• Journal of Radiation Research and Radiation Processing
  • Vol. 41, Issue 6, 060702 (2023)
Jin XU1, Feng CHENG2,*, and Xiaoxiang JIN2
Author Affiliations
  • 1CGN Huizhou Nuclear Power Co., Ltd., Huizhou 516353, China
  • 2Yangjiang Nuclear Power Co., Ltd., Yangjiang 529941, China
  • show less
    DOI: 10.11889/j.1000-3436.2023-0054 Cite this Article
    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 Copy Citation Text show less
    Flowchart of analysis of γ radionuclides by gamma spectrometry in biological samples
    Fig. 1. Flowchart of analysis of γ radionuclides by gamma spectrometry in biological samples
    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 1. Heating parameters of microwave apparatus

    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 2. Comparison of pre-treatment speed between the two methods
    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 3. Results of recoveries test

    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 4. Comparison of analysis results of two methods

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

    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 6. Results of waste gas detection

    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

    Table 7. Comparison of two pre-treatment methods
    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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