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

Jin XU; Feng CHENG; Xiaoxiang JIN

doi:10.11889/j.1000-3436.2023-0054

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

105

150

180

240

280

300

350

360

380

1 800~4 800

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Chicken

8.23

6.40

6.11

淡水鱼

Freshwater fish

10.8

10.2

10.0

海鱼Sea fish

9.70

12.2

11.7

海虾Sea shrimp

10.5

17.4

13.6

青口Mussel

7.55

17.4

16.6

牡蛎Oysters

13.0

6.66

6.92

紫菜Laver

11.4

6.08

5.38

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

⁵⁴Mn

430.7

388.4

424.7

90.2

98.6

4.47

⁵⁷Co

82.10

91.26

95.04

111

116

2.03

⁶⁰Co

622.5

644.4

641.8

104

103

0.20

⁶⁵Zn

1178

1263

1282

107

109

0.76

¹⁰⁹Cd

1763

1761

100

99.9

0.01

¹³⁷Cs

429.0

373.3

374.7

87.0

87.3

0.18

²⁴¹Am

170.6

169.3

168.3

99.2

98.7

0.29

¹³⁹Ce

99.94

104.3

91.46

104

91.5

6.54

样品类型

Sample type

制样方法

Preparation method

核素（鲜重）/ (Bq·kg^-1)

Nuclide (fresh weight)

⁷Be

⁵⁴Mn

⁵⁸Co

⁶⁰Co

^110mAg

¹³⁴Cs

¹³⁷Cs

⁴⁰K

²²⁶Ra

²³²Th

²³⁸U

鸡

Chicken

<0.056

<0.008

<0.011

<0.007

0.014

62.3

0.055

<0.023

<0.307

<0.057

<0.009

<0.008

<0.010

<0.007

0.016

63.4

0.041

<0.024

<0.309

C / %

6.67

0.88

14.6

<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

<0.088

<0.016

<0.015

<0.023

<0.013

<0.011

0.036

93.9

<0.029

<0.040

<0.121

<0.092

<0.016

<0.024

<0.013

<0.011

0.035

96.2

<0.025

<0.040

<0.125

C / %

1.41

1.21

<0.027

<0.004

<0.006

<0.004

<0.003

<0.004

<0.120

<0.010

<0.014

<0.026

海鱼

Sea fish

<0.107

<0.019

<0.027

<0.016

<0.014

0.030

120

<0.029

<0.047

<0.145

<0.098

<0.018

<0.027

<0.014

<0.013

0.030

117

<0.027

<0.044

<0.138

C / %

0.00

1.27

<0.030

<0.005

<0.004

<0.006

<0.004

<0.005

<0.133

<0.011

<0.015

<0.028

海虾

Sea shrimp

<0.126

<0.021

<0.022

<0.031

<0.018

<0.015

0.026

77.8

0.099

0.101

<0.159

<0.097

<0.017

<0.016

<0.024

<0.014

<0.012

0.023

63.5

0.089

0.075

<0.122

C / %

6.12

10.1

5.32

14.8

<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

<0.099

<0.017

<0.024

<0.014

<0.012

<0.018

48.9

0.151

0.104

<0.135

<0.099

<0.018

<0.016

<0.023

<0.014

<0.013

<0.018

50.0

0.130

0.107

<0.130

C / %

1.11

7.47

1.42

<0.039

<0.006

<0.005

<0.008

<0.005

<0.006

<0.171

<0.014

<0.020

<0.037

牡蛎

Oysters

<0.051

<0.008

<0.011

<0.007

<0.006

<0.008

19.9

0.055

0.111

0.393

<0.047

<0.008

<0.007

<0.011

<0.006

<0.008

24.5

0.045

0.109

0.346

C / %

10.4

10.0

0.91

6.36

<0.023

<0.004

<0.003

<0.005

<0.003

<0.004

<0.099

<0.008

<0.011

<0.021

紫菜

Laver

<0.036

<0.005

<0.007

<0.005

<0.004

<0.005

33.1

0.061

0.093

<0.388

<0.039

<0.006

<0.005

<0.007

<0.005

<0.006

38.9

0.059

0.094

<0.454

C / %

8.06

1.67

0.53

<0.026

<0.004

<0.005

<0.004

<0.003

<0.004

<0.108

<0.009

<0.013

<0.026

样品类型

Sample type

放射性核素 Radionuclide

⁷Be

⁵⁴Mn

⁵⁸Co

⁶⁰Co

^110mAg

¹³⁴Cs

¹³⁷Cs

⁴⁰K

²²⁶Ra

²³²Th

²³⁸U

鸡Chicken

0.98

0.89

1.00

1.10

1.00

0.88

0.98

1.34

0.96

0.99

淡水鱼Freshwater fish

1.05

1.00

1.07

1.04

1.00

0.97

1.02

0.86

1.00

1.03

海鱼Sea fish

1.09

1.06

1.00

1.14

1.08

1.00

1.03

1.07

1.05

海虾Sea shrimp

1.30

1.24

1.38

1.29

1.25

1.13

1.23

1.11

1.35

1.30

青口Mussel

1.00

1.06

0.94

0.96

1.00

1.08

1.00

1.02

0.86

1.03

0.96

牡蛎Oysters

1.09

1.00

1.14

1.00

1.17

1.00

0.81

1.22

1.02

1.14

紫菜Laver

0.92

0.83

1.00

0.80

0.83

0.85

1.03

0.99

0.85

平均值Mean value(

{\bar{x}}_{A / B}

)

1.06

1.01

1.08

1.06

1.09

1.03

0.97

0.99

1.07

1.06

1.05

标准偏差

Standard deviation（S）

0.11

0.12

0.13

0.10

0.11

0.12

0.09

0.13

0.16

0.12

0.13

t值 t-Value (t_A/B)

1.22

0.19

1.40

1.20

1.79

0.54

0.67

0.14

0.99

1.07

0.81

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

苯

Benzene

<0.004

合格

Pass

氨

Ammonia

0.023

4.9

合格Pass

甲苯

Toluene

0.273

合格

Pass

三甲胺

Trimethylamine

<1.0×10^-3

0.54

合格Pass

对二甲苯

Paraxylene

<0.009

合格

Pass

硫化氢

Hydrogen sulfide

<1.7×10^-6

0.33

合格Pass

间二甲苯

M-xylene

<0.009

合格

Pass

甲硫醇

Methyl mercaptan

<4.3×10^-6

0.04

合格Pass

邻二甲苯

O-xylene

<0.004

合格

Pass

甲硫醚

Methyl sulfide

<1.7×10^-4

0.33

合格Pass

甲醛

Formaldehyde

<0.025

合格

Pass

二甲二硫

Dimethyl disulfide

<3.5×10^-6

0.43

合格Pass

非甲烷总烃

NMHC

84.6

120

合格

Pass

二硫化碳

Carbon disulfide

<2.6×10^-4

1.5

合格Pass

臭气浓度(无量纲)

Odor concentration

(dimensionless)

741

2 000

合格

Pass

苯乙烯

Styrene

1.1×10^-3

6.5

合格Pass

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)

无

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

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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