Detelogy土壤中多环芳烃的测定前处理方案

萃取溶剂

丙酮：正己烷=1:1

加热温度

100℃

萃取池压力

1500 psi

预加热平衡

5 min

静态萃取时间

5 min

溶剂淋洗体积

60% 池体积

氮气吹扫时间

60 s

静态萃取次数

2次

总萃取时间

45min

活化

二氯甲烷

4

2

-

活化

正己烷

5.0

2

-

浸泡

-

-

-

300s

活化

正己烷

5.0

2

-

上样

样品

2

2

-

洗瓶

正己烷

2

2

-

洗脱

二氯甲烷：正己烷=1:1

5

2

-

浸泡

-

-

-

120s

洗脱

二氯甲烷：正己烷=1:1

5

2

-

进样口温度

280℃

进样方式

不分流进样至0.75 min 后打开分流，分流出口流量为 50 mL/min

载气

高纯氦气，1.0 mL/min，恒流

柱温升温程序

初始温度 80℃，保持2min，以20℃/min 升温至180℃，保持5 min；以10℃/min升温至 290℃，保持 40 min；

进样量

1.0 μL

离子源温度

230℃

离子化能量

70 eV

接口温度

280℃

四级杆温度

150℃

质量扫描范围

45 amu~450 amu

溶剂延迟时间

5 min

扫描模式

全扫描 Scan

萘

58.76%

66.45%

62.48%

62.14%

65.65%

61.39%

4.52%

2-氟联苯

76.79%

73.21%

70.34%

79.76%

73.78%

70.38%

4.98%

苊烯

70.76%

81.63%

81.18%

79.73%

75.44%

77.79%

5.30%

苊

64.50%

66.52%

70.16%

72.79%

65.40%

73.29%

5.56%

芴

83.87%

78.89%

84.59%

83.70%

78.33%

83.67%

3.39%

菲

106.61%

94.02%

105.11%

104.96%

94.05%

103.61%

5.70%

蒽

96.05%

83.49%

94.56%

94.42%

83.52%

93.07%

6.35%

荧蒽

100.01%

98.35%

88.38%

96.29%

98.76%

96.42%

4.32%

芘

97.70%

85.59%

95.26%

92.54%

82.97%

93.15%

6.27%

4,4’三联苯-d14

107.77%

94.47%

107.53%

104.92%

95.05%

105.29%

5.96%

苯并（a）蒽

92.02%

87.39%

97.94%

88.03%

98.60%

103.47%

6.81%

䓛

103.53%

97.58%

103.00%

102.55%

98.12%

103.64%

2.75%

苯并（b）荧蒽

102.98%

96.09%

104.76%

103.42%

97.08%

104.67%

3.82%

苯并（k）荧蒽

101.85%

95.60%

103.97%

103.15%

96.59%

100.12%

3.45%

苯并（a）芘

88.02%

83.04%

91.55%

90.17%

93.37%

91.76%

4.13%

茚并（123-c，d）芘

93.99%

96.89%

101.98%

97.43%

98.32%

84.89%

6.11%

二苯并（a，h）蒽

103.78%

90.73%

94.33%

97.25%

92.08%

97.25%

4.88%

苯并（g，h，i）苝

100.59%

86.24%

92.54%

92.58%

87.53%

92.29%

5.50%