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HJ 816-2016 English PDF

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HJ 816-2016: Radiochemical analysis of caesium-137 in water and ash of biological samples
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Standard similar to HJ 816-2016

GB/T 4214.1   GB 1495   HJ 814   HJ 815   HJ 813   

Basic data

Standard ID HJ 816-2016 (HJ816-2016)
Description (Translated English) Radiochemical analysis of caesium-137 in water and ash of biological samples
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z33
Word Count Estimation 10,191
Date of Issue 2016-10-12
Date of Implementation 2016-11-01
Older Standard (superseded by this standard) GB/T 6767-1986; GB/T 11221-1989
Regulation (derived from) Ministry of Environmental Protection Notice No.62 of 2016
Issuing agency(ies) Ministry of Ecology and Environment

HJ 816-2016: Radiochemical analysis of caesium-137 in water and ash of biological samples

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(Radiochemical analysis of cesium - 137 in water and biological samples) National Environmental Protection Standard of the People 's Republic of China Replacing GB 6767-86, GB 11221-89 Water and biological samples of ash in cesium-137 Radiochemical analysis method Radiochemical analysis of caesium-137 In water and ash of biological samples 2016-10-12 released 2016-11-01 implementation Issued by the Ministry of Environmental Protection Directory

Foreword

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 samples

8 Analysis Step 4 9 blank experiment 5 10 results calculated .5 Analysis error Appendix A (informative) Supplementary note on the implementation of the standard

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 radiochemical analysis method for the determination of cesium-137 in water and bio-sample ash. This standard is the "water cesium -137 radiochemical analysis method" (GB 6767-86) and "biological sample ash cesium -137 radiation Chemical analysis method "(GB 11221-89) of the integrated revision, the use of analytical principles and the original standard is basically the same. "Water cesium -137 radiochemical analysis method" (GB 6767-86) was first released in 1986, the original standard drafting unit for the National Institute of Radiation Protection, "Method for Radiochemical Analysis of Cesium-137 in Biological Gray" (GB 11221-89) was first published in 1989 Year, the original standard drafting unit for the China Radiation Protection Research Institute, the state-owned eight one two plants. This is the first revision. Revision main ones As follows. - the two original standards were integrated, merged into a standard; - Optimized cesium -137 detection efficiency scale method; - made clear requirements for blank experiments; - The preparation of ammonium pyromolybdate [(NH4) 3PO4 • 12MoO3 • xH2O] in the standard method was modified. - Revised some of the content in the standard methodology. This standard since the date of implementation, the former State Environmental Protection Agency on September 4, 1986 approved the release of the national environmental protection standards "water (GB 6767-86) and the former State Environmental Protection Agency March 16, 1989 approved the release of the country Home environmental protection standard "biological sample ash cesium -137 radiochemical analysis method" (GB 11221-89) abolished. Appendix A 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. Radiochemical analysis of cesium - 137 in water and biological samples

1 Scope of application

This standard specifies the radiochemical analysis method for the determination of cesium-137 in water and bio-sample ash. This standard applies to the determination of cesium-137 in water and biological samples. The measurement range of this method is. water samples 10-2 ~ 10 Bq/L, biological samples ash 10-1 ~ 10Bq.

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

3 Principle of the method

In an acidic medium, cesium is selectively adsorbed selectively with an inorganic ion exchanger, ammonium phosphomolybdate, to allow cesium to concentrate and remove interference. And then dissolved with sodium hydroxide solution after adsorption of cesium ammonium phosphomolybdate, and converted to citric acid and acetic acid system to form iodine Calcium bismuth precipitate. Dried to constant weight, measured with a low background beta-ray meter and then calculated for the radioactivity concentration of cesium-137 degree.

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 nitric acid. mass fraction of 65.0% ~ 68.0%. 4.2 nitric acid solution. c = 1.0 mol/L. 4.3 Nitric acid solution. (1 9). 4.4 hydrochloric acid. mass fraction of 35.0% ~ 38.0%. 4.5 ammonium nitrate. 4.6 glacial acetic acid (CH3COOH). the mass fraction of not less than 98%. 4.7 Ethanol (C2H5OH). mass fraction of 99.5%. 4.8 Ammonium phosphomolybdate [(NH4) 3PO4 • 12MoO3 • xH2O] 8 g of diammonium phosphate was dissolved in 250 mL of water and the solution was mixed with 50 mL of 10 g of ammonium nitrate and 30 mL of concentrated nitric acid Of the solution were mixed and heated to about 50 ° C. 500 mL of a solution containing 70 g of ammonium molybdate was slowly added with stirring. Cool to room temperature. Dump the supernatant and filter with a Buchner funnel. Followed by 100 mL of 5% nitric acid solution and 50 mL of absolute ethanol Washed, dried at room temperature in the dark, stored in a brown bottle. 4.9 Hydrogen peroxide. 30% mass fraction. 4.10 citric acid solution. 30% mass fraction. 4.11 sodium hydroxide solution. c = 2 mol/L. 4.12 saturated ammonium nitrate solution. 4.13 cesium carrier solution (about 20 mg/mL) 4.13.1 Preparation method. Weigh 12.7 g Cesium chloride (CsCl) dried at 110 ° C was dissolved in 100 mL of water and 7.5 mL Nitric acid (4.1), into a 500 mL volumetric flask, dilute to the mark with water. 4.13.2 Calibration method. Remove 4 copies of 5.00 mL cesium carrier solution (4.13.1) were placed in a conical flask, add 1 mL Nitric acid (4.1) and 5 mL of perchloric acid (HClO4). Heated to evaporate to smoke thick white smoke, cooled to room temperature, add 15 mL B Alcohol (4.7), stirred and placed in an ice-water bath for 10 min. The cesium perchlorate was precipitated by filtration into a constant weight G4 glass sand The core funnel was washed with 10 mL of ethanol (4.7). Dried in a 105 ° C oven to constant weight. 4.14 solution of sodium iodoborate solution 20 g of bismuth iodide (BiI3) was dissolved in 48 mL of water, 20 g of sodium iodide (NaI) and 2 mL of glacial acetic acid (4.6) were added, Stir. The insoluble material was filtered off with a quick filter paper. The filtrate is stored in a brown bottle. 4.15 nitric acid - ammonium nitrate wash solution Weigh 8.0 g ammonium nitrate (4.5), dissolve in 100 mL of water, add 67 mL nitric acid (4.1), move into 1000 mL Volumetric flask, diluted with water to the mark. 4.16 cesium-137 standard solution (about 15 Bq/mL).

5 instruments and equipment

5.1 low background beta meter, the background is less than 1 cpm. 5.2 Electric stirrer. 5.3 Removable funnel. 5.4 G4 glass sand core funnel. 5.5 Analytical balance, readability 0.1 mg. 5.6 Oven. 5.7 Ma Fu furnace. 5.8 commonly used laboratory equipment.

6 the scale of the instrument

6.1 The counter used to measure the activity of cesium-137 should be calibrated to determine the response of the measuring device to the known activity of cesium-137 Should, it can be used to detect efficiency. The method is. 6.1.1 cesium -137 detection efficiency - the quality curve of the drawing. take five 50 mL beaker, respectively, by adding 0.40,0.60,0.80, 1.00 mL, 1.20 mL cesium carrier solution (4.13), each added 1.00 mL of known activity of cesium-137 standard solution (4.16) Were placed in an ice-water bath and 2 mL of glacial acetic acid (4.6) and 2.5 mL of sodium iodoborate solution (4.14) were added. Press the following operation 8.4 to 8.6. The standard source should be the same size as the sample source area. Divide the count rates of the five standard sources by dividing them The cesium-137 recovery rate of cesium after chemical recovery is the detection efficiency. 6.1.2 Detection efficiency, calculated according to formula (1). DY E sf  (1) Where. Ef - cesium-137 detection efficiency, s-1.Bq-1; Ns - cesium -137 standard source of the net count rate, s-1; D - 1.00 mL activity of cesium - 137 standard solution (4.16), Bq; Y - Chemical recovery of cesium. 6.1.3 Draw the detection efficiency - the quality curve for inspection purposes. 6.1.4 in the measuring plate evenly into a certain amount of cesium -137 standard solution (4.16), in the infrared light drying, made with the sample Source of the same size of the inspection source. At the same time, the counting rate of cesium-137 check source was measured. In the routine Analysis should be used cesium -137 check the source to check the instrument status is normal. Can also be used to stabilize the state and surface emissivity (not Will change with time, sub-body pollution, half-life long) plane source (such as plating source) as a check source.

7 samples

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 7.2.1 Water samples 7.2.1.1 Take 1 L ~ 100 L water sample, adjust to pH < 3 with nitric acid (4.1), add 1.00 mL of cesium carrier solution (4.13). 7.2.1.2 Ammonium phosphomolybdate (4.8) was added at a rate of 1 g per 5 L of water, stirred for 30 min, and clarified for more than 12 h. 7.2.1.3 Rainbow discard the supernatant, the remaining solution into the G4 glass sand core funnel (5.4) filter, with nitric acid solution (4.2) Wash the container, all the precipitation into the funnel, discard the filtrate. 7.2.1.4 with sodium hydroxide solution (4.11) (according to 1g ammonium phosphomolybdate about 10 mL ratio) dissolved precipitation, filtration, Into the 400 mL beaker. Diluted with water to about 300 mL. Add the same amount of solid citric acid as ammonium phosphomolybdate added in 7.2.1.2 After dissolving, add 10 mL of nitric acid (4.1). 7.2.2 Biological samples 7.2.2.1 Weigh 5 ~ 20 g of sample which is completely ashed after pretreatment at 450 ° C, accurate to 0.01 g, placed in 150 mL porcelain vapor Inside the dish. Add a little water wetting. Add 1.00 mL of cesium carrier solution (4.13), then slowly add 10 mL of nitric acid (4.1) And 3 mL of hydrogen peroxide (4.9). Stir evenly, cover the glass table dish, evaporated in the sand bath. Placed in a low temperature electric furnace heating To catch the yellow smoke, into the horse furnace (5.7), at 450 ℃ ashing 1 ~ 2 h, cooling. If the ashing is not complete, available full And ammonium nitrate solution (4.12), placed in an electric furnace and evaporated to dry the ammonium nitrate. The sample should be ashed until no carbon particles. 7.2.2.2 Leaching the gray sample with nitric acid solution (4.3) several times. Heating and hot filtration or centrifugation, discard the residue, merge the liquid. So that the volume of leaching solution control in about 250 mL.

8 Analysis steps

8.1 Add 0.8 g of ammonium phosphomolybdate (4.8) to the sample solution after the pretreatment and stir for 30 min. With G4 glass core The funnel (5.4) was filtered and the vessel was washed with nitric acid-ammonium nitrate wash solution (4.15). Discard the filtrate and keep the precipitate. 8.2 Dissolve ammonium phosphomolybdate in the funnel with 10 mL of sodium hydroxide solution (4.11). Wash the funnel with 10 mL of water, The filtrate and washings were collected in a 25 mL test tube in a suction flask. The collected solution was transferred to a 50 mL beaker and 5 mL of citric acid was added Solution (4.10). 8.3 Carefully evaporate the solution to 5 to 8 mL on the electric furnace. After cooling, place in an ice-water bath, add 2 mL of glacial acetic acid (4.6) and 2.5 mL solution of sodium iodoborate (4.14). The glass rod was wiped and stirred to form iodobenzoate to precipitate and was allowed to stand in an ice-water bath for 10 min. 8.4 Dilute the precipitate into a removable funnel (5.3) with constant weight filter paper. Washed with glacial acetic acid (4.6) to the filtrate Colorless, and then 10 mL of ethanol (4.7) washed once, discard the filtrate. 8.5 Dipotassium iodoborate precipitation with filter paper at 110 ℃ drying, weighing, until constant weight. Cesium bismuth acid (Cs3Bi2I9) shape Calculate the chemical recovery of cesium. 8.6 Place the precipitate together with the filter paper on the measuring plate and count on the low background beta meter (5.1). 8.7 Measuring cesium-137 reference source.

9 blank experiment

9.1 blank experiments on a regular basis, each time the reagent should be replaced, each batch of samples should be empty White 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. 9.1.1 Add 250 mL of nitric acid (water sample 4.2, biomass 4.3) to a 500 mL beaker and add 1.00 mL of cesium Body solution (4.13). 9.1.2 According to the method specified in 8.1 to 8.6, the counting rate of the blank specimen is measured under the same conditions as the sample. 9.1.3 Calculate the mean and standard deviation of the blank sample count rate and verify that it is 95% confidence with the instrument count rate Whether there is a significant difference in the level. 10 results calculated 10.1 Calculate the radioactivity concentration of cesium-137 in water samples according to formula (2). VYJE NJ 0  (2) Where. A - radioactive activity concentration of cesium-137 in water, Bq/L; N - sample source net count rate, s-1; J0 - the net counting rate of the cesium-137 reference source measured at the detection efficiency of the scale measuring instrument, s -1; Ef - instrument detection efficiency, s -1.Bq-1, detected by the cesium -137 detection efficiency-mass curve; V - water sample volume, L; Y - chemical recovery of cesium; J - the net count rate of cesium-137 reference source for sample measurement, s-1. 10.2 Calculate the radioactivity concentration C of cesium-137 in the ash of biological samples according to formula (3). FJEmY NJ A 0  (3) Where. A - the radioactive activity concentration of cesium-137 in the ash of biological samples, Bq/g; M - the amount of ash taken, g; Other symbols and codes - see equations (1) and (2). Note. If you want to represent the activity concentration of cesium-137 in the biological sample, multiply the final result by the sample's ashes (g/kg). 11 precision When the activity concentration of water sample cesium-137 is 1 Bq/L, the maximum error and the relative standard deviation of the same experiment should reach Table 1 Column requirements. Table 1 Method error and relative standard deviation Cesium -137 activity concentration, Bq/L error,% relative standard deviation,% 1 ≤ 10 ≤ 10 Bio-gray-like repeatability and reproducibility should meet the requirements listed in Table 2. Table 2 Reproducibility and reproducibility of the method Total activity of cesium-137, Bq repeatability,% reproducibility,% < 1.0 25 40 1.0 to 10 15 30 > 10 10 15

7 Appendix A

(Informative) Supplement to the implementation of the standard A.1 samples such as cesium-134, cesium -136, cesium -138 in the presence of low background γ spectrometer for cesium -137 determination. A.2 When radioactive iodine is present in the water sample, in addition to the measurement of cesium-137 by the low background gamma spectrometer, 7.2.1.4 After adding 20 mg of iodine support to the solution, the solution was heated to near boiling and 3 mL to 5 mL of 10% nitric acid Silver solution, boil to silver iodide agglomeration, when the supernatant clear and transparent, stop heating. Cool to room temperature and remove the precipitate. The filtrate is analyzed by 8.1. A.3 by adding ammonium phosphomolybdate adsorption of cesium adsorption, such as the discovery of ammonium phosphomolybdate from yellow to blue-green, you can add a few drops of saturated high Potassium permanganate solution, so that ammonium phosphomolybdate remained yellow. A.4 If the sample volume is less than 5 L, steps 7.2.1.2 to 7.2.1.4 can be omitted. A.5 The ash of the sample analyzed by this standard shall be obtained by ashing in the Ma Fu furnace below 450 ℃. A.6 If the time from sampling to measurement exceeds 1 a, denominator in equation (2) of clause 10 and 10.2 of formula (3) Should be multiplied by cesium -137 decay correction factor, which is equal to e-0.693t/T. Where t is the time (a) from sampling to measurement; T is the half-life of cesium-137, 30.17 a. A.7 Calculate the time of sample counting according to formula (A.1). 22EN NNN T bccc   (A.1) 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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