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HJ 840-2017: Technical guidelines for environmental impact assessment Analytical methods for micro-quantity of uranium in environmental samples
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Technical guidelines for environmental impact assessment Analytical methods for micro-quantity of uranium in environmental samples
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Standard similar to HJ 840-2017 GB/T 4214.1 GB 1495 HJ 842 HJ 843 HJ 841 Basic data | Standard ID | HJ 840-2017 (HJ840-2017) | | Description (Translated English) | Technical guidelines for environmental impact assessment Analytical methods for micro-quantity of uranium in environmental samples | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z33 | | Word Count Estimation | 34,354 | | Date of Issue | 7/7/2017 | | Date of Implementation | 8/1/2017 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 840-2017: Technical guidelines for environmental impact assessment Analytical methods for micro-quantity of uranium in environmental samples
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Technical guidelines for environmental impact assessment Analytical methods for micro-quantity of uranium in environmental samples
National Environmental Protection Standard of the People 's Republic of China
Replace GB 6768-86, GB 11220.1-89, GB 11223.2-89, GB 11223.1-89, GB 12378-90, GB 12377-90
Analytical method of trace uranium in environmental samples
Technical guidelines for environmental impact assessment Analytical methods
For micro-quantity of uranium in environmental samples
2017-7-7 release
2017-8-1 implementation
release
Ministry of Environmental Protection
I directory
Preface ..II
1 Scope of application 1
2 normative reference document 1
3 laser fluorescence method
4 N-235 Extraction-Spectrophotometry
5 tributyl phosphate extraction or tri-n-octylphosphine extraction-solid fluorescence method
6 Tributyl phosphate extraction - spectrophotometric method
7 tributyl phosphate extraction - solid fluorescence method.17
8 TBP extraction - solid fluorescence method
9 CL-5209 Extraction resin separation - 2 - (5-bromo-2-pyridylazo) -5-diethylaminophenol spectrophotometry.
Appendix A (normative appendix) Supplementary note on the implementation of the standard
Appendix B (Normative Appendix) Method for the determination of thorium using N-235 extraction-spectrophotometry.
Appendix C (Normative Appendix) Instructions for the Proper Use of Standards 29
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,
Quantity management, standardize environmental monitoring methods, the development of this standard.
This standard specifies the analytical methods for trace uranium in environmental water samples, air, biological and soil samples.
The technical content of this standard to GB 6768-86 "trace uranium analysis method", GB 11223.1-89 "biological samples of gray uranium
Determination of uranium in biological samples by laser liquid fluorescence method ", GB 11220.1-89" GB 11223.2-89 "
"Determination of uranium in soil CL-5209 Extraction resin Separation of 2- (5-bromo-2-pyridylazo) -5-diethylaminophenol spectrophotometry"
GB 12378-90 "Methods for Analysis of Trace Uranium in the Air TBP Extraction Fluorescence Method", GB 12377-90 "Analytical side of trace uranium in the air
Method of laser fluorescence "integration. The integration process with reference to GB 14883.7-2016 "food safety national standard food radiation
Determination of natural thorium and uranium in substances ", EJ/T 550-2000" Determination of uranium in soils, rocks and other samples "and" HJ "
168-2010 "Environmental Monitoring and Analysis Methods Standardization Technical Guidelines" and other information.
"Trace uranium analysis method" (GB 6768-86) was first released in 1986, the original standard drafting unit for the state-owned 504 factory
And the third research institute of the Ministry of Nuclear Industry; "Determination of uranium in biological samples of solid fluorescence method" (GB 11223.1-89) first published in 1989
Year, the original standard drafting unit for the Ministry of Nuclear Industry State-owned 814 factory; "biological samples of uranium uranium determination laser liquid fluorescence method" (GB
11223.2-89) was first released in 1989, the original standard drafting unit for the Ministry of Nuclear Industry State-owned 814 factory; "soil uranium determination
Separation of 2- (5-bromo-2-pyridylazo) -5-diethylaminophenol spectrophotometry by CL-5209 extraction resin (GB 11220.1-89)
Was released in 1989, the original standard drafting unit for the Ministry of Nuclear Industry Beijing Institute of the fifth; "analysis of trace uranium in the air TBP
(GB 12378-90) and "Analytical Methods for Trace Uranium in the Air" (GB 12377-90)
Quasi-first published in.1990, the original standard drafting unit for the Ministry of Nuclear Industry State-owned eight one two plants. This is the first revision. Revised
main content.
- the integration of the above six scattered standards, merged into a standard;
- Determination of trace uranium in environmental water samples, air, biological and soil samples by laser fluorescence method.
- the addition of uranium in biological samples of the determination of uranium N-235 extraction - spectrophotometric method, and gives the uranium thorium combined analysis
sequence;
- increased individual steps in the sample pretreatment and analysis process;
- Specification of part of the text and parameter units according to the current standard requirements.
Since the implementation of this standard, "trace uranium analysis method" (GB 6768-86), "Determination of uranium in soil CL-5209
Separation of 2- (5-bromo-2-pyridylazo) -5-diethylaminophenol spectrophotometric method (GB 11220.1-89), "
(GB 11223.2-89), "Determination of uranium in bio-sample ash solid-state fluorescence method" (GB
11223.1-89), "Analytical Methods for Trace Uranium in the Air TBP Extraction Fluorescence" (GB 12378-90), "
Method of laser fluorescence method "(GB 12377-90) abolished.
The appendix to this standard is an informative appendix.
This standard is proposed by the Safety Supervision Division of the Ministry of Environmental Protection.
This standard is organized by the Ministry of Environmental Protection Nuclear Safety Management Division, Science and Technology Standards Division.
The main drafting unit of this standard. Zhejiang Province, radiation environmental monitoring station, Qingdao Environmental Monitoring Center Station, Guangxi Radiation Environmental Supervision
management station.
The Environmental Protection Department of this standard was approved on July 7,.2017.
This standard has been implemented since August 1,.2017.
This standard is explained by the Ministry of Environmental Protection.
Analysis of Trace Uranium in Environmental Samples
1 Scope of application
This standard specifies the analytical methods for trace uranium in environmental water samples, air, biological and soil samples.
This standard applies to environmental water samples, air, biological, soil samples of trace uranium analysis, also applies to the nuclear facilities camp
Transport units, nuclear technology utilization units, uranium (thorium) mines and associated radioactive minerals development and utilization units of uranium pollution monitoring.
2 normative reference documents
The contents of this standard refer to the terms of the following documents. For those who do not specify a date, the valid version applies to this
standard.
GB 12997 water quality sampling program design technical specifications
Technical Guidance for Water Quality Sampling
Technical specification for preservation and management of sampled samples of water quality GB 12999
GB 12379 Environmental nuclear radiation monitoring regulations
GB 14883.7 Determination of natural thorium and uranium in radioactive substances in foodstuffs
Technical specification for radiation environmental monitoring of HJ/T 61
EJ/T 550 Determination of uranium in soils, rocks and other samples - Laser fluorescence method
3 laser fluorescence method
This method is applicable to environmental water samples (including surface water, groundwater, pollution sources), air, biology, soil
Analysis of trace uranium in samples.
The measurement range of uranium in environmental water, air, biology and soil samples by laser fluorescence method was 2.0 × 10-8 ~
2.0 × 10-5 g/L (water sample), 2.0 × 10-11 to 2.0 × 10-8 g/m3 (air sampling volume of 10 m3), 1.0 × 10-8 ~
1.0 × 10-5 g/g ash (when the amount of silica was 0.05 g) and 1.0 × 10-7 to 1.0 × 10-4 g/g (soil sample amount
0.10 g).
3.1 Principle of the method
The uranium enrichment enhancer added to the liquid sample forms a stable complex with the uranyl ions in the sample. In the UV pulse
Light intensity can be excited to produce fluorescence, and uranium content within a certain range, the fluorescence intensity and uranium content is proportional to,
By measuring the fluorescence intensity, the calculated uranium content was calculated.
3.2 Reagents
2 Unless otherwise stated, analytical pure chemical reagents conforming to national standards are used for the analysis, and the test water is freshly prepared.
Ionized water or distilled water. The acid used in the absence of specified concentration refers to the analysis of pure acid. Nitric acid acidification is pH 2 nitrate
Acid solution. When the reagent content is to be indicated, the following method is shown.
When the concentration of the solution is expressed as the mass concentration of the substance, the unit is in moles per liter (mol/L), and the sign of the quantity is c [for example, c
(G/L), micrograms per milliliter (μg/mL) when the concentration of the solution is expressed as the mass concentration,
(Ρ (U) = 10.0 μg/mL]; if the solution concentration is given by the mass fraction, the sign is ω
Such as ω (NaCl) = 10%, that 100 g of the solution containing 10 g of sodium chloride, that is, 10 g of sodium chloride dissolved in 90 g of water]
The unit is dimensionless; if the solution concentration is given in volume fraction, the symbol of the amount is ψ [for example, ψ (HCl) = 5%], indicating 100 mL
The solution contains 5 mL of concentrated hydrochloric acid, the unit dimensionless.
The reagents used in the trace uranium analysis method should be used for the determination of uranium content, uranium content higher than the level of the reagent can not
Used for the experimental process.
3.2.1 hydrofluoric acid (HF). mass concentration ≥ 40%.
3.2.2 nitric acid (HNO3). mass concentration of 65.0% ~ 68.0%.
3.2.3 Nitric acid solution. c (HNO3) = 1 mol/L.
3.2.4 nitric acid solution. 1 1.
3.2.5 Nitric acid solution. 1 2.
3.2.6 Nitric acid acidified water. pH = 2.
3.2.7 perchloric acid (HClO4). mass concentration of 70.0% ~ 72.0%.
3.2.8 Sodium persulfate (Na2S2O8).
3.2.9 Sodium hydroxide (NaOH).
3.2.10 Sodium hydroxide solution. ω (NaOH) = 4%.
3.2.11 uranium fluorescence enhancer.
3.2.12 Anti-interference uranium fluorescence enhancer use liquid (soil sample determination)
Weigh 2.5 g sodium hydroxide (3.2.9), dissolve with 100 mL uranium fluorescence enhancer (3.2.11), then water to volume
1000 mL, shake, placed in a plastic bottle to keep the spare.
3.2.13 uranium oxide (baseline or spectral purity, uranium octaoxide content greater than 99.97%)
3.2.14 uranium standard stock solution. ρ (U) = 1.00 mg/mL
3.2.14.1 Exempted uranium standard stock solution
Purchase a uranium standard solution with a standard substance certificate as a uranium standard stock solution.
3.2.14.2 Preparation of uranium standard stock solution
The uranium octaoxide (3.2.13) was placed in a furnace at 850 ° C for 0.5 h and removed in a desiccator to cool to room temperature.
3 Weigh 0.1179 g in 50 mL beaker, with 2 to 3 drops of water wet after adding 5 mL of nitric acid (3.2.2), on the hot plate
Dissolved in heat and evaporated to near dryness (controlled temperature to prevent spillage), then dissolved with nitric acid (3.2.6), quantitatively transferred
100mL volumetric flask, diluted with nitric acid (3.2.6) to the mark.
3.2.15 uranium standard intermediate solution. ρ (U) = 10.0 μg/mL
Take a 1.00 mL 1.00 mg/mL uranium standard stock solution (3.2.14) and dilute to 100 with nitric acid (3.2.6)
ML.
3.2.16 uranium standard working solution. ρ (U) = 0.500 μg/mL
Take the uranium standard intermediate solution (3.2.15) at 5.00 mL 10.0 μg/mL and dilute to 100 with nitric acid (3.2.6)
ML.
3.2.17 uranium standard working solution. ρ (U) = 0.100 μg/mL
Take the uranium standard intermediate solution (3.2.15) at 1.00 mL 10.0 μg/mL, dilute to 100 with nitric acid (3.2.6)
ML.
3.3 The main equipment
3.3.1 uranium analyzer
Range. 1 × 10-11 ~ 2 × 10-8 g/mL;
Detection limit. ≤2 × 10-11g/mL;
Linearity. r≥0.995.
3.3.2 Micro Sampler. 50 μL, 100 μL.
3.3.3 Analytical Balance. Readability 0.1 mg.
3.3.4 Quartz cuvette. (1 × 2 × 4) cm.
3.3.5 Teflon crucible (covered). 20 mL to 30 mL.
3.3.6 Platinum crucible. 20 mL.
3.3.7 Ma Fu furnace. temperature control accuracy of ± 3 ℃.
3.3.8 Air sampler.
3.3.9 Acidity meter.
3.4 sample collection, transportation, preservation and pretreatment
3.4.1 Sample collection, transport and storage
In accordance with GB 12997, GB 12998, GB 12999, GB 12379 and HJ/T 61 and other standards in the relevant provisions
Water samples, air, biological samples and soil samples collected and preserved. Wherein the air sample sampling membrane is a perchlorethylene resin
Fiber filter cloth, sampler diameter φ100 mm, sampling head from the ground height of 1.5m, flow rate of 50 ~ 100 cm/s. Sample volume root
4 According to the determination of uranium in the air (usually not less than 10 m3), record the sampling temperature, pressure, sampling volume, the need to convert
Into the standard condition of the volume. At the end of the sampling, the filter cloth is stored in the sample box.
3.4.2 Sample pretreatment
3.4.2.1 Water samples
After the water sample is left, the supernatant is taken as the sample to be tested. If there is suspended solids in water, filter with a pore size of 0.45 μm is required
Remove the filtrate as the sample to be tested.
3.4.2.2 Air samples
3.4.2.2.1 Uncover and discard the sampled filter gauze, place the perchlorethylene resin synthetic fiber filter cloth in a platinum crucible,
Ma Fu furnace slowly heated to 700 ℃, burning 1 h.
3.4.2.2.2 After removing the crucible, add 5 mL of nitric acid (3.2.2), heat it on an electric sand bath,
Hydrofluoric acid (3.2.1) 0.5 mL, continue heating to near dry (control temperature to prevent spillage). If the ash is large, you can add another drop
Hydrofluoric acid (3.2.1) until desilicon is complete.
3.4.2.2.3 Remove the crucible, then add 2 mL nitric acid (3.2.2), evaporate to near dry (control the temperature to prevent spill).
3.4.2.2.4 The crucible was washed three times with nitric acidified water (3.2.6) and combined in a 10 mL volumetric flask. According to the uranium
The use of light enhancer conditions, sodium hydroxide and nitric acid to adjust the filtrate pH to the appropriate range, to achieve the use of uranium fluorescence enhancement
Agent requirements, and constant capacity to the capacity of the bottle mark, shake as a sample to be tested.
3.4.2.3 Biological samples
3.4.2.3.1 The collected biological samples are pretreated by sample, pre-treated (including dry, carbonized, ashed, etc.) hands
Section, get a biological sample gray sample. Sample treatment should control the carbonization, ashing temperature, to prevent the fire, to prevent the sample burning
Knot
Bio-sample ash analysis should be uniform when weighing, and the sample ash should have the exact weight (or dry weight) of the biological sample
Conversion factor (gray ratio or ash ratio, ie 1 kg fresh or dry weight of the biological sample pretreated, pretreated after the ash
Heavy, expressed in g/kg), except that the results of the gray sample content are given only.
3.4.2.3.2 Weigh 0.0200 to 0.0500 g (depending on the uranium content in the sample) Bio-sample Gray on 50 mL of porcelain crucible
Pot, placed in the furnace at 600 ℃ burning to ashing completely (no obvious carbon particles), remove the slightly cold, add 20 mL of water and
2.0 g sodium persulfate (3.2.8), heated on the hot plate, stirred until the bubbles were exhausted and evaporated to dryness. If still in the process of drying
There are bubbles, can be slightly cold and then add about 15 mL of water, heated on the hot plate until no bubbles after drying, solid completely melt
melt. Remove the crucible, cool to room temperature, add 15 mL of water, dissolve the solid, after a little heat into the centrifuge tube centrifuged or too
filter. Wash the container with water and insoluble. The filtrate and washings were collected in a 25 mL volumetric flask. Discard insoluble matter.
3.4.2.3.3 Adjust the pH of the filtrate to sodium hydroxide and nitric acid according to the conditions of use of the uranium fluorescence enhancer used
Range, and constant capacity to the capacity of the bottle mark, shake after the sample to be tested.
53.4.2.4 Soil samples
3.4.2.4.1 take a certain amount of soil samples through the 140 mesh sieve, in a constant temperature oven, at 105 ℃ ~ 110 ℃ temperature
Under conditions of baking 2 h, remove the dryer placed in the dryer to room temperature.
3.4.2.4.2 Weigh 0.0100 to 0.1000 g samples in 20 mL to 30 mL polytetrafluoroethylene crucible, with a little water wetting,
Add 3.2 mL of nitric acid (3.2.2), 3 mL of perchloric acid (3.2.7), 2 mL of hydrofluoric acid (3.2.1), shake slowly and add crucible
Cover, in the thermostat heating plate about 1 h (note that the control temperature does not exceed 220 ℃), until the sample is completely decomposed, to crucible
The lid is evaporated to white smoke. Remove the crucible, slightly cold along the wall by adding nitric acid (3.2.2) 1 mL, then the crucible placed in the thermostat
Hot plate heating (note that the control temperature does not exceed 220 ℃) to the sample was wet salt (pay attention to prevent dry). Remove the crucible slightly
After cooling, add 5 mL of preheated (60 ° C to 70 ° C) (1 2) nitric acid (3.2.5) along the wall, then add to the hot plate
Heat to immediately remove the solution clear, rinse the crucible wall with water, put room temperature, turn in 50 mL volumetric flask, washed with water crucible
Three times, the washing liquid combined in the volumetric flask, and water volume to the capacity of the bottle marking, shake, clear.
3.4.2.4.3 Remove 5 mL of the clarified sample solution in a 50 mL volumetric flask and use the uranium fluorescence enhancer
Pieces, sodium hydroxide and nitric acid to adjust the pH value of the filtrate to the appropriate range, diluted with water volume to the volumetric flask mark, shake after
Sample to be tested.
3.5 Analysis steps
3.5.1 Linear range determination
To blank samples, according to the sample analysis steps, before the measurement in accordance with the requirements of the instrument, the instrument's photocell negative pressure
Adjusted to the appropriate range, the uranium standard solution was added several times and the recorded fluorescence intensity was measured. With the fluorescence intensity as the ordinate,
Uranium content is the abscissa, draw the fluorescence intensity - uranium content standard curve, determine the fluorescence intensity - uranium content linear range,
In the linear range, r > 0.995. Calculate the standard ratio of fluorescence intensity to uranium content.
The actual sample is measured using the standard addition method and should be carried out within the linear range.
This standard does not require that each time the determination of the linear range, but if the instrument photoelectric tube negative pressure adjustment and other indicators change
Or uranium fluorescence enhancer, and the fluorescence intensity measurement should be heavier when the original linear range boundary is determined
Newly determined linear range.
3.5.2 Sample determination
3.5.2.1 in accordance with the instrument operating procedures to the instrument and stable, check the instrument to confirm the photoelectric tube negative pressure and other indicators and
The state of the linear range is the same.
3.5.2.2 Transfer 5.00 mL The sample to be tested is placed in a quartz cuvette and placed in a micro uranium analyzer to measure the chamber.
And record the reading N0.
63.5.2.3 Add 0.5 mL of uranium fluorescence enhancer to the sample (3.2.11) [Anti-interference uranium fluorescence for soil samples
(3.2.12)], mix well and observe that, if precipitation occurs, the sample is discarded (note that
The sample is diluted or other methods of treatment, until no precipitation, before entering the measurement step).
3.5.2.4 Measurement of recorded fluorescence intensity N1.
3.5.2.5 Add 50 μL 0.100 μg/mL uranium to the sample Standard working solution (3.2.17) [When uranium content is high, add
Into the 50 μL 0.500 μg/mL uranium standard solution (3.2.16)], and mix thoroughly to determine the recorded fluorescence intensity of N2.
3.5.2.6 Check that N2 should be within the linear range of the standard curve. If the linear range is exceeded, the sample should be diluted and re-determined.
3.5.2.7 Check that the ratio of N2-N1 to the added uranium standard should be consistent with the standard curve B value.
3.5.3 Result calculation
3.5.3.1 Water sample uranium content calculated according to formula (1).
) (
) (
Water VNN
KVCNN
C (1)
Where. uranium concentration in water - water sample, μg/L;
N0 - the fluorescence intensity measured before the sample was not added to the uranium fluorescence enhancer;
N1 - Fluorescence intensity measured after sample addition to uranium fluorescence enhancer;
N2 - the fluorescence intensity of the sample after uranium standard working solution;
C1 - concentration of uranium standard working solution at a fluorescence intensity of N2, μg/mL;
V1 - volume of uranium standard working solution added when measuring fluorescence intensity N2, mL;
V0 - volume of analytical water samples, mL;
K - water sample dilution factor.
V1 - volume of uranium standard working solution added when measuring fluorescence intensity N2, mL;
K - water sample dilution factor.
3.5.3.2 Uranium content in air samples calculated according to formula (2).
VYV
VVKC
NN
NN
NN
NN
Gas
 €
distance (2)
Where. the concentration of uranium in the C gas-air sample, μg/m3;
N0
', N1
', N2
'- the corresponding instrument readings when determining the reagent blank sample;
V2 - volume of volume at sample trea...
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