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HJ 841-2017: Analytical method for 131I in water, milk, plant and animal thyroid gland
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Analytical method for 131I in water, milk, plant and animal thyroid gland
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HJ 841-2017
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Standard similar to HJ 841-2017 GB/T 4214.1 GB 1495 HJ 842 HJ 843 HJ 840 Basic data | Standard ID | HJ 841-2017 (HJ841-2017) | | Description (Translated English) | Analytical method for 131I in water, milk, plant and animal thyroid gland | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z33 | | Word Count Estimation | 21,279 | | Date of Issue | 7/7/2017 | | Date of Implementation | 8/1/2017 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 841-2017: Analytical method for 131I in water, milk, plant and animal thyroid gland---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.
Analytical method for 131I in water, milk, plant and animal thyroid gland
National Environmental Protection Standard of the People 's Republic of China
Instead of GB/T 13272-91, GB/T 14674-93, GB/T 13273-91
Water, milk, plant, animal thyroid
Iodine-131 analysis method
Analytical method for 131I
In water, milk, plant and animal thyroid gland
2017-7-7 release
2017-8-1 implementation
Ministry of Environmental Protection released
I directory
Preface to the Secretary-General ...
1 Scope of application ...1
2 Methodological Summary ...1
3 Reagents and Materials ...1
4 Instruments and equipment ...2
5 Sampling ...
6 Analysis steps ...
7 Measurement and calculation ...
8 method to detect the lower limit of the calculation of the ...9
9 Quality Control ...
Appendix A (informative) Correct use of the description of this standard ... 13
Appendix B (informative) Equipment diagram ...
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 analysis of iodine-131 in water, milk, plants, and animal thyroids.
This standard on "water iodine-131 analysis method" (GB/T 13272-91), "milk iodine -131 analysis method"
(GB/T 13273-93), "Plant, animal thyroid iodine-131 analysis method" (GB/T 13273-91) were integrated, its
The main technical content is basically the same as the original standard.
"Analysis method of iodine-131 in water" (GB/T 13272-91) was first published in.1991, "Analysis of iodine-131 in milk
Law "(GB/T 14674-93) was first published in.1993," plant, animal thyroid iodine-131 analysis method "
(GB/T 13273-91) was first released in.1991, the standard drafting units are China Atomic Energy Research Institute. This time for the first time
Revised, revised the main content.
- Integrate the above three criteria into one standard;
- increased the efficiency scale of the gamma spectrometer;
- increase the calculation of the lower limit of the method;
- the decay correction coefficients during the measurement period are introduced in the calculation formulas (1), (4), (7) and (8)
- Revised part of the content.
Appendix A of this standard is an informative appendix.
Appendix B to this standard is an informative appendix.
From the date of implementation of this standard, "analysis method of iodine-131 in water" (GB/T 13272-91), "Analysis of iodine-131 in milk
Method "(GB/T 14674-93)," plant, animal thyroid iodine-131 analysis method "(GB/T 13273-91) abolished.
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. radiation environment monitoring station in Zhejiang Province, Guangxi Zhuang Autonomous Region Radiation Environmental Supervision and 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.
1 water, milk, plant, animal thyroid iodine-131 analysis method
1 Scope of application
This standard specifies the analysis of iodine-131 in water, milk, plants, and animal thyroids.
This standard applies to the environment of water, milk, goat milk and other liquid milk samples and plants, animal thyroid iodine -131 activity concentration
analysis.
2 method summary
Water and milk samples of iodine-131, concentrated with a strong alkaline anion exchange resin, sodium hypochlorite desorption, carbon tetrachloride extraction, sulfur
Sodium hydrogen acid reduction, water stripping, made of silver iodide precipitation. Measured with a low background beta meter or a low background gamma spectrometer.
Plant samples, animal thyroid iodine-131, fixed with iodine iodine, hydrogen peroxide to help ash, water extraction, carbon tetrachloride extraction
Take, water stripping, made of silver iodide precipitation. Measured with a low background beta meter or a low background gamma spectrometer.
3 reagents and materials
Unless otherwise stated, analytical analytical reagents and distilled water or equivalent purity water are used in accordance with national or professional standards.
Other grades of reagents can be used as long as they are preliminarily determined to have a sufficiently high purity and are not used to reduce the measurement accuracy.
3.1 iodine carrier solution
Dissolved in 13.070 g of potassium iodide in distilled water, transferred to 1L volumetric flask. Add a little anhydrous sodium carbonate, diluted to the mark.
3.2 iodine-131 reference solution. nuclear pure;
3.3 sodium hypochlorite (NaClO). active chlorine content of 5.2% or more, preserved at low temperature;
3.4 sodium hypochlorite (NaClO). active chlorine content of 2.6% or more, preserved at low temperature;
3.5 carbon tetrachloride (CCl4). mass concentration 99.5%;
3.6 Hydroxylamine Hydrochloride Solution. c (NH2OH • HCl) = 3 mol/L;
3.7 Silver nitrate solution (AgNO3). mass concentration 1%;
3.8 sodium bisulfite solution (NaHSO3). mass concentration of 5%;
3.9 Sodium hydroxide solution (NaOH). mass concentration 5%;
3.10 Sodium hydroxide solution. c (NaOH) = 1 mol/L;
3.11 nitric acid (HNO3). mass concentration 65.0% ~ 68.0%
3.12 Nitric acid solution (HNO3). 1 1;
3.13 hydrochloric acid solution. c (HCl) = 1 mol/L;
23.14 sodium nitrite solution. c (NaNO2) = 5 mol/L;
3.15 Hydrogen peroxide (H2O2). 30% mass concentration;
3.16 2 mol/L sodium hydroxide solution 2 mol/L solution of potassium hydroxide solution. (3 2);
Follow steps 3.18.1.2.
4 equipment
4.1 low background β measuring instrument. the background is less than 1cpm;
4.2 low background gamma spectrometer;
4.2.1 NaI γ spectrometer. cylindrical NaI (Tl) crystal with size not less than Φ7.5cm × 7.5cm, and 661.6keV of 137Cs
The energy peak resolution is less than 9%.
4.2.2 high purity germanium γ spectrometer. sensitive volume should be greater than 50cm3, 60Co 1332.5keV gamma ray energy resolution is less than
32.2 keV.
4.3 Analysis of balance. readability 0.1 mg;
4.4 electric stirrer;
4.5 high frequency heat sealing machine;
4.6 Glass exchange column. see Figure B.1 in Appendix B;
4.7 glass desorption column. see Figure B.2 in Appendix B;
4.8 Glass Removable Funnel. See Appendix B, Figure B.3;
4.9 stainless steel pressure source mold. see Figure B.4 in Appendix B;
4.10 Seal copper ring. see Figure B.5 in Appendix B;
4.11 mortar hammer;
4.12 porcelain evaporative dish. 600 ml ~ 750 ml.
5 sampling
5.1 Water sample. Select representative point sampling. Rivers or lakes are generally selected for their central area sampling, tap water to collect the end of the water pipe
Phase acidity to pH 1 (aqueous phase acidity with a fine pH test strip from the bottom of the separatory funnel to take a little water phase test). Oscillation 2 min
(Note the air), standing. The organic phase was transferred to a 250 ml separatory funnel and the extract was repeated twice. Each time with carbon tetrachloride (3.5) 15 ml,
The organic phase was combined and the aqueous phase was separated and the organic phase was transferred to another 250 ml separatory funnel.
The following steps in 6.2.5 ~ 6.2.9 washing, stripping, precipitation, sample preparation and sealing, to be tested.
6.4 plants, animal thyroid
6.4.1 Sample preparation
6.4.1.1 Plant samples
6.4.1.1.1 Collect all kinds of plant samples, take 250 g of fresh sample, chopped into 750 ml porcelain evaporator. Plus 20 mg
6 iodine carrier (6.1), and 1 g of the sample by adding 1 ml of mixed solution (3.16), the mixture was evenly stirred.
6.4.1.1.2 After the sample was evaporated to dryness on the electric furnace, the porcelain evaporated dish was shredded at 450 ° C for 1 h. Cooling, grinding, with 30%
Hydrogen peroxide (3.15) was completely evaporated to dryness and placed in a furnace at 450 ° C for 30 min. Such as gray still obvious carbon particles, and then added to help
Ashing agent Hydrogen peroxide (3.15), continue to ashes in the furnace at 450 ° C until the sample is gray.
6.4.1.2 Animal thyroid
Called 5 g thyroid samples of glandular tissue. Cut, placed in 600 ml porcelain evaporates. Add 10 mg of iodine carrier (6.1) and 10 ml
Mix the solution (3.16). Mix evenly, as per step in 6.4.1.1.2.
6.4.2 leaching
The gray sample was transferred to a 100 ml centrifuge tube, three times with 30 ml of water. Centrifuge the supernatant transferred to a 250 ml separatory funnel
in.
6.4.3 Extraction
To the separatory funnel (6.4.2) was added 20 ml of carbon tetrachloride (3.5), 2 ml of sodium nitrite solution (3.14), nitric acid (3.11)
Adjust the acidity of the water phase to pH 1 (water phase acidity with a fine pH test paper from the bottom of the separatory funnel to take a little water phase test). The oscillation
2 min (note the deflation), static phase separation. The organic phase was transferred to a 100 ml separatory funnel. With 15 ml and 5 ml of carbon tetrachloride (3.5), respectively
Perform a second, third extraction. Each oscillation for 2 min, after standing combined organic phase.
The following steps in 6.2.5 ~ 6.2.9 washing, stripping, precipitation, sample preparation and sealing, to be tested.
7 Measurement and calculation
7.1 beta measurement
7.1.1 Draw the self-absorption curve
Take 0.1 ml of the appropriate activity of iodine-131 reference solution (3.2) drop in the stainless steel plate. Add 1 drop of sodium hydroxide solution (3.10) to slow it
Slow drying, made with the sample measurement conditions consistent with the thin source. On a low background beta meter (4.1), the radioactivity is I0.
Take 6 100 ml beaker, add 0.5,1.0,1.5,2.0,2.5,3.0 ml iodine carrier solution (3.1), add appropriate amount of distilled water.
Add 0.1 ml of iodine-131 reference solution (3.2), add nitric acid (3.11) under stirring, when the solution was golden yellow, immediately add 7ml nitro
Silver acid solution (3.7). Heated to micro-boiling, remove and cool to room temperature. Follow the steps 6.2.8 to 6.2.9 to operate the source. Will be thin source and prepared by 6
And the radioactivity was measured on a low background beta instrument. The radioactivity of each source is corrected to I by chemical yield
As the standard, the self-absorption coefficient of the silver iodide precipitation source with different sample thickness was obtained. Then, the self-absorption coefficient is the ordinate, with iodine
The mass thickness of the silver precipitation source is the abscissa, and the self - absorption standard curve is drawn.
7.1.2 Instrument detection efficiency
7 A thin source was prepared with a known reference activity of cesium-137 reference solution for the determination of beta detection efficiency.
7.1.3 Calculation
Calculate the concentration of iodine-131 in water and milk by formula (1). Calculate the concentration of iodine-131 in the thyroid of plants and animals by the formula (4).
Bc
Where.
W1 - measured the weight of the iodine carrier in the sample, mg;
W2 - the weight of the iodine carrier added to the sample, mg.
The decay correction factor F of the sample during the measurement is calculated as.
Te
F
(3)
Where.
Λ - the decay constant of iodine -131, s-1;
T - sample measurement time, s.
Bc
EWYE
FNN
A
) ((4)
8 where.
Aβ - iodine - 131 activity concentration, Bq/kg or Bq/g;
W - the weight of the test sample, kg or g;
The rest of the formula (1).
7.2 γ measurement
7.2.1 Efficiency scale of gamma spectrometer
7.2.1.1 The efficiency scale of the gamma spectrometer refers to the relationship between the gamma ray energy and its energy efficiency at a given measurement, or
Determine the scale factor for some specific nuclides.
7.2.1.2 The selected scale source is exactly the same as the geometry of the sample to be tested and the box material, and the nuclide content and the energy
Do know, and have good uniformity and stability.
7.2.1.3 The geometry of the scale source and the sample (including the background) must be consistent. According to the accuracy requirements of the scale to determine
The total number of omnipotent peaks of the scale is generally not less than 10,000 for each gamma ray full peak.
7.2.1.4 Using the formula (5) to calculate the energy efficiency of the gamma ray energy E.
PA
NN bs
. (5)
Where.
Ηγ - γ ray energy is the all - round peak detection efficiency of E, s - 1 · Bq - 1;
A - the scale of the source in the measurement of the corresponding nuclide activity, Bq;
Ns - γ ray energy is the universal peak count rate of E, s -1;
The Nb - γ ray energy is the corresponding background count rate under the E -
P - γ ray energy is the emission probability of E all - peak.
7.2.1.5 After a set of all-round peak efficiency ηγ and corresponding energy E experimental points are determined, the experimental point is used as the least squares fitting
Find the efficiency curve, in the 50keV ~ 3MeV energy range with the formula (6).
Ln () =
IEln
Ia) ((6)
Where.
Ηγ - γ ray energy is the all - round peak detection efficiency of E, s - 1 · Bq - 1;
Ai - fitting coefficient;
N-1 - fit order, generally take n-1 = 2 or 3.
97.2.2 Calculation
The count rate of the 0.364 MeV allotron peak was measured with a low background gamma spectrometer (4.2). Calculate the activity of iodine-131 in water and milk by formula (7)
Concentration, using the formula (8) to calculate the plant, animal thyroid iodine-131 activity concentration.
Bc
EpVY
FNN
A
) (. (7)
Where.
Aγ - Iodine - 131 activity concentration, Bq/L;
Nc - 0.364 MeV universal peak count rate, s -1;
Nb - 0.364 MeV all - round peak corresponding to the background count rate, s -1;
Η γ - detection efficiency of spectrometer, s-1 · Bq-1;
Y - Chemical yield (calculated as formula 2);
V - the volume of the test sample, L;
P - 0.364 MeV omnipotent peak emission probability, desirable 81.1%;
Λ - the decay constant of iodine -131, s-1;
T - sampling to the start of the measurement interval, s;
F - the decay correction factor of the sample during the measurement (calculated as Equation 3).
Bc
EpWY
FNN
A
) ((8)
Where.
Aγ - iodine - 131 activity concentration, Bq/kg or Bq/g;
W - the weight of the test sample, kg or g;
The rest of the formula (7).
8 method to detect the lower limit of the calculation
8.1 Low background beta meter measurement
Low-cost beta measuring instrument, the formula (9) is used to calculate the detection limit of iodine-131 in water and milk, calculate the plant with formula (10)
The lower limit of iodine-131 detection in animal thyroid.
D t
EVY
L
65.4
..(9)
Where.
LD - iodine - 131 detection limit, Bq/L;
Ηβ - β detection efficiency, s - 1 · Bq - 1;
Y - chemical yield;
V - the volume of the test sample, L;
E - iodine -131 self-absorption coefficient;
Nb - background count rate, s-1;
Tb - background measurement time, s.
D t
EWY
L
65.4
(10)
Where.
LD - iodine -131 detection limit, Bq/kg or Bq/g;
W - the weight of the test sample, kg or g;
The rest with the formula (9).
8.2 Low background gamma spectrometer
(11), the lower limit of detection of iodine-131 in water and milk is calculated by the formula (12). The plant,
The lower limit of detection of iodine-131 in the thyroid gland.
D t
PVY
L
65.4
(11)
Where.
LD - iodine - 131 detection limit, Bq/L;
Η γ - detection efficiency of spectrometer, s-1 · Bq-1;
Y - chemical yield;
V - the volume of the test sample, L;
P - 0.364 MeV omnipotent peak emission probability, desirable 81.1%;
Nb - 0.364 MeV all - round peak corresponding to the background count rate, s - 1;
T b - background measurement time, s
D t
PWY
L
65.4
(12)
Where.
LD - iodine -131 detection limit, Bq/kg or Bq/g;
W - the weight of the test sample, kg or g;
The rest of the formula (11).
9 quality control
9.1 blank test
Whenever the reagent is replaced, a blank test must be carried out.
9.1.1 Water samples
The number of samples can not be less than 6, the amount of 10 L distilled water in 10 L under the mouth of the bottle. Operate from 6.2.2 to 6.2.9 and calculate blank test
The average count rate and the standard deviation, and test whether the instrument count rate of 95% of the confidence rate is significant difference.
9.1.2 Milk
The number of samples of not less than 6, take the uncontaminated milk sample 4 L in the 5 L beaker. According to analysis steps 6.3.1 ~ 6.3.4 operation, and count
Calculate the average count rate and standard deviation of the blank sample and check whether there is a significant difference between the background count rate and the 95% confidence ratio
difference.
9.1.3 plants, animal thyroid
The number of samples can not be less than 6, take uncontaminated plant samples 250 g, or sheep thyroid 5 g. According to 6.4.1 ~ 6.4.3 operation, and count
Calculate the average count rate and standard deviation of the blank sample, and test whether it has a significant difference with the instrument count rate at 95% confidence level
different.
9.2 precision
9.2.1 Water samples
The precision data were determined by three labs for three levels of the sample. Each laboratory has three levels each
Make four parallel test samples.
Table 1 Precision test results Unit. Bq
Level Ⅰ Ⅱ Ⅲ
Mean m 6.38 51.25 112.23
Repetitive r 0.78 7.31 13.30
Reproducibility R 3.25 16.94 29.23
9.2.2 Milk
The precision data were determined by three labs for three levels of the sample. Each lab is done at three levels
4 parallel test samples.
Table 2 Precision test results Unit. Bq
Level Ⅰ Ⅱ Ⅲ
Mean value m 6.14 52.10 112.44
Repetitive r 0.87 5.91 5.96
Reproducibility R 1.51 23.90 35.31
9.2.3 plants, animal thyroid
The precision data were determined by three labs for three levels of the sample. Each laboratory has three levels each
Make four parallel test samples.
Table 3 Plant-like precision test results Unit. Bq
Level Ⅰ Ⅱ Ⅲ
Mean value m 7.05 49.93 108.12
Repetitive r 0.95 5.99 6.97
Reproducibility R 2.3 15.23 25.96
Table 4 sheep thyroid precision test results Unit. Bq
Level Ⅰ Ⅱ Ⅲ
Mean value m 6.57 48.17 109.88
Repetitive r 1.74 5.64 11.83
Reproducibility R 2.8 15.63 17.47
Appendix A
(Informative)
Correctly use the instructions in this standard
A.1 Determine the time at which the sample is measured by the formula (A.1) tc (s).
22) (SNN
NNN
Bc
Bcc
C
+ mi (A.1)
Where.
Tc - sample counting time, s;
Nc-sample source plus the count rate of the background, s -1;
Nb - background count rate, s -1;
S-predetermined relative standard deviation.
A.2 If a resin is easily desorbed, 6.3.2 of the analytical procedure can be omitted during the analysis of the milk sample.
A.3 animal thyroid must be the determination of the stable iodine content of the sample itself. Corresponding to their glands (such as submandibular gland, etc.) as a control.
And deducts it when calculating the chemical yield of iodine.
A.4 If there is no high-frequency heat sealing machine, the precipitation source can be sandwiched in plastic film, cover a layer of yellow wax silk, with 5W electric iron along the precipitation source
Draw a circle of closure, cut the outer edge, to be measured.
A.5 on the use of cesium -137 thin source instead of iodine -131 source scale β detection efficiency of the problem. According to cesium -137 β decay of the emission probability, weighted
The average maximum energy value of the subsequent β particles is 0.547 MeV, and the average maximum energy of iodine-131β particles is 0.576 MeV.
The deviation is 4.9%. Which causes the detection efficiency (including the absorption of the air layer, anti-scattering, etc.) deviation within the experimental error range, so
Can be used cesium -137 thin source instead of iodine -131 source scale β detection efficiency.
Appendix B
(Informative)
Device diagram
Figure B.1 Glass exchange column (unit. mm)
Figure B.2 Glass Desorption Column (Unit. mm)
Figure B.3 Glass Removable Funnel (Unit. mm)
Figure B.4 stainless steel pressure source mold (unit. mm)
Figure B.5 Seal copper ring (unit. mm)
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