Analyte | Mass | #1 | #2 | #3 | #4 | #5 | 平均值 | SD | rsd |
Cr | 50 | 541.456 | 551.265 | 586.945 | 553.046 | 584.61 | 563.5 | 20.9 | 3.70% |
Cr | 52 | 540.136 | 557.958 | 606.738 | 564.482 | 592.188 | 572.3 | 26.8 | 4.69% |
Cr | 53 | 554.493 | 561.792 | 610.139 | 567.176 | 592.489 | 577.2 | 23.3 | 4.04% |
Rh | 103 | ||||||||
Cr-1 | 50 | 515.482 | 522.928 | 554.886 | 521.568 | 550.306 | 533.0 | 18.1 | 3.40% |
Cr-1 | 52 | 514.782 | 529.669 | 574.007 | 532.681 | 557.839 | 541.8 | 23.7 | 4.38% |
Cr-1 | 53 | 528.288 | 533.073 | 577.058 | 534.969 | 557.831 | 546.2 | 20.7 | 3.78% |
Sc | 45 | ||||||||
Cr-2 | 50 | 462.525 | 477.821 | 477.214 | 484.475 | 493.575 | 479.1 | 11.4 | 2.38% |
Cr-2 | 52 | 462.275 | 484.366 | 494.295 | 495.14 | 500.8 | 487.4 | 15.2 | 3.12% |
Cr-2 | 53 | 473.891 | 487.122 | 496.256 | 496.984 | 500.421 | 490.9 | 10.7 | 2.18% |
填加量 | ppb | 517.5907 | 515.519 | 504.2498 | 495.3418 | 501.8025 | |||
Cr | 50 | 104.6% | 106.9% | 116.4% | 111.6% | 116.5% | |||
Cr | 52 | 104.4% | 108.2% | 120.3% | 114.0% | 118.0% | |||
Cr | 53 | 107.1% | 109.0% | 121.0% | 114.5% | 118.1% | |||
Rh | 103 | 0.0% | 0.0% | 0.0% | 0.0% | 0.0% | |||
Cr-1 | 50 | 99.6% | 101.4% | 110.0% | 105.3% | 109.7% | |||
Cr-1 | 52 | 99.5% | 102.7% | 113.8% | 107.5% | 111.2% | |||
Cr-1 | 53 | 102.1% | 103.4% | 114.4% | 108.0% | 111.2% | |||
Sc | 45 | 0.0% | 0.0% | 0.0% | 0.0% | 0.0% | |||
Cr-2 | 50 | 89.4% | 92.7% | 94.6% | 97.8% | 98.4% | |||
Cr-2 | 52 | 89.3% | 94.0% | 98.0% | 100.0% | 99.8% | |||
Cr-2 | 53 | 91.6% | 94.5% | 98.4% | 100.3% | 99.7% |
Analyte | Mass | #1 | #2 | #3 | #4 | #5 | #6 | #7 | 平均值 | SD | rsd |
Cr | 50 | 1047.487 | 1074.877 | 1065.711 | 1053.264 | 1064.65 | 1096.89 | 1062.65 | 1066.504 | 16.06902 | 1.51% |
Cr | 52 | 1092.12 | 1096.89 | 1103.366 | 1094.855 | 1098.058 | 1111.056 | 1091.046 | 1098.199 | 6.988511 | 0.64% |
Cr | 53 | 1101.411 | 1104.978 | 1114.248 | 1103.762 | 1107.522 | 1115.295 | 1096.657 | 1106.268 | 6.716219 | 0.61% |
Rh | 103 | ||||||||||
Cr-1 | 50 | 997.001 | 1018.223 | 995.72 | 1001.967 | 1000.615 | 1006.015 | 995.98 | 1002.217 | 7.97458 | 0.80% |
Cr-1 | 52 | 1039.806 | 1039.481 | 1031.307 | 1042.058 | 1032.618 | 1019.555 | 1023.048 | 1032.553 | 8.677538 | 0.84% |
Cr-1 | 53 | 1048.399 | 1046.92 | 1041.174 | 1050.255 | 1041.204 | 1023.1 | 1028.004 | 1039.865 | 10.45474 | 1.01% |
Sc | 45 | ||||||||||
Cr-2 | 50 | 883.428 | 947.359 | 914.414 | 888.233 | 906.968 | 975.474 | 913.97 | 918.5494 | 32.64762 | 3.55% |
Cr-2 | 52 | 921.895 | 967.41 | 947.282 | 924.172 | 936.248 | 988.634 | 939.009 | 946.3786 | 24.07687 | 2.54% |
Cr-2 | 53 | 929.081 | 974.038 | 956.046 | 931.021 | 943.686 | 991.938 | 943.255 | 952.7236 | 23.10995 | 2.43% |
填加量 | ppb | 995.272 | 1011.761 | 1005.801 | 1013.548 | 1009.575 | 1006.993 | 1015.138 | |||
Cr | 50 | 104.24% | 105.25% | 104.96% | 102.93% | 104.46% | 107.93% | 103.70% | |||
Cr | 52 | 108.73% | 107.43% | 108.71% | 107.04% | 107.77% | 109.34% | 106.49% | |||
Cr | 53 | 109.66% | 108.23% | 109.79% | 107.91% | 108.71% | 109.76% | 107.05% | |||
Cr-1 | 50 | 99.17% | 99.65% | 98.00% | 97.87% | 98.12% | 98.91% | 97.13% | |||
Cr-1 | 52 | 103.47% | 101.75% | 101.54% | 101.83% | 101.29% | 100.25% | 99.79% | |||
Cr-1 | 53 | 104.33% | 102.49% | 102.52% | 102.63% | 102.14% | 100.61% | 100.28% | |||
Cr-2 | 50 | 87.76% | 92.65% | 89.92% | 86.65% | 88.85% | 95.88% | 89.05% | |||
Cr-2 | 52 | 91.62% | 94.63% | 93.19% | 90.20% | 91.75% | 97.18% | 91.52% | |||
Cr-2 | 53 | 92.34% | 95.28% | 94.06% | 90.87% | 92.48% | 97.51% | 91.93% |
Analyte | Mass | #1 | #2 | #3 | #4 | #5 | 平均值 | SD | rsd |
Cr | 50 | 1739.289 | 1718.659 | 1603.773 | 1611.835 | 1681.698 | 1671.1 | 61.4 | 3.67% |
Cr | 52 | 1729.58 | 1766.922 | 1666.061 | 1662.587 | 1759.501 | 1716.9 | 50.0 | 2.91% |
Cr | 53 | 1729.36 | 1764.347 | 1658.448 | 1663.238 | 1757.019 | 1714.5 | 50.7 | 2.96% |
Rh | 103 | ||||||||
Cr-1 | 50 | 1554 | 1629.708 | 1508.232 | 1509.512 | 1581.892 | 1556.7 | 51.4 | 3.30% |
Cr-1 | 52 | 1546.162 | 1675.855 | 1567.192 | 1557.851 | 1655.847 | 1600.6 | 60.5 | 3.78% |
Cr-1 | 53 | 1545.463 | 1673.104 | 1559.643 | 1558.199 | 1653.052 | 1597.9 | 60.2 | 3.77% |
Sc | 45 | ||||||||
Cr-2 | 50 | 1545.134 | 1459.446 | 1420.147 | 1422.036 | 1393.999 | 1448.2 | 59.0 | 4.08% |
Cr-2 | 52 | 1537.163 | 1501.237 | 1475.904 | 1467.429 | 1459.152 | 1488.2 | 31.6 | 2.12% |
Cr-2 | 53 | 1536.523 | 1498.448 | 1468.716 | 1467.514 | 1456.47 | 1485.5 | 32.5 | 2.19% |
填加量 | 1504.133 | 1517.14 | 1513.301 | 1503.852 | 1525.613 | ||||
Cr | 50 | 115.6% | 113.3% | 106.0% | 107.2% | 110.2% | |||
Cr | 52 | 115.0% | 116.5% | 110.1% | 110.6% | 115.3% | |||
Cr | 53 | 115.0% | 116.3% | 109.6% | 110.6% | 115.2% | |||
Rh | 103 | 0.0% | 0.0% | 0.0% | 0.0% | 0.0% | |||
Cr-1 | 50 | 103.3% | 107.4% | 99.7% | 100.4% | 103.7% | |||
Cr-1 | 52 | 102.8% | 110.5% | 103.6% | 103.6% | 108.5% | |||
Cr-1 | 53 | 102.7% | 110.3% | 103.1% | 103.6% | 108.4% | |||
Sc | 45 | 0.0% | 0.0% | 0.0% | 0.0% | 0.0% | |||
Cr-2 | 50 | 102.7% | 96.2% | 93.8% | 94.6% | 91.4% | |||
Cr-2 | 52 | 102.2% | 99.0% | 97.5% | 97.6% | 95.6% | |||
Cr-2 | 53 | 102.2% | 98.8% | 97.1% | 97.6% | 95.5% |
yangsm
第2楼2018/05/27
抱歉,单位为ug/Kg,补充
因为定量是以50毫升抛弃式消化瓶定量,故样品包含检量线皆以重量/重量为单位,
不知您为何认为以Rh为内标的数据较好?
因为有消化及赶酸前处理,回收率皆大于100%好像不太可能(空白值大约为20ppb以下)(我是空白基质称重0.45g后,分别加入标准品99.3285mg / Kg 0.25mL,0.5mL,0.75mL,以天平计算重量差换算加入量,消化赶酸後以抛弃式消化瓶定量至50毫升,再计算定量后净重,故样品及检量线皆以ppb即ug/Kg为单位)(添加1000ppb的样品在检测一星期前消化并定量完成)
检量线标准品浓度为2000、1500、1000、500、200、100、0 ppb
上机前,取标准品(样品亦同)10mL,加入Sc,Rh内标混合液200ppb 1mL,以VORTEX批次混合10秒,上机检测。
yangsm
第4楼2018/05/29
是1组Rh内标,2组Sc内标,3组无内标
我是使用PE DRC II,反应气体为NH3,
52Cr,53Cr反应气体流量开0.3;50Cr,铑,SC为标准模式。
推想好像是
1. 52Cr,53Cr反应气体流量开太大(52-17 = 38Ar,52-17 = 39K),
2.赶酸不完全(赶完酸后,消化瓶大约余2mL液体,定量至50mL,则定量后酸浓度大约是4%,理想是定量50mL赶酸后剩余体积约为0.5mL)
3.流洗时间1min好像不是很够(?),目标物浓度偏高,样品酸度大于标准液酸度,造成记忆效应之目标物流洗出来。
4.赶完酸后需静置,让氮化合物逸散?(50-14 = 36 Ar,Cl,S)
功率= 1350W,torch温度在点火后40分钟的变动会趋于稳定(30分至1小时不变),interface及cooling温度会基本不变。
我的经验告诉我酸度高,铑的感度会下降(好像是比重高,气动式进样量降低的缘故)
现在正逐步检讨中,希望先进能多指点一二。