固体废物 金属元素 电感耦合等离子体质谱法HJ766.docx

方法验证报告检测项目：铝、金、硼、铁、钙、铋、铈、铯、镝、铒、铕、镓、钆、锗、铪、钬、铟、铱、钡、锡、镧、锂、镥、铌、钕、磷、镨、铂、铷、铼、铑、钌、钪、钐、锶、铽、碲、钍、钛、 铥、铀、钨、钇、镱、锆、钽方法名称及编号：固体废物 金属元素的测定 电感耦合等离子体质谱仪 HJ766-2015二 O 一七年二月、 实验目的以固体废物 金属元素的测定 电感耦合等离子体质谱仪 HJ766-2015 为标准对固体废物和固体废物浸出液中的铝、金、硼、铁、钙、铋、铈、 铯、镝、铒、铕、镓、钆、锗、铪、钬、铟、铱、钡、锡、镧、锂、镥、 铌、钕、磷、钯、镨、铂、铷、铼、铑、钌、钪、钐、锶、铽、碲、钍、 钛、铥、铀、钨、钇、镱、锆、钽进行实验本实验室现有条件基本符合 标准方法规定的条件，按照该方法进行基础实验，以验证本实验室开展该 项目的适用性二、 方法原理固体废物或固体废物浸出液经消解后，试样由载气带入雾化系统进行 雾化后，目标元素以气溶胶形式进入等离子的轴向通道，在高温和惰性气 体中被蒸发、解离、原子化和电离，转化成带电荷的正离子经离子采集系 统进入质谱仪，质谱仪根据离子的质荷比进行分离并定性、定量分析。

在 一定浓度范围内，离子的质荷比所对应的响应值与其浓度成正比三、 内容及结果1、标准曲线取浓度为100mg/L的多元素标准储备液10.0m L用1%硝酸定容至100mL，配制成浓度为10.0mg/L的标准中间液，取标准中间液1.0mL于 100mL 容量瓶中，用 1%硝酸稀释至刻度，配制的标准使用液浓度为 100ug/L，依次配制一系列待测元素标准溶液，可根据测量需要的调整校准 曲线的浓度范围在容量瓶中取一定体积的标准使用液，使用硝酸溶液配 制系列标准曲线，铝、金、硼、铁、钙、铋、铈、铯、镝、铒、铕、镓、 钆、锗、铪、钬、铟、铱、钡、锡、镧、锂、镥、铌、钕、磷、钯、镨、铂、铷、铼、铑、钌、钪、钐、锶、铽、碲、钍、钛、铥、铀、钨、钇、镱、锆浓度为 0pg/L、.5pg/L、1.0pg/L、5.0pg/L、10.0pg/L、20.0pg/L、40.0pg/L、50.0pg/L、100.0pg/L,钽浓度为 0.0pg/L、4.0pg/L、8.0pg/L、16.0pg/L、40.0pg/L、80.0yg/L、100.0yg/L ；线性结果见表 1表 1 线性实验结果序号元素 标准曲线方程序号元素标准曲线方程1铝AlY=0.2359 x+0.3533 ,r= 0.993425钪ScY=7056x+2333,r=0.99992金AuY= 139.6x+1.222 ,r=0.998626钐SmY=3413x+1.110 ,r=1.00003硼BY=1030 x+7336 ,r=1.000027锶SrY=0.6211x+0.2506,r=0.99994钡BaY=0.02865x+0.006801,r=1.00028锡SnY= 337.7x+919.0 ,r=0.99985铋BiY=11680 x+101.1 ,r=0.999929铽TbY=23150x+360.0 ,r=1.00006铈CeY= 19610x+2453 ,r=0.999930碲TeY=2.443 x+1.110 ,r=0.99987铯CsY=0.8516 x+0.09311 ,r=0.999931钍ThY= 16310x+ 255.6,r=0.99998镝DyY=5539 x+3.333 ,r=1.000032钛TiY=415.3 x+421.1 ,r=0.99999铒ErY= 7438x+3.333 ,r=1.000033铥TmY=22340 x+3.333 ,r=1.000010铕EuY=12500x+3.330 ,r=1.000034铀UY=0.1853x+0.001631,r=1.000011铁FeY=0.3965 x+4.623 ,r=0.990735钒VY= 0.3516x+0.6038 ,r=0.999912镓GaY=0.05620x+0.001515,r=1.00036钨WY=4095 x+161.1 ,r=0.999813钆GdY=4612x+1.556 ,r=1.000037钇YY= 16100x+1850 ,r=1.000014锗GeY=1722 x+1479 ,r=0.999938镱YbY=4978 x+ 2.220,r=1.000015铪HfY=422.5 x+ 104.5,r=0.998439钯PdY=123.1 x+6.667 ,r=0.989016钦HoY=22490 x+1.110 ,r=1.000040镨PrY=2310x+2.778 ,r=1.000017铟InY=13570 x+3.778 ,r=0.999941铷RbY=0.1223x+0.1863,r=0.999118铱IrY= 827.2x+5.553 ,r=0.999942铼ReY=6131 x+1.110 ,r=1.000019镧LaY=21260 x+153.3 ,r=1.000043钉RuY= 228.3x+3.333 ,r=0.999320锂LiY=0.06916x+0.1236,r=1.00044铑RhY= 12560x+7.445 ,r=0.999921镥LuY=21810 x+164.5 ,r=1.000045铂PtY= 286.2x+4.443 ,r=0.999822铌NbY= 9567x+1726 ,r=0.994646钽TaY=4.578x-7.733,r=0.999523钕NdY=4022x+1.555 ,r=1.000047锆ZrY= 7262x+3561 ,r=0.999524磷PY=4197x+48460 ,r=0.999748钙CaY=3.491x+1.093 ,r=0.99962、方法检出限2.1 固体废物分解法称取 0.1000~0.2000g 样品，置于聚四氟乙烯坩埚中，用少量水冲洗内 壁润湿试样后，加入硝酸4.0m 1、盐酸1.0m 1、氢氟酸1.0m 1、双氧水1.0ml, 在石墨消解仪上进行消解，消解后冷却至室温，打开盖子，进行赶酸，直 至尽干，用去离子水定容至50.0ml，分别测定，求得标准偏差SD,按照下 式计算检出限MDL,检出限试验结果见表2.1-1,表2.1-2：MDL=3.143*SD表 2.1-1 方法检出限元素检出浓度(mg/kg)标准偏差(SD)方法检出限(MDL) mg/kg1金Au0.1050.0970.1050.0810.1260.0810.0990.0140.042硼B0.1700.0960.1190.1440.1990.1830.2680.0530.173钮Bi0.5740.1640.1210.1050.0940.0890.0890.1640.524肺Ce14.37215.15215.46015.59615.69515.86715.9090.4951.565链Cs1.6031.6181.6381.6481.6611.7051.6450.0300.096鏑Dy0.9831.0001.0391.0281.0441.0441.0650.0260.087餌Er0.7530.7990.7970.8160.8070.8130.8260.0220.078错Eu0.1930.1970.2040.2010.2060.2090.2040.0050.029镣Ga3.8053.9283.8714.0013.9974.2354.0650.1300.4110轧Gd1.1631.2321.2531.2521.2361.2821.2780.0370.1211错Ge1.4101.3971.4151.4951.5341.5191.5540.0610.1912诒Hf3.0713.0223.1843.2803.9243.9253.7820.3751.1813钦Ho0.2100.2150.2230.2220.2250.2230.2270.0060.0214锢In0.0200.0100.0110.0100.0110.0120.0100.0030.0115铁Ir0.0510.0260.0160.0150.0150.0160.0180.0120.0416鋼La6.2346.5876.7236.7586.8366.9046.9060.2190.6917锂Li9.7799.7019.94510.16910.20710.63410.0890.2890.91元素检出浓度(mg/kg)标准偏差(SD)方法检出限(MDL) mg/kg18镥Lu0.1670.1780.1810.1780.1810.1820.1840.0050.0219铌Nb1.4171.3541.4471.6091.5811.5381.5180.0850.2720钕Nd5.5645.8596.0015.9616.0376.0626.1230.1730.5421钪Sc1.1391.1571.1461.1621.1841.1801.1840.0170.0522钐Sm1.1161.1881.1981.1961.2281.2251.2280.0370.1223锶Sr4.2204.1954.2044.2144.1914.3354.1840.0480.1524锡Sn16.02017.72017.70117.11415.15014.86015.62316.3133.4825铽Tb0.1720.1790.1860.1830.1870.1850.1840.0050.0226碲Te0.6640.5760.2660.3990.3210.2550.2100.1610.5027钍Th8.1598.772。