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HJ 814-2016: Radiochemical analysis of plutonium inwater and soil samples
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Radiochemical analysis of plutonium inwater and soil samples
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Standard similar to HJ 814-2016 GB/T 4214.1 GB 1495 HJ 815 HJ 816 HJ 813 Basic data | Standard ID | HJ 814-2016 (HJ814-2016) | | Description (Translated English) | Radiochemical analysis of plutonium inwater and soil samples | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z33 | | Word Count Estimation | 17,125 | | Date of Issue | 2016-10-12 | | Date of Implementation | 2016-11-01 | | Older Standard (superseded by this standard) | GB/T 11225-1989; GB/T 11219.1-1989; GB/T 11219.2-1989 | | Regulation (derived from) | Ministry of Environmental Protection Notice No.62 of 2016 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 814-2016: Radiochemical analysis of plutonium inwater and soil 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 plutonium in water and soil samples)
National Environmental Protection Standard of the People 's Republic of China
Replacing GB 11225-89, GB 11219.1-89 and GB 11219.2-89
Water and soil samples of plutonium
Radiochemical analysis method
Radiochemical analysis of plutonium
In water and soil samples
2016-10-12 released
2016-11-01 implementation
release
Ministry of Environmental Protection
Directory
Preface ..II
1 Scope of application
2 normative reference documents
3 Extraction chromatography
3.1 Principle of the method
3.2 Reagents and materials
3.3 Instruments and equipment
3.4 samples
3.5 Analysis Step 5
3.6 Results Calculation 5
3.7 Determination of full radiochemical recovery of plutonium
3.8 Method validation 6
4 ion exchange method
4.1 Principle of the method
4.2 Reagents and Materials
4.3 Instruments and equipment
4.4 samples .9
4.5 Analysis steps
4.6 Results Calculation 10
Determination of the full radiochemical recovery of plutonium
4.8 Method validation 10
Appendix A (informative) Supplementary note on the implementation of the standard 11
Appendix B (informative) Instrument and equipment
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,
Human health, regulate environmental monitoring methods, the development of this standard.
This standard specifies the method for the determination of plutonium in water and soil samples.
This standard is the "analysis method of plutonium in water" (GB 11225-89), "determination of plutonium in soil - extraction chromatography" (GB 11219.1
-89), "determination of plutonium in soil - ion exchange method" (GB 11219.2-89) three standards of the integrated revision, the use of the analysis
Principle and the original standard is basically the same.
The three standards were first released in 1989, the original standard drafting unit for the China Atomic Energy Research Institute. This is the first revision.
The main contents of the amendment are as follows.
- the integration of the three original standards, merged into a standard;
- the contents of the original standard on the sampling part are deleted;
- increased individual steps in the pretreatment and analysis of water and soil samples;
- Added 242Pu as a tracer to determine the full radiochemical recovery rate;
- increased the requirements for blank experiments;
- Added instructions for the use of the sample amount and the chemical yield indicator.
Since the implementation of this standard, the former State Environmental Protection Agency approved on March 16, 1989, issued three environmental protection standards "plutonium in water
(GB 11225-89), "Determination of plutonium in soil - Extraction chromatography" (GB 11219.1-89), "plutonium in soil
Of the determination - ion exchange method "(GB 11219.2-89) abolished.
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 plutonium in water and soil samples
1 Scope of application
This standard specifies the radiochemical analysis methods for the determination of plutonium in groundwater, surface water and soil. Nuclear industry in wastewater
The determination of plutonium may be referred to the present method.
The extraction chromatography method in this standard is suitable for the determination of plutonium in water and soil samples. The ion exchange method is suitable for soil
Determination and determination of plutonium in.
The minimum detectable limit of this method is water sample 1 × 10-5Bq/L, soil type 1.5 × 10-5Bq/g.
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
GB/T 6379 Accuracy of measurement methods and results (accuracy and precision)
Technical specification for preservation and management of samples for water quality sampling
3 extraction chromatography
3.1 Principle of the method
The pretreated samples were prepared into 6 ~ 8mol/L HNO3 sample solution. After reduction, oxidation regulates the valence of plutonium
After plutonium with Pu (NO3) 5
- or Pu (NO3) 62
- Anionic form is present in the solution. With tri-n-octylamine-polychlorochloro-ethyl chloride
The enriched powder extraction layer adsorbs plutonium and is rinsed with hydrochloric acid and nitric acid to further purify plutonium. Dissolve with oxalic acid-nitric acid mixed solution.
The source of the electrodeposition is carried out at low acidity. Finally, the activity of plutonium was measured with a low background alpha spectrometer.
3.2 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.
3.2.1 anhydrous calcium chloride. the content of not less than 96.0%.
3.2.2 magnesium chloride. the content of not less than 97.0%.
3.2.3 Ammonium sulfonate. HO · SO2 · NH2, the content of not less than 99.5%.
3.2.4 reduced iron powder. the content of not less than 97.0%.
3.2.5 sodium nitrite. the content of not less than 99.0%.
3.2.6 oxalic acid. H2C2O4 · 2H2O, the content of not less than 99.8%.
3.2.7 Polychlorotrifluoroethylene powder. irradiation synthesis, 40 to 60 mesh.
3.2.8 nitric acid. mass fraction of 65.0% ~ 68.0%.
3.2.9 hydrochloric acid. mass fraction of 36.0% ~ 38.0%
3.2.10 Ammonium hydroxide. mass fraction of 25.0% ~ 28.0%.
3.2.11 xylene. C6H4 (CH3) 2, the content of not less than 80.0%.
3.2.12 Ethanol. mass fraction of not less than 99.5%.
3.2.13 Hydrochloric acid. c = 10 mol/L.
3.2.14 Nitric acid. (1 1).
3.2.15 nitric acid. c = 3 mol/L.
3.2.16 nitric acid. c = 0.1 mol/L.
3.2.17 Ammonium hydroxide. (1 1).
3.2.18 0.025 mol/L oxalic acid - 0.150 mol/L nitric acid solution.
3.2.19 sodium nitrite solution. c = 4mol/L.
3.2.20 Tri-n-octylamine (TOA). [CH3 (CH2) 7] 3N, the content of not less than 95.0% to 99.0%.
3.2.21 ferrous sulfamate solution
Weigh 3.0g of reduced iron powder (3.2.4) and 12.0 g of sulfamic acid (3.2.3), and dissolved about 40 mL of nitric acid (3.2.16)
Solution, filtered to remove insoluble matter, the filtrate diluted with nitric acid (3.2.16) to 50mL brown volumetric flask, stored in the refrigerator,
spare. The use of not more than 30d.
3.2.22 hydroiodic acid. mass fraction of not less than 45.0%.
3.2.23 0.4mol/L hydroiodic acid - 6.0mol/L hydrochloric acid solution.
3.2.24 precision test paper. measuring range of pH = 0.5 ~ 5.0.
3.2.25 sulfuric acid. mass fraction of 95.0% ~ 98.0%.
3.2.26 perchloric acid. mass fraction of 70.0% ~ 72.0%.
3.2.27 hydrofluoric acid. mass fraction of not less than 40.0%.
3.2.28 aluminum nitrate. Al (NO3) 3 · 9H2O, the content of not less than 99.0%.
3.2.29 TOA-xylene solution. 1 part of TOA and 9 parts xylene mixed by volume ratio.
3.2.30 239Pu, 242Pu Standard Indicator. Uncertainty ≦ 2%.
3.2.31 239Pu Standard Plane Plating Source. Uncertainty ≦ 2%.
3.3 Instruments and equipment
3.3.1 Low background alpha spectrometer.
3.3.2 Analysis of balance. readability 0.1mg.
3.3.3 Centrifuge. the maximum speed of 4000r/min, capacity 250mL × 4,100mL × 4.
3.3.4 electric stirrer. 25 ~ 60W, the maximum speed of 2 000r/min.
3.3.5 Polyethylene plastic bucket. capacity 60L.
3.3.6 Glass Extraction Columns. See Appendix B (informative) Figure B.1.
3.3.7 Electrodeposition apparatus. see Appendix B (informative) Figure B.2.
3.3.8 Teflon Beaker. Capacity 100mL.
3.3.9 Preparation of glass extraction chromatography
3.3.9.1 Preparation of color powder. 2.0 mL of the solution of TOA-xylene (3.2.29) was added to each 1.0 g of polychlorotrifluoroethylene powder (3.2.7)
Stir evenly after placing or baking in the infrared light, so that xylene volatiles and loose, with water suspension to remove the suspension
Of the fine powder stored in a brown glass bottle in reserve.
3.3.9.2 Preparation of color column. the color powder (3.3.9.1) into the column (3.3.6) by wet method, the upper and lower columns of the two
End with a small amount of PTFE filament packing, bed height 60mm, before use with 20mL nitric acid (3.2.14) to 2mL/min
Flow through the column to balance the acidity of the column.
3.3.9.3 color column regeneration. followed by 10mL0.025mol/L oxalic acid -0.150mol/L nitric acid solution (3.2.18), 20mL
Water, 20 mL nitric acid (3.2.14) was passed through a color column at a flow rate of 2 mL/min.
3.4 samples
3.4.1 Acquisition and storage
Samples were collected and stored in accordance with the relevant provisions in GB 12997, GB 12998 and HJ 493.
3.4.2 Pretreatment of samples
Water samples
3.4.2.1 Set the water sample for more than 12 hours.
3.4.2.2 from the standing water samples were taken 50L supernatant into the 60L polyethylene plastic bucket, add a certain amount of
Plutonium chemical yield indicator 242Pu (3.2.30), adding 50mL ammonium hydroxide (3.2.10), stirring evenly after adding 15g
Water calcium chloride (3.2.1), 30g magnesium chloride (3.2.2), to be completely dissolved, stirring evenly, then slowly adding ammonium hydroxide
(3.2.10), adjust the pH value of 9 to 10, continue to stir more than 60min, and then rest for more than 12h.
3.4.2.3 take the supernatant, the remaining small amount of supernatant and precipitation together into 250mL centrifuge tube, centrifugal
10 ~ 15min (speed of 3000r/min) discard the supernatant, and then.200 ~ 300mL distilled water washing plastic barrels after the turn
Into the original centrifuge tube, and the sediment stirred and then centrifuged 10 ~ 15min (speed 3000r/min), discard the washing liquid.
3.4.2.4 Wash the stir bar and plastic drum wall with 80 mL nitric acid (3.2.15), then pour the wash solution into 250 mL of glass
Glass beaker, and then once again with 70 mL nitric acid (3.2.14), twice the combined wash solution and used to dissolve the centrifuge tube
, The dissolved solution was filtered using fast filter paper and the filter paper and residue were washed with 10 mL of nitric acid (3.2.14)
The filtrate was collected and purified by step 3.5.
Soil type
3.4.2.5 nitric acid leaching method. from the soil sample weighed 30.0g of the sample, accurate to 0.1 g, placed in a 250mL beaker,
Adding a certain amount of plutonium chemical yield indicator 242Pu (3.2.30), slowly adding nitric acid (3.2.14) 70mL, stirring evenly
After heating on the electric furnace to boil for 10 ~ 15min (to prevent splashing and overflow), cooled to room temperature after the leachate and precipitation transfer
Centrifuge to 100 mL centrifuge tube 10 ~ 15min (speed 3000r/min), the collection of supernatant. And then 40mL nitric acid
(3.2.14) The precipitate was transferred to the original beaker and heated again for one time, and the supernatant was combined twice. Precipitation with 30mL
Nitric acid (3.2.15), 30mL water were washed once, centrifuged, the supernatant and the previous two supernatant combined (known as A liquid)
Purify by 3.5 steps.
3.4.2.6 sulfuric acid - perchloric acid - nitric acid - hydrofluoric acid - hydrochloric acid dissolution method. from the soil sample weighed 5.00g sample, accurate to
0.01 g, placed in a.200 mL beaker, adding a certain amount of plutonium indicator 242Pu (3.2.30), adding 5 mL of sulfuric acid (3.2.25)
5mL perchloric acid (3.2.26) stir evenly on the surface of the dish in the electric furnace sand bath for 1h, then hot by adding 5mL high chlorine
Acid (3.2.26) continue to heat digestion 1 ~ 1.5h, remove the surface pan evaporated. The residue was then transferred to 100 mL of polytetrafluoroethylene
The beaker was washed several times with 10 mL of perchloric acid (3.2.26) and 10 mL of nitric acid (3.2.8). Wash the liquid
Into the polytetrafluoroethylene beaker, then add 20mL hydrofluoric acid (3.2.27), capped at about.200 ℃ sand bath on the micro-boiling 3 ~ 4h
Go to the lid and evaporate to dry. The residue is pale green or light yellow. The residue was transferred to a 100 mL beaker with 50 mL of nitric acid (3.2.15)
Heating and dissolving, centrifuging (speed 3000r/min) 10 ~ 15min, collecting supernatant. With 25 mL of nitric acid (3.2.15)
Precipitation transferred to the original beaker, repeat the above operation, combined twice the supernatant. With 10mL hydrochloric acid (3.2.9) and then precipitation
Transferred to the original beaker, heated to dry, with 10 ~ 15mL nitric acid (3.2.15) heating dissolved residue, and with the previous two
The supernatant is combined. At the same time by adding 5g aluminum nitrate (3.2.28) (called B liquid) by 3.5 steps separation and purification.
If the residue is completely dissolved by 50 mL and 25 mL nitric acid (3.2.15), the 10 mL salt can be omitted
Acid (3.2.9) to deal with this step.
3.5 Analysis steps
3.5.1 separation and purification
3.5.1.1 Add 100 mL of the above solution (3.4.2.4 or 3.4.2.5 A solution or 3.4.2.6 B solution) to 0.5 mL of amino sulfide
Ferric acid solution (3.2.21), the reduction, placed 5 ~ 10min, then add 0.5mL sodium nitrite solution (3.2.19),
Oxidize, place for 5 ~ 10min, then boil the solution in the electric furnace, so that excessive sodium nitrite completely decomposed, cooled to
Room temperature.
3.5.1.2 The acidity of the above solution (3.5.1.1) was adjusted to 6 to 8 mol/L and passed at a flow rate of 2 mL/min.
Of the color column. The original beaker was washed several times with 10 mL of nitric acid (3.2.14), and the washing solution was passed through the chromatography column at the same flow rate.
3.5.1.3 The chromatographic column was washed with 20 mL of hydrochloric acid (3.2.13), 30 mL of nitric acid (3.2.15) at a flow rate of 2 mL/min,
Finally, the chromatographic column was washed with 2 mL of distilled water at a flow rate of 1 mL/min.
3.5.1.4 Under a condition of not less than 10 ° C, 0.025 mol/L oxalic acid - 0.150 mol/L nitric acid solution (3.2.18)
1 mL/min, and the desiccant was collected into a ready-made electrodeposition bath (3.3.7), washed with ammonium hydroxide
(3.2.17) The pH of the desorbed solution in the electrodeposition bath is adjusted to 1.5 to 2.0.
3.5.2 Electrodeposition system source and measurement
3.5.2.1 The electrodeposition bath (3.5.1.4) is placed in a flowing cold water bath with a distance between 4 and 5 mm, a current density
Dried at 500 to 800 mA/cm2 for 60 min, and then 1 to 2 mL of ammonium hydroxide (3.2.10) was added to continue the electrodeposition
1 ~ 3min, disconnect the power, discard the electrodeposition solution, and then washed with water and ethanol (3.2.12) plating, and then in the infrared light
Under the drying. In the electric furnace at 400 ℃ for 1 ~ 3min.
3.5.2.2 Place the plated sheet (3.5.2.1) on a low background alpha spectrometer (3.3.1).
3.6 Results calculation
The radioactivity concentration of plutonium in the sample was calculated according to equation (1).
EYV m
(or) (1)
Where.
A - the radioactivity concentration of plutonium in the sample, Bq/L (or Bq/kg);
N - the net count rate of the sample source, S-1;
E - instrument detection efficiency of plutonium, S-1 Bq-1;
Y - plutonium full recovery rate,%;
V - the volume used to analyze the sample, L;
(Or m - soil sample quality, kg).
Determination of full - range radiochemical recovery of plutonium
In the analysis of water samples (or soil samples that were quantitatively analyzed by drying and grinding), a certain amount of plutonium (242Pu)
The agent is operated according to 3.4.2 to 3.5.2 of this standard and the total radiochemical recovery of plutonium is calculated according to formula (2).
(2)
Where.
N1 - the activity of 242Pu in the sample source, Bq;
N0 - the sample added 242Pu activity, Bq.
3.8 Method validation
3.8.1 Blank experiment
Regular blank experiment; whenever the replacement of reagents, should be blank experiment; each batch of samples should be blank
experiment.
3.8.1.1 Water samples
The number of samples can not be less than 5. Measure 50L distilled water in polyethylene barrels, according to this standard 3.4.2 water sample ~ 3.5.2 operation
For. And calculate the average count rate and standard deviation of the blank sample.
3.8.1.2 Soil samples
The number of samples can not be less than four.
(1) acid leaching method. measure 120mL nitric acid (3.2.14) placed in.200mL beaker, according to the standard 3.5.1 ~ 3.5.2
Bar operation, taking the same conditions as the sample to measure the count rate of the blank sample. Calculate the average count rate and standard for blank samples
deviation. Verify that there is a significant difference between the background count rate of the instrument and the 95% confidence level.
(2) acid dissolution method. without the sample according to the standard 3.4.2.6 ~ 3.5.2 operation, the measurement, calculation and testing are the same with the
Standard 3.7.
3.8.2 precision
3.8.2.1 Water samples
According to the relevant provisions of GB/T 6379, the experimental determination of the precision, see Table 1.
Table 1 The precision of the method
Precision function relation
Level (x 10-3Bq)
Lg (r) = lg (0.65) 0.821 g (m) lg (R) = lg (0.81) 0.89 lg (m)
M Reproducibility (r) Reproducibility (R)
61.8
7.30
0.296
19.4
3.34
0.239
29.3
4.42
0.258
3.8.2.2 Soil samples
Reproducibility and reproducibility should meet the requirements listed in Table 2.
Table 2 Reproducibility and reproducibility of the method
The total activity of plutonium,
Bq
Repeatability,% reproducibility,%
Acid leaching acid - dissolving acid leaching acid - dissolving method
< 0.01
0.01 ~ < 10
4 ion exchange method
4.1 Principle of the method
The pretreated samples were prepared with 7 to 8 mol/L HNO3 sample solution and then treated with a strong basic anion exchange resin
The purified plutonium was separated and rinsed with hydrochloric acid and nitric acid to further purify plutonium. Dissolve plutonium with hydrochloric acid - hydrofluoric acid solution. In nitric acid - nitric acid
Preparation of Electrodeposition in Ammonium Solution. Measured with a low background alpha spectrometer.
4.2 Reagents and materials
Unless otherwise stated, analytical analytical reagents in accordance with national standards are used for the analysis, and the test water is freshly prepared
Deionized water or distilled water.
4.2.1 sodium nitrite. the content of not less than 99.0%.
4.2.2 Ammonium hydroxide. mass fraction of 25.0% to 28.0%.
4.2.3 anhydrous ethanol. the mass fraction of not less than 99.5%.
4.2.4 hydrochloric acid. mass fraction of 36.0% ~ 38.0%.
4.2.5 nitric acid. mass fraction of 65.0% ~ 68.0%.
4.2.6 hydrofluoric acid. mass fraction of not less than 40.0%.
4.2.7 precision test paper. measuring range of pH = 0.5 ~ 5.0.
4.2.8 Ammonium sulfonate. HO · SO2 · NH2, the content of not less than 99.5%.
4.2.9 reduced iron powder. the content of not less than 97.0%.
4.2.10 Amine Hydroxide. (1 1).
4.2.11 Hydrochloric acid. c = 8.0 mol/L.
4.2.12 nitric acid. (1 1).
4.2.13 nitric acid. c = 3.0 mol/L.
4.2.14 nitric acid. c = 0.1mol/L.
4.2.15 sodium nitrite solution. c = 4.0mol/L.
4.2.16 0.36 mol/L hydrochloric acid -0.01 mol/L hydrofluoric acid solution.
4.2.17 ferrous sulfamate solution
Weigh 3.0g of reduced iron powder (4.2.9) and 12.0 g of sulfamic acid (4.2.8) were weighed with nitric acid solution (4.2.14) and filtered
Remove the insoluble matter, the filtrate diluted to 50mL with water, sealed in a brown bottle in the low temperature preservation, spare. The use of not more than 30d.
4.2.18 Anion exchange resin 251 × 8.
4.2.19 0.150mol/L ammonium nitrate - 0.150mol/L nitric acid solution.
4.2.20 239Pu, 242Pu Standard Indicator. Uncertainty ≦ 2%.
4.2.21 239Pu Standard Plane Plating Source. Uncertainty ≦ 2%.
4.3 Instruments and equipment
4.3.1 Low background alpha spectrometer.
4.3.2 Analysis of balance. readability 0.1mg.
4.3.3 Centrifuge. the maximum speed of 4000r/min, capacity 400mL × 4.
4.3.4 Glass exchange column. see Appendix B (informative) Figure B.1.
4.3.5 Electrodeposition apparatus. see Appendix B (informative) Figure B.2.
4.3.6 Teflon beaker. capacity 100mL.
4.3.7 ion exchange resin activation. the anion exchange resin (4.2.18) grinding and screening 60 to 80 mesh, with anhydrous B
Alcohol (4.2.3) soak for 24 hours, drain the floats and rinse several times with distilled water, drift off the suspended matter, and finally use nitric acid (4.2.14)
Soak, bottled.
4.3.8 Ion exchange resin column. the ion exchange resin (4.3.7) natural sinking into the exchange column, the column
Of the upper and lower ends with a small amount of PTFE filament packing, bed height 70mm. Then treated with 20 mL of nitric acid (4.2.12) in 3 mL
/ Min flow through the column, ready for separation and purification.
4.4 samples
4.4.1 Acquisition and storage
The collection and storage of samples shall be in accordance with the provisions of GB 12997, GB 12998 and HJ 493.
4.4.2 Pretreatment of the sample
Soil samples from the soil sample weighed 30.0g,...
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