仪器条件 | 仪器 | gc 5890F | 编号 | WHBP-E-06 | |||||||
毛细管柱 | DB-1701 | 30m*0.25mm*0.25μm | |||||||||
柱前压 | 0.15MPa | 柱流量 | 恒流 | 2.0ml/min | |||||||
检测器 | FID | ||||||||||
进样口 | 260℃ | 隔垫吹扫 | 3.0mi/min | ||||||||
柱箱升温方式 | 程序升温 | ||||||||||
升温梯度 | 50℃(5min)--8℃/min--250℃(1min) | ||||||||||
检测器 | 300℃ | 尾吹 | 30nl/min | ||||||||
进样量 | 1.0μL | ||||||||||
校准曲线 | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | |
单位 | 浓度/目标化合物 | 氯苯 | 2-氯甲苯 | 3-氯甲苯 | 4-氯甲苯 | 1,3-二氯苯 | 1,4-二氯苯 | 1,2-二氯苯 | 1,3,5-三氯苯 | 1,2,4-三氯苯 | 1,2,3-三氯苯 |
mg/L | |||||||||||
2.0 | 1932 | 2148 | 2030 | 2044 | 1576 | 1620 | 1486 | 1348 | 1197 | 1335 | |
5.0 | 4710 | 5383 | 5159 | 5328 | 3917 | 3896 | 4053 | 3385 | 3225 | 3314 | |
10.0 | 9552 | 10061 | 9670 | 9875 | 7526 | 8215 | 7239 | 6361 | 6280 | 6052 | |
20.0 | 18758 | 21040 | 20622 | 20771 | 15886 | 15567 | 15578 | 13549 | 12517 | 12975 | |
100.0 | 95847 | 107724 | 103612 | 104823 | 78982 | 78264 | 78941 | 68071 | 64190 | 65843 | |
校准曲线 | Y=959.2X-123.3 | Y=1080X-312.9 | Y=1038X-230.2 | Y=1050X-200.4 | Y=790.8X-91.08 | Y=781.6X+96.23 | Y=791.4X-224.4 | Y=682.1X-145.8 | Y=642.9X-133.6 | Y=659.9X-177.9 | |
r | 0.99999 | 0.99997 | 0.99997 | 0.99998 | 0.99998 | 0.99998 | 0.99996 | 0.99997 | 0.99998 | 0.99996 | |
1 | 检出限 | 无组织标况采样体积30L,解析液体积1.00ml,向7只同批次空白活性炭吸附管中加入1.0μg标准品,后采集清洁空气30L,用胶帽密封两端, 将A,B两段分别转移至5ml具塞玻璃试管中,各加入1.0ml色谱纯二硫化碳,于超声清洗仪中超声解吸1min,静置30min,取1.0μL上机测试。 | |||||||||
1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | ||
测定次数 | 氯苯 | 2-氯甲苯 | 3-氯甲苯 | 4-氯甲苯 | 1,3-二氯苯 | 1,4-二氯苯 | 1,2-二氯苯 | 1,3,5-三氯苯 | 1,2,4-三氯苯 | 1,2,3-三氯苯 | |
1 | 1.0516 | 1.0100 | 0.9547 | 0.9298 | 0.9928 | 0.9610 | 0.9496 | 0.9308 | 0.9470 | 1.0741 | |
2 | 1.0263 | 1.0101 | 0.9608 | 0.9281 | 0.9771 | 1.0017 | 0.9495 | 0.9470 | 0.9304 | 1.0419 | |
3 | 1.0753 | 1.0391 | 0.9979 | 1.0018 | 1.0115 | 0.9737 | 0.9976 | 1.0160 | 0.9596 | 0.9761 | |
4 | 1.0016 | 1.0391 | 0.9576 | 0.9573 | 1.0034 | 1.0017 | 0.9624 | 1.0185 | 0.9602 | 1.0069 | |
5 | 1.0183 | 1.0409 | 1.0212 | 1.0018 | 1.0115 | 1.0962 | 0.9976 | 0.9798 | 0.9959 | 1.0305 | |
6 | 0.9787 | 1.0239 | 0.9647 | 0.9846 | 0.9657 | 1.0539 | 0.9882 | 1.0275 | 1.0106 | 0.9722 | |
7 | 1.0160 | 0.9883 | 0.9995 | 0.9573 | 0.9877 | 1.0017 | 0.9976 | 0.9886 | 1.0070 | 0.9924 | |
平均值 | 1.0240 | 1.0216 | 0.9795 | 0.9658 | 0.9928 | 1.0128 | 0.9775 | 0.9869 | 0.9730 | 1.0134 | |
标准偏差 | 0.0318 | 0.0199 | 0.0263 | 0.0311 | 0.0174 | 0.0470 | 0.0228 | 0.0372 | 0.0314 | 0.0373 | |
t值 | 3.143 | 3.143 | 3.143 | 3.143 | 3.143 | 3.143 | 3.143 | 3.143 | 3.143 | 3.143 | |
检出限μg/ml | 0.0998 | 0.0624 | 0.0826 | 0.0978 | 0.0547 | 0.1476 | 0.0716 | 0.1168 | 0.0988 | 0.1173 | |
无组织检出限 (采样体积30L, 解吸液体积1.0ml) | 0.0033 | 0.0021 | 0.0028 | 0.0033 | 0.0018 | 0.0049 | 0.0024 | 0.0039 | 0.0033 | 0.0039 | |
无组织方法检出限(采样体积30L, 解吸液体积1.0ml) | 0.008 | 0.009 | 0.008 | 0.008 | 0.008 | 0.008 | 0.01 | 0.008 | 0.007 | 0.008 | |
无组织测定下限 (采样体积30L, 解吸液体积1.0ml) | 0.013 | 0.008 | 0.011 | 0.013 | 0.007 | 0.020 | 0.010 | 0.016 | 0.013 | 0.016 | |
无组织方法测定下限(采样体积30L, 解吸液体积1.0ml) | 0.032 | 0.036 | 0.032 | 0.032 | 0.032 | 0.032 | 0.040 | 0.032 | 0.028 | 0.032 | |
结果判定 | 符合 | 符合 | 符合 | 符合 | 符合 | 符合 | 符合 | 符合 | 符合 | 符合 | |
有组织检出限 (采样体积10L, 解吸液体积2.00ml) | 0.020 | 0.012 | 0.017 | 0.020 | 0.011 | 0.030 | 0.014 | 0.023 | 0.020 | 0.023 | |
有组织方法检出限 (采样体积10L, 解吸液体积2.00ml) | 0.03 | 0.03 | 0.03 | 0.03 | 0.03 | 0.03 | 0.04 | 0.03 | 0.02 | 0.03 | |
有组织测定下限(采样体积10L, 解吸液体积2.00ml) | 0.08 | 0.05 | 0.07 | 0.08 | 0.04 | 0.12 | 0.06 | 0.09 | 0.08 | 0.09 | |
有组织方法测定下限(采样体积10L, 解吸液体积2.00ml) | 0.12 | 0.12 | 0.12 | 0.12 | 0.12 | 0.12 | 0.16 | 0.12 | 0.08 | 0.12 | |
结果判定 | 符合 | 符合 | 符合 | 符合 | 符合 | 符合 | 符合 | 符合 | 符合 | 符合 | |
2.精密度 | 无组织标况采样体积30L,解析液体积1.00ml,向6只同批次空白活性炭吸附管中分别加入4.0μg、30.0μg、75.0μg标准品,后采集清洁空气30L,用胶帽密封两端,即得0.13mg/m3、1.00mg/m3、2.50mg/m3样品 将A,B两段分别转移至5ml具塞玻璃试管中,各加入1.0ml色谱纯二硫化碳,于超声清洗仪中超声解吸1min,静置30min,取1.0μL上机测试,计算6次测定平均值,标准偏差和相对标准偏差 | ||||||||||
低浓度 | |||||||||||
4ppm | 0.13mg/m3 | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
测定次数 | 氯苯 | 2-氯甲苯 | 3-氯甲苯 | 4-氯甲苯 | 1,3-二氯苯 | 1,4-二氯苯 | 1,2-二氯苯 | 1,3,5-三氯苯 | 1,2,4-三氯苯 | 1,2,3-三氯苯 | |
1 | 3.9344 | 4.0236 | 3.8415 | 3.9303 | 3.968 | 4.0098 | 3.987 | 3.8355 | 3.9149 | 4.073 | |
2 | 3.8455 | 3.9204 | 4.0806 | 3.9106 | 3.8205 | 3.9202 | 3.8561 | 3.8607 | 4.0296 | 4.0192 | |
3 | 3.9339 | 3.9784 | 3.8149 | 3.9538 | 3.8823 | 3.9275 | 3.9631 | 3.8959 | 3.8974 | 4.0352 | |
4 | 3.8457 | 3.9204 | 3.9941 | 3.9645 | 3.9427 | 3.9595 | 3.918 | 3.8774 | 4.0295 | 4.0083 | |
5 | 3.8957 | 3.9916 | 3.8413 | 3.9682 | 3.8429 | 3.9575 | 3.9179 | 3.8959 | 3.8646 | 3.9745 | |
6 | 3.9235 | 4.0406 | 3.8780 | 3.9464 | 3.8183 | 3.9687 | 3.9671 | 3.8959 | 4.0182 | 3.9179 | |
平均值 | 3.8965 | 3.9792 | 3.9084 | 3.9456 | 3.8791 | 3.9572 | 3.9349 | 3.8769 | 3.9590 | 4.0047 | |
标准偏差 | 0.0418 | 0.0506 | 0.1055 | 0.0219 | 0.0639 | 0.0321 | 0.0476 | 0.0247 | 0.0750 | 0.0534 | |
相对标准偏差 | 1.07% | 1.27% | 2.70% | 0.55% | 1.65% | 0.81% | 1.21% | 0.64% | 1.89% | 1.33% | |
精密度 | 中浓度 | 1.00mg/m3 | |||||||||
30ppm | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | |
测定次数 | 氯苯 | 2-氯甲苯 | 3-氯甲苯 | 4-氯甲苯 | 1,3-二氯苯 | 1,4-二氯苯 | 1,2-二氯苯 | 1,3,5-三氯苯 | 1,2,4-三氯苯 | 1,2,3-三氯苯 | |
1 | 30.5506 | 29.9573 | 29.9787 | 29.0788 | 29.6828 | 29.5559 | 29.0831 | 30.1608 | 30.7018 | 30.6368 | |
2 | 29.6234 | 29.7784 | 30.4558 | 29.2545 | 29.5246 | 29.0616 | 29.1327 | 29.6411 | 30.2844 | 30.2963 | |
3 | 29.51 | 29.6047 | 29.9651 | 29.0423 | 29.4718 | 29.2927 | 28.951 | 28.9743 | 30.2823 | 29.981 | |
4 | 29.0144 | 29.4982 | 30.212 | 29.1648 | 29.8973 | 28.8866 | 29.1327 | 29.4063 | 30.5222 | 31.1708 | |
5 | 29.6434 | 30.2085 | 30.3508 | 29.2171 | 29.8973 | 29.0616 | 29.4659 | 30.2227 | 30.6588 | 30.5143 | |
6 | 29.9932 | 30.2794 | 30.5591 | 29.7051 | 29.9403 | 29.6542 | 30.1093 | 29.6842 | 30.9153 | 31.233 | |
平均值 | 29.7225 | 29.8878 | 30.2536 | 29.2438 | 29.7357 | 29.2521 | 29.3125 | 29.6816 | 30.5608 | 30.6387 | |
标准偏差 | 0.5141 | 0.3178 | 0.2467 | 0.2399 | 0.2055 | 0.3039 | 0.4258 | 0.4691 | 0.2492 | 0.4902 | |
相对标准偏差 | 1.73% | 1.06% | 0.82% | 0.82% | 0.69% | 1.04% | 1.45% | 1.58% | 0.82% | 1.60% | |
精密度 | 高浓度 | 2.50mg/m3 | |||||||||
75ppm | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | |
测定次数 | 氯苯 | 2-氯甲苯 | 3-氯甲苯 | 4-氯甲苯 | 1,3-二氯苯 | 1,4-二氯苯 | 1,2-二氯苯 | 1,3,5-三氯苯 | 1,2,4-三氯苯 | 1,2,3-三氯苯 | |
1 | 67.834 | 67.9884 | 68.6393 | 67.3826 | 68.1336 | 69.5451 | 67.8193 | 68.2225 | 69.8883 | 68.9351 | |
2 | 68.3433 | 68.2472 | 69.9157 | 67.9231 | 68.3485 | 69.9052 | 68.0601 | 69.0802 | 70.2668 | 69.143 | |
3 | 68.3907 | 69.0446 | 69.9736 | 68.6303 | 68.5183 | 69.9052 | 68.3934 | 68.9606 | 70.6764 | 69.0555 | |
4 | 68.5238 | 68.499 | 70.4886 | 70.9412 | 69.6326 | 70.0937 | 69.4147 | 69.1863 | 70.6222 | 70.5871 | |
5 | 69.1939 | 69.2914 | 69.4552 | 69.0369 | 69.6326 | 70.8362 | 70.7162 | 68.7395 | 72.0808 | 69.2237 | |
6 | 68.1164 | 69.5319 | 70.3168 | 69.4345 | 69.3925 | 70.8362 | 68.3437 | 69.0699 | 71.4560 | 70.6663 | |
平均值 | 68.4004 | 68.7671 | 69.7982 | 68.8914 | 68.9430 | 70.1869 | 68.7912 | 68.8765 | 70.8318 | 69.6018 | |
标准偏差 | 0.4582 | 0.6141 | 0.6709 | 1.2490 | 0.6844 | 0.5334 | 1.0892 | 0.3545 | 0.8034 | 0.8000 | |
相对标准偏差 | 0.67% | 0.89% | 0.96% | 1.81% | 0.99% | 0.76% | 1.58% | 0.51% | 1.13% | 1.15% | |
3.准确度 | 无组织标况采样体积30L,解析液体积1.00ml,向6只同批次空白活性炭吸附管中分别加入7.50μg、60.0μg、90.0μg标准品,后采集清洁空气30L,用胶帽密封两端,即得0.25mg/m3、2.00mg/m3、3.00mg/m3样品 将A,B两段分别转移至5ml具塞玻璃试管中,各加入1.0ml色谱纯二硫化碳,于超声清洗仪中超声解吸1min,静置30min,取1.0μL上机测试,计算6次测定平均值,标准偏差和相对标准偏差和加标回收率 | ||||||||||
低浓度 | |||||||||||
准确度 | 低浓度 | 2.50mg/m3 | |||||||||
7.5ppm | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | |
测定次数 | 氯苯 | 2-氯甲苯 | 3-氯甲苯 | 4-氯甲苯 | 1,3-二氯苯 | 1,4-二氯苯 | 1,2-二氯苯 | 1,3,5-三氯苯 | 1,2,4-三氯苯 | 1,2,3-三氯苯 | |
1 | 6.691 | 7.3729 | 7.077 | 6.6665 | 6.6557 | 6.401 | 7.0328 | 6.4512 | 7.4542 | 7.022 | |
2 | 6.7972 | 6.9915 | 7.521 | 6.9597 | 6.9851 | 7.0067 | 7.1283 | 7.7727 | 6.8627 | 7.2135 | |
3 | 6.7482 | 7.2128 | 7.2977 | 7.3634 | 6.8651 | 6.8374 | 7.083 | 6.8627 | 7.3865 | 7.152 | |
4 | 6.9708 | 7.2364 | 7.1195 | 6.6799 | 7.0076 | 7.152 | 6.9925 | 6.6287 | 7.1047 | 6.8315 | |
5 | 6.9778 | 7.4891 | 7.1054 | 7.2364 | 6.8046 | 6.9726 | 6.9755 | 6.8193 | 7.2963 | 7.152 | |
6 | 6.8681 | 7.3130 | 6.9570 | 6.6262 | 6.8046 | 6.8374 | 6.9344 | 6.5873 | 7.2005 | 7.3369 | |
平均值 | 6.8422 | 7.2693 | 7.1796 | 6.9220 | 6.8538 | 6.8679 | 7.0244 | 6.8537 | 7.2175 | 7.1180 | |
标准偏差 | 0.1177 | 0.1688 | 0.1998 | 0.3183 | 0.1305 | 0.2572 | 0.0718 | 0.4753 | 0.2143 | 0.1736 | |
相对标准偏差 | 1.72% | 2.32% | 2.78% | 4.60% | 1.90% | 3.75% | 1.02% | 6.93% | 2.97% | 2.44% | |
加标量 | 7.50 | 7.50 | 7.50 | 7.50 | 7.50 | 7.50 | 7.50 | 7.50 | 7.50 | 7.50 | |
回收率 | 91.23% | 96.92% | 95.73% | 92.29% | 91.38% | 91.57% | 93.66% | 91.38% | 96.23% | 94.91% | |
准确度 | 中浓度 | 2.00mg/m3 | |||||||||
60.0ppm | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | |
测定次数 | 氯苯 | 2-氯甲苯 | 3-氯甲苯 | 4-氯甲苯 | 1,3-二氯苯 | 1,4-二氯苯 | 1,2-二氯苯 | 1,3,5-三氯苯 | 1,2,4-三氯苯 | 1,2,3-三氯苯 | |
1 | 61.3855 | 61.4926 | 62.3214 | 62.08 | 62.2168 | 62.1589 | 60.9554 | 60.8366 | 63.8338 | 63.2238 | |
2 | 61.1936 | 61.489 | 62.0157 | 61.9752 | 62.1096 | 61.658 | 60.8142 | 60.7193 | 62.8742 | 62.886 | |
3 | 61.1547 | 60.8488 | 62.0121 | 61.9752 | 62.0047 | 61.9444 | 60.6072 | 60.8595 | 62.9686 | 63.3598 | |
4 | 61.2162 | 61.789 | 61.9915 | 61.9674 | 61.8157 | 61.6717 | 60.9179 | 60.3049 | 63.5243 | 62.482 | |
5 | 61.8262 | 61.995 | 62.5601 | 62.5784 | 62.2031 | 61.658 | 60.7964 | 60.5744 | 63.5154 | 62.2769 | |
6 | 61.6640 | 61.7561 | 62.4186 | 62.1033 | 62.2586 | 61.658 | 60.8775 | 60.6703 | 63.4628 | 62.5229 | |
平均值 | 61.4067 | 61.5618 | 62.2199 | 62.1133 | 62.1014 | 61.7915 | 60.8281 | 60.6608 | 63.3632 | 62.7919 | |
标准偏差 | 0.2785 | 0.3989 | 0.2460 | 0.2354 | 0.1670 | 0.2127 | 0.1239 | 0.2040 | 0.3675 | 0.4362 | |
相对标准偏差 | 0.45% | 0.65% | 0.40% | 0.38% | 0.27% | 0.34% | 0.20% | 0.34% | 0.58% | 0.69% | |
加标量 | 60.00 | 60.00 | 60.00 | 60.00 | 60.00 | 60.00 | 60.00 | 60.00 | 60.00 | 60.00 | |
回收率 | 102.34% | 102.60% | 103.70% | 103.52% | 103.50% | 102.99% | 101.38% | 101.10% | 105.61% | 104.65% | |
准确度 | 高浓度 | 3.00mg/m3 | |||||||||
90.0ppm | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | |
测定次数 | 氯苯 | 2-氯甲苯 | 3-氯甲苯 | 4-氯甲苯 | 1,3-二氯苯 | 1,4-二氯苯 | 1,2-二氯苯 | 1,3,5-三氯苯 | 1,2,4-三氯苯 | 1,2,3-三氯苯 | |
1 | 87.5800 | 88.3600 | 87.9700 | 84.6400 | 86.8900 | 89.9900 | 85.5200 | 85.2000 | 88.3700 | 85.0400 | |
2 | 86.7159 | 87.1692 | 88.1087 | 87.6414 | 87.9892 | 88.3147 | 86.7899 | 86.6228 | 88.1320 | 87.6355 | |
3 | 87.0434 | 87.5221 | 87.8939 | 87.5662 | 88.4716 | 88.5945 | 86.9751 | 86.9240 | 89.1677 | 88.0790 | |
4 | 86.8849 | 87.6250 | 88.0238 | 87.4742 | 88.2040 | 88.4081 | 87.0541 | 86.7808 | 88.5321 | 88.2255 | |
5 | 87.3790 | 87.7248 | 88.0981 | 87.8216 | 88.7811 | 89.0492 | 87.4596 | 87.2456 | 89.3372 | 88.5529 | |
6 | 88.4467 | 87.6743 | 88.2959 | 87.6602 | 89.8993 | 89.1828 | 87.4156 | 87.1249 | 90.2937 | 88.6238 | |
平均值 | 87.3417 | 87.6792 | 88.0651 | 87.1339 | 88.3725 | 88.9232 | 86.8691 | 86.6497 | 88.9721 | 87.6928 | |
标准偏差 | 0.6275 | 0.3882 | 0.1388 | 1.2272 | 0.9880 | 0.6269 | 0.7098 | 0.7451 | 0.7975 | 1.3476 | |
相对标准偏差 | 0.72% | 0.44% | 0.16% | 1.41% | 1.12% | 0.70% | 0.82% | 0.86% | 0.90% | 1.54% | |
加标量 | 90.00 | 90.00 | 90.00 | 90.00 | 90.00 | 90.00 | 90.00 | 90.00 | 90.00 | 90.00 | |
回收率 | 97.05% | 97.42% | 97.85% | 96.82% | 98.19% | 98.80% | 96.52% | 96.28% | 98.86% | 97.44% |