主题:【第十届原创】葡萄酒中稀土元素的测定

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葡萄酒中稀土元素的测定



摘要:选用三种典型葡萄酒(红葡萄酒、白葡萄酒和起泡酒),采用湿法消解进行样品前处理,用ICP-MS对其中的稀土元素进行测定,各元素的检出限分别为La 0.0028 μg/L、Ce0.0034μg/L、Y 0.0018 μg/L、Pr 0.0010 μg/L、Nd  0.0037 μg/L、Sm 0.0026 μg/L、Eu 0.0009 μg/L、Gd 0.0019 μg/L、Tb 0.0004 μg/L、Dy 0.0011 μg/L、Ho 0.0003 μg/L、Er 0.0012 μg/L、Tm 0.0003 μg/L、Yb 0.0010 μg/L、Lu 0.0003 μg/L、Ge 0.0065 μg/L、Sc 0.2431 μg/L,三类葡萄酒样品进行三个水平添加回收率在92.0%-106.3%之间;相对标准偏差在0.49%-8.60%之间。本方法快速准确,可用于葡萄酒稀土元素的测定。
关键词:葡萄酒稀土 ICP-MS
稀土元素是指元素周期表中原子序数57-71的15种元素以及钪(Sc)和钇(Y)共17种元素。我国是稀土储藏、生产及应用大国,葡萄种植土壤中会有一定量的稀土元素,同时由于稀土元素对植物的生长具有促进作用,被广泛运用到种植业,通过植物迁移作用,进入到植物体内,葡萄酒通过葡萄酿制而成,酿酒葡萄受到品种、土壤、气候以及所施肥料的影响,其元素特性会迁入到葡萄酒中,再加上葡萄酒的酿制过程需要用到硅藻土等,也会带进无机元素,有研究表明葡萄酒中稀土元素含量具有表征其地理标志的作用。
随着电感耦合等离子体质谱仪不断迅速发展,凭借其背景低,灵敏度高的特点,样品经直接消解进入检测系统,不需要富集分离就可达到ppd级的检出限,在稀土元素的检测中独居鳌头,难以替代。我们在葡萄酒的检测过程中研究建立了葡萄酒稀土检测的电感耦合等离子体质谱法,不仅能为葡萄酒中影响人体健康的稀土元素含量提供有效的检测结果,同时检测结果还可以为葡萄酒地理标志乃至于甄别其真假提供数据依据。
实验部分
1、 实验材料
1.1  葡萄酒样品 市售红葡萄酒、白葡萄酒、起泡酒
1.2  试剂:硝酸(优级纯);
稀土元素标准溶液(100mg/L)(加拿大SCP分公司)
铑元素标准储备液(1000mg/L)(加拿大SCP分公司)
1.3  仪器:电感耦合等离子体质谱仪ELAN DRC-e美国PE公司
2方法的建立
  2.1前处理方法的选择及优化
2.1.1消解方式的选择
参考相关葡萄酒元素测定以及植物性食品稀土元素检测的样品处理方式,针对葡萄酒含有酒精和其他有机质的特点,主要是从消除酒精,消化有机质两方面重点切入。参照葡萄酒中元素检测的前处理方法(GB/T15038-2006 葡萄酒、果酒通用分析方法中铜、铁测定的处理方法,直接稀释法和酸消解法,通过实验我们发现由于葡萄酒基质的影响,直接酸稀释法检测结果不稳定,加标回收率也不理想,如果采用基质匹配法配制标准溶液,难以找到合适的基质,特别是其中的有机质容易在锥上积碳影响仪器的使用寿命和检测的稳定性,选用酸消解法进行样品前处理,结果非常理想,基本消除了基质的影响。(见表1)。
表1 直接酸稀释进样检测和酸消解进样检测结果
 

直接酸稀释进样检测

元素

1

2

3

4

5

平均值

回收率%

RSD%

La

9.15

8.78

9.04

8.35

8.92

8.85

83.33

3.5

Ce

9.78

9.54

9.77

8.92

9.74

9.55

85.21

3.83

Y

10.37

11.12

11.50

11.57

11.39

11.19

100.4

3.35

Pr

8.70

8.56

8.82

8.03

8.70

8.56

84.49

3.65

Nd

9.16

8.94

9.04

8.58

9.27

9.00

85.19

2.94

Sm

9.13

8.82

9.06

8.23

8.74

8.79

85.42

4.05

Eu

8.64

8.70

8.72

8.16

8.71

8.51

85.07

2.79

Gd

9.29

8.37

9.18

8.61

9.33

9.05

89.12

3.47

Tb

9.20

8.96

9.18

8.43

9.17

8.99

89.74

3.61

Dy

9.01

8.84

9.21

8.37

9.21

8.93

87.94

3.90

Ho

9.16

9.13

9.26

8.51

9.28

9.07

90.43

3.51

Er

9.76

9.32

9.64

8.89

9.54

9.28

92.84

3.23

Tm

9.34

9.15

9.38

8.66

9.43

9.16

91.56

3.32

Yb

9.61

9.31

9.37

8.73

9.47

9.13

91.29

3.32

Lu

9.44

9.22

9.29

8.81

9.41

9.19

91.88

2.47

Ge

12.01

11.67

12.05

11.05

11.59

11.47

114.71

3.38

Sc

64.6

64.01

62.67

57.32

61.71

10.13

101.33

28.46

   

酸消解进样检测

元素

1

2

3

4

5

平均值

回收率%

RSD%

La

9.93

10.27

10.62

10.37

10.36

10.31

95.74

2.41

Ce

11.03

11.24

10.51

11.37

10.95

11.02

95.43

2.97

Y

10.98

11.21

11.03

11.28

11.38

11.18

99.82

1.51

Pr

9.90

9.94

10.11

10.13

10.25

10.06

98.95

1.44

Nd

9.85

10.29

10.23

10.16

10.31

10.13

95.28

1.83

Sm

9.81

10.12

10.31

10.20

10.14

10.17

98.85

1.84

Eu

9.67

9.97

9.85

10.00

9.56

9.81

97.49

1.92

Gd

9.75

10.15

10.11

10.32

9.99

10.06

98.90

2.11

Tb

9.86

10.28

10.26

9.92

10.08

10.08

100.46

1.88

Dy

10.33

10.48

10.31

10.12

10.20

10.29

101.17

0.135

Ho

9.68

10.22

10.13

10.04

9.84

9.98

99.44

2.22

Er

9.83

10.39

9.96

10.02

10.13

10.07

99.27

2.10

Tm

9.84

10.04

10.04

9.97

10.00

9.98

99.55

0.85

Yb

9.36

9.88

9.84

9.92

10.02

9.80

96.52

2.61

Lu

9.80

10.06

10.08

10.09

10.04

10.01

99.85

1.24

Ge

9.31

9.40

9.80

9.56

9.50

9.51

95.00

1.94

Sc

8.91

9.74

9.84

9.15

9.30

9.39

93.88

4.19


2.1.2消解试剂的选择
参照GB 5009.94-2012 植物性食品中稀土元素的测定中样品处理方法,结合葡萄酒的特殊性,如果直接用酸进行消解,由于酒精的存在,会使反应异常剧烈,因此我们选择在100℃(酒精沸点78.3℃)进行低温加热挥发,待溶液挥发三分之二后,冷却加酸消解。
硝酸是一种强氧化性酸,为食品无机分析最主要的消解试剂,可以有效的分解大多数食品样品,目前成为较好的食品消解试剂,同时,由于其产生的质谱干扰小,被认为是ICP-MS分析最好的酸介质,因此,我们选取硝酸作为消解酸。检测中未发现酸介质干扰。
2.4 消解试剂用量的选择
我们本着保证完全消解样品,尽量减少消解试剂用量的原则,结合其他方法选用的试剂用量,分别选取0mL、3mL、5mL、8mL和10mL对添加量10μg/L的样品进行进行实验,结果见表2。
表2 硝酸用量对检测的影响
 

元素

 

硝酸用量

 

红葡萄酒

 

白葡萄酒

 

起泡酒

含量(μg/L)

回收率

含量(μg/L)

回收率

含量(μg/L)

回收率

 

La

0mL

9.021

82.8

9.211

83.1

10.27

94.4

3mL

10.551

98.1

11.023

101.2

10.87

100.4

5mL

10.362

96.2

11.017

101.2

10.726

99.0

8mL

10.246

95.1

10.989

100.9

10.753

99.2

10mL

10.328

95.9

10.966

100.7

10.733

99.0

 

Ce

0mL

10.311

88.3

10.16

79.3

10.98

92.2

3mL

11.385

99.1

12.135

99.1

11.373

96.1

5mL

11.274

97.9

12.126

99.0

11.59

98.3

8mL

11.032

95.5

12.093

98.6

11.663

99.0

10mL

11.221

97.4

12.119

98.9

11.594

98.3

 

Y

0mL

10.349

91.6

12.55

105.1

11.72

101.4

3mL

10.922

97.3

12.101

100.6

11.692

101.1

5mL

10.857

96.7

12.028

99.9

11.523

99.4

8mL

10.963

97.7

12.022

99.8

11.533

99.5

10mL

10.951

97.6

12.029

99.9

11.551

99.7

 

Pr

0mL

8.611

78.7

8.89

79.9

9.77

95.7

3mL

9.090

83.5

9.976

90.8

10.052

98.5

5mL

10.142

94.0

10.017

91.2

10.036

98.4

8mL

10.287

95.5

10.023

91.2

10.044

98.4

10mL

10.203

94.6

10.019

91.2

10.029

98.3

 

Nd

0mL

9.541

89.2

9.541

84.6

10.217

93.7

3mL

10.444

98.2

11.034

99.5

10.454

96.0

5mL

10.536

99.2

11.062

99.8

10.615

97.7

8mL

10.623

100.0

11.073

99.9

10.739

98.9

10mL

10.579

99.6

11.029

99.5

10.626

97.8

 

Sm

0mL

9.342

91.1

9.032

87.6

8.891

86.9

3mL

10.521

102.9

10.033

97.6

9.799

96.0

5mL

10.090

98.6

10.124

98.5

9.853

96.5

8mL

10.111

98.8

10.372

101.0

9.692

94.9

10mL

10.185

99.6

10.195

99.3

9.781

95.8

 

Eu

0mL

8.864

88.0

8.793

87.4

9.581

92.4

3mL

10.020

99.6

9.798

97.5

10.011

96.7

5mL

10.070

100.1

9.664

96.1

9.969

96.3

8mL

10.110

100.5

9.821

97.7

9.953

96.1

10mL

9.560

95.0

9.563

95.1

9.972

96.3

 

Gd

0mL

9.560

93.8

9.62

93.3

9.38

91.3

3mL

10.230

100.5

10.176

98.9

10.126

98.8

5mL

10.090

99.1

10.126

98.4

10.098

98.5

8mL

10.170

99.9

10.203

99.1

10.158

99.1

10mL

10.380

102.0

10.225

99.4

10.244

99.9

 

Tb

0mL

9.150

91.2

8.376

83.4

8.011

79.9

3mL

10.270

102.4

10.008

99.7

9.852

98.3

5mL

10.190

101.6

9.793

97.5

9.962

99.4

8mL

10.130

101.0

9.991

99.5

9.754

97.3

10mL

10.050

100.2

9.855

98.2

9.822

98.0

 

Dy

0mL

9.140

89.7

9.69

94.1

9.25

90.4

3mL

10.570

104.0

10.191

99.1

10.199

99.9

5mL

10.460

102.9

10.232

99.5

10.18

99.7

8mL

10.330

101.6

10.263

99.8

10.262

100.5

10mL

10.450

102.8

10.241

99.6

10.269

100.6

 

Ho

0mL

9.100

90.6

9.522

94.6

9.181

91.4

3mL

10.210

101.7

10.021

99.6

10.008

99.7

5mL

10.100

100.6

10.173

101.1

10.026

99.9

8mL

10.150

101.1

10.192

101.3

10.031

99.9

10mL

10.060

100.2

10.202

101.4

10.028

99.9

 

Er

0mL

9.150

90.1

9.79

95.5

9.38

92.2

3mL

10.120

99.8

10.185

99.5

10.091

99.3

5mL

10.050

99.1

10.199

99.6

10.122

99.6

8mL

9.870

97.3

10.204

99.6

10.131

99.7

10mL

10.000

98.6

10.115

98.8

10.155

100.0

 

Tm

0mL

9.110

90.9

9.6

95.7

9.25

92.3

3mL

10.200

101.8

9.973

99.4

10.003

99.8

5mL

9.970

99.5

10.021

99.9

9.945

99.3

8mL

9.880

98.6

10.121

100.9

9.765

97.5

10mL

9.930

99.1

10.104

100.7

9.832

98.1

 

Yb

0mL

9.020

88.6

9.5

91.8

9.26

90.4

3mL

10.020

98.6

9.983

96.6

9.823

96.0

5mL

9.860

97.0

10.155

98.4

9.996

97.8

8mL

9.950

97.9

10.282

99.6

10.125

99.1

10mL

9.830

96.7

10.102

97.8

10.062

98.4

 

Lu

0mL

9.216

91.9

9.135

91.0

9.28

92.5

3mL

9.750

97.2

9.936

99.0

10.002

99.7

5mL

10.037

100.1

9.821

97.8

9.933

99.0

8mL

10.063

100.3

9.885

98.5

9.985

99.6

10mL

10.131

101.0

10.011

99.7

9.878

98.5

 

Ge

0mL

8.943

89.2

9.54

93.8

9.24

90.0

3mL

9.667

96.5

10.083

99.2

10.255

100.2

5mL

9.770

97.5

9.992

98.3

10.236

100.0

8mL

9.823

98.0

10.122

99.6

10.139

99.0

10mL

9.452

94.3

10.093

99.3

10.131

98.9

 

Sc

0mL

60.230

基体干扰大

56.69

基体干扰大

61.91

基体干扰大

3mL

9.537

95.4

16.047

110.4

12.239

101.4

5mL

9.862

98.6

15.136

101.3

12.011

99.1

8mL

9.655

96.6

15.063

100.5

12.025

99.3

10mL

9.780

97.8

15.069

100.6

12.113

100.1


从实验中可以看出,不加入酸,检测回收率差于加酸消解,3-10mL硝酸量相对于本实验选取的样品,回收率影响不大,通过本实验结合其他标准方法选取的消解试剂用量,我们选取5mL硝酸作为消解样品消解液的用量。酒精挥发酸消解相对于有文献报道的微波消解方法,我们认为更具安全性,在时效上也不输于微波消解法,是一种更经济适用的样品处理方法。通过实验证明,方法的回收率和稳定性都非常理想。
3.1仪器测定条件
    按照仪器操作规程用多元素调谐液优化仪器,使其背景值、稳定性、氧化物、双电荷、灵敏度、分辨率等参数达到仪器要求。
    使用稀土标准溶液优化雾化器流量、RF功率。我们使用的仪器分析条件为射频功率1500W;等离子气流量载气流量为0.94L/min;辅助器流量为1.2L/min;等离子气流量为15L/min,;透镜电压5.5V,采样流量0.8mL/min。
3.2 基体干扰及消除
    机体干扰主要来源于样品的机体,对待测元素产生增强或抑制作用,产生系统偏差。选择适当的内标元素能有效的克服机体效应,内标元素选择我们遵循:样品中不含的元素;不受样品中基体及分析物的干扰;与待测元素质量相近电离能相近原则。在常作为内标元素的元素中我们选取Rh 的质量数为103电离能为719.7与大部分稀土元素质量数和电离能相近,作为内标元素。
4方法的线性范围、回归方程与定量限
4.1线性范围和回归方程和方法的定量限
    将仪器调整至最佳状态,分别测定空白溶液、标准系列溶液(0μg/L、0.5μg/L、1.0μg/L、2.0μg/L、5.0μg/L、10.0μg/L、25.0μg/L、50.0μg/L)得到线性方程的相关系数、检出限、定量限。其中检出限为实际流程空白连续测定10次的响应值3倍标准偏差所对应的的浓度值,定量限为10倍标准偏差对应的浓度值(见表3)。
表3 线性范围、相关系数、检出限

元素

线性范围(μg/L)

相关系数

溶液检出限μg/L

溶液定量限μg/L

139La

0-50

0.999941

0.0028

0.01

140Ce

0-50

0.999986

0.0034

0.01

89Y

0-50

0.999931

0.0018

0.01

141Pr

0-50

0.999951

0.0010

0.01

142Nd

0-50

0.999883

0.0037

0.01

152Sm

0-50

0.999739

0.0026

0.01

153Eu

0-50

0.999913

0.0009

0.01

158Gd

0-50

0.999949

0.0019

0.01

159Tb

0-50

0.999899

0.0004

0.01

164Dy

0-50

0.999920

0.0011

0.01

165Ho

0-50

0.999891

0.0003

0.01

166Er

0-50

0.999935

0.0012

0.01

169Tm

0-50

0.999923

0.0003

0.01

174Yb

0-50

0.999960

0.0010

0.01

175Lu

0-50

0.999851

0.0003

0.01

74Ge

0-50

0.999899

0.0065

0.02

45Sc

0-50

0.999793

0.2431

1.00


方法的定量限由溶液定量限以及样品取样量和最后稀释体积计算得出。
4.3检测方法精密度和回收率验证
采用三类样品加标回收来考察方法的准确性,每个加标水平平行测定10次考察方法的精密度,检验结果见表4。三类所有元素三个添加水平的回收率平均值在92.0%-106.3%之间;相对标准偏差在0.49%-8.60%之间。
表4 -1红葡萄酒加标回收和精密度实验

0.

 

元素

 

样品

 

添加水平

 

1(μg/L)

 

10(μg/L)

 

40(μg/L)

测定值

测定值

回收率

测定值

回收率

测定值

回收率

 

La

0.725

1.712

97.4

10.576

98.4

40.694

99.9

0.784

1.800

106.2

11.012

102.7

40.704

99.9

0.692

1.756

101.8

11.460

107.2

41.710

102.4

0.676

1.722

98.4

11.371

106.3

40.952

100.5

0.800

1.703

106.5

11.303

105.6

40.167

98.6

0.736

1.795

105.7

11.116

103.7

41.021

100.7

0.729

1.753

101.5

10.940

102.1

39.663

97.3

0.736

1.713

97.5

10.763

100.2

39.434

96.7

0.745

1.783

104.5

10.895

101.5

39.772

97.6

0.755

1.755

101.7

10.722

99.9

39.567

97.1

平均值

0.738

1.789

102.1

11.016

102.8

40.368

99.1

RSD%

 

2.28

 

2.66

 

1.88

 
 

Ce

1.524

2.456

97.6

11.18

97.0

39.872

96.0

1.476

2.552

107.2

11.624

101.4

38.872

93.5

1.384

2.572

109.2

11.912

104.3

40.056

96.4

1.536

2.577

109.7

11.823

103.4

39.962

96.2

1.564

2.473

99.3

11.767

102.9

39.933

96.1

1.502

2.601

112.1

11.441

99.6

39.858

95.9

1.535

2.581

110.1

11.502

100.2

39.776

95.7

1.503

2.532

105.2

11.322

98.4

39.895

96.0

1.428

2.538

105.8

11.531

100.5

39.622

95.4

1.352

2.522

104.2

11.620

101.4

39.599

95.3

平均值

1.480

2.560

106.2

11.572

100.9

39.745

95.7

RSD%

 

2.46

 

1.96

 

0.85

 
 

Y

1.272

2.124

93.0

11.116

99.2

40.634

98.6

1.176

2.196

100.2

11.748

105.5

39.632

96.1

1.168

2.336

114.2

11.58

103.9

40.744

98.9

1.160

2.253

105.9

11.597

104.0

39.693

96.2

1.132

2.265

107.1

11.466

102.7

39.701

96.3

1.179

2.167

97.3

11.325

101.3

40.557

98.4

1.236

2.199

100.5

11.202

100.1

40.622

98.6

1.193

2.148

95.4

11.684

104.9

40.456

98.1

1.216

2.235

104.1

11.529

103.3

39.852

96.6

1.203

2.263

106.9

11.561

103.8

40.236

97.6

平均值

1.194

2.219

102.5

11.481

102.9

40.213

97.5

RSD% 

2.88

 

1.79

 

1.11

 
 

Pr

0.168

1.152

98.4

9.860

96.9

39.264

97.7

0.168

1.208

104

10.180

100.1

38.396

95.6

0.156

1.252

108.4

10.576

104.1

39.668

98.8

0.180

1.283

111.5

10.366

102.0

39.785

99.0

0.160

1.291

112.3

10.323

101.6

39.996

99.6

0.173

1.188

102.0

10.115

99.5

40.037

99.7

0.179

1.181

101.3

10.173

100.1

40.122

99.9

0.168

1.175

100.7

10.028

98.6

39.237

97.7

0.155

1.163

99.5

9.965

98.0

39.899

99.3

0.168

1.204

103.6

10.205

100.4

39.109

97.4

平均值

0.168

1.210

104.2

10.179

100.1

39.551

98.5

RSD% 

4.07

 

2.04

 

1.38

 
 

Nd

0.660

1.576

95.5

10.292

96.7

39.016

96.0

0.644

1.56

93.9

10.928

103.1

38.528

94.8

0.624

1.696

107.5

10.872

102.5

39.264

96.6

0.632

1.655

103.4

10.697

100.8

39.736

97.8

0.536

1.693

107.2

10.736

101.2

39.569

97.4

0.622

1.576

95.5

10.885

102.6

39.245

96.6

0.597

1.593

97.2

10.264

96.4

38.994

95.9

0.603

1.498

87.7

10.794

101.7

39.982

98.4

0.647

1.594

97.3

10.362

97.4

39.391

96.9

0.640

1.611

99.0

10.697

100.8

38.936

95.8

平均值

0.621

1.605

98.4

10.653

100.3

39.266

96.6

RSD% 

3.83

 

2.37

 

1.08

 
 

Sm

0.224

1.224

99.2

10.040

98.1

38.463

95.6

0.236

1.188

95.6

10.352

101.2

37.629

93.5

0.200

1.288

105.6

10.540

103.1

38.794

96.4

0.264

1.233

100.1

10.311

100.8

39.262

97.6

0.252

1.262

103.0

10.326

100.9

39.553

98.3

0.232

1.306

107.4

10.175

99.4

39.765

98.8

0.248

1.119

88.7

10.239

100.1

39.331

97.7

0.217

1.169

93.7

10.463

102.3

38.545

95.8

0.211

1.230

99.8

10.174

99.4

38.465

95.6

0.231

1.233

100.1

10.311

100.8

38.328

95.2

平均值

0.232

1.225

99.3

10.293

100.6

38.814

96.5

RSD%

 

4.54

 

1.41

 

1.69

 
 

Eu

0.072

1.108

104.5

9.736

96.7

39.42

98.4

0.068

1.092

102.9

10.032

99.7

38.852

97.0

0.056

1.120

105.7

9.916

98.5

39.356

98.2

0.056

1.102

103.9

9.895

98.3

38.876

97.0

0.060

1.092

102.9

9.996

99.3

38.667

96.5

0.065

1.085

102.2

9.945

98.8

38.974

97.3

0.063

1.099

103.6

10.009

99.5

39.221

97.9

0.059

1.107

104.4

10.022

99.6

39.376

98.3

0.065

1.111

104.8

10.053

99.9

39.152

97.7

0.070

1.062

99.9

9.798

97.4

38.262

95.5

平均值

0.063

1.098

103.5

9.940

98.8

39.016

97.4

RSD%

 

1.48

 

1.06

 

0.94

 
 

Gd

0.172

1.196

101.6

9.924

97.4

39.168

97.5

0.176

1.204

102.4

10.32

101.4

38.792

96.5

0.156

1.192

101.2

10.288

101.1

39.332

97.9

0.192

1.197

101.7

10.177

100.0

39.097

97.3

0.206

1.189

100.9

10.105

99.3

39.665

98.7

0.195

1.178

99.8

10.112

99.3

39.926

99.4

0.186

1.193

101.3

10.096

99.2

39.453

98.2

0.178

1.165

98.5

10.052

98.7

39.282

97.8

0.169

1.21

103.0

10.136

99.6

38.955

96.9

0.174

1.197

101.7

10.177

100.0

39.097

97.3

平均值

0.180

1.192

101.2

10.139

99.6

39.277

97.7

RSD%

 

1.07

 

1.12

 

0.86

 
 

Tb

0.032

1.016

98.4

9.892

98.6

39.116

97.7

0.036

1.036

100.4

10.312

102.8

37.576

93.8

0.032

1.108

107.6

10.288

102.6

39.492

98.6

0.032

1.042

101.0

10.160

101.3

38.728

96.7

0.028

1.053

102.1

10.055

100.2

38.662

96.6

0.037

1.072

104.0

10.017

99.9

38.451

96.0

0.029

1.044

101.2

10.561

105.3

38.785

96.9

0.035

1.021

98.9

10.688

106.6

38.412

95.9

0.033

1.036

100.4

10.028

100.0

39.262

98.1

0.029

1.102

107.0

9.795

97.6

38.565

96.3

平均值

0.032

1.053

102.1

10.180

101.5

38.705

96.7

RSD%

 

3.00

 

2.80

 

1.38

 
 

Dy

0.148

1.240

107.4

10.504

103.4

40.039

99.7

0.180

1.240

107.4

10.652

104.9

39.672

98.8

0.168

1.248

108.2

10.480

103.1

39.960

99.5

0.192

1.243

107.7

10.535

103.7

39.899

99.3

0.148

1.252

108.6

10.526

103.6

39.388

98.1

0.163

1.251

108.5

10.497

103.3

39.545

98.4

0.156

1.264

109.8

10.433

102.7

39.852

99.2

0.162

1.282

111.6

10.520

103.5

39.876

99.3

0.175

1.236

107.0

10.531

103.7

39.774

99.0

0.172

1.233

106.7

10.62

104.5

39.982

99.5

平均值

0.166

1.249

108.3

10.530

103.6

39.799

99.1

RSD%

 

1.18

 

0.58

 

0.49

 
 

Ho

0.04

1.068

102.7

9.72

96.8

39.904

99.7

0.04

1.06

101.9

10.264

102.2

38.932

97.2

0.04

1.096

105.5

10.172

101.3

39.736

99.2

0.036

1.085

104.4

10.092

100.5

39.224

98.0

0.044

1.08

103.9

10.085

100.4

39.392

98.4

0.042

1.077

103.6

10.117

100.8

38.736

96.7

0.041

1.072

103.1

10.231

101.9

38.958

97.3

0.045

1.064

102.3

10.005

99.6

39.285

98.1

0.041

1.059

101.8

9.956

99.2

39.753

99.3

0.037

1.066

102.5

9.785

97.4

39.262

98.0

平均值

0.041

1.073

103.2

10.043

100.0

39.318

98.2

RSD%

 

1.10

 

1.70

 

0.93

 
 

Er

0.128

1.116

97.3

9.968

98.25

39.948

99.5

0.152

1.220

107.7

10.532

103.89

39.612

98.6

0.140

1.180

103.7

10.104

99.61

39.952

99.5

0.140

1.172

102.9

10.201

100.58

39.437

98.2

0.142

1.169

102.6

10.017

98.74

39.342

98.0

0.147

1.165

102.2

10.121

99.78

38.947

97.0

0.147

1.168

102.5

10.136

99.93

39.375

98.1

0.145

1.175

103.2

10.362

102.19

39.221

97.7

0.136

1.106

96.3

10.452

103.09

38.568

96.1

0.150

1.112

96.9

10.111

99.68

39.026

97.2

平均值

0.143

1.158

101.5

10.200

100.6

39.343

98.0

RSD%

 

3.11

 

1.83

 

1.10

 
 

Tm

0.024

1.004

98.0

9.860

98.36

39.624

99.0

0.020

1.044

102.0

10.06

100.36

38.132

95.3

0.020

1.08

105.6

10.068

100.44

39.504

98.7

0.025

1.043

101.9

9.996

99.72

39.087

97.7

0.023

1.026

100.2

10.022

99.98

38.94

97.3

0.022

1.056

103.2

10.056

100.32

37.96

94.8

0.025

1.043

101.9

10.011

99.87

38.81

97.0

0.027

1.031

100.7

10.019

99.95

39.03

97.5

0.025

1.053

102.9

10.035

100.11

39.56

98.8

0.024

1.029

100.5

10.023

99.99

39.25

98.1

平均值

0.024

1.041

101.7

10.015

99.91

38.990

97.4

RSD%

 

1.96

 

0.59

 

1.46

 
 

Yb

5

      

0.184

1.184

102.0

10.032

98.7

38.764

96.5

0.148

1.256

109.2

9.992

98.3

38.572

96.0

0.148

1.180

101.6

9.877

97.1

38.596

96.1

0.172

1.166

100.2

9.820

96.6

38.647

96.2

0.165

1.141

97.7

9.955

97.91

37.904

94.4

0.158

1.138

97.4

9.895

97.31

37.771

94.0

0.177

1.133

96.9

9.936

97.72

38.562

96.0

0.162

1.151

98.7

9.977

98.13

38.455

95.7

0.159

1.162

99.8

9.997

98.33

38.326

95.4

平均值

0.164

1.161

99.71

9.900

97.36

38.405

95.6

RSD%

 

3.57

 

1.51

 

0.84

 
 

Lu

0.028

1.032

100.3

9.824

98.0

38.288

95.6

0.028

1.004

97.5

10.092

100.6

38.244

95.5

0.036

1.084

105.5

10.112

100.8

39.344

98.3

0.024

1.040

101.1

10.009

99.8

38.959

97.3

0.032

1.023

99.4

10.005

99.8

38.304

95.7

0.030

1.019

99.0

9.996

99.7

38.566

96.3

0.026

1.028

99.9

9.983

99.5

38.852

97.1

0.029

1.033

100.4

10.052

100.2

39.078

97.6

0.029

1.049

102.0

10.066

100.4

39.263

98.1

0.031

1.052

102.3

10.043

100.1

39.223

98.0

平均值

0.029

1.036

100.7

10.018

99.9

38.812

97.0

RSD%

 

2.11

 

0.80

 

1.11

 
 

Ge

0.012

0.956

93.6

9.324

93.0

37.124

92.8

0.023

0.928

90.8

9.412

93.9

36.400

91.0

0.020

1.040

102.0

9.808

97.9

36.656

91.6

0.024

0.975

95.5

9.598

95.8

36.925

92.3

0.016

0.966

94.6

9.685

96.7

36.706

91.7

0.020

0.973

95.3

9.785

97.7

36.765

91.9

0.021

0.952

93.2

9.803

97.8

37.235

93.0

0.018

0.944

92.4

9.660

96.4

37.126

92.8

0.022

0.948

92.8

9.326

93.1

36.895

92.2

0.021

0.965

94.5

9.455

94.4

36.563

91.4

平均值

0.020

0.965

94.5

9.586

95.7

36.840

92.0

RSD%

 

3.12

 

2.01

 

0.73

 
 

Sc

ND

5.012

100.2

9.786

97.9

38.756

96.9

ND

5.101

102.0

9.925

99.3

38.962

97.4

ND

5.006

100.1

10.011

100.1

39.263

98.2

ND

4.956

99.1

10.076

100.8

38.922

97.3

ND

4.768

95.4

10.036

100.4

38.757

96.9

ND

4.899

98.0

10.267

102.7

38.269

95.7

ND

4.929

98.6

10.133

101.3

39.332

98.3

ND

4.957

99.1

10.021

100.2

38.926

97.3

ND

5.111

102.2

9.995

100.0

38.356

95.9

ND

5.286

105.7

9.895

99.0

38.022

95.1

平均值

ND

5.003

100.1

10.015

100.1

38.757

96.9

RSD%

 

0.14

 

0.13

 

0.42

 

表4 -2白葡萄酒加标回收和精密度实验

 

元素

 

样品

 

添加水平

 

1(μg/L)

 

10(μg/L)

 

40(μg/L)

测定值

测定值

回收率

测定值

回收率

测定值

 

回收率

 

La

0.906

1.895

99.5

10.889

99.89

40.299

 

98.5

0.910

1.786

88.6

10.523

96.23

40.383

 

98.7

0.893

1.908

100.8

10.902

100.02

40.766

 

99.7

0.881

1.912

101.2

10.789

98.89

40.932

 

100.1

0.892

1.883

98.3

10.868

99.68

40.263

 

98.4

0.913

1.896

99.6

10.793

98.93

40.252

 

98.4

0.915

1.922

102.2

10.045

91.45

39.836

 

97.3

0.903

1.901

100.1

10.916

100.16

39.966

 

97.7

0.912

1.91

101.0

10.778

98.78

39.942

 

97.6

0.877

1.882

98.2

10.862

99.62

39.981

 

97.7

平均值

0.900

1.890

99.0

10.737

98.4

40.262

 

98.4

RSD%

 

2.04

 

2.50

 

0.90

 
 

Ce

2.124

3.151

92.2

11.939

97.1

39.872

 

94.1

2.276

3.233

100.4

12.022

97.9

39.396

 

92.9

2.384

3.098

86.9

12.152

99.2

39.875

 

94.1

2.211

3.122

89.3

12.566

103.4

40.013

 

94.5

2.528

3.306

107.7

12.461

102.3

40.033

 

94.5

2.088

3.192

96.3

12.066

98.4

40.121

 

94.7

2.106

3.144

91.5

12.269

100.4

40.172

 

94.9

2.233

3.258

102.9

12.453

102.2

39.951

 

94.3

2.159

3.306

107.7

12.373

101.4

39.888

 

94.1

2.185

3.077

84.8

12.019

97.9

39.792

 

93.9

平均值

2.229

3.189

96.0

12.232

100.0

39.911

 

94.2

RSD%

 

2.62

 

1.81

 

0.54

 
 

Y

1.983

2.905

86.5

11.993

99.53

39.634

 

94.0

2.013

3.012

97.2

12.011

99.71

39.866

 

94.6

2.239

2.897

85.7

11.875

98.35

39.532

 

93.7

1.966

2.966

92.6

11.962

99.22

40.127

 

95.2

1.833

3.131

109.1

12.102

100.62

40.059

 

95.0

1.856

3.152

111.2

12.033

99.93

40.166

 

95.3

1.974

3.011

97.1

12.041

100.01

40.072

 

95.1

2.125

2.962

92.2

11.872

98.32

38.252

 

90.5

2.169

2.989

94.9

11.855

98.15

39.771

 

94.3

2.231

2.885

84.5

11.922

98.82

40.052

 

95.0

平均值

2.0389

2.991

95.1

11.967

99.3

39.753

 

94.3

RSD% 

3.06

 

0.70

 

1.43

 
 

Pr

0.219

1.119

86.9

10.091

98.4

39.036

 

97.0

0.237

1.156

90.6

10.235

99.9

38.396

 

95.4

0.241

1.323

107.3

10.363

101.1

38.792

 

96.4

0.301

1.184

93.4

10.161

99.1

39.013

 

96.9

0.322

1.175

92.5

10.202

99.5

39.265

 

97.5

0.282

1.372

112.2

10.012

97.6

38.976

 

96.8

0.209

1.109

85.9

10.173

99.2

39.162

 

97.3

0.237

1.158

90.8

10.266

100.2

39.214

 

97.4

0.255

1.223

97.3

10.137

98.9

39.565

 

98.3

0.218

1.204

95.4

10.159

99.1

39.477

 

98.1

平均值

0.2521

1.2023

95.23

10.1799

99.3

39.090

 

97.1

RSD% 

4.07

 

2.04

  

1.38

 
 

Nd

0.941

1.971

89.1

10.932

98.5

39.145

 

95.2

0.99

2.034

95.4

10.898

98.2

39.033

 

94.9

1.053

2.053

97.3

11.108

100.3

38.796

 

94.3

1.173

2.039

95.9

10.793

97.1

38.665

 

94.0

1.231

2.172

109.2

10.869

97.9

39.215

 

95.3

1.265

2.111

103.1

10.532

94.5

39.552

 

96.2

0.917

1.993

91.3

10.774

96.9

39.368

 

95.7

0.863

2.105

102.5

11.016

99.4

40.023

 

97.4

1.126

2.006

92.6

11.053

99.7

40.055

 

97.4

1.212

2.025

94.5

11.005

99.3

39.757

 

96.7

平均值

1.077

2.051

97.1

10.898

98.2

39.361

 

95.7

RSD% 

3.00

 

1.55

 

1.23

 
 

Sm

0.285

1.211

94.1

10.114

98.44

38.925

 

96.6

0.273

1.193

92.3

10.236

99.66

39.011

 

96.9

0.292

1.206

93.6

10.259

99.89

39.254

 

97.5

0.266

1.239

96.9

10.066

97.96

39.441

 

97.9

0.238

1.262

99.2

9.758

94.88

39.599

 

98.3

0.245

1.273

100.3

10.055

97.85

40.102

 

99.6

0.285

1.282

101.2

10.176

99.06

40.113

 

99.6

0.251

1.301

103.1

10.836

105.66

40.292

 

100.1

0.277

1.264

99.4

9.898

96.28

39.735

 

98.7

0.247

1.197

92.7

10.005

97.35

38.988

 

96.8

平均值

0.266

1.243

97.3

10.140

98.7

39.546

 

98.2

RSD%

 

3.13

 

2.84

  

1.28

 
 

Eu

0.066

1.036

98.6

9.665

96.2

38.663

 

96.5

0.053

1.102

105.2

9.739

96.9

39.787

 

99.3

0.055

1.093

104.3

9.798

97.5

39.594

 

98.9

0.046

1.072

102.2

9.856

98.1

38.838

 

97.0

0.049

1.055

100.5

9.823

97.7

39.271

 

98.1

0.058

1.042

99.2

10.01

99.6

39.146

 

97.7

0.061

1.056

100.6

10.023

99.7

38.889

 

97.1

0.053

1.022

97.2

10.066

100.2

38.564

 

96.3

0.061

1.037

98.7

10.41

103.6

38.248

 

95.5

0.045

1.044

99.4

9.892

98.4

39.229

 

97.9

平均值

0.0547

1.056

100.6

9.93

98.8

39.023

 

97.4

RSD%

 

2.45

 

2.14

  

1.21

 
 

Gd

0.273

1.177

88.8

10.033

97.4

38.557

 

95.7

0.329

1.209

92

10.135

98.5

38.899

 

96.5

0.295

1.235

94.6

10.266

99.8

39.263

 

97.4

0.301

1.293

100.4

10.378

100.9

39.483

 

98.0

0.266

1.326

103.7

10.352

100.6

39.182

 

97.2

0.286

1.348

105.9

10.295

100.1

39.736

 

98.6

0.281

1.198

90.9

10.034

97.4

39.566

 

98.2

0.305

1.347

105.8

10.052

97.6

38.793

 

96.3

0.262

1.202

91.3

10.247

99.6

38.866

 

96.4

0.292

1.363

107.4

10.119

98.3

39.251

 

97.4

平均值

0.289

1.270

98.08

10.191

99.0

39.160

 

97.2

RSD%

 

5.74

 

1.30

  

0.96

 
 

Tb

0.039

1.003

96.3

10.125

100.9

38.662

 

96.6

0.038

1.006

96.6

10.03

99.9

39.263

 

98.1

0.045

1.105

106.5

10.111

100.7

39.134

 

97.7

0.043

1.105

106.5

10.056

100.2

39.026

 

97.5

0.035

1.103

106.3

10.006

99.7

38.775

 

96.8

0.036

1.002

96.2

9.982

99.4

38.528

 

96.2

0.033

1.005

96.5

9.917

98.8

38.962

 

97.3

0.029

1.013

97.3

9.832

97.9

39.261

 

98.1

0.046

1.021

98.1

9.575

95.4

38.864

 

97.1

0.052

1.008

96.8

9.874

98.3

39.423

 

98.5

平均值

0.040

1.037

99.7

9.951

99.1

38.990

 

97.4

RSD%

 

4.50

 

1.64

 

0.74

 
 

Dy

0.269

1.201

92.1

10.308

100.28

39.569

 

98.2

0.283

1.218

93.8

10.402

101.22

39.443

 

97.9

0.267

1.302

102.2

10.451

101.71

38.972

 

96.7

0.303

1.313

103.3

10.127

98.47

39.122

 

97.1

0.326

1.209

92.9

10.188

99.08

39.267

 

97.5

0.291

1.166

88.6

10.263

99.83

39.331

 

97.6

0.282

1.319

103.9

10.317

100.37

38.698

 

96.0

0.303

1.306

102.6

10.294

100.14

38.766

 

96.2

0.262

1.283

100.3

10.311

100.31

39.026

 

96.9

0.253

1.292

101.2

10.262

99.82

39.138

 

97.1

平均值

0.284

1.261

98.09

10.292

100.123

39.133

 

97.1

RSD%

 

4.45

 

0.91

  

0.72

 
 

Ho

0.076

1.092

103.2

9.785

97.25

39.833

 

99.43

0.072

1.113

105.3

9.893

98.33

39.695

 

99.09

0.089

1.069

100.9

9.668

96.08

39.748

 

99.22

0.051

1.053

99.3

9.568

95.08

39.526

 

98.67

0.065

1.08

102

9.975

99.15

38.783

 

96.81

0.046

1.043

98.3

10.063

100.03

38.296

 

95.59

0.059

1.106

104.6

10.005

99.45

38.565

 

96.26

0.066

1.037

97.7

10.012

99.52

38.587

 

96.32

0.062

1.009

94.9

10.126

100.66

39.244

 

97.96

0.049

1.062

100.2

10.201

101.41

39.369

 

98.27

平均值

0.064

1.066

100.6

9.930

98.70

39.1646

 

97.76

RSD%

 

3.05

 

2.03

  

1.43

 
 

Er

0.257

1.143

90.3

10.36

101.2

39.948

 

99.3

0.245

1.135

89.5

10.256

100.2

39.612

 

98.4

0.242

1.188

94.8

10.273

100.3

39.952

 

99.3

0.226

1.236

99.6

10.169

99.3

39.437

 

98.0

0.213

1.247

100.7

10.179

99.4

39.342

 

97.8

0.226

1.316

107.6

10.088

98.5

38.947

 

96.8

0.237

1.126

88.6

10.164

99.2

39.375

 

97.8

0.241

1.269

102.9

10.295

100.6

39.221

 

97.5

0.249

1.115

87.5

10.356

101.2

38.568

 

95.8

0.256

1.217

97.7

10.149

99.1

39.026

 

97.0

平均值

0.239

1.199

95.9

10.229

99.9

39.343

 

97.8

RSD%

 

3.11

 

1.83

  

1.10

 
 

Tm

0.027

1.013

98.3

10.023

99.9

39.352

 

98.3

0.027

1.026

99.6

10.108

100.8

38.966

 

97.3

0.023

1.029

99.9

10.202

101.7

38.973

 

97.4

0.039

1.032

100.2

10.026

100.0

39.02

 

97.5

0.035

1.044

101.4

10.005

99.8

38.794

 

96.9

0.025

1.035

100.5

10.318

102.9

38.735

 

96.8

0.032

1.042

101.2

10.201

101.7

38.926

 

97.2

0.029

1.029

99.9

10.051

100.2

38.783

 

96.9

0.026

1.017

98.7

10.017

99.9

39.261

 

98.1

0.026

1.013

98.3

9.893

98.6

39.177

 

97.9

平均值

0.0289

1.028

99.8

10.084

100.5

38.999

 

97.4

RSD%

  

1.07

 

1.23

 

0.53

 

Yb

0.326

1.193

87.3

10.423

101.03

38.989

 

96.67

0.317

1.295

97.5

10.288

99.68

39.562

 

98.11

0.309

1.196

87.6

10.265

99.45

39.747

 

98.57

0.341

1.259

93.9

10.427

101.07

39.616

 

98.24

0.295

1.356

103.6

10.214

98.94

39.56

 

98.10

0.304

1.402

108.2

10.159

98.39

38.779

 

96.15

0.327

1.371

105.1

10.365

100.45

39.026

 

96.77

0.295

1.366

104.6

10.055

97.35

39.149

 

97.07

0.305

1.251

93.1

10.26

99.4

39.533

 

98.03

0.339

1.178

85.8

10.047

97.27

39.125

 

97.01

平均值

0.316

1.287

96.7

10.250

99.3

39.309

 

97.5

RSD%

 

6.47

 

1.32

  

0.84

 
 

Lu

0.007

1.035

99.5

9.769

97.29

37.986

 

94.9

0.005

1.052

101.2

9.885

98.45

38.211

 

95.4

0.006

1.029

98.9

10.005

99.65

38.363

 

95.8

0.003

1.012

97.2

10.102

100.62

38.569

 

96.3

0.003

1.035

99.5

9.936

98.96

38.745

 

96.8

0.003

1.039

99.9

9.925

98.85

39.021

 

97.5

0.004

1.041

100.1

9.955

99.15

38.155

 

95.3

0.004

1.037

99.7

9.986

99.46

38.557

 

96.3

0.004

1.050

101

10.023

99.83

39.262

 

98.1

0.002

1.026

98.6

10.011

99.71

39.104

 

97.7

平均值

0.004

1.036

99.6

9.960

99.2

38.597

 

96.4

RSD%

  

1.12

 

0.91

 

1.12

 

Ge

0.019

1.012

85.2

10.106

99.46

37.351

 

92.98

0.012

1.010

85

10.093

99.33

37.467

 

93.27

0.015

1.131

97.1

10.121

99.61

37.599

 

93.60

0.010

1.117

95.7

10.098

99.38

37.195

 

92.59

0.013

1.103

94.3

10.203

100.43

38.026

 

94.67

0.021

1.261

110.1

10.253

100.93

38.151

 

94.98

0.026

1.230

107

10.224

100.64

37.833

 

94.18

0.019

1.252

109.2

10.175

100.15

37.864

 

94.26

0.016

1.088

92.8

10.077

99.17

37.566

 

93.52

0.013

1.023

86.3

10.159

99.99

38.195

 

95.09

平均值

0.016

1.123

96.3

10.151

99.9

37.725

 

93.9

RSD%

 

8.60

 

0.60

 

0.91

 
 

Sc

5.026

10.137

102.54

15.017

100.07

43.695

 

96.71

5.159

9.277

85.34

15.026

100.16

44.122

 

97.78

4.952

10.174

103.28

14.866

98.56

43.863

 

97.13

4.895

10.062

101.04

14.753

97.43

43.772

 

96.91

5.103

9.869

97.18

14.539

95.29

43.919

 

97.27

5.214

10.023

100.26

14.826

98.16

44.082

 

97.68

4.826

10.111

102.02

14.838

98.28

43.956

 

97.37

4.802

9.969

99.18

15.102

100.92

44.269

 

98.15

4.959

9.653

92.86

15.114

101.04

43.833

 

97.06

5.142

10.017

100.14

14.377

93.67

43.975

 

97.41

平均值

5.01

9.929

98.4

14.846

98.36

43.949

 

97.3

RSD%

 

2.76

 

1.62

 

0.39

 

表4 -3起泡酒加标回收和精密度实验

 

元素

 

样品

 

添加水平

 

1(μg/L)

 

10(μg/L)

 

40(μg/L)

测定值

测定值

回收率

测定值

回收率

测定值

回收率

 

La

0.812

1.835

100.5

10.856

100.26

39.569

96.8

0.826

1.802

97.2

10.91

100.8

39.265

96.1

0.836

1.901

107.1

10.743

99.13

38.782

94.9

0.851

1.795

96.5

10.696

98.66

38.963

95.3

0.829

1.833

100.3

10.638

98.08

39.029

95.5

0.864

1.869

103.9

10.655

98.25

39.111

95.7

0.821

1.795

96.5

10.629

97.99

38.785

94.9

0.815

1.802

97.2

10.855

100.25

38.822

95.0

0.809

1.902

107.2

10.796

99.66

38.691

94.7

0.832

1.858

102.8

10.963

101.33

38.462

94.1

平均值

0.830

1.839

100.9

10.774

99.4

38.948

95.3

RSD%

 

2.27

 

1.11

 

0.81

 
 

Ce

1.816

2.801

104.1

11.822

100.6

39.269

93.8

1.812

2.735

97.5

11.834

100.7

39.563

94.5

1.825

2.699

93.9

11.752

99.9

39.925

95.4

1.736

2.783

102.3

11.645

98.9

39.196

93.6

1.739

2.791

103.1

11.483

97.2

39.776

95.0

1.722

2.759

99.9

11.774

100.1

39.206

93.6

1.734

2.739

97.9

11.802

100.4

39.757

95.0

1.729

2.694

93.4

11.836

100.8

40.006

95.6

1.742

2.615

85.5

11.526

97.7

40.236

96.2

1.733

2.703

94.3

11.479

97.2

40.269

96.3

平均值

1.759

2.732

97.2

11.529

99.4

40.157

94.9

RSD%

 

2.07

 

1.29

 

1.00

 
 

Y

1.492

2.601

102.1

11.462

98.82

39.561

95.0

1.507

2.593

101.3

11.55

99.7

39.606

95.1

1.563

2.585

100.5

11.399

98.19

39.277

94.2

1.515

2.602

102.2

11.417

98.37

39.751

95.4

1.568

2.499

91.9

11.452

98.72

39.862

95.7

1.602

2.507

92.7

11.462

98.82

39.665

95.2

1.637

2.589

100.9

11.591

100.11

38.269

91.7

1.628

2.575

99.5

11.601

100.21

38.956

93.4

1.611

2.563

98.3

11.482

99.02

38.788

93.0

1.655

2.591

101.1

11.516

99.36

38.769

93.0

平均值

1.5778

2.5705

99.05

11.493

99.1

39.250

94.2

RSD% 

1.46

 

0.60

 

1.35

 
 

Pr

0.222

1.281

107.1

10.113

99.0

38.836

96.6

0.206

1.225

101.5

10.186

99.8

38.748

96.3

0.213

1.267

105.7

10.236

100.3

38.692

96.2

0.202

1.249

103.9

10.161

99.5

38.575

95.9

0.235

1.251

104.1

10.213

100.0

38.626

96.0

0.233

1.206

99.6

10.233

100.2

39.132

97.3

0.206

1.22

101

10.309

101.0

39.087

97.2

0.201

1.209

99.9

10.321

101.1

38.265

95.1

0.217

1.212

100.2

10.291

100.8

39.117

97.3

0.203

1.231

102.1

10.142

99.3

39.326

97.8

平均值

0.214

1.235

102.5

10.221

100.1

38.840

96.6

RSD% 

4.07

 

2.04

 

1.38

 
 

Nd

0.846

1.782

93.2

10.663

98.1

39.145

95.7

0.829

1.833

98.3

10.706

98.6

39.033

95.5

0.833

1.901

105.1

10.923

100.7

38.796

94.9

0.857

1.856

100.6

10.976

101.3

38.665

94.5

0.862

1.839

98.9

10.863

100.1

39.215

95.9

0.839

1.792

94.2

11.026

101.8

39.552

96.8

0.849

1.833

98.3

11.134

102.8

39.368

96.3

0.847

1.897

104.7

11.109

102.6

40.023

97.9

0.862

1.877

102.7

11.243

103.9

40.055

98.0

0.859

1.862

101.2

11.036

101.9

39.757

97.3

平均值

0.848

1.847

99.7

10.968

101.2

39.361

96.3

RSD% 

2.16

 

1.68

 

1.23

 
 

Sm

0.19

1.211

101.1

10.114

99.1

39.112

97.3

0.221

1.206

100.6

10.236

100.4

39.107

97.3

0.209

1.195

99.5

10.259

100.6

38.826

96.6

0.192

1.201

100.1

10.066

98.7

38.937

96.8

0.183

1.245

104.5

9.758

95.6

38.965

96.9

0.189

1.219

101.9

10.055

98.6

39.166

97.4

0.196

1.243

104.3

10.176

99.8

38.526

95.8

0.209

1.226

102.6

10.836

106.4

38.317

95.3

0.201

1.231

103.1

9.898

97.0

38.472

95.7

0.227

1.217

101.7

10.005

98.1

37.269

92.7

平均值

0.202

1.219

101.9

10.140

99.4

38.670

96.2

RSD%

 

1.39

 

2.84

 

1.48

 
 

Eu

0.319

1.402

106.2

10.239

99.0

39.216

97.2

0.327

1.441

110.1

10.217

98.8

39.033

96.7

0.335

1.393

105.3

10.069

97.3

38.935

96.5

0.351

1.385

104.5

10.133

97.9

38.759

96.0

0.355

1.366

102.6

10.275

99.4

38.734

96.0

0.362

1.372

103.2

10.201

98.6

39.262

97.3

0.349

1.347

100.7

10.308

99.7

38.563

95.6

0.333

1.357

101.7

10.325

99.9

38.293

94.9

0.347

1.326

98.6

10.269

99.3

38.445

95.3

0.326

1.328

98.8

10.417

100.8

38.397

95.1

平均值

0.3404

1.372

103.2

10.25

99.1

38.764

96.1

RSD%

 

2.57

 

0.96

 

0.88

 
 

Gd

0.229

1.206

95.6

10.019

97.7

38.469

95.5

0.242

1.231

98.1

10.139

98.9

38.366

95.3

0.262

1.241

99.1

10.117

98.7

38.201

94.9

0.251

1.229

97.9

10.205

99.6

38.097

94.6

0.266

1.251

100.1

10.146

99.0

38.568

95.8

0.253

1.233

98.3

10.187

99.4

39.252

97.5

0.271

1.239

98.9

10.236

99.9

39.483

98.1

0.236

1.26

101

10.256

100.1

38.926

96.7

0.238

1.208

95.8

10.195

99.5

39.585

98.3

0.248

1.317

106.7

10.242

99.9

39.776

98.8

平均值

0.250

1.242

99.2

10.174

99.2

38.872

96.6

RSD%

 

2.53

 

0.70

 

1.58

 
 

Tb

0.013

1.013

99.3

10.006

99.9

38.972

97.4

0.016

1.006

98.6

10.009

99.9

39.211

98.0

0.02

0.925

90.5

9.839

98.2

39.265

98.1

0.028

0.984

96.4

9.926

99.1

39.073

97.6

0.019

0.996

97.6

9.667

96.5

38.563

96.4

0.018

1.039

101.9

9.967

99.5

38.726

96.8

0.015

1.026

100.6

10.031

100.1

38.696

96.7

0.024

1.007

98.7

10.042

100.2

38.526

96.3

0.018

1.027

100.7

10.107

100.9

39.225

98.0

0.021

1.036

101.6

10.201

101.8

39.305

98.2

平均值

0.019

1.006

98.6

9.980

99.6

38.447

97.3

RSD%

 

3.32

 

1.47

 

0.79

 
 

Dy

0.205

1.213

100.3

10.166

99.56

38.667

96.1

0.213

1.219

100.9

10.153

99.43

37.953

94.4

0.204

1.206

99.6

10.187

99.77

37.665

93.6

0.189

1.226

101.6

10.251

100.41

38.265

95.1

0.195

1.224

101.4

10.098

98.88

38.196

95.0

0.193

1.251

104.1

10.123

99.13

38.432

95.6

0.217

1.301

109.1

10.202

99.92

37.895

94.2

0.211

1.203

99.3

10.245

100.35

38.066

94.6

0.229

1.213

100.3

10.097

98.87

39.132

97.3

0.225

1.218

100.8

10.088

98.78

38.696

96.2

平均值

0.208

1.227

101.74

10.161

99.510

38.297

95.2

RSD%

 

2.37

 

0.59

 

1.15

 
 

Ho

0.029

1.007

96.7

9.933

98.93

38.863

97.06

0.033

1.002

96.2

9.825

97.85

38.265

95.56

0.042

1.039

99.9

9.965

99.25

38.217

95.44

0.036

1.044

100.4

10.022

99.82

38.225

95.46

0.039

1.041

100.1

10.027

99.87

39.033

97.48

0.045

1.052

101.2

10.019

99.79

38.269

95.57

0.036

1.055

101.5

10.005

99.65

38.137

95.24

0.031

1.049

100.9

9.989

99.49

37.266

93.07

0.042

1.051

101.1

9.978

99.38

37.563

93.81

0.046

1.039

99.9

9.666

96.26

36.989

92.37

平均值

0.038

1.038

99.8

9.943

99.0

38.083

95.1

RSD%

 

1.78

 

1.15

 

1.70

 
 

Er

0.146

1.162

100.2

10.112

99.5

38.696

96.3

0.151

1.149

98.9

10.093

99.3

38.753

96.5

0.169

1.144

98.4

10.026

98.7

38.926

96.9

0.155

1.156

99.6

10.044

98.8

38.335

95.4

0.158

1.159

99.9

10.131

99.7

38.269

95.3

0.179

1.171

101.1

10.159

100.0

37.569

93.5

0.151

1.166

100.6

10.009

98.5

39.457

98.2

0.149

1.163

100.3

10.022

98.6

38.745

96.5

0.156

1.182

102.2

10.026

98.7

38.699

96.3

0.157

1.19

103

10.37

102.1

39.117

97.4

平均值

0.157

1.164

100.4

10.099

99.4

38.657

96.2

RSD%

 

1.21

 

1.07

 

1.33

 
 

Tm

0.015

1.009

98.9

10.003

99.8

38.776

96.9

0.019

1.013

99.3

10.011

99.9

38.632

96.5

0.024

1.03

101

9.966

99.5

38.921

97.3

0.022

1.026

100.6

9.753

97.3

39.126

97.8

0.017

1.029

100.9

9.851

98.3

39.255

98.1

0.013

1.044

102.4

9.969

99.5

38.751

96.8

0.026

1.051

103.1

10.037

100.2

38.636

96.5

0.023

1.029

100.9

10.021

100.0

38.211

95.5

0.019

1.023

100.3

10.006

99.9

38.736

96.8

0.023

1.045

102.5

9.639

96.2

38.755

96.8

平均值

0.0201

1.0299

100.99

9.583

99.1

38.780

96.9

RSD%

 

1.32

 

1.40

 

0.74

 
 

Yb

0.203

1.202

98.2

10.017

97.97

39.011

96.98

0.198

1.217

99.7

10.056

98.36

39.236

97.54

0.211

1.159

93.9

10.106

98.86

39.175

97.39

0.235

1.207

98.7

10.227

100.07

38.688

96.17

0.204

1.301

108.1

10.204

99.84

38.923

96.76

0.239

1.262

104.2

10.139

99.19

39.137

97.29

0.213

1.246

102.6

10.228

100.08

39.206

97.47

0.206

1.253

103.3

10.305

100.85

38.565

95.86

0.219

1.202

98.2

10.416

101.96

38.821

96.50

0.242

1.239

101.9

10.3

100.8

39.02

97.00

平均值

0.217

1.229

100.9

10.200

99.8

38.978

96.9

RSD%

 

3.24

 

1.21

 

0.58

 
 

Lu

0.034

1.029

99.9

9.922

98.92

38.986

97.4

0.033

1.022

99.2

9.956

99.26

38.623

96.5

0.023

1.031

100.1

9.693

96.63

39.112

97.7

0.029

1.039

100.9

9.598

95.68

38.757

96.8

0.026

1.028

99.8

9.775

97.45

37.926

94.7

0.022

1.035

100.5

9.869

98.39

37.969

94.8

0.03

1.042

101.2

10.106

100.76

38.441

96.0

0.032

1.037

100.7

10.063

100.33

38.206

95.4

0.037

1.051

102.1

10.028

99.98

37.83

94.5

0.032

1.066

103.6

10.035

100.05

37.958

94.8

平均值

0.030

1.038

100.8

9.976

98.7

38.381

95.9

RSD%

 

1.23

 

1.70

 

1.23

 
 

Ge

0.175

1.251

101.1

10.233

99.93

39.228

97.47

0.192

1.226

98.6

10.221

99.81

39.314

97.69

0.261

1.263

102.3

10.258

100.18

39.88

99.10

0.24

1.269

102.9

10.3

100.6

38.869

96.57

0.266

1.217

97.7

10.413

101.73

38.785

96.36

0.293

1.309

106.9

10.433

101.93

39.269

97.57

0.225

1.197

95.7

10.396

101.56

39.566

98.32

0.242

1.207

96.7

10.502

102.62

39.476

98.09

0.281

1.305

106.5

10.519

102.79

39.526

98.22

0.264

1.288

104.8

10.447

102.07

39.777

98.84

平均值

0.244

1.253

101.3

10.372

101.3

39.369

97.8

RSD%

 

3.23

 

1.07

 

0.90

 
 

Sc

2.063

7.205

103.9

12.008

99.08

41.088

97.47

1.958

7.175

103.3

12.351

102.51

39.867

94.42

1.866

7.008

99.96

12.201

101.01

40.036

94.84

2.131

6.935

98.5

12.19

100.9

41.937

99.59

2.206

6.984

99.48

12.245

101.45

42.665

101.41

2.093

6.869

97.18

12.306

102.06

41.939

99.60

2.147

7.021

100.22

12.177

100.77

40.086

94.97

2.008

7.032

100.44

12.401

103.01

39.856

94.39

2.317

7.157

102.94

12.473

103.73

39.206

92.77

2.249

7.149

102.78

12.259

101.59

41.572

98.68

平均值

2.10

7.054

100.9

12.261

101.61

40.825

96.8

RSD%

 

1.60

 

1.07

 

2.84

 

结论
采用低温赶酸,硝酸消解,用ICP-MS测定葡萄酒中的稀土元素,快速准确,可用于葡萄酒的稀土元素检测。
该帖子作者被版主 wangjstw2积分, 2经验,加分理由:发帖奖励
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