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Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 898-2017: Water quality. Determination of gross alpha activity. Thick source method Status: Valid
Basic dataStandard ID: HJ 898-2017 (HJ898-2017)Description (Translated English): Water quality. Determination of gross alpha activity. Thick source method Sector / Industry: Environmental Protection Industry Standard Classification of Chinese Standard: Z16 Classification of International Standard: 13.060 Word Count Estimation: 16,183 Date of Issue: 2017-12-21 Date of Implementation: 2018-02-01 Quoted Standard: GB 12379; GB/T 11682; HJ 493; HJ 494; HJ 495; HJ/T 61; HJ/T 91 Regulation (derived from): Ministry of Environmental Protection Announcement 2017 No. 77 Issuing agency(ies): Ministry of Ecology and Environment Summary: This standard specifies the thick source method for the determination of total alpha radioactivity in water. This standard applies to the determination of total alpha radioactivity in surface water, groundwater, industrial wastewater and domestic sewage. The lower detection limit of the method depends on the total mass of the residue contained in the sample, the detection efficiency of the measuring instrument, the background count rate, and the measurement time. Under typical conditions, the lower detection limit can reach 4.3��10^(-2)Bq/L. HJ 898-2017: Water quality. Determination of gross alpha activity. Thick source method---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.(Water quality - Determination of total radioactivity - Thick source method) People's Republic of China national environmental protection standards Water quality - Determination of total radioactivity - Thick source method Water quality-Determination of gross alpha activity -Thick source method 2017-12-21 Published 2018-02-01 implementation Ministry of Environmental Protection released i directory Foreword .ii 1 Scope 1 2 Normative references 1 3 Terms and definitions4 method principle 2 5 Reagents and materials .26 instruments and equipment7 samples .3 8 Analysis Step 5 9 results calculated and said 6 10 precision and accuracy .6 11 Quality Assurance and Quality Control .7 12 Waste treatment .8 13 Matters needing attention .8 Appendix A (informative) Correct use of the standard instructions Appendix B (Normative) total α, total β radioactive simultaneous measurement of total α radioactivity correction .14ForewordIn order to carry out the "Law of the People's Republic of China on Environmental Protection" and the "Law of the People's Republic of China on Prevention and Control of Radioactive Pollution", the protection Environment, protect human health, standardize the determination of total radioactivity in water, the development of this standard. This standard specifies the thick source method for the determination of total alpha radioactivity in surface water, groundwater, industrial waste water and domestic sewage. Appendix A of this standard is informative, Appendix B is a normative appendix. 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. Nuclear and Radiation Safety Administration of Jiangsu Province. This standard verification unit. Zhejiang Provincial Environmental Monitoring Station radiation, radioactive environmental monitoring station in Shanghai, Anhui Province Environmental Radiation Supervision Governor Station, Jiangsu Provincial Center for Disease Control and Prevention, Tianwan Nuclear Power Station Health and Physical Department and Jiangsu Provincial Radiation Environment Monitoring and Management Station. This standard MEP approved on December 21,.2017. This standard since February 1,.2018 come into operation, This standard is interpreted by the MEP.1 water quality determination of total radioactive thick source methodWarning. nitric acid, sulfuric acid, acetone and trace radioactive substances used in the experiment are corrosive, toxic and radioactive, Reagent preparation process should be carried out in a fume hood, operation should wear protective equipment as required to avoid inhalation of respiratory and skin contact Skin, clothing.1 scope of applicationThis standard specifies the thick source method for the determination of total alpha radioactivity in water. This standard applies to the determination of total alpha radioactivity in surface water, groundwater, industrial wastewater and domestic sewage. The method detection limit depends on the total mass of the residue contained in the sample, the detection efficiency of the measuring instrument, the background count rate, the measurement Time, etc. Under typical conditions, the detection limit of up to 4.3 × 10-2 Bq/L.2 Normative referencesThis standard references the following documents or the terms. For undated references, the effective version applies to this book standard. GB 12379 Environmental Nuclear Radiation Monitoring Regulations GB/T 11682 low background α and/or β measuring instrument HJ 493 Technical Specifications for the Preservation and Management of Water Quality Samples HJ 494 water sampling technical guidance HJ 495 water quality sampling program design specifications HJ/T 61 radiation environmental monitoring technical specifications HJ/T 91 Technical Specifications for Surface Water and Sewerage Monitoring3 Terms and definitionsThe following terms and definitions apply to this standard. 3.1 Total alpha radioactivity gross alpha activity Refers to the sample preparation conditions specified in this standard, the sample is not volatile all natural and artificial radionuclide alpha radiator General 3.2 Effective thickness of saturated layer Refers to a radioactive ray emission rate increases with the increase of radioactive material thickness, when the radioactive material thickness reaches a To a certain extent, the radiation emissivity will no longer increase with the thickness of the radioactive material, and the thickness is the Effective saturation thickness. 23.3 Thick source method According to different diameter measuring disc, when the shop thickness reaches the effective saturation thickness of radioactive rays, the corresponding sampling volume To pave the amount of "minimum sampling volume", this paving method is thick source method.4 method principleThe sample was slowly evaporated and concentrated, converted to sulfate and evaporated to dryness, and then placed in a muffle furnace to give a solid Residue. Weigh accurately not less than the "minimum sampling volume" of the residue evenly spread in the measuring plate, placed in a low background α, β measuring instrument The total alpha count rate is measured to calculate the total alpha radioactivity concentration in the sample.5 Reagents and materialsUnless otherwise specified, the analysis of the use of analytical reagents in line with national standards, experimental water for the newly prepared deionized Water or distilled water, the total alpha radioactivity of all reagents should be below the detection limit of the method. 5.1 Nitric acid (HNO3). p = 1.42 g/ml. 5.2 nitric acid solution. 1 1. Measure 100 ml nitric acid (5.1) and dilute to.200 ml. 5.3 Sulfuric acid (H2SO4). p = 1.84 g/ml. 5.4 Organic solvents. Absolute ethanol (C2H5OH). purity ≥95%; Or acetone (C3H6O). Purity ≥95%. 5.5 calcium sulfate (CaSO4). excellent grade pure. Before use should be dried at 105 ℃ constant weight, stored in a desiccator. The calcium sulfate powder may contain traces of 226Ra And 210Pb, before use, should be weighed with the same quality sample of calcium sulfate powder in the measuring plate paved the bottom of the low α, β test The total alpha count rate measured on the meter should be kept within 3 times the standard deviation of the average total background count rate of the instrument, otherwise Replacing the calcium sulfate powder or using the total alpha count rate of the calcium sulfate powder instead of the instrument background count rate. 5.6 certified reference material. 241Am standard solution for the total alpha standard material, the recommended concentration of activity 5.0 Bq/g ~ 100.0 Bq/g.6 instruments and equipment6.1 low background α, β measuring instrument. Instrument performance indicators should meet the relevant requirements GB/T 11682. 6.2 Analytical Balance. Sense of 0.1 mg. 6.3 adjustable temperature electric hot plate. You can also use electric furnace or other heating equipment. 6.4 oven. 6.5 infrared box or infrared light. 6.6 muffle furnace. to maintain a constant temperature at 350 ℃. 6.7 Measuring disc. stainless steel disc with edge, disc mass thickness of at least 2.5 mg/mm2, measuring disc diameter 3 Depends on the diameter of the instrument detector and the size of the sample source holder. 6.8 evaporating dish. quartz or porcelain material,.200 ml. Wash pan, dry or in oven (6.4) before use After drying at 105 ℃, placed in a muffle furnace (6.6) at 350 ℃ burning 1 h, removed after cooling in the dryer weighing, and even Continued weighing two (more than 3 h interval, usually less than 6 h) difference of less than ± 1 mg, that is, constant weight, record constant weight the amount. 6.9 Mortar and grinding stick. 6.10 polyethylene barrel. 10 L. 6.11 common laboratory equipment and equipment.7 samples7.1 sample collection and preservation Sample representative, sampling methods and preservation methods according to GB 12379, HJ 493, HJ 494, HJ 495, HJ/T 61 And HJ/T 91 of the relevant provisions of the implementation. Sampling equipment before sampling to clean, and 3 times with raw water sample polyethylene barrel. After the sample is collected, sample per liter Add 20 ml nitric acid solution (5.2) Acidified samples to reduce the loss of radioactive material absorbed by the wall. sample After collection, analysis should be determined as soon as possible, the sample shelf life of generally not more than 2 months. Sampling capacity recommended not less than 6L. If a clear sample is to be measured, the supernatant can be taken after the suspension is allowed to settle by filtration or standing. 7.2 Sample Preparation 7.2.1 Concentration Estimate the volume of sample required for experimental analysis based on the residue content (see A.3 in Appendix A). To prevent the operation The loss in the process ensures that the sample is evaporated to dryness. The total mass of the residue after burning is slightly greater than 0.1 A mg (A is the area of the measuring disk, mm-2) After burning the total mass of residue by 0.13A mg estimated sample size. Measure the volume of the sample under test in a beaker, placed on the adjustable temperature hot plate (6.3) on the slow heating, hot plate temperature Degree control at about 80 ℃, so that the sample was concentrated under micro-boiling conditions. To prevent spillage of the sample during the micro-boiling, beaker In the sample volume must not exceed half the capacity of the beaker, if the sample size is larger, you can add one after another in succession. All samples are concentrated To about 50 ml, place the cooling. Transfer the concentrated sample to the evaporating dish (6.8) with a little more than 80 ° C Hot deionized water to wash the beaker to prevent the salt crystals from adhering to the wall of the cup, and pour the lotion into the evaporating dish together. For samples with very low hardness (eg less than 30 mg/L in terms of calcium carbonate), measure as much as practicable The maximum sample volume collected to evaporate and concentrate, if you really can not get the actual amount of sample can also be added to the sample Slightly more than 0.13A mg of calcium sulfate (5.5), and then evaporated, concentrated, sulfated, burning and other processes made of Test sample source. 7.2.2 Sulfation Slowly add 1 ml of sulfuric acid (5.3) to the evaporating dish along the wall of the vessel. To prevent splashing, place the evaporating dish in a red box or Infrared light (6.5) or water bath on the heating until the sulfuric acid smoke, and then put the evaporating dish temperature adjustable hot plate (6.3) (temperature Degree below 350 ℃), continue heating until the smoke cleared. 47.2.3 Burning Place the evaporating dish with the residue in a muffle furnace (6.6), ignite it at 350 ° C for 1 h, remove and place it in the desiccator Cooling, accurate weighing after cooling, according to the difference with the evaporating dish (6.8) to obtain the total mass of the residue after burning. 7.2.4 Preparation of sample source The residue was transferred to a mortar, ground into a fine powder, accurately weighed not less than 0.1A mg of the powder to the test The middle of the pan, with a dropper to draw organic solvents (5.4), dripped onto the residue powder, the infiltration of residual powder in organic solvents The end of the uniform tile in the measuring plate, and then the measuring plate to dry or placed in the oven drying, made of sample source. 7.2.5 blank sample preparation Accurately weigh the same mass of calcium sulphate (5.5) as the source of the sample and make it by the same procedure as in the preparation of the sample source (7.2.4) Blank sample. 7.2.6 laboratory blank sample preparation process Measure 1 L deionized water to 2 L glass beaker, add 20 ml nitric acid solution (5.2), stir, add 0.13A mg of calcium sulfate (5.5), according to 7.2.1 ~ 7.2.4 operation, and then weighed with the sample source of the same quality of the residue, made of Laboratory whole process blank sample. 7.2.7 Preparation of standard source Weigh accurately 2.5 g of calcium sulfate (5.5) in a 150 ml beaker, add 10 ml of nitric acid solution (5.2), stir After adding 100 ml of hot water (above 80 ℃), carefully heated on a hot plate to dissolve the solid material. Turn all solutions Into a.200 ml evaporating dish (6.8), accurately add about 5 Bq ~ 10 Bq standard material (5.6), in the red box or red Slowly evaporated to dryness under the external light, and then placed in a muffle furnace at 350 ℃ for 1 h, removed, placed in a desiccator cooled and weighed, were Have to contain 241Am of calcium sulfate standard powder. According to the total activity of 241Am added and the total mass of calcium sulfate residue obtained after burning The total α-radioactivity concentration αs (Bq/g) of the calcium sulfate standard powder is calculated according to the formula (1). ss sm MA (1) Where. αs - calcium sulfate standard powder total α radioactivity concentration, Bq/g; As - added 241Am standard solution activity concentration, Bq/g; Ms - added 241Am standard solution mass, mg; ms - after burning the total mass of calcium sulfate residue, mg. The standard calcium sulfate powder fine, weighed sample source with the same quality in the measuring plate, according to the sample source preparation (7.2.4) The same steps, made of standard source, record the date and time shop. Can also be purchased directly Certificate 241Am solid powder standard material, before use at 105 ℃ dry constant weight, weighed directly, Shop, measuring. 58 analysis steps 8.1 Determination of instrument background Take unused, non-polluting measuring disc (6.7), after washing with alcohol immersion more than 1 h, remove, drying, placed Low background α, β measuring instrument (6.1) on the continuous measurement of the total instrument α background count rate of 8 h ~ 24 h, to determine the stability of the instrument background Sex, taking the average, with the count rate R0 (s-1) said. 8.2 Determination of effective saturation thickness (minimum shop volume) The actual measurement. Weigh 80 mg, 100 mg, 120 mg, 140 mg, 160 mg, 180 mg,.200 mg, 220 mg, 240 mg of the standard source (7.2.7) in the measuring plate, according to the same procedure for the preparation of the sample source (7.2.4), made of different thickness The series of standard sources, evenly tiled at the bottom of the measuring plate, after drying, placed on a low background α, β measuring instrument (6.1) on each measurement The total alpha count rate for a standard source. Taking the total α net counting rate as the ordinate and the paving amount as the abscissa, the α self-absorption curve is drawn. when When the amount of pavement reached a certain value, the net total count rate ceased to increase with the increase in the amount of pavement and the slanted line of the self-absorption curve was prolonged Section and the horizontal section, the intersection of the corresponding bedding shop is the standard source of effective saturation thickness, which is the method of the minimum shop volume. Theoretical Estimation. If effective saturation thickness measurement difficulties, can be directly calculated by 0.1A mg. 8.3 Blank sample determination The blank sample (7.2.5) is measured on a low background α, β meter (6.1) for total α count rate. The total alpha count rate should be maintained Within 3 times the standard deviation of the average total background count of the instrument, otherwise calcium sulphate should be replaced (5.5) or a blank test The total α count rate instead of the instrument background count rate. 8.4 The whole process of the laboratory blank sample determination The total laboratory blank sample (7.2.6) is measured on a low background alpha, beta meter (6.1) for total alpha count rate. Total α The counting rate should be kept within 3 times of the standard deviation of the average total background count of the instrument, otherwise the radioactive level should be used more Low chemical reagents, or use the whole laboratory blank sample total α count instead of instrument background count rate. 8.5 Determination of standard sources The standard alpha count (7.2.7) is measured on a low background alpha, beta meter (6.1) with a count rate Rs (s-1) Show, and record count time, time interval and date. 8.6 Determination of sample source Sample source (7.2.4) Immediately after drying, the total α count rate Rx (s-1) should be measured on a low background α, β meter (6.1) And record count time, time interval and date. The length of the measurement depends on the count rate of the sample and the background and the required accuracy. See Appendix A for calculation method A.1. Instruments on the same sample source count rate of the existence of fluctuations in the measurement, to be measured more than 5 times, take the arithmetic mean. 69 Results Calculation and Presentation 9.1 Calculation Results The concentration of total α radioactive activity in the sample Cα (Bq/L), calculated according to equation (2), the formula derived see appendix A in A.7. If the measuring instrument can measure α and β counts at the same time, and the ratio of β-ray to α-channel can not be neglected, Road than the amendment, correction formula in Appendix B. 02.1 ) RR ) RR C s 0s 0x (2) Where. Cα - total α radioactivity in the sample concentration, Bq/L; Rx - the total alpha count rate of the sample source, s-1; R0 - total background count rate, s-1; αs - the total alpha radioactivity concentration of the standard source, Bq/g; m - sample evaporated, the total mass of the residue after burning, mg; 1.02 - Correction factor, ie 1020 ml acidified sample equivalent to 1000 ml original sample; Rs - the total alpha count of the standard source, s-1; V - sampling volume, L. 9.2 results indicated When the measurement result is less than 0.1 Bq/L, keep three digits after the decimal point. When the measurement result is 0.1 Bq/L or more, Keep three significant figures. 10 precision and accuracy 10.1 Precision Six laboratories performed six rounds of a uniform sample containing 0.046 Bq/L of total alpha radioactivity and 25.6 Bq/L Repeated determination, the relative standard deviations in the laboratory were 8.5% ~ 26% and 3.7% ~ 14%, respectively; relative standard deviation The differences were 8.8% and 10%, respectively; the repeatability limits r were 0.021 Bq/L and 5.29 Bq/L respectively; the reproducibility limits R were 0.022 Bq/L and 8.69 Bq/L. 10.2 Accuracy Six laboratories added 241Am of uniform samples containing 0.046 Bq/L of total alpha radioactivity and 25.6 Bq/L Standard solution, the recovery rate of the measurement method, the spiked recovery range of 94.8% to 120% and 96.9% to 110%; plus The final values of standard recoveries were (105 ± 17.6)% and (103 ± 11.6)%, respectively. 711 Quality Assurance and Quality Control 11.1 Instrument Stability 11.1.1 Apparatus Poisson distribution test At least once a year Poisson distribution of the instrument background count test, if the background is very low, a certain activity standard Source instead. 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