柱温: 40℃保持19min,以30℃/min升温至200℃,保持15min;
检测器类型: FID ; 检测器温度: 280 ℃; 载气: 氮气 ;
进样口温度: 220 ℃;流速: 5.0 ml/min; ; 进样量: 1 ml;
2.4顶空条件的选择:
样品盘温度: 110 ℃;定量环温度: 120℃ ;管线温度: 130 ℃;
样品平衡时间: 25 min;加压时间:0.3 min;管线充满时间: 0.3 min;
乙醛浓度(ug/ml) | 20.016 | 40.032 | 50.04 | 80.064 | 100.08 | 150.12 |
A乙醛 | 240648.3 | 490168.6 | 617084.2 | 1003729.3 | 1285942.1 | 1883606.5 |
回归方程及相关系数 | ||||||
环氧乙烷浓度(ug/ml) | 0.042 | 0.084 | 0.105 | 0.168 | 0.21 | 0.315 |
A环氧乙烷 | 1584.9 | 2989.5 | 3582.8 | 5794.6 | 7426.7 | 10107.1 |
回归方程及相关系数 | ||||||
二氯甲烷(ug/ml) | 2.004 | 4.008 | 5.01 | 8.016 | 10.02 | 15.03 |
A二氯甲烷 | 11095.7 | 22903.2 | 28387.7 | 47033.8 | 60036.9 | 85360 |
回归方程及相关系数 | ||||||
正己烷(ug/ml) | 11.624 | 23.248 | 29.06 | 46.496 | 58.12 | 87.18 |
A正己烷 | 3988411.9 | 7923793.6 | 10021283 | 15696633 | 20194122 | 31978061.3 |
回归方程及相关系数 | ||||||
三氯甲烷(ug/ml) | 0.406 | 0.812 | 1.015 | 1.624 | 2.03 | 3.045 |
A三氯甲烷 | 368.5 | 938.1 | 1529.2 | 2357.9 | 2822.7 | 4541.4 |
回归方程及相关系数 | ||||||
1,1,2-三氯乙烯(ug/ml) | 0.404 | 0.808 | 1.01 | 1.616 | 2.02 | 3.03 |
A1,1,2-三氯乙烯 | 3651.5 | 9917.7 | 11750.5 | 19609.2 | 23556.2 | 33857.1 |
回归方程及相关系数 | ||||||
1,4-二氧六环(ug/ml) | 0.408 | 0.808 | 1.01 | 1.616 | 2.02 | 3.03 |
A1,4-二氧六环 | 2832.5 | 5652 | 7767.1 | 11166.2 | 14136.1 | 19666.1 |
回归方程及相关系数 |
杂质名称 | 乙醛 | 环氧乙烷 | 二氯甲烷 | 正己烷 | 三氯甲烷 | 1,1,2-三氯乙烯 | 1,4-二氧六环 |
峰高 | 233.9 | 271.5 | 279.1 | 271.6 | 247.3 | 267.6 | 272.3 |
S/N | 9.0 | 10.4 | 10.7 | 10.4 | 9.5 | 10.3 | 10.5 |
浓度(ppm) | 0.061 | 0.03 | 0.17 | 0.0052 | 1.2 | 0.28 | 0.73 |
噪音(N) | 26微伏 |
杂质名称 | 乙醛 | 环氧乙烷 | 二氯甲烷 | 正己烷 | 三氯甲烷 | 1,1,2-三氯乙烯 | 1,4-二氧六环 |
峰高 | 53.3 | 97.8 | 97.7 | 100.5 | 101.5 | 54.5 | 95.6 |
S/N | 2.1 | 3.8 | 3.8 | 3.9 | 3.9 | 2.1 | 3.7 |
浓度(ppm) | 0.012 | 0.082 | 0.049 | 0.0013 | 0.39 | 0.053 | 0.21 |
噪音(N) | 26微伏 |
相对浓度 | 序号 | 称样量(mg) | 已知量(ug) | 加入量(ug) | 测得量(ug) | 回收率% | |
乙醛 | 30% | 1 | 2003.5 | 8.014 | 301.86 | 284.1 | 91.5 |
2 | 2001.8 | 8.0072 | 301.86 | 264.5 | 85.0 | ||
3 | 1998.5 | 7.994 | 301.86 | 255.9 | 82.1 | ||
50% | 1 | 2004.5 | 8.018 | 503.1 | 455 | 88.8 | |
2 | 2003.1 | 8.0124 | 503.1 | 458.8 | 89.6 | ||
3 | 2000.7 | 8.0028 | 503.1 | 456.6 | 89.2 | ||
100% | 1 | 1998.3 | 7.9932 | 1006.2 | 949.1 | 93.5 | |
2 | 1999.2 | 7.9968 | 1006.2 | 962 | 94.8 | ||
3 | 2003.9 | 8.0156 | 1006.2 | 971.8 | 95.8 | ||
环氧乙烷 | 30% | 1 | 2003.5 | 0 | 0.66 | 0.63 | 95.5 |
2 | 2001.8 | 0 | 0.66 | 0.64 | 97.0 | ||
3 | 1998.5 | 0 | 0.66 | 0.63 | 95.5 | ||
50% | 1 | 2004.5 | 0 | 1.1 | 1.11 | 100.9 | |
2 | 2003.1 | 0 | 1.1 | 1.16 | 105.5 | ||
3 | 2000.7 | 0 | 1.1 | 1.06 | 96.4 | ||
100% | 1 | 1998.3 | 0 | 2.2 | 2.15 | 97.7 | |
2 | 1999.2 | 0 | 2.2 | 2.13 | 96.8 | ||
3 | 2003.9 | 0 | 2.2 | 2.17 | 98.6 | ||
二氯甲烷 | 30% | 1 | 2003.5 | 0 | 30.63 | 26.4 | 86.2 |
2 | 2001.8 | 0 | 30.63 | 27.2 | 88.8 | ||
3 | 1998.5 | 0 | 30.63 | 26.4 | 86.2 | ||
50% | 1 | 2004.5 | 0 | 51.05 | 46.3 | 90.7 | |
2 | 2003.1 | 0 | 51.05 | 46.2 | 90.5 | ||
3 | 2000.7 | 0 | 51.05 | 47.3 | 92.7 | ||
100% | 1 | 1998.3 | 0 | 102.1 | 98.3 | 96.3 | |
2 | 1999.2 | 0 | 102.1 | 95.7 | 93.7 | ||
3 | 2003.9 | 0 | 102.1 | 98.8 | 96.8 | ||
正己烷 | 30% | 1 | 2003.5 | 0.621085 | 175.8 | 159.3 | 90.6 |
2 | 2001.8 | 0.620558 | 175.8 | 164.6 | 93.6 | ||
3 | 1998.5 | 0.619535 | 175.8 | 157.5 | 89.6 | ||
50% | 1 | 2004.5 | 0.621395 | 293 | 275 | 93.9 | |
2 | 2003.1 | 0.620961 | 293 | 278.7 | 95.1 | ||
3 | 2000.7 | 0.620217 | 293 | 281 | 95.9 | ||
100% | 1 | 1998.3 | 0.619473 | 586 | 552 | 94.2 | |
2 | 1999.2 | 0.619752 | 586 | 558.9 | 95.4 | ||
3 | 2003.9 | 0.621209 | 586 | 557.6 | 95.2 | ||
三氯甲烷 | 30% | 1 | 2003.5 | 0 | 6.33 | 6.1 | 96.4 |
2 | 2001.8 | 0 | 6.33 | 5.6 | 88.5 | ||
3 | 1998.5 | 0 | 6.33 | 5.5 | 86.9 | ||
50% | 1 | 2004.5 | 0 | 10.55 | 8.7 | 82.5 | |
2 | 2003.1 | 0 | 10.55 | 8.9 | 84.4 | ||
3 | 2000.7 | 0 | 10.55 | 9.5 | 90.0 | ||
100% | 1 | 1998.3 | 0 | 21.1 | 17.9 | 84.8 | |
2 | 1999.2 | 0 | 21.1 | 17.1 | 81.0 | ||
3 | 2003.9 | 0 | 21.1 | 19.9 | 94.3 | ||
1,1,2-三氯乙烯 | 30% | 1 | 2003.5 | 0 | 6.9 | 6.7 | 97.1 |
2 | 2001.8 | 0 | 6.9 | 6 | 87.0 | ||
3 | 1998.5 | 0 | 6.9 | 6.8 | 98.6 | ||
50% | 1 | 2004.5 | 0 | 11.5 | 10.8 | 93.9 | |
2 | 2003.1 | 0 | 11.5 | 10.2 | 88.7 | ||
3 | 2000.7 | 0 | 11.5 | 9.8 | 85.2 | ||
100% | 1 | 1998.3 | 0 | 23 | 22.2 | 96.5 | |
2 | 1999.2 | 0 | 23 | 22.3 | 97.0 | ||
3 | 2003.9 | 0 | 23 | 22.8 | 99.1 | ||
1,4-二氧六环 | 30% | 1 | 2003.5 | 0 | 6.57 | 6.1 | 92.8 |
2 | 2001.8 | 0 | 6.57 | 7.7 | 117.2 | ||
3 | 1998.5 | 0 | 6.57 | 6.9 | 105.0 | ||
50% | 1 | 2004.5 | 0 | 10.95 | 10.7 | 97.7 | |
2 | 2003.1 | 0 | 10.95 | 11.4 | 104.1 | ||
3 | 2000.7 | 0 | 10.95 | 11 | 100.5 | ||
100% | 1 | 1998.3 | 0 | 21.9 | 23.7 | 108.2 | |
2 | 1999.2 | 0 | 21.9 | 22.7 | 103.7 | ||
3 | 2003.9 | 0 | 21.9 | 24.3 | 111.0 |
批号 | 乙醛% | 环氧乙烷% | 二氯甲烷% | 正己烷% | 三氯甲烷% | 1,1,2-三氯乙烯% | 1,4-二氧六环% |
120801 | 0.00039 | --- | --- | 0.000031 | --- | --- | --- |
120802 | 0.00038 | --- | --- | 0.000033 | --- | --- | --- |
120803 | 0.00041 | --- | --- | 0.000041 | --- | --- | --- |