Journal of Radiation Research and Radiation Processing, Volume. 41, Issue 6, 060702(2023)

Rapid determination of radionuclides by gamma spectrometry in biological samples using a microwave pretreatment technique

Jin XU1... Feng CHENG2,* and Xiaoxiang JIN2 |Show fewer author(s)
Author Affiliations
  • 1CGN Huizhou Nuclear Power Co., Ltd., Huizhou 516353, China
  • 2Yangjiang Nuclear Power Co., Ltd., Yangjiang 529941, China
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    Figures & Tables(8)
    Flowchart of analysis of γ radionuclides by gamma spectrometry in biological samples
    • Table 1. Heating parameters of microwave apparatus

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      Table 1. Heating parameters of microwave apparatus

      加热参数设定 Heating parameters

      加热时段

      Heating period

      加热温度 / ℃

      Heating

      temperature

      加热功率 / %

      Heating power

      保温温度 / ℃

      Holding

      temperature

      保温功率 / %

      Holding power

      保温偏差 / ℃

      Temperature

      deviation

      保温时间 / min

      Holding time

      18080806025
      21058010560215
      31508015060220
      41808018060240
      52408024060240
      62808028060260
      73008030065260
      835085350652360
      9380853806521 800~4 800
    • Table 2. Comparison of pre-treatment speed between the two methods

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      Table 2. Comparison of pre-treatment speed between the two methods

      样品类型

      Sample type

      样品

      量 / kg

      Sample

      weight

      传统灰样制备法

      Traditional ash sample preparation method

      微波灰样制备法

      Microwave ash sample preparation method

      前处理

      总时间 /d

      Total pretreat-

      ment time

      灰鲜比

      /(g·kg-1)

      Ash to fresh ratio

      分批处理

      次数

      Batch proce-

      ssing times

      前处理

      总时间/d

      Total pretreat-

      ment time

      灰鲜比

      /(g·kg-1)

      Ash to fresh ratio

      分批处理

      次数

      Batch processing times

      鸡Chicken8.23406.402126.112

      淡水鱼

      Freshwater fish

      10.83510.221010.02
      海鱼Sea fish9.704012.221011.72
      海虾Sea shrimp10.52017.42813.62
      青口Mussel7.551417.42416.61
      牡蛎Oysters13.0256.66256.921
      紫菜Laver11.4206.08285.382
    • Table 3. Results of recoveries test

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      Table 3. Results of recoveries test

      中国毛虾Acetes Chinensis

      核素

      Nuclide

      原样测定值

      / (Bq·kg-1)

      Original value

      加标量/(Bq·kg-1)

      Added scalar quantity

      加标测定值1

      / (Bq·kg-1)

      Measured value 1

      加标测定值2

      / (Bq·kg-1)

      Measured value 2

      加标回收率1

      / %

      Recovery rate 1

      加标回收率2

      / %

      Recovery rate 2

      相对偏差/%

      Relative

      deviation

      54MnND430.7388.4424.790.298.64.47
      57CoND82.1091.2695.041111162.03
      60CoND622.5644.4641.81041030.20
      65ZnND1178126312821071090.76
      109CdND17631761176110099.90.01
      137CsND429.0373.3374.787.087.30.18
      241AmND170.6169.3168.399.298.70.29
      139CeND99.94104.391.4610491.56.54
    • Table 4. Comparison of analysis results of two methods

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      Table 4. Comparison of analysis results of two methods

      样品类型

      Sample type

      制样方法

      Preparation method

      核素(鲜重)/ (Bq·kg-1)

      Nuclide (fresh weight)

      7Be54Mn58Co60Co110mAg134Cs137Cs40K226Ra232Th238U

      Chicken

      A<0.056<0.008<0.008<0.011<0.007<0.0070.01462.30.055<0.023<0.307
      B<0.057<0.009<0.008<0.010<0.007<0.0070.01663.40.041<0.024<0.309
      C / %//////6.670.8814.6//
      DL<0.036<0.006<0.005<0.008<0.005<0.004<0.006<0.157<0.013<0.018<0.034

      淡水鱼

      Freshwater fish

      A<0.088<0.016<0.015<0.023<0.013<0.0110.03693.9<0.029<0.040<0.121
      B<0.092<0.016<0.016<0.024<0.013<0.0110.03596.2<0.025<0.040<0.125
      C / %//////1.411.21///
      DL<0.027<0.004<0.004<0.006<0.004<0.003<0.004<0.120<0.010<0.014<0.026

      海鱼

      Sea fish

      A<0.107<0.019<0.019<0.027<0.016<0.0140.030120<0.029<0.047<0.145
      B<0.098<0.018<0.018<0.027<0.014<0.0130.030117<0.027<0.044<0.138
      C / %//////0.001.27///
      DL<0.030<0.005<0.004<0.006<0.004<0.004<0.005<0.133<0.011<0.015<0.028

      海虾

      Sea shrimp

      A<0.126<0.021<0.022<0.031<0.018<0.0150.02677.80.0990.101<0.159
      B<0.097<0.017<0.016<0.024<0.014<0.0120.02363.50.0890.075<0.122
      C / %//////6.1210.15.3214.8/
      DL<0.028<0.005<0.004<0.006<0.004<0.003<0.004<0.123<0.010<0.014<0.026

      青口

      Mussel

      A<0.099<0.017<0.017<0.024<0.014<0.012<0.01848.90.1510.104<0.135
      B<0.099<0.018<0.016<0.023<0.014<0.013<0.01850.00.1300.107<0.130
      C / %///////1.117.471.42/
      DL<0.039<0.006<0.005<0.008<0.005<0.005<0.006<0.171<0.014<0.020<0.037

      牡蛎

      Oysters

      A<0.051<0.008<0.008<0.011<0.007<0.006<0.00819.90.0550.1110.393
      B<0.047<0.008<0.007<0.011<0.006<0.006<0.00824.50.0450.1090.346
      C / %///////10.410.00.916.36
      DL<0.023<0.004<0.003<0.005<0.003<0.003<0.004<0.099<0.008<0.011<0.021

      紫菜

      Laver

      A<0.036<0.005<0.005<0.007<0.005<0.004<0.00533.10.0610.093<0.388
      B<0.039<0.006<0.005<0.007<0.005<0.005<0.00638.90.0590.094<0.454
      C / %///////8.061.670.53/
      DL<0.026<0.004<0.004<0.005<0.004<0.003<0.004<0.108<0.009<0.013<0.026
    • Table 5. Ratio of t-value for method A and method B

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      Table 5. Ratio of t-value for method A and method B

      样品类型

      Sample type

      放射性核素 Radionuclide
      7Be54Mn58Co60Co110mAg134Cs137Cs40K226Ra232Th238U
      鸡Chicken0.980.891.001.101.001.000.880.981.340.960.99
      淡水鱼Freshwater fish1.051.001.071.041.001.000.971.020.861.001.03
      海鱼Sea fish1.091.061.061.001.141.081.001.031.071.071.05
      海虾Sea shrimp1.301.241.381.291.291.251.131.231.111.351.30
      青口Mussel1.001.060.940.961.001.081.001.020.861.030.96
      牡蛎Oysters1.091.001.141.001.171.001.000.811.221.021.14
      紫菜Laver0.920.831.001.001.000.800.830.851.030.990.85
      平均值Mean value(x¯A/B)1.061.011.081.061.091.030.970.991.071.061.05

      标准偏差

      Standard deviation(S

      0.110.120.130.100.110.120.090.130.160.120.13
      tt-Value (tA/B)1.220.191.401.201.790.540.670.140.991.070.81
    • Table 6. Results of waste gas detection

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      Table 6. Results of waste gas detection

      检测项目

      Test items

      实测浓度

      /(mg/m³)

      Measured

      value

      最高允许排放浓度/(mg/m³) Maximum allowable emission concentration

      检测结果

      Detection

      result

      检测项目

      Test items

      实测排放

      量/(kg/h)

      Measured emission

      排放量标准值/(kg/h)

      Emission standard value

      检测结果

      Detection

      result

      Benzene

      <0.00412

      合格

      Pass

      Ammonia

      0.0234.9合格Pass

      甲苯

      Toluene

      0.27340

      合格

      Pass

      三甲胺

      Trimethylamine

      <1.0×10-30.54合格Pass

      对二甲苯

      Paraxylene

      <0.00970

      合格

      Pass

      硫化氢

      Hydrogen sulfide

      <1.7×10-60.33合格Pass

      间二甲苯

      M-xylene

      <0.009

      合格

      Pass

      甲硫醇

      Methyl mercaptan

      <4.3×10-60.04合格Pass

      邻二甲苯

      O-xylene

      <0.004

      合格

      Pass

      甲硫醚

      Methyl sulfide

      <1.7×10-40.33合格Pass

      甲醛

      Formaldehyde

      <0.02525

      合格

      Pass

      二甲二硫

      Dimethyl disulfide

      <3.5×10-60.43合格Pass

      非甲烷总烃

      NMHC

      84.6120

      合格

      Pass

      二硫化碳

      Carbon disulfide

      <2.6×10-41.5合格Pass

      臭气浓度(无量纲)

      Odor concentration

      (dimensionless)

      7412 000

      合格

      Pass

      苯乙烯

      Styrene

      1.1×10-36.5合格Pass
    • Table 7. Comparison of two pre-treatment methods

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      Table 7. Comparison of two pre-treatment methods

      方法

      Methods

      传统灰样制备法

      Traditional ash sample preparation method

      微波灰样制备法

      Microwave ash sample preparation method

      加热方式

      Heating mode

      热传导、对流和辐射原理使热量从外部传至物料内部(存在温度梯度,故加热的物料不均匀)

      Heat is transferred from the outside to the inside through three ways: heat conduction, convection, and radiation (Temperature gradient leads to uneven heating)

      被加热体内部偶极分子高频往复运动,产生“内摩擦热”,物料内外部同时加热和升温(加热速度快且均匀)

      Material is heated by 'internal friction heat', caused by high frequency reciprocating motion of dipole molecules inside the heated body. Material internal and external heating and heating-up at the same time (heating speed is fast and uniform)

      制样时间和效率

      Sample preparation time and efficiency

      制样时间较长,单个样品约2~6周,劳动强度大

      Sample preparation time is long, 2 ~ 6 weeks for a single sampling process, higher labour intensity

      制样时间缩短,单个样品约1~2周,制样效率高

      Sample preparation time is shortened, 1 ~ 2 weeks for a single sample preparation, high sample preparation efficiency

      温度控制

      Temperature control

      电炉(含电炉丝)不能定量控制温度

      Electric furnace (including electric wire) cannot control temperature quantitatively

      测温元件热电偶,可控制干燥、碳化和灰化各个阶段的温度,使得温度不超过400 ℃

      Thermocouple used for temperature measuring element. Able to control temperature in various stages of the drying, carbonization and ashing, temperature does not exceed 400 ℃

      核素损失可能性

      Nuclide loss probability

      大(炒锅底部长时间高温容易凸凹变形,收集转移可能会损失)Large (the bottom of the frying pan is prone to convex and concave deformation. Loss could be happen during collection and transfer)

      小(石英玻璃坩埚,灰样可全部收集)

      Small (quartz glass crucible, ash samples can be fully collected)

      样品处理量

      Sample handling capacity

      较大

      The larger

      大(油脂类样品除外)

      Large (except for oil samples)

      沾污可能性

      Contamination possibility

      小(通风橱易结垢油污,清洗难度大)

      Small (ventilation cabinet is easy to scale oil, cleaning is difficult)

      无(石英坩埚易清洗,且含油烟回收系统)

      No (quartz crucible is easy to be cleaned, and oily smoke recovery system is integrated)

      对设备腐蚀性

      Corrosivity to equipment

      小(海洋生物腐蚀铁制品)

      Small (marine biological corrosion of iron products)

      No

      安全系数

      Safety factor

      低(容易着火)

      Low (easy to catch fire)

      高(碳化阶段不通氧气,不易着火)

      High (no oxygen in the carbonization stage, not easy to catch fire)

      健康危害程度

      Health hazard degree

      高,对呼吸道有刺激

      High, irritating to the respiratory tract

      无(全封闭式,含净化装置)

      No (fully enclosed, with purification device)

      设备操作

      Equipment operation

      操作工序繁琐,需3种设备完成干燥、碳化和灰化等前处理工序

      Operation process is complicated, and three kinds of equipment are needed to complete the pretreatment process such as drying, carbonization and ashing

      操作简单,自动升降,一键启动,全过程无需人员值守

      The equipment is easy to be operated, automatic lifting, one key start, Unattended throughout the entire process

      设备费用

      Equipment cost

      较贵,电消耗量大

      More expensive, larger power consumption

      较便宜,电消耗量低

      Cheaper, lower power consumption

      测量准确度

      Measurement

      accuracy

      较高(长半衰期放射性核素)

      High (long half-life radionuclides)

      高(长、短半衰期放射性核素)

      High (long and short half-life radionuclides)

      适用范围

      Scope of application

      长半衰期核素

      Long half-life nuclides

      短、长半衰期核素

      Short and long half-life nuclides

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    Jin XU, Feng CHENG, Xiaoxiang JIN. Rapid determination of radionuclides by gamma spectrometry in biological samples using a microwave pretreatment technique[J]. Journal of Radiation Research and Radiation Processing, 2023, 41(6): 060702

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    Paper Information

    Category: Research Articles

    Received: Jun. 30, 2023

    Accepted: Aug. 7, 2023

    Published Online: Jan. 3, 2024

    The Author Email: CHENG Feng (成丰)

    DOI:10.11889/j.1000-3436.2023-0054

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