HJ 815-2016 English PDFUS$509.00 · In stock
Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 815-2016: Radiochemical analysis of strontium-90 in water and ash of biological samples Status: Valid
Basic dataStandard ID: HJ 815-2016 (HJ815-2016)Description (Translated English): Radiochemical analysis of strontium-90 in water and ash of biological samples Sector / Industry: Environmental Protection Industry Standard Classification of Chinese Standard: Z33 Word Count Estimation: 22,274 Date of Issue: 2016-10-12 Date of Implementation: 2016-11-01 Older Standard (superseded by this standard): GB/T 6766-1986; GB/T 6764-1986; GB/T 6765-1986; GB/T 11222.1-1989 Regulation (derived from): Ministry of Environmental Protection Notice No.62 of 2016 Issuing agency(ies): Ministry of Ecology and Environment HJ 815-2016: Radiochemical analysis of strontium-90 in water and ash of biological samples---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.(Radiochemical analysis of strontium - 90 in water and biological samples) National Environmental Protection Standard of the People 's Republic of China Replacing GB 6766-86, GB 6764-86, GB 6765-86 and GB 11222.1-89 Water and biological samples of gray strontium-90 Radiochemical analysis method Radiochemical analysis of strontium-90 in water and ash of biological samples 2016-10-12 released 2016-11-01 implementation Ministry of Environmental Protection released Directory Preface ..II 1 Scope of application2 normative reference documents3 - di - (2 - ethylhexyl) phosphoric acid extraction chromatography 3.1 Principle of the method 1 3.2 Reagents and materials 3.3 Instruments and equipment 3.4 Collection and storage of samples 3.5 Analysis Step 44 Smoke Nitric Acid Precipitation Method4.1 Principle of the method 6 4.2 Reagents and materials 4.3 Instruments and equipment 4.4 Collection and storage of samples 4.5 Analysis Step 85 ion exchange method5.1 Principle of the method 9 5.2 Reagents and Materials 10 5.3 Instruments and equipment 11 5.4 Collection and storage of samples 11 5.5 Analysis steps 6 instrument scale 12 7 Results Calculate 13 8 Method validation 14 8.1 blank experiment .14 8.2 Precision Appendix A (informative) yttrium-90 decay and growth factor Appendix B (informative) Supplementary note on the implementation of the standardForewordIn 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, Human health, regulate environmental monitoring methods, the development of this standard. This standard specifies the radiochemical analysis method for the determination of strontium-90 in water and bio-sample ash. This standard is a method for the determination of di- (2-ethylhexyl) phosphoric acid extraction by the method of radiochemical analysis of strontium-90 in water (GB 6766-86) "Radiochemical analysis of strontium-90 in water Smoke nitric acid precipitation method" (GB 6764-86), "Radiochemical analysis of strontium-90 in water Sub-exchange method "(GB 6765-86)," Radiochemical analysis of strontium-90 in ash of biological samples Extraction of di- (2-ethylhexyl) phosphate Color method "(GB 11222.1-89) four standards of the integration of amendments, the use of analytical principles and the original standard is basically the same. "Radiochemical analysis of strontium-90 in water 2 - (2-ethylhexyl) phosphoric acid extraction chromatography" (GB 6766-86) first release In 1986, the original standard drafting unit for the Ministry of Nuclear Industry Radiation Protection Institute; "water strontium-90 radiochemical analysis method smoke nitric acid Precipitation method "(GB 6764-86) was first released in 1986, the original standard drafting unit for the state-owned eight one two plants, the Ministry of Nuclear Industry radiation protection research And the China Atomic Energy Research Institute; "ion exchange of strontium-90 in the water ion exchange method" (GB 6765-86) first published in 1986 Year, the original standard drafting unit for the Southwest Institute of Nuclear Physics and Chemistry, the Ministry of Nuclear Industry Institute of Radiation Protection, China Atomic Energy Research Institute; (2-ethylhexyl) phosphate extraction chromatography "(GB 11222.1-89) for the first time, the method of radiochemical analysis of strontium-90 in the sample ash Published in 1989, the original standard drafting unit for the China Institute of Radiation Protection. This is the first revision. The main contents of the amendment are as follows. - the four original standards were integrated, merged into a standard; - increased the requirements for blank experiments; - Revised some of the contents of the original standard method. This standard since the date of implementation, the former State Environmental Protection Agency on September 4, 1986 approved the release of the three national environmental protection standards "water (2-ethylhexyl) phosphoric acid extraction chromatography "(GB 6766-86)," radiation of strontium-90 in water Chemical analysis method fuming nitric acid precipitation method "(GB 6764-86) and" water strontium-90 radiochemical analysis method ion exchange method "(GB 6765-86), as well as the former State Environmental Protection Agency approved on March 16, 1989, issued a national environmental protection standards "biological sample ash Determination of strontium-90 by radiochemical analysis of di- (2-ethylhexyl) phosphate extraction chromatography "(GB 11222.1-89). Appendix A and Appendix B of this standard are informative. 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. Radiochemical analysis of strontium - 90 in water and biological samples1 Scope of applicationThis standard specifies the radiochemical analysis method for the determination of strontium-90 in water and bio-sample ash. The 2 - (2 - ethylhexyl) phosphoric acid extraction chromatography method in this standard is suitable for the determination of strontium - 90 in water and animal and plant ash. Smoke nitric acid precipitation method and ion exchange method for the determination of strontium-90 in water. The measurement range of this method is. the activity concentration of strontium-90 in water is 10-2 ~ 10Bq/L, the activity of strontium-90 in plant ash For 10-1 to 10Bq.2 normative reference documentsThe contents of this standard refer to the terms of the following documents. For undated references, the valid version applies to this standard quasi. GB/T 6379 Accuracy of measurement methods and results (accuracy and precision) Technical specification for preservation and management of samples for water quality sampling Technical specification for radiation environmental monitoring of HJ/T 61 3 - di - (2 - ethylhexyl) phosphoric acid extraction chromatography 3.1 Principle of the method The activity of strontium-90 in the sample was determined by the activity of yttrium-90, which is a radionuclide nuclide in its radioactive equilibrium. 3.1.1 rapid method. the sample by pretreatment, adjust the acidity, the solution by coating with di - (2 - ethylhexyl) phosphoric acid (referred to as HDEHP) of the polychlorotrifluoroethylene (kel-F) chromatography column adsorption of yttrium, and then 1.5mol/L nitric acid leaching chromatography column, elution Yttrium other than the adsorption of strontium, cesium, cerium, 钷 plasma, and 6mol/L nitric acid desorption yttrium, yttrium oxalate precipitation in the form Perform beta counting and weighing. 3.1.2 Placement method. sample pretreatment method and fast method. After adjusting the acidity of the solution, through the HDEHP-kel-F color column, Remove yttrium, iron and rare earth and other elements. The effluent for 14d or more, so that yttrium -90 and strontium-90 to achieve radioactive balance, Column chromatography, separation and determination of yttrium-90. 3.2 Reagents and materials Unless otherwise stated, analytical reagents and distilled water or equivalent purity are used in accordance with national or professional standards Of water. The activity of the radioactive material in the reagent shall ensure that the count rate measured by the blank sample does not exceed the statistical error of the background of the instrument. 3.2.1 bis - (2 - ethylhexyl) phosphoric acid (C16H35O4P). chemically pure, the content of not less than 95%, ρ = 0.969 ~ 0.975g/mL. 3.2.2 n-heptane (C7H16). ρ = 0.681 ~ 0.687g/mL. 3.2.3 polychlorotrifluoroethylene powder (kel-F). 60 to 100 mesh. 3.2.4 nitric acid. mass fraction of 65.0% ~ 68.0%. 3.2.5 Hydrogen peroxide. mass fraction of not less than 30%. 3.2.6 oxalic acid. 3.2.7 anhydrous ethanol. mass fraction of not less than 95%. 3.2.8 hydrochloric acid. mass fraction of 36.0% ~ 38.0%. 3.2.9 precision test paper. pH = 0.5 ~ 5.0. 3.2.10 Ammonium hydroxide (or ammonia). mass fraction of 25.0% ~ 28.0%. 3.2.11 Ammonium hydroxide (or ammonia). no carbon dioxide. 3.2.12 nitric acid. (1 1.5). 3.2.13 Nitric acid. (1 9). 3.2.14 nitric acid. c = 0.1mol/L. 3.2.15 Ammonium carbonate. 3.2.16 saturated ammonium carbonate solution. 3.2.17 Saturated oxalic acid solution Weigh 110g oxalic acid dissolved in 1L water, slightly heated, stirring, cooling and placed in the reagent bottle. 3.2.18 oxalic acid solution. mass fraction of 0.5%. 3.2.19 Wangshui. hydrochloric acid (3.2.8) and nitric acid (3.2.4) were mixed in a volume ratio of 3. 1. 3.2.20 HDEHP-n-heptane solution. HDEHP (3.2.1) and n-heptane (3.2.2) were mixed at a volume ratio of 1. 4. 3.2.21 Hydrochloric acid. (1 5). 3.2.22 Hydrochloric acid. c = 0.1 mol/L. 3.2.23 Strontium carrier solution (about 50 mg Sr/mL) 3.2.23.1 preparation method. Weigh 153g strontium chloride (SrCl2 · 6H2O) dissolved in nitric acid (3.2.14), transferred to 1L capacity Bottle and diluted with nitric acid (3.2.14) to the mark. 3.2.23.2 Calibration method. take 4 copies of 2.00mL strontium carrier solution (3.2.23.1) were placed in a beaker, add 20mL of water, The solution was adjusted to pH 8.0 with ammonium hydroxide (3.2.10), 5 mL of saturated ammonium carbonate solution (3.2.16) was added, heated to near boiling Teng, so that precipitation condensate, cooling. Filtered with a heated G4 glass sand core funnel, filtered with water and absolute ethanol (3.2.7) 10 mL wash the precipitate. Dry at 105 ° C for 1 h. Cooling, weighing, until constant weight. 3.2.24 Strontium standard solution (about 100 μg Sr/mL) Accurately remove 1.00 mL of strontium carrier solution (3.2.23) into a 500 mL volumetric flask and dilute to a scale with nitric acid (3.2.14). 3.2.25 yttrium carrier solution (about 20 mg Y/mL) 3.2.25.1 Preparation method. Weigh 86.2g of yttrium nitrate [Y (NO3) 3 · 6H2O] dissolved in 100mL nitric acid (3.2.12) , Into the 1L volumetric flask, diluted with water to the mark. 3.2.25.2 Calibration method. take 4 copies of 2.00mL yttrium carrier solution (3.2.25.1) were placed in a beaker, add 30mL of water and 5 mL of saturated oxalic acid solution (3.2.17) and the pH of the solution was adjusted to 1.5 with ammonium hydroxide (3.2.10). Heated in a water bath to make sink Agglomeration. Cool to room temperature. Precipitation Filtration In a triangular funnel with quantitative filter paper, water, anhydrous ethanol (3.2.7) Each 10mL washing. Remove the filter paper placed in the porcelain crucible, in the electric furnace drying, carbonization, placed in 900 ℃ Ma Fu furnace burning 30min. Cool in a dryer. Weighing until constant weight. 3.2.26 Strontium-90-yttrium-90 standard solution (about 10Bq/mL). in 0.1mol/L nitric acid medium. 3.2.27 lanthanum solution. mass fraction of 5% 15.5 g of lanthanum nitrate [La (NO3) 3 · 6H2O] was dissolved in water, and a few drops of nitric acid (3.2.4) were added and transferred to a capacity of 100 mL Bottle, diluted with water to the mark. 3.3 Instruments and equipment 3.3.1 Low background beta meter. 3.3.2 Analysis of balance, readability 0.1mg. 3.3.3 Atomic Absorption Spectrophotometer. 3.3.4 HDEHP-kel-F color column (diameter 8 ~ 10mm, about 150mm high) Preparation of color powder. Weigh 3.0g kel-F powder (3.2.3) into a 50mL beaker and add 5.0mL HDEHP-n-heptane Solution (3.2.20) repeatedly stirring, placed more than 10h. Bake at 80 ° C to a loose shape. The lower part of the column is filled with glass wool and the piston is closed. The above prepared colored layer was washed with nitric acid (3.2.14) Into the column. Open the piston, so that the color powder naturally sink. The column to maintain a certain level of the liquid level. spare. Note. After each use, wash the column with 50 mL nitric acid (3.2.12) at a flow rate of 1 mL/min. Washed with water to the effluent The pH was 1.0. 3.3.5 Removable funnel. 3.3.6 Oven. 3.3.7 Ma Fu furnace. 3.3.8 Centrifuge, the maximum speed of 4000r/min, capacity 100mL × 4. 3.3.9 General laboratory equipment commonly used. 3.4 Collection and storage of samples Samples are collected and stored in accordance with the relevant regulations in HJ 493 and HJ/T 61. 3.5 Analysis steps 3.5.1 Pretreatment of samples Water samples 3.5.1.1 water samples 1 ~ 50L, with nitric acid to adjust pH = 1.0, adding 2.00mL strontium carrier solution (3.2.23) and 1.00mL yttrium Carrier solution (3.2.25), calcium content of the sample should be added to the appropriate amount of calcium. Adjust the pH to 8 ~ 9 with ammonia, stir the water per liter Add 8 g of ammonium carbonate. The water sample is heated to near boiling, so that the precipitate is agglomerated, removed and cooled, and allowed to stand overnight. 3.5.1.2 Absorb the supernatant with siphon, centrifuge the remainder, or filter it through a medium speed filter in a cloth funnel. The mass fraction is 1% ammonium carbonate solution to wash the precipitate. Discard the liquid. Precipitate into the beaker, add dropwise 6mol/L nitric acid to Shen The starch is completely dissolved, heated, and the insoluble matter is filtered off. The filtrate was adjusted to pH 1.0 with ammonia. Biological gray sample 3.5.1.3 Weigh 5 ~ 30g gray sample, accurate to 0.01g, placed in 100mL porcelain crucible, adding 2.00mL strontium carrier solution (3.2.23) And 1.00 mL of yttrium carrier solution (3.2.25). After wetting with a little water, add 5 ~ 10mL nitric acid (3.2.4), 3mL hydrogen peroxide (3.2.5). Placed on the hot plate evaporated. Into the 600 ℃ Ma Fu furnace burning to the sample without carbon black so far. 3.5.1.4 Remove the sample and cool to room temperature. With 30 ~ 80mL hydrochloric acid (3.2.21) heating leaching twice. After centrifugation or filtration, The leachate was collected in a 250 mL beaker. The insoluble material and the vessel were washed with hydrochloric acid (3.2.22). Centrifuge or filter. Wash the liquid and Into the leachate. Discard the residue. 3.5.1.5 Add 5 to 15 g of oxalic acid (3.2.6) and adjust the pH of the solution to 3 with ammonium hydroxide (3.2.10). Heat in a water bath for 30 min. Cool to room temperature. 3.5.1.6 The precipitate was filtered through a medium speed filter and washed twice with 20 mL of oxalic acid solution (3.2.18). Discard the filtrate. Will precipitate Together with the filter paper into the 100mL porcelain crucible, in the electric furnace drying, carbonization, moved into the Ma Fu furnace at 600 ℃ to keep burning 1h. 3.5.1.7 Remove the crucible and cool it. Dissolve the precipitate with a small amount of nitric acid (3.2.12) until no more bubbles are generated. Join again 40 mL of nitric acid (3.2.13) to completely dissolve the precipitate. The solution was filtered through slow filter paper and the filtrate was collected in a 150 mL beaker Nitric acid (3.2.13) Wash the precipitate and the vessel. The washings are filtered and combined in the same beaker and the residue is discarded. Filtrate volume control In about 60mL. 3.5.2 Separation and Purification of Samples Fast method 3.5.2.1 The solution was passed through a HDEHP-kel-F column (3.3.4) at a flow rate of 2 mL/min. Write down from the beginning to the pillar The middle of the time, as the strontium, yttrium separation time. 3.5.2.2 The effluent is collected in a 150 mL beaker. The chromatographic column was washed with 40 mL of nitric acid (3.2.13) at a flow rate of 2 mL/min, Collect the preceding 10 mL effluent into the same 150 mL beaker. The effluent (referred to as effluent A) is left for release Use. Discard the remaining effluent. 3.5.2.3 Dissolve yttrium at 30 mL nitric acid (3.2.12) at a flow rate of 1 mL/min. The solution was collected in a 100 mL beaker. 3.5.2.4 Add 5 mL of saturated oxalic acid solution (3.2.17) to the desorption solution, adjust the pH of the solution to 1.5-2.0 with ammonium hydroxide (3.2.10) The water bath was heated for 30 min and allowed to cool to room temperature. 3.5.2.5 Filter by suction on a removable funnel with a constant weight filter with constant weight. Followed by oxalic acid solution (3.2.18), Water and absolute ethanol (3.2.7) each washed with 10 mL. 3.5.2.6 The precipitate is dried at 45 to 50 ° C to constant weight. The yttrium was calculated from the molecular formula of yttrium oxalate [Y2 (C2O4) 3 · 9H2O] Recovery rate. Only the rapid method of the test method, the placement method can be omitted. Placement method 3.5.2.7 Use the effluent A obtained from step 3.5.2.2 of this standard and adjust the pH to 1.0 with ammonium hydroxide (3.2.10) 2 mL/min flow through the HDEHP-kel-F column (3.3.4). The effluent was collected in a 100 mL volumetric flask with 10 mL of nitrate Acid (3.2.14) leaching chromatography column, the effluent into the same volumetric flask. 3.5.2.8 To the volumetric flask in the standard 3.5.2.7, add 1.00 mL of yttrium carrier solution (3.2.25), add nitric acid (3.2.14) Dilute to the mark. Write down the volume V0, remove the 1.00mL solution (note the volume of V1) to 50mL volumetric flask, keep this solution Liquid (called solution B) for this step 3.5.2.9. The remaining solution (called solution C) is retained for this standard 3.5.2.10 Step with. 3.5.2.9 Determination of chemical recovery of strontium 3.5.2.9.1 Solution B added to the standard 3.5.2.8 step was added 3.0 mL of lanthanum solution (3.2.27) and 1.0 mL of nitric acid (3.2.4) Diluted with water to the mark. Write down the volume V2. The absorbance value was determined on an atomic absorption spectrophotometer. 3.5.2.9.2 Drawing of the working curve. Add 0, 2.50, 5.00, 10.0, 15.0, 20.0 to 7 50 mL volumetric flasks And 25.0 mL of strontium standard solution (3.2.24) were added 3.0 mL of lanthanum solution (3.2.27), diluted with nitric acid (3.2.14) degree. The absorbance value was measured on an atomic absorption spectrophotometer. To absorb the value of the vertical axis, strontium concentration for the abscissa, drawing works line. 3.5.2.9.3 Strontium concentration is detected from the working curve based on the absorbance of the sample solution. Calculate the recovery of strontium according to formula (1). 1000V VCV Q . (1) Where. Q - the recovery of strontium, mg; C - the concentration of strontium found in the working curve, μg/mL; V0--3.5.2.8 volume of the sample solution after dilution, mL; V1 - the volume of solution drawn from V0, mL; V2 - the volume after V1 dilution, mL; 1000 - the conversion factor in which the microgram becomes milligrams. 3.5.2.9.4 Calculate the chemical recovery of strontium according to formula (2). 0q YSr . (2) Where. Ysr - chemical recovery of strontium; Q0 - the amount of strontium carrier added to the sample, mg; Q - formula (1) calculated the recovery of strontium, mg. 3.5.2.10 The solution C obtained in step 3.5.2.8 of this standard is allowed to stand for more than 14 days. And then passed through the chromatography column at a flow rate of ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 815-2016_English be delivered?Answer: Upon your order, we will start to translate HJ 815-2016_English as soon as possible, and keep you informed of the progress. The lead time is typically 2 ~ 4 working days. The lengthier the document the longer the lead time.Question 2: Can I share the purchased PDF of HJ 815-2016_English with my colleagues?Answer: Yes. The purchased PDF of HJ 815-2016_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet.Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. If you need your currency to be printed on the invoice, please write an email to Sales@ChineseStandard.net. In 2 working-hours, we will create a special link for you to pay in any currencies. Otherwise, follow the normal steps: Add to Cart -- Checkout -- Select your currency to pay. |
