chloride solution (4.7) and stir until the solution is homogeneous and heated to 600 ° C on the hot plate. under. 8.3 Slowly add ammonia (4.8) with stirring until pH = 9.2 (measured with a precision pH test strip), stir every half hour Once, until no floating suspension, standing overnight. 8.4 Dilute (or siphon) the supernatant and filter. Wash the beaker and filter paper 3 times with deionized water and discard the filtrate. 8.5 with 6 ~ 8 mL hydrochloric acid (4.4) dissolved precipitate, the filtrate collected in 100 mL beaker. Followed by 10 mL of hydrochloric acid (4.6) And 5 mL of deionized water to clean the filter paper and the cleaning solution is combined into the beaker. 8.6 Add 2 to 3 drops of hydrogen peroxide (4.9) to the beaker and slightly soak for 3 min on the hot plate. 8.7 After the solution is slightly cold, add 2 ~ 3 g ascorbic acid (4.1) and 0.5 mL hydroxylamine hydrochloride (4.10), add 30 ~ 40 mL Hydrochloric acid (4.6), control acidity of 0.2 ~ 0.5 mol/L, the total volume of about 70 mL. 8.8 Place the stirrer into the beaker, bracket, surface dish and silver (4.14). The whole beaker is placed in the crystal dish and filled Water, open heating and stirring function, self-deposition 1 ~ 2 h. 8.9 Remove the silver, first with deionized, and then immersed in anhydrous ethanol (4.11) soak for about 20 min. Remove, deionize After the water rinse naturally dry, coated with paint on the sample label, and then placed in the 1100C constant temperature drying oven for 1 h. 8.10 silver chip into the alpha spectrometer continuous counting 48 h.

9 blank experiment

Regular blank experiment, whenever the replacement of reagents, should be blank experiments; each batch of samples should be blank Experiment; under normal circumstances the number of blank samples should not be less than 5% of the total number of sample analysis. The method is as follows. 9.1 take four 5 L of deionized water, with hydrochloric acid to adjust the pH < 2, standing. 9.2 Complete the experiment according to the procedure specified in 8.2 to 8.10 and measure the total number of blanks on the alpha spectrometer. 9.3 Calculate the mean and standard deviation of the blank sample count and verify that the instrument count is 95% confidence level No significant difference. 10 results calculated When calculating the 210Po peak corresponding to the net count in the ROI, the background spectrum should be subtracted first. The concentration of 210Po activity in water samples may be To be calculated as follows. VN AA Where. A0 - 210Po activity concentration in water samples, Bq/L; A1 - Tracer 209Po activity, Bq; N0 - 210Po peak corresponding to the net area of interest; N1--209Po peak corresponding to the net area of interest; V - water sample volume, L. 11 quality control 11.1 The instrument is used within the valid period of the test. 11.2 scale with a standard mixed plating surface source annual self-test 1 times. 11.3 209Po tracer standard solution is checked once a year. 11.4 Perform a blank test on a regular basis, and a blank test must be performed whenever the reagent is replaced. 12 Uncertainty assessment The establishment of mathematical model The concentration of 210Po activity in water is calculated as follows. VN AA Where. A0 - 210Po activity concentration in water samples, Bq/L; A1 - Tracer 209Po activity, Bq; N0 - 210Po peak corresponding to the net area of interest; N1--209Po peak corresponding to the net area of interest; V - water sample volume, L. Determination of Uncertainty Component According to the mathematical model, the total uncertainty consists of the following four parts. the uncertainty of the instrument measurement u1, tracer Activity uncertainty u2, sample sampling uncertainty u3, and 210Po decay correction uncertainty u4. which is. 1 uuuuu  + 12.1 Uncertainty of instrument measurement u1 111 uuu   12.1.1 210Po net count rate N0 uncertainty u11 11 nn U  Where. T0 - sample source measurement time, s; Tb - background measurement time, s; N0 - the total count rate in the region of interest corresponding to the 210Po peak in the sample source; The background count rate in the region of interest corresponding to the 210Po peak in the sample source. 12.1.2 Uncertainty of net count rate of 209Po u12 Nn U  Where. T1 - standard source measurement time, s; Tb - background measurement time, s; N1 - the total count rate in the region of interest corresponding to the 209Po peak in the standard source; The base count rate in the region of interest corresponding to the 209Po peak in the standard source. 12.2 Tracer 209Po Uncertainty of radioactivity u2 12.2.1 Tracer The uncertainty of the radioactivity of 209po is given by the scale certificate, and its extended uncertainty is Us1, The coefficient is k, u21 can be calculated according to the following formula. U s121  12.2.2 Uncertainty of adding 209Po activity to water samples u22 The formula for adding 209Po activity to the water sample is as follows. 111 VAa  Where. A1 - 209Po standard solution of the activity concentration, Bq/L; V1 - the volume of the 209Po standard solution added, L. U22 can be calculated as follows. 22122 uuu   Where. U221--209Po standard solution activity concentration uncertainty; U222 - Uncertainty of pipetting removal of 209Po standard solution. 12.2.3 Uncertainty of pipetting removal of 209Po standard solution u23 221 cj uuu   Where. Uj - the uncertainty of the removal of the 209Po standard solution from the pipette; Uc - temperature uncertainty of pipette correction. Uj is calculated as follows. 1Vk U Yj   Where. UY - expansion uncertainty of pipette test; K - expansion factor; V1 - remove the volume of the 209Po standard solution, mL. Laboratory room temperature changes in the range of 20 ° C ~ 24 ° C, due to the expansion of the liquid volume can cause changes in water The volume expansion coefficient is 2.1 × 10-4/° C. Assuming that the temperature distribution is a rectangular distribution, the temperature is not corrected for the pipette The degree of determination uc can be calculated as follows. 109.4 4101.2  cu 12.3 Uncertainty of sample volume Sampling volume of 5 L, need to use 1000 mL cylinder to take 5 times. The uncertainty of the sampling volume includes the accuracy of the cylinder sampling The degree of temperature, sampling temperature, sampling repeatability, can be calculated according to the following formula. 313 uuu   Where. U31 - Uncertainty of cylinder sampling; U32 - Uncertainty of temperature correction of the cylinder. 12.3.1 Uncertainty of cylinder sampling The uncertainty of the extension of the cylinder test is UL, the expansion factor k, and the sampling 5 times, then the uncertainty of the cylinder can be According to the following formula. 531  k U L 12.3.2 Temperature on the cylinder correction uncertainty u32 Laboratory room temperature changes in the range of 20 ° C ~ 24 ° C, due to the expansion of the liquid volume can cause changes in water The volume expansion coefficient is 2.1 × 10-4/° C. Assuming that the temperature distribution is a rectangular distribution, the temperature is correct for the cylinder correction The degree u32 can be calculated as follows. 32 109.4 4101.2  u 12.4 Instrument Uncertainty u4 The instrument is regularly verified, according to the uncertainty of the unit given by the unit U4 = U instrument/k, k = 2. 12.5 Uncertainty calculation From 12.1 to 12.4, it can be seen that the synthetic standard uncertainty u can be given by. 1 uuuuu  + The extended uncertainty U is given by. U = u × k, k = 2

Appendix A

(Informative) Supplement to the implementation of the standard A.1 If the solution becomes black during self deposition, deionized water may be added and the self-deposition time may be reduced. A.2 Self-deposition If you find a lot of foam above the solution, you can use glass rods or filter paper to clean up. A.3 ferric hydroxide precipitation filter should be dissolved as soon as possible after overnight, the difficulty of dissolution increased. A.4 If the 210Po content in the water sample is greater than 0.2Bq/L, 50mL sample can be taken directly, the acidity is 0.2 ~ 0.5M with hydrochloric acid, After adding the tracer, follow the procedure of 8.7 ~ 8.10. A.5 If the 210Po peak area of the alpha spectrometer is large, there is overlap interference to 209Po, the sample can be diluted or reduced, and then Re-analysis once, can effectively reduce the 210Po peak to 209Po peak interference. A.6 If silver appears black, indicating that self-deposition is not ideal, should be re-analysis. A.7 If the silver plate caused by the surface is not flat, will increase the α-ion scattering, affecting the tail. A.8 Calculate the time of sample counting according to the following formula. 22EN NNN T bccc   Where. Tc - the time of sample counting, s; Nc - the total count rate of the sample source plus the background, s-1; Nb - background count rate, s-1; N - sample net count rate, s-1; E - the predetermined relative standard error. ......

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