固体废物金属元素电感耦合等离子体质谱法HJ766-2023年

方法验证报告检测工程：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HJ766-2023O一七年二月一、试验目的HJ766-2023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、钽进展试验。本试验室现有条件根本符合标准方法规定的条件，依据该方法进展根底试验，以验证本试验室开展该工程的适用性。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展雾化后，目标元素以气溶胶形式进入等离子的轴向通道，在高温顺惰性气体中被蒸发、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，质谱仪依据离子的质荷比进展分别并定性、定量分析。在肯定浓度范围内，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100mg/L10.0mL1%硝酸定容至100mL，配制成浓度为10.0mg/L1.0mL于100mL1%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，可依据测量需要的调整校准曲线的浓度范围。在容量瓶中取肯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、0μg/L0.5μg/L1.0μg/L5.0μg/L10.0μg/L20.0μg/L40.0μg/L、50.0μg/100.0.4.8.16.40.、、100.0μg/L1。表1 线性试验结果序号元素标准曲线方程序号元素标准曲线方程1AlY=0.2359x+0.3533,r=0.993425ScY=7056x+2333,r=0.99992AuY=139.6x+1.222,r=0.998626SmY=3413x+1.110,r=1.00003BY=1030x+7336,r=1.000027SrY=0.6211x+0.2506,r=0.99994BaY=0.02865x+0.006801,r=1.00028SnY=337.7x+919.0,r=0.99985BiY=11680x+101.1,r=0.999929TbY=23150x+360.0,r=1.00006CeY=19610x+2453,r=0.999930TeY=2.443x+1.110,r=0.99987CsY=0.8516x+0.09311,r=0.999931ThY=16310x+255.6,r=0.99998DyY=5539x+3.333,r=1.000032TiY=415.3x+421.1,r=0.99999ErY=7438x+3.333,r=1.000033TmY=22340x+3.333,r=1.000010EuY=12500x+3.330,r=1.000034UY=0.1853x+0.001631,r=1.000011FeY=0.3965x+4.623,r=0.990735VY=0.3516x+0.6038,r=0.999912GaY=0.05620x+0.001515,r=1.00036WY=4095x+161.1,r=0.999813GdY=4612x+1.556,r=1.000037YY=16100x+1850,r=1.000014GeY=1722x+1479,r=0.999938YbY=4978x+2.220,r=1.000015HfY=422.5x+104.5,r=0.998439钯PdY=123.1x+6.667,r=0.989016HoY=22490x+1.110,r=1.000040镨PrY=2310x+2.778,r=1.000017InY=13570x+3.778,r=0.999941RbY=0.1223x+0.1863,r=0.999118IrY=827.2x+5.553,r=0.999942ReY=6131x+1.110,r=1.000019LaY=21260x+153.3,r=1.000043RuY=228.3x+3.333,r=0.999320LiY=0.06916x+0.1236,r=1.00044RhY=12560x+7.445,r=0.999921LuY=21810x+164.5,r=1.000045铂PtY=286.2x+4.443,r=0.999822NbY=9567x+1726,r=0.994646TaY=4.578x-7.733,r=0.999523NdY=4022x+1.555,r=1.000047ZrY=7262x+3561,r=0.999524磷PY=4197x+48460,r=0.999748CaY=3.491x+1.093,r=0.99962、方法检出限固体废物分解法0.1000~0.2023g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，参加硝酸4.0ml、盐酸1.0ml、氢氟酸1.0ml、双氧水1.0ml，在石墨消解仪上进展消解，消解后冷却至室温，翻开盖子，进展赶酸，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，依据下式计算检出限MDL2.1-12.1-2：MDL=3.143*SD元素〔mg/kg〕元素〔mg/kg〕标准偏差〔SD〕方法检出限1Au0.1050.0970.1050.0810.1260.0810.0990.0140.042B0.1700.0960.1190.1440.1990.1830.2680.0530.173Bi0.5740.1640.1210.1050.0940.0890.0890.1640.524Ce14.37215.15215.46015.59615.69515.86715.9090.4951.565Cs1.6031.6181.6381.6481.6611.7051.6450.0300.096Dy0.9831.0001.0391.0281.0441.0441.0650.0260.087Er0.7530.7990.7970.8160.8070.8130.8260.0220.078Eu0.1930.1970.2040.2010.2060.2090.2040.0050.029Ga3.8053.9283.8714.0013.9974.2354.0650.1300.4110Gd1.1631.2321.2531.2521.2361.2821.2780.0370.1211Ge1.4101.3971.4151.4951.5341.5191.5540.0610.1912Hf3.0713.0223.1843.2803.9243.9253.7820.3751.1813Ho0.2100.2150.2230.2220.2250.2230.2270.0060.0214In0.0200.0100.0110.0100.0110.0120.0100.0030.0115Ir0.0510.0260.0160.0150.0150.0160.0180.0120.0416La6.2346.5876.7236.7586.8366.9046.9060.2190.6917Li9.7799.7019.94510.16910.20710.63410.0890.2890.91元素 度〔mg/kg〕

〔SD〕

方法检出限〔MDL〕mg/kg18Lu0.1670.1780.1810.1780.1810.1820.1840.0050.0219Nb1.4171.3541.4471.6091.5811.5381.5180.0850.2720Nd5.5645.8596.0015.9616.0376.0626.1230.1730.5421Sc1.1391.1571.1461.1621.1841.1801.1840.0170.0522Sm1.1161.1881.1981.1961.2281.2251.2280.0370.1223Sr4.2204.1954.2044.2144.1914.3354.1840.0480.1524Sn16.02017.72017.70117.11415.15014.86015.62316.3133.4825Tb0.1720.1790.1860.1830.1870.1850.1840.0050.0226Te0.6640.5760.2660.3990.3210.2550.2100.1610.5027Th8.1598.7728.8528.8168.7988.8018.8160.2290.7228Tm0.1300.1370.1370.1360.1360.1410.1410.0040.0129U5.0085.3255.3575.5885.4735.6715.3690.1990.6230W0.5420.5360.5260.5100.5000.5070.5540.0190.0631Y4.6504.8764.9694.9745.0515.0675.0930.1420.4532Yb1.0011.0411.0801.0561.0701.0971.0690.0290.0933钯Pd6.0725.8155.6395.5805.4775.5405.7820.1900.6034镨Pr1.5161.5981.6341.6231.6571.6591.6570.0480.1535Rb76.10678.39277.65080.22580.89585.73882.5511.4904.6836Re0.0080.0020.0030.0010.0010.0010.0010.0020.00837Ru0.0300.0360.0390.0490.0380.0380.0260.0070.0238Rh0.0090.0050.0050.0040.0040.0040.0040.0020.00539铂Pt0.0600.0480.0420.0430.0460.0340.0480.0070.0240Ta0.4970.4960.4960.4970.4970.5000.4990.0020.00541Zr11.47112.76012.52212.31112.1809.39110.0401.2153.82元素标准偏差元素标准偏差〔SD〕方法检出限1Al5.1594.9154.9204.8684.8144.9614.7560.1190.372Fe6.7176.6796.4296.6336.7646.3736.7000.1400.443Ti0.5430.5430.5670.5810.5850.5910.5890.0190.064磷P0.7180.7220.7030.7180.7140.7180.7030.0070.025Ca41.87440.18842.21339.70143.18141.87440.1881.2974.08元素元素标准偏差〔SD〕方法检出限150~200g1：10的比例参加浸提剂，于翻转振荡2318h50.0ml，置于消4.0ml1.0ml盐酸，将消解罐放入装置内进展消解，，50.0ml容量瓶中。分SDMDL，检出限试验结果2.2-12.2-2：MDL=3.143*SD元素标准偏差元素标准偏差〔SD〕方法检出限1Au1.4251.2341.0111.4251.2341.0111.4250.0870.272B6.4695.5624.7187.2196.4695.5624.7180.8752.753Bi0.0690.1410.1010.0690.0740.0570.0390.0870.274Ce8.8538.1597.9587.6097.2986.9736.6598.8538.165Cs17.31617.80917.85018.43219.04618.06820.8791.0993.456Dy9.1258.7408.4318.2597.9687.6717.3800.2800.887Er9.2258.9428.6258.3807.9977.7077.4430.3451.098Eu10.51210.1069.8489.5499.2748.9068.6170.3130.989Ga14.16915.18914.47414.74916.39614.16916.3860.8932.8110Gd9.0328.7058.4938.2078.0057.6877.2770.2670.8411Ge0.2320.2140.2340.1410.1740.1450.1320.0410.1312Hf6.5236.3135.9795.8605.8296.5235.8650.2920.9213Ho9.1618.8018.4888.2857.9877.6547.3480.2960.9314In0.0080.0070.0050.0040.0050.0040.0010.0020.006元素

〔SD〕

方法检出限〔MDL〕μg/L15Ir0.0310.0030.0120.0030.0010.0030.0310.0110.0316La8.7808.2607.9887.6137.3547.0616.7500.3471.0917Lu9.3088.9838.6778.4148.1477.8947.5680.3100.9818Nd9.0278.5938.1888.0767.6017.3986.9540.3541.1119磷P5.8745.6355.6175.7165.5455.7765.8740.1090.3420Sc8.3337.9357.6347.2636.9056.4576.0090.3871.2221Sm9.1168.6558.3418.1137.7907.4447.1560.3160.9922Ti0.8670.8960.9440.6580.7620.7200.7250.0990.3123Sn5.8575.9825.7685.4335.5945.2155.8570.2600.8224Tb9.1248.6658.4218.2017.8617.5717.2340.2960.9325Te3.9574.8674.8213.9114.1844.6853.4560.4971.5626Th9.0678.8128.5858.2758.0527.7409.0670.2920.9227Tm9.1668.8618.5758.3308.0097.7187.4380.3140.9928U5.9985.7625.9465.6545.9985.7625.2450.2460.7729W14.86514.13513.62013.19712.80012.41614.8650.8212.5830Y8.6158.0637.7047.3596.9336.6616.2820.4181.3131Yb9.1968.8658.6648.3147.9737.6547.4000.3401.0732钯Pd0.6170.6080.5900.6170.6080.5900.6170.0110.0433镨Pr8.7778.3168.0547.7797.3787.1216.8390.3471.0934Re0.1260.1180.1190.1140.1040.1050.0930.0100.0335Ru2.4142.1512.0982.0251.9081.9372.1660.1580.5036Rh1.1121.0430.9840.9510.9170.9540.9430.0630.2037铂Pt0.0430.0000.0000.0080.0160.0000.0190.0140.0438Zr8.4597.8747.5137.0778.4597.8747.5130.5061.5939Fe153.730153.379158.179159.109153.730155.615153.9252.3587.412.2-2方法检出限元素〔mg/L〕标准偏差〔SD〕方法检出限1Li1.4501.4671.4061.4501.4671.4061.3420.0260.082Al2.3072.3172.2122.2402.1482.2392.3980.0760.24素〔SD〕〔MDL〕mg/L3铷Rb0.5090.5500.5280.5390.5550.5570.6000.0260.084Sr5.4785.6115.5605.6375.4665.5275.8360.1170.37元〔元〔mg/L〕标准偏差方法检出限、固体废物分解法0.1000~0.2023g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，参加硝酸4.0ml、盐酸1.0ml、氢氟酸1.0ml、双氧水1.0ml，在石墨消解仪上进展消解，消解后冷却至室温，翻开盖子，进展赶酸，直3.1-2。

元素土壤样品溶液检出浓度〔mg/kg〕相对标准偏差元素土壤样品溶液检出浓度〔mg/kg〕相对标准偏差〔RSD%〕Ag0.2820.2860.2900.2880.2920.2970.2840.2881.68Au0.1050.0970.1050.0810.1260.0810.0990.09914.4B0.1700.1190.1440.1990.1830.165--0.16317.4Bi0.1210.1050.0940.0890.0890.098--0.09912.3Ce14.37215.15215.46015.59615.69515.86715.90915.4363.21Cs1.6031.6181.6381.6481.6611.7051.6451.6461.83Dy0.9831.0001.0391.0281.0441.0441.0651.0292.54Er0.7530.7990.7970.8160.8070.8130.8260.8022.74Eu0.1930.1970.2040.2010.2060.2090.2040.2022.51Ga3.8053.9283.8714.0013.9974.2354.0653.9863.26Gd1.1631.2321.2531.2521.2361.2821.2781.2422.97Ge1.4101.3971.4151.4951.5341.5191.5541.4754.12Hf3.0713.0223.1843.2803.9243.9253.7823.45510.9Ho0.2100.2150.2230.2220.2250.2230.2270.2212.56In0.0200.0100.0110.0100.0110.0120.0100.0114.72Ir0.0160.0150.0150.0160.0180.017--0.0167.23元素 土壤样品溶液检出浓度〔mg/kg〕

相对标准偏差〔RSD%〕La6.2346.5876.7236.7586.8366.9046.9066.7073.26Li9.7799.7019.94510.16910.20710.63410.08910.0752.87Lu0.1670.1780.1810.1780.1810.1820.1840.1792.87Nb1.4171.3541.4471.6091.5811.5381.5181.4955.70Nd5.5645.8596.0015.9616.0376.0626.1235.9442.91Sc1.1391.1571.1461.1621.1841.1801.1841.1651.48Sm1.1161.1881.1981.1961.2281.2251.2281.1973.06Sr4.2204.1954.2044.2144.1914.3354.1844.2201.14Sn16.02017.72017.70117.11417.10517.12616.58217.0533.52Tb0.1720.1790.1860.1830.1870.1850.1840.1822.74Te0.2660.3990.3210.2550.3150.302--0.31016.5Th8.1598.7728.8528.8168.7988.8018.8168.7162.62Tm0.1300.1370.1370.1360.1360.1410.1410.1372.67U5.0085.3255.3575.5885.4735.6715.3695.3993.68W0.5420.5360.5260.5100.5000.507--0.5203.00Y4.6504.8764.9694.9745.0515.0675.0934.9542.86Yb1.0011.0411.0801.0561.0701.0971.0691.0592.72钯Pd6.0725.8155.6395.5805.4775.5405.7825.7013.33镨Pr1.5161.5981.6341.6231.6571.6591.6571.6212.94Rb78.39280.22580.89582.55181.23479.365--80.4441.82Re0.0010.0010.0010.0010.0010.001--0.00117.6Ru0.0300.0360.0390.0380.0380.026--0.03414.1Rh0.0050.0050.0040.0040.0040.004--0.00410.6铂Pt0.0480.0420.0430.0460.0340.048--0.04411.3Zr11.47112.76012.52212.31112.18012.251--12.2493.56元素〔g/kg〕元素〔g/kg〕相对标准偏差〔RSD〕Al5.1594.9154.9204.8684.8144.9614.7564.9132.43Fe6.7176.6796.4296.6336.7646.3736.7006.6142.12Ti0.5430.5430.5670.5810.5850.5910.5890.5713.40磷P0.7180.7220.7030.7180.7140.718--0.7150.92Ca41.87440.18842.21339.70143.18141.874--41.4313.13元素元素〔g/kg〕相对标准偏差〔RSD〕150~200g1：10的比例参加浸提剂，于翻转振荡2318h50.0ml，置于消4.0ml1.0ml盐酸，将消解罐放入装置内进展消解，，50.0ml容量瓶中。分3.2-13.2-2。元素〔μg/L〕元素〔μg/L〕相对标准偏差〔RSD%〕Au1.4251.2341.0111.4251.2341.0111.4251.22313.83B6.4695.5624.7186.4695.5624.718--5.58312.8Bi0.0690.1410.1010.0690.0740.057--0.07621.5Ce8.8538.1597.9587.6097.2986.9736.6597.7564.25Cs17.31617.80917.85018.43219.04618.068--18.0873.00Dy9.1258.7408.4318.2597.9687.6717.3808.3503.35Er9.2258.9428.6258.3807.9977.7077.4438.4864.07Eu10.51210.1069.8489.5499.2748.9068.6179.6943.22Ga14.16915.18914.47414.74916.39614.169--15.0124.73Gd9.0328.7058.4938.2078.0057.6877.2778.3523.20Ge0.2320.2140.2340.1410.1740.1450.1320.17322.1Hf6.5236.3135.9795.8605.8296.523--6.1014.46Ho9.1618.8018.4888.2857.9877.6547.3488.3903.53In0.0080.0070.0050.0040.0050.004--0.6051.82Ir0.0310.0030.0120.0030.0010.0030.0310.00224.7La8.7808.2607.9887.6137.3547.0616.7507.8044.44Lu9.3088.9838.6778.4148.1477.8947.5688.5553.62元素 土壤样品溶液检出浓度〔μg/L〕 元素 土壤样品溶液检出浓度〔μg/L〕 〔RSD%〕Nd9.0278.5938.1888.076 7.601 7.3986.9548.1144.36磷P5.8745.6355.6175.716 5.545 5.7765.8745.6941.91Sc8.3337.9357.6347.263 6.905 6.4576.0097.4345.21Sm9.1168.6558.3418.113 7.790 7.4447.1568.2253.84Ti0.8670.8960.9440.658 0.762 0.7200.7250.79612.4Sn5.8575.9825.7685.433 5.594 5.2155.8575.6424.61Tb9.1248.6658.4218.201 7.861 7.5717.2348.2873.57Te3.9574.8674.8213.911 4.184 4.6853.4564.26911.6Th9.0678.8128.5858.275 8.052 7.7409.0678.6853.36Tm9.1668.8618.5758.330 8.009 7.7187.4388.4443.72U5.9985.7625.9465.654 5.998 5.762--5.8402.38W14.86514.13513.62013.197 12.800 12.41614.86513.5066.10Y8.6158.0637.7047.359 6.933 6.6616.2827.5155.56Yb9.1968.8658.6648.314 7.973 7.6547.4008.4544.03钯Pd0.6170.6080.5900.617 0.608 0.5900.6170.6051.82镨Pr8.7778.3168.0547.779 7.378 7.1216.8397.8824.41Re0.1260.1180.1190.114 0.104 0.1050.0930.1119.40Ru2.4142.1512.0982.025 1.908 1.9372.1662.1007.52Rh1.1121.0430.9840.951 0.917 0.9540.9430.9866.41铂Pt0.0430.0000.0000.008 0.016 0.0000.0190.01711.1Zr8.4597.8747.5137.077 8.459 7.8747.5137.7316.5Fe153.730153.379158.179159.109 153.730 155.615--155.6241.60元素表3.2-2 方法周密度土壤样品溶液检出浓度〔mg/L〕相对标准偏差〔RSD〕Li1.4501.4671.4061.4501.4671.406--1.4411.80Al2.3072.3172.2122.240------2.2691.96Rb0.5090.5500.5280.5390.555----0.5363.08Sr5.4785.6115.5605.6375.466----5.5501.244、方法准确度4.1、固体废物准确度测定分析方法同前面一样，分别测定，计算方法准确度，准确度测定结果4.1-14.1-2。表4.1-1 土壤标样GBW07408计算方法准确度标准值元素

〔g〕

样品浓度

平均值

相对误差〔%〕Sc11.7±0.70.113411.431--11.431-2.30Y26±20.113423.958--23.958-7.86Ho0.97±0.080.11341.088--1.08812.21Tm0.46±0.070.11340.464--0.4640.78Yb2.8±0.20.11343.046--3.0468.80Lu0.43±0.040.11340.457--0.4576.19La36±30.158633.031--33.031-8.25Ce66±70.158666.042--66.0420.06Pr8.3±0.80.15867.708--7.708-7.14Nd32±20.158629.632--29.632-7.40Sm5.9±0.40.15865.799--5.799-1.72Tb0.89±0.080.15860.834--0.834-6.24Dy4.8±0.40.15864.647--4.647-3.18Er2.8±0.20.15862.756--2.756-1.56Eu1.2±0.10.18861.346--1.34612.2Gd5.4±0.50.18865.296--5.296-1.93Th11.8±0.70.188611.111--11.111-5.84Ge1.27±0.200.42151.341--1.3415.60Nb15±20.123514.290--14.290-4.73W1.7±0.20.20231.5431.5521.543-9.20Ti3800±1200.20233683.923--3683.923-3.05Zr229±120.1395222.436--222.436-2.87In0.044±0.0130.17150.0460.0440.0451.95Hf7.0±0.80.33157.563--7.5638.04Bi0.30±0.040.17150.3390.2640.3144.65-9.20%~12.2%之间。元素〔μg/L〕元素〔μg/L〕加标量〔μg/L〕平均加标回收率〔%〕Li41.38888.06589.086----50.094.4Al17.15938.48438.484----20.091.5Fe27.59440.28440.284----15.087.4Ga16.37422.12221.462----5.0108Rb329.554419.515412.631----10086.5Sr17.33743.41144.097----30.088.1Cs6.76011.64711.942----5.0101U22.17727.26926.116----5.090.3B0.6704.6954.856----4.0103Re0.0033.280