石墨炉测沉积物中重金属元素的升温程序.pdf

实验小结实验小结实验小结实验小结:THGA原子原子原子原子吸收光谱升温程序吸收光谱升温程序吸收光谱升温程序吸收光谱升温程序-沉积物中重金属元素Cu、Pb、Cr、Cd、Co、Ni样品与进样量的选择?GSD-9（长江沉积物）?称重0.2-0.25g?湿法消化(HNO3+HClO3+HF)?0.5%HNO3定容至50ml进样量的选择1 1 1 1100100100100倍倍倍倍3 3 3 3倍倍倍倍3 3 3 3倍倍倍倍1 1 1 1加液加液加液加液40ul40ul40ul40ul稀释稀释稀释稀释20202020倍倍倍倍11.9 11.9 11.9 11.9 0.1 0.1 0.1 0.1 4.8 4.8 4.8 4.8 5.7 5.7 5.7 5.7 10.7 10.7 10.7 10.7 0.7 0.7 0.7 0.7 V GSD9 20(ul)V GSD9 20(ul)V GSD9 20(ul)V GSD9 20(ul)17.8 17.8 17.8 17.8 0.2 0.2 0.2 0.2 7.2 7.2 7.2 7.2 8.5 8.5 8.5 8.5 16.1 16.1 16.1 16.1 1.1 1.1 1.1 1.1 V GSD9 30(ul)V GSD9 30(ul)V GSD9 30(ul)V GSD9 30(ul)1363.6 1363.6 1363.6 1363.6 45.5 45.5 45.5 45.5 772.7 772.7 772.7 772.7 909.1 909.1 909.1 909.1 772.7 772.7 772.7 772.7 59.1 59.1 59.1 59.1 318.2 318.2 318.2 318.2 Mass for 0.2(pg)Mass for 0.2(pg)Mass for 0.2(pg)Mass for 0.2(pg)2045.5 2045.5 2045.5 2045.5 68.2 68.2 68.2 68.2 1159.1159.1159.1159.1 1 1 1 1363.6 1363.6 1363.6 1363.6 1159.1 1159.1 1159.1 1159.1 88.6 88.6 88.6 88.6 477.3 477.3 477.3 477.3 Mass for 0.3(pg)Mass for 0.3(pg)Mass for 0.3(pg)Mass for 0.3(pg)303030301 1 1 11717171720202020171717171.31.31.31.37 7 7 7CharactCharactCharactCharact MassMassMassMass8508508508507007007007001200120012001200110011001100110014001400140014007007007007001500150015001500Char TempChar TempChar TempChar Temp1500150015001500180018001800180019001900190019002300230023002300240024002400240014001400140014002300230023002300atom Tempatom Tempatom Tempatom Temp0.1150.1150.1150.1150.390.390.390.390.160.160.160.160.160.160.160.160.0720.0720.0720.0720.4250.4250.4250.425GSD9/200GSD9/200GSD9/200GSD9/2004 4 4 45 5 5 53 3 3 34 4 4 41.81.81.81.810101010GSDGSDGSDGSD-9 9 9 9-SDSDSDSD2323232378787878323232323232323214.414.414.414.485858585GSDGSDGSDGSD-9 9 9 9PbPbPbPbZnZnZnZnCuCuCuCuNiNiNiNiCoCoCoCoCdCdCdCdCrCrCrCrCr20ul进样灰化温度的选择Char temp1400oCTemp-PA00.050.10.150.2900100011001200130014001500160017001800Char TempPeak areaTemp-PA/BA0510152025900100011001200130014001500160017001800Char TempPeak/BK Temp-BA00.0020.0040.0060.0080.010.0120.014900100011001200130014001500160017001800Char tempBK areaChar Temp-PH00.050.10.150.20.250.3900100011001200130014001500160017001800Char tempPeak HighBH-Char temp00.0050.010.0150.020.0250.030.035900100011001200130014001500160017001800Char tempBK HighChar Temp-PH/BH05101520900100011001200130014001500160017001800Char tempPH/BHCr灰化升温梯度Char ramp time=10sPeak area-ramp time00.040.080.120.1651015202530Chart ramp timePeak areaBKA-ramp time00.0020.0040.0060.0080.010.01251015202530Chart ramp timeBK areaPeak/BK-ramp time036912151851015202530Chart ramp timePeak/BKPeak High-ramp time00.060.120.180.240.351015202530Chart ramp timePeak areaBKH-ramp time00.0050.010.0150.020.0250.0351015202530Chart ramp timeBK areaPeak/BK-ramp time03691251015202530Chart ramp timePeak/BKCr灰化时间Char time=20sPA-Chart hold time00.040.080.120.16510152025303540Chart Hold timePeak areaBA-Chart hold time00.0030.0060.0090.012510152025303540Chart hold timeBK areaPA/BA-Chart hold time0369121518510152025303540Chart hold timePeak/BK areaPH-Chart hold time00.050.10.150.20.250.3510152025303540Chart Hold timePeak HighBH-Chart hold time00.010.020.030.04510152025303540Chart hold timeB HighPH/BH-Chart hold time0246810510152025303540Chart hold timePH/BHCr原子化温度Atom temp=2100Atom temp-Peak area00.050.10.150.217001800190020002100220023002400Atom TempPeak areaAtom temp-Bk area00.0050.010.0150.0217001800190020002100220023002400Atom TempBackground AreaPA/BA-Atom temp0510152017001800190020002100220023002400Atom tempPA/BAAtom temp-Peak High00.050.10.150.20.250.317001800190020002100220023002400Atom TempPeak HighAtom temp-Bk High00.010.020.0317001800190020002100220023002400Atom TempBK HighPH/BH-Atom temp05101517001800190020002100220023002400Atom tempPH/BHCrCo10ul进样灰化温度的选择Char temp=1300oCTemp-PA00.020.040.060.080.110001100120013001400150016001700Char TempPeak areaTemp-PA/BA00.40.81.21.6210001100120013001400150016001700Char TempPeak/BK Temp-BA00.020.040.0610001100120013001400150016001700Char tempBK areaChar Temp-PH00.020.040.060.080.10.120.1410001100120013001400150016001700Char tempPeak HighBH-Char temp00.040.080.120.1610001100120013001400150016001700Char tempBK HighChar Temp-PH/BH00.40.81.21.6210001100120013001400150016001700Char tempPH/BHCo灰化升温梯度Char ramp time=10sPeak area-ramp time00.020.040.060.080.151015202530Char ramp timePeak areaBKA-ramp time00.010.020.030.040.050.0651015202530Char ramp timeBK areaPeak/BK-ramp time00.511.5251015202530Char ramp timePeak/BKPeak High-ramp time00.050.10.1551015202530Char ramp timePeak areaBKH-ramp time00.020.040.060.080.10.1251015202530Char ramp timeBK areaPeak/BK-ramp time00.511.551015202530Char ramp timePeak/BKCo灰化时间Char time=20sPA-Chart hold time00.020.040.060.080.101020304050Char Hold timePeak areaBA-Chart hold time00.020.040.060.0801020304050Char hold timeBK areaPA/BA-Chart hold time012345678901020304050Char hold timePeak/BK areaPH-Chart hold time0.00000.05000.10000.150001020304050Char Hold timePeak HighBH-Chart hold time00.050.10.1501020304050Char hold timeBK HPH/BH-Chart hold time00.511.522.533.5401020304050Char hold timePH/BHCo原子化温度Atom temp=2400Atom temp-Peak area0.000.050.100.1518001900200021002200230024002500Atom TempPeak areaAtom temp-Bk area0.000.100.200.300.400.5018001900200021002200230024002500Atom TempBK AreaPA/BA-Atom temp0.00.20.40.60.81.01.218001900200021002200230024002500Atom tempPA/BAAtom temp-Peak High0.000.050.100.150.200.250.300.3518001900200021002200230024002500Atom TempPeak HighAtom temp-Bk High0.000.050.100.150.200.2518001900200021002200230024002500Atom TempBK HighPH/BH-Atom temp0.00.51.01.52.018001900200021002200230024002500Atom tempPH/BHCoPb20ul进样灰化温度的选择Char temp=500oC00.020.040.060.080.10.12300400500600700800900100011001200灰化温度灰化温度灰化温度灰化温度峰面积峰面积峰面积峰面积00.511.522.53300400500600700800900100011001200灰化温度灰化温度灰化温度灰化温度峰面积峰面积峰面积峰面积/背景背景背景背景 00.010.020.030.040.050.060.07300400500600700800900100011001200灰化温度灰化温度灰化温度灰化温度背 景 峰 面 积背 景 峰 面 积背 景 峰 面 积背 景 峰 面 积00.050.10.150.20.25300400500600700800900100011001200灰化温度灰化温度灰化温度灰化温度峰高峰高峰高峰高00.010020.030.040.050.060.07300400500600700800900100011001200灰化温度灰化温度灰化温度灰化温度背景峰高背景峰高背景峰高背景峰高00.511.522.533.54300400500600700800900100011001200灰化温度灰化温度灰化温度灰化温度峰高峰高峰高峰高/背景背景背景背景Pb灰化升温梯度Char ramp time=10s00.020.040.060.080.10.1251015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温峰面积峰面积峰面积峰面积00.010.020.030.040.050.0651015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温背景峰面积背景峰面积背景峰面积背景峰面积00.511.522.551015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温峰面积峰面积峰面积峰面积/背景背景背景背景00.050.10.150.251015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温峰高峰高峰高峰高00.010.020.030.040.050.060.0751015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温背景峰高背景峰高背景峰高背景峰高00.511.522.533.551015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温峰高峰高峰高峰高/背景背景背景背景Pb灰化时间Char time=20s00.020.040.060.080.10.12510152025303540灰化时间灰化时间灰化时间灰化时间峰面积峰面积峰面积峰面积00.020.040.060.08510152025303540灰化时间灰化时间灰化时间灰化时间背景峰面积背景峰面积背景峰面积背景峰面积0123510152025303540灰化时间灰化时间灰化时间灰化时间峰面积峰面积峰面积峰面积/背景背景背景背景0.000.050.100.150.200.25510152025303540灰化时间灰化时间灰化时间灰化时间峰高峰高峰高峰高00.020.040.060.08510152025303540灰化时间灰化时间灰化时间灰化时间背景峰高背景峰高背景峰高背景峰高01234510152025303540灰化时间灰化时间灰化时间灰化时间峰高峰高峰高峰高/背景背景背景背景Pb原子化温度Atom temp=15000.000.050.100.151000110012001300140015001600170018001900原子化温度原子化温度原子化温度原子化温度峰 面 积峰 面 积峰 面 积峰 面 积0.000.020.040.060.080.101000110012001300140015001600170018001900原子化温度原子化温度原子化温度原子化温度背景峰面积背景峰面积背景峰面积背景峰面积0.00.51.01.52.02.53.01000110012001300140015001600170018001900原子化温度原子化温度原子化温度原子化温度峰 面 积峰 面 积峰 面 积峰 面 积/背 景背 景背 景背 景0.000.050.100.150.201000110012001300140015001600170018001900原子化温度原子化温度原子化温度原子化温度峰 高峰 高峰 高峰 高0.000.010.020.030.040.050.060.070.081000110012001300140015001600170018001900原子化温度原子化温度原子化温度原子化温度背景峰高背景峰高背景峰高背景峰高0.00.51.01.52.02.53.03.51000110012001300140015001600170018001900原子化温度原子化温度原子化温度原子化温度峰 高峰 高峰 高峰 高/背 景背 景背 景背 景PbNi10ul进样灰化温度的选择Char temp=1400oC00.050.10.150.20.259001000110012001300 14001500160017001800灰化温度灰化温度灰化温度灰化温度峰面积峰面积峰面积峰面积00.40.81.21.62900100011001200130014001500160017001800灰化温度灰化温度灰化温度灰化温度峰 面 积峰 面 积峰 面 积峰 面 积/背 景背 景背 景背 景00.040.080.120.16900100011001200130014001500160017001800灰化温度灰化温度灰化温度灰化温度背 景 峰 面 积背 景 峰 面 积背 景 峰 面 积背 景 峰 面 积00.10.20.30.4900100011001200130014001500160017001800灰化温度灰化温度灰化温度灰化温度峰 高峰 高峰 高峰 高00.050.10.150.20.250.30.35900100011001200130014001500160017001800灰化温度灰化温度灰化温度灰化温度背 景 峰 高背 景 峰 高背 景 峰 高背 景 峰 高00.40.81.21.62900100011001200130014001500160017001800灰化温度灰化温度灰化温度灰化温度峰 高峰 高峰 高峰 高/背 景背 景背 景背 景Ni灰化升温梯度Char ramp time=10s00.050.10.150.20.2551015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温峰面积峰面积峰面积峰面积00.040.080.120.1651015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温背景峰面积背景峰面积背景峰面积背景峰面积00.40.81.21.6251015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温峰面积峰面积峰面积峰面积/背景背景背景背景00.10.20.30.451015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温峰高峰高峰高峰高00.050.10.150.20.2551015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温背景峰高背景峰高背景峰高背景峰高00.40.81.21.6251015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温峰高峰高峰高峰高/背景背景背景背景Ni灰化时间Char time=20s00.050.10.150.20.25510152025303540灰化时间灰化时间灰化时间灰化时间峰面积峰面积峰面积峰面积00.020.040.060.080.1510152025303540灰化时间灰化时间灰化时间灰化时间背景峰面积背景峰面积背景峰面积背景峰面积01234510152025303540灰化时间灰化时间灰化时间灰化时间峰面积峰面积峰面积峰面积/背景背景背景背景00.10.20.30.4510152025303540灰化时间灰化时间灰化时间灰化时间峰高峰高峰高峰高00.050.10.150.20.25510152025303540灰化时间灰化时间灰化时间灰化时间背景峰高背景峰高背景峰高背景峰高00.511.522.5510152025303540灰化时间灰化时间灰化时间灰化时间峰高峰高峰高峰高/背景背景背景背景Ni原子化温度Atom temp=23000.000.050.100.150.200.250.3017001800190020002100220023002400原子化温度原子化温度原子化温度原子化温度峰面积峰面积峰面积峰面积0.000.050.100.150.200.250.301700 18001900 2000 2100 22002300 2400原子化温度原子化温度原子化温度原子化温度背景峰面积背景峰面积背景峰面积背景峰面积0.00.20.40.60.81.01.21.417001800190020002100220023002400原子化温度原子化温度原子化温度原子化温度峰面积峰面积峰面积峰面积/背景背景背景背景0.000.050.100.150.200.250.3017001800190020002100220023002400原子化温度原子化温度原子化温度原子化温度峰高峰高峰高峰高0.000.050.100.150.200.251700 18001900 2000 2100 22002300 2400原子化温度原子化温度原子化温度原子化温度背景峰高背景峰高背景峰高背景峰高0.00.20.40.60.81.01.21.417001800190020002100220023002400原子化温度原子化温度原子化温度原子化温度峰高峰高峰高峰高/背景背景背景背景NiCu7ul进样灰化温度的选择Char temp=1000oCTemp-PA00.050.10.150.20.2570080090010001100 12001300140015001600灰化温度灰化温度灰化温度灰化温度峰面积峰面积峰面积峰面积Temp-PA/BA00.10.20.30.40.50.60.70.80.970080090010001100 120013001400 15001600灰化温度灰化温度灰化温度灰化温度PeakA/BK Temp-BA00.050.10.150.20.250.37008009001000110012001300140015001600灰化温度灰化温度灰化温度灰化温度BK areaChar Temp-PH00.050.10.150.27008009001000110012001300140015001600灰化温度灰化温度灰化温度灰化温度峰高峰高峰高峰高BH-Char temp00.050.10.150.20.257008009001000110012001300140015001600灰化温度灰化温度灰化温度灰化温度BK HighChar Temp-PH/BH00.20.40.60.811.27008009001000110012001300140015001600灰化温度灰化温度灰化温度灰化温度PH/BHCu灰化升温梯度Char ramp time=10s00.050.10.150.20.2551015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温峰面积峰面积峰面积峰面积00.050.10.150.20.250.351015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温BK area00.20.40.60.851015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温PeakA/BK00.050.10.150.251015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温峰高峰高峰高峰高00.050.10.150.20.2551015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温BK H00.20.40.60.8151015202530灰化斜坡升温灰化斜坡升温灰化斜坡升温灰化斜坡升温PeakH/BKCu灰化时间Char time=20sPA-Chart hold time00.050.10.150.20.25510152025303540灰化时间灰化时间灰化时间灰化时间峰面积峰面积峰面积峰面积BA-Chart hold time00.10.20.3510152025303540灰化时间灰化时间灰化时间灰化时间BK areaPA/BA-Chart hold time0123456789510152025303540灰化时间灰化时间灰化时间灰化时间Peak/BK areaPH-Chart hold time0.00000.05000.10000.15000.2000510152025303540灰化时间灰化时间灰化时间灰化时间峰高峰高峰高峰高BH-Chart hold time00.050.10.150.2510152025303540灰化时间灰化时间灰化时间灰化时间B HighPH/BH-Chart hold time00.511.522.5510152025303540灰化时间灰化时间灰化时间灰化时间PH/BHCu原子化温度Atom temp=1900Atom temp-Peak area0.000.050.100.150.20140015001600170018001900200021002200原子化温度原子化温度原子化温度原子化温度峰 面 积峰 面 积峰 面 积峰 面 积Atom temp-Bk area0.000.050.100.150.200.25140015001600170018001900200021002200原子化温度原子化温度原子化温度原子化温度Background AreaPA/BA-Atom temp0.00.20.40.60.81.01.2140015001600170018001900200021002200原子化温度原子化温度原子化温度原子化温度PA/BAAtom temp-Peak High0.000.050.100.150.20140015001600170018001900200021002200原子化温度原子化温度原子化温度原子化温度峰 高峰 高峰 高峰 高Atom temp-Bk High0.000.050.100.150.20140015001600170018001900200021002200原子化温度原子化温度原子化温度原子化温度BK HighPH/BH-Atom temp0.00.20.40.60.81.01.2140015001600170018001900200021002200原子化温度原子化温度原子化温度原子化温度PH/BHCuCdwithout matrix modifier40ul进样灰化温度的选择Char temp=500oCTemp-A s00.010.020.030.040.05200300400500600700800900Chart TempA-sTemp-Peak/BK00.050.10.150.20.25200300400500600700800900Chart TempPeak/BKTemp-BK00.050.10.150.20.250.3200300400500600700800900Chart tempBK areaCd灰化升温梯度Char ramp time=10sPeak area-ramp time00.020.040.060.080.151015202530Chart ramp timePeak areaBK-ramp time00.050.10.150.251015202530Chart ramp timeBK areaPeak/BK-ramp time00.10.20.30.451015202530Chart ramp timePeak/BKCd灰化时间Char time=20sAs-Chart hold time00.020.040.060.080.151015202530Chart Hold timePeak areaBK-Chart hold time00.050.10.150.251015202530Chart hold timeBK areaP/BK-Chart hold time00.10.20.30.40.551015202530Chart hold timePeak/BK areaCd原子化温度Atom temp=1000Atom temp-As00.010.020.030.040.050.0610001100120013001400150016001700180019002000210022002300Atom TempAsAtom temp-Bk area00.10.20.30.40.50.610001100120013001400150016001700180019002000210022002300Atom TempBackground AreaPeak/Bk-Atom temp00.050.10.150.20.250.30.350.40.4510001100120013001400150016001700180019002000210022002300Atom tempPeak/BkCd