大佬救助,在用
ICP-MS测定未受污染的土壤金属浓度 ,质控样7408,7402,大部分金属的回收率都非常低(最低百分之10),个别金属回收率爆炸百分之几百,使用了四个内标
Sc,Rh,Re,Ge,内标回收率:空白样都是70%左右,7402样Sc120%,Ge257%Rh30%Re30%,7408样Sc110%,Ge78%Rh30%Re29%。
消解方法是6硝酸2盐酸1高氯酸2氢氟酸在石墨炉闭盖3h(120-140-160度梯度升温),开盖赶酸2h(120-140-160度梯度升温),除7408复加一次酸外,其他样都复加2次酸(一次1.5氢氟酸3硝酸,第二次3硝酸1高氯酸),最后剩0.5-0.8ml剩余溶液定容11ml
52Cr (KED) [μg/l] | 55Mn (KED) | 59Co (KED) | 60Ni (KED) | 63Cu (KED) | 66Zn (KED) | 77Se (KED) | 88Sr (KED) | 111Cd (KED) | 137Ba (KED) | 208Pb (KED) | 75As (KED) | 202Hg (KED) |
Sc,Rh,Re,Ge内标 | Cr | Mn | Co | Ni | Cu | Zn | Se | Sr | Cd | Ba | Pb | As | Hg |
33(7402) | 12.13974661 | 145.360189 | 2.122495226 | 4.308646342 | 2.766639964 | -3.479733044 | 15.36073074 | 42.79706547 | 0.073546209 | 834.9329363 | 16.85894077 | -17.19808467 | 0.014302905 |
7402真值 | 47 | 510 | 8.7 | 19.4 | 16.3 | 42 | 0.16 | 187 | 0.071 | 930 | 20 | 13.7 | 0.015 |
回收率 | 0.258292481 | 0.285019978 | 0.243964968 | 0.222095172 | 0.169732513 | -0.082850787 | 96.00456715 | 0.228861313 | 1.035862097 | 0.897777351 | 0.842947039 | -1.255334647 | 0.953527015 |
34(7408) | 25.78178274 | 267.0954838 | 5.48130984 | 13.14444089 | 9.509971765 | 15.07871183 | 17.13871509 | 149.7606418 | 0.0995013 | 473.5366436 | 17.1573733 | -10.04842431 | 0.02416819 |
7408真值 | 68 | 650 | 12.7 | 31.5 | 24.3 | 68 | 0.1 | 236 | 0.13 | 480 | 21 | 12.7 | 0.017 |
回收率 | 0.379143864 | 0.410916129 | 0.4315992 | 0.417283838 | 0.391356863 | 0.221745762 | 171.3871509 | 0.634578991 | 0.765394615 | 0.986534674 | 0.817017776 | -0.791214512 | 1.421658258 |