固體廢物 金屬元素 電感耦合等離子體質(zhì)譜法HJ766-2015

1、方法驗(yàn)證報(bào)告檢測(cè)項(xiàng)目：鋁、金、硼、鐵、鈣、鉍、鈰、銫、鏑、鉺、銪、鎵、釓、鍺、鉿、鈥、銦、銥、鋇、錫、鑭、鋰、镥、鈮、釹、磷、鐠、鉑、銣、錸、銠、釕、鈧、釤、鍶、鋱、碲、釷、鈦、銩、鈾、鎢、釔、鐿、鋯、鉭方法名稱及編號(hào)：固體廢物金屬元素的測(cè)定電感耦合等離子體質(zhì)譜儀HJ766-2015二O一七年二月、實(shí)驗(yàn)?zāi)康囊怨腆w廢物金屬元素的測(cè)定電感耦合等離子體質(zhì)譜儀HJ766-2015為標(biāo)準(zhǔn)對(duì)固體廢物和固體廢物浸出液中的鋁、金、硼、鐵、鈣、鉍、鈰、銫、鏑、鉺、銪、鎵、釓、鍺、鉿、鈥、銦、銥、鋇、錫、鑭、鋰、镥、鈮、釹、磷、鈀、鐠、鉑、銣、錸、銠、釕、鈧、釤、鍶、鋱、碲、釷、鈦、銩、鈾、鎢、釔、鐿、鋯、鉭進(jìn)行

2、實(shí)驗(yàn)。本實(shí)驗(yàn)室現(xiàn)有條件基本符合標(biāo)準(zhǔn)方法規(guī)定的條件，按照該方法進(jìn)行基礎(chǔ)實(shí)驗(yàn)，以驗(yàn)證本實(shí)驗(yàn)室開(kāi)展該項(xiàng)目的適用性。二、方法原理固體廢物或固體廢物浸出液經(jīng)消解后，試樣由載氣帶入霧化系統(tǒng)進(jìn)行霧化后，目標(biāo)元素以氣溶膠形式進(jìn)入等離子的軸向通道，在高溫和惰性氣體中被蒸發(fā)、解離、原子化和電離，轉(zhuǎn)化成帶電荷的正離子經(jīng)離子采集系統(tǒng)進(jìn)入質(zhì)譜儀，質(zhì)譜儀根據(jù)離子的質(zhì)荷比進(jìn)行分離并定性、定量分析。在一定濃度范圍內(nèi)，離子的質(zhì)荷比所對(duì)應(yīng)的響應(yīng)值與其濃度成正比。三、內(nèi)容及結(jié)果1、標(biāo)準(zhǔn)曲線取濃度為100mg/L的多元素標(biāo)準(zhǔn)儲(chǔ)備液10.0mL用1%硝酸定容至100mL，配制成濃度為10.0mg/L的標(biāo)準(zhǔn)中間液，取標(biāo)準(zhǔn)中間液1.0mL

3、于100mL容量瓶中，用1%硝酸稀釋至刻度，配制的標(biāo)準(zhǔn)使用液濃度為100ug/L，依次配制一系列待測(cè)元素標(biāo)準(zhǔn)溶液，可根據(jù)測(cè)量需要的調(diào)整校準(zhǔn)曲線的濃度范圍。在容量瓶中取一定體積的標(biāo)準(zhǔn)使用液，使用硝酸溶液配制系列標(biāo)準(zhǔn)曲線，鋁、金、硼、鐵、鈣、鉍、鈰、銫、鏑、鉺、銪、鎵、釓、鍺、鉿、鈥、銦、銥、鋇、錫、鑭、鋰、镥、鈮、釹、磷、鈀、鐠、鉑、銣、錸、銠、釕、鈧、釤、鍶、鋱、碲、釷、鈦、銩、鈾、鎢、釔、鐿、鋯濃度為0pg/L、.5pg/L、1.0yg/L、5.0pg/L、10.0pg/L、20.0pg/L、40.0pg/L、50.0pg/L、100.0pg/L,鉭濃度為0.0pg/L、4.0pg/L、.0

4、pg/L、16.0pg/L、40.0pg/L、8O.Oyg/L、lOO.Og/L；線性結(jié)果見(jiàn)表1。表1線性實(shí)驗(yàn)結(jié)果序號(hào)元素標(biāo)準(zhǔn)曲線方程序號(hào)元素標(biāo)準(zhǔn)曲線方程1鋁A1Y=0.2359x+0.3533,r=0.993425鈧ScY=7056x+2333,r=0.99992金AuY=139.6x+1.222,r=0.998626釤SmY=3413x+1.110,r=1.00003硼B(yǎng)Y=1030 x+7336,r=1.000027鍶SrY=0.6211x+0.2506,r=0.99994鋇BaY=0.02865x+0.006801,r=1.00028錫SnY=337.7x+919.0,r=0.9998

5、5鉍BiY=11680 x+101.1,r=0.999929鋱TbY=23150 x+360.0,r=1.00006鈰CeY=19610 x+2453,r=0.999930碲TeY=2.443x+1.110,r=0.99987銫CsY=0.8516x+0.09311,r=0.999931釷ThY=16310 x+255.6,r=0.99998鏑DyY=5539x+3.333,r=1.000032鈦TiY=415.3x+421.1,r=0.99999鉺ErY=7438x+3.333,r=1.000033銩TmY=22340 x+3.333,r=1.000010銪EuY=12500 x+3.330

6、,r=1.000034鈾UY=0.1853x+0.001631,r=1.000011鐵FeY=0.3965x+4.623,r=0.990735釩VY=0.3516x+0.6038,r=0.999912鎵GaY=0.05620 x+0.001515,r=1.00036鎢WY=4095x+161.1,r=0.999813釓GdY=4612x+1.556,r=1.000037釔YY=16100 x+1850,r=1.000014鍺GeY=1722x+1479,r=0.999938鐿YbY=4978x+2.220,r=1.000015鉿HfY=422.5x+104.5,r=0.998439鈀PdY=1

7、23.1x+6.667,r=0.989016欽HoY=22490 x+1.110,r=1.000040鐠PrY=2310 x+2.778,r=1.000017銦InY=13570 x+3.778,r=0.999941銣RbY=0.1223x+0.1863,r=0.999118銥IrY=827.2x+5.553,r=0.999942錸ReY=6131x+1.110,r=1.000019鑭LaY=21260 x+153.3,r=1.000043釘RuY=228.3x+3.333,r=0.999320鋰LiY=0.06916x+0.1236,r=1.00044銠RhY=12560 x+7.445,r

8、=0.999921镥LuY=21810 x+164.5,r=1.000045鉑PtY=286.2x+4.443,r=0.999822鈮NbY=9567x+1726,r=0.994646鉭TaY=4.578x-7.733,r=0.999523釹NdY=4022x+1.555,r=1.000047鋯ZrY=7262x+3561,r=0.999524磷PY=4197x+48460,r=0.999748鈣CaY=3.491x+1.093,r=0.99962、方法檢出限2.1固體廢物分解法稱取0.10000.2000g樣品，置于聚四氟乙烯坩堝中，用少量水沖洗內(nèi)壁潤(rùn)濕試樣后，加入硝酸4.0m1、鹽酸1.0

9、m1、氫氟酸1.0m1、雙氧水1.0ml,在石墨消解儀上進(jìn)行消解，消解后冷卻至室溫，打開(kāi)蓋子，進(jìn)行趕酸，直至盡干，用去離子水定容至50.0ml，分別測(cè)定，求得標(biāo)準(zhǔn)偏差SD,按照下式計(jì)算檢出限MDL，檢出限試驗(yàn)結(jié)果見(jiàn)表2.1-1，表2.1-2：MDL=3.143*SD表2.1-1方法檢出限元素檢出濃度（mg/kg）標(biāo)準(zhǔn)偏差（SD）方法檢出限（MDL）mg/kg1金Au0.1050.0970.1050.0810.1260.0810.0990.0140.042硼B(yǎng)0.1700.0960.1190.1440.1990.1830.2680.0530.173鉍Bi0.5740.1640.1210.1050

10、.0940.0890.0890.1640.524鈰Ce14.37215.15215.46015.59615.69515.86715.9090.4951.565銫Cs1.6031.6181.6381.6481.6611.7051.6450.0300.096鏑Dy0.9831.0001.0391.0281.0441.0441.0650.0260.087鉺Er0.7530.7990.7970.8160.8070.8130.8260.0220.078銪Eu0.1930.1970.2040.2010.2060.2090.2040.0050.029鎵Ga3.8053.9283.8714.0013.9974

11、.2354.0650.1300.4110釓Gd1.1631.2321.2531.2521.2361.2821.2780.0370.1211鍺Ge1.4101.3971.4151.4951.5341.5191.5540.0610.1912鉿Hf3.0713.0223.1843.2803.9243.9253.7820.3751.1813欽Ho0.2100.2150.2230.2220.2250.2230.2270.0060.0214銦In0.0200.0100.0110.0100.0110.0120.0100.0030.0115銥Ir0.0510.0260.0160.0150.0150.0160.

12、0180.0120.0416鑭La6.2346.5876.7236.7586.8366.9046.9060.2190.6917鋰Li9.7799.7019.94510.16910.20710.63410.0890.2890.91元素檢出濃度(mg/kg)標(biāo)準(zhǔn)偏差(SD)方法檢出限(MDL)mg/kg18镥Lu0.1670.1780.1810.1780.1810.1820.1840.0050.0219鈮Nb1.4171.3541.4471.6091.5811.5381.5180.0850.2720釹Nd5.5645.8596.0015.9616.0376.0626.1230.1730.5421鈧

13、Sc1.1391.1571.1461.1621.1841.1801.1840.0170.0522釤Sm1.1161.1881.1981.1961.2281.2251.2280.0370.1223鍶Sr4.2204.1954.2044.2144.1914.3354.1840.0480.1524錫Sn16.02017.72017.70117.11415.15014.86015.62316.3133.4825鋱Tb0.1720.1790.1860.1830.1870.1850.1840.0050.0226碲Te0.6640.5760.2660.3990.3210.2550.2100.1610.502

14、7釷Th8.1598.7728.8528.8168.7988.8018.8160.2290.7228銩Tm0.1300.1370.1370.1360.1360.1410.1410.0040.0129鈾U5.0085.3255.3575.5885.4735.6715.3690.1990.6230鎢W0.5420.5360.5260.5100.5000.5070.5540.0190.0631釔Y4.6504.8764.9694.9745.0515.0675.0930.1420.4532鐿Yb1.0011.0411.0801.0561.0701.0971.0690.0290.0933鈀Pd6.072

15、5.8155.6395.5805.4775.5405.7820.1900.6034鐠Pr1.5161.5981.6341.6231.6571.6591.6570.0480.1535銣Rb76.10678.39277.65080.22580.89585.73882.5511.4904.6836錸Re0.0080.0020.0030.0010.0010.0010.0010.0020.00837釘Ru0.0300.0360.0390.0490.0380.0380.0260.0070.0238銠Rh0.0090.0050.0050.0040.0040.0040.0040.0020.00539鉑Pt0.

16、0600.0480.0420.0430.0460.0340.0480.0070.0240鉭Ta0.4970.4960.4960.4970.4970.5000.4990.0020.00541鋯Zr11.47112.76012.52212.31112.1809.39110.0401.2153.82表2.1-2方法檢出限元素檢出濃度(g/kg)標(biāo)準(zhǔn)偏差(SD)方法檢出限(MDL)g/kg1鋁Al5.1594.9154.9204.8684.8144.9614.7560.1190.372鐵Fe6.7176.6796.4296.6336.7646.3736.7000.1400.443鈦Ti0.5430.5

17、430.5670.5810.5850.5910.5890.0190.06元素檢出濃度(g/kg)標(biāo)準(zhǔn)偏差(SD)方法檢出限(MDL)g/kg4磷P0.7180.7220.7030.7180.7140.7180.7030.0070.025鈣Ca41.87440.18842.21339.70143.18141.87440.1881.2974.082.2、固體廢物浸出液稱取150200g樣品，按固液比1：10的比例加入浸提劑，于翻轉(zhuǎn)振蕩器上，在溫度23C下振蕩18h,過(guò)濾；取固體廢物浸出液50.0m1,置于消解罐中，加入4.0m1硝酸和1.0ml鹽酸，將消解罐放入裝置內(nèi)進(jìn)行消解，消解后冷卻至室溫，打

18、開(kāi)蓋子進(jìn)行趕酸，溶液定容至50.0ml容量瓶中。分別測(cè)定，求得標(biāo)準(zhǔn)偏差SD，按照下式計(jì)算檢出限MDL，檢出限試驗(yàn)結(jié)果見(jiàn)表2.2-1，表2.2-2：MDL=3.143*SD表2.2-1方法檢出限元素檢出濃度（gg/L）標(biāo)準(zhǔn)偏差(SD)方法檢出限(MDL)昭/L1金Au1.4251.2341.0111.4251.2341.0111.4250.0870.272硼B(yǎng)6.4695.5624.7187.2196.4695.5624.7180.8752.753鉍Bi0.0690.1410.1010.0690.0740.0570.0390.0870.274鈰Ce8.8538.1597.9587.6097.29

19、86.9736.6598.8538.165銫Cs17.31617.80917.85018.43219.04618.06820.8791.0993.456鏑Dy9.1258.7408.4318.2597.9687.6717.3800.2800.887鉺Er9.2258.9428.6258.3807.9977.7077.4430.3451.098銪Eu10.51210.1069.8489.5499.2748.9068.6170.3130.989鎵Ga14.16915.18914.47414.74916.39614.16916.3860.8932.8110釓Gd9.0328.7058.4938.20

20、78.0057.6877.2770.2670.8411鍺Ge0.2320.2140.2340.1410.1740.1450.1320.0410.1312鉿Hf6.5236.3135.9795.8605.8296.5235.8650.2920.9213欽Ho9.1618.8018.4888.2857.9877.6547.3480.2960.9314銦In0.0080.0070.0050.0040.0050.0040.0010.0020.006元素檢出濃度(昭/L)標(biāo)準(zhǔn)偏差(SD)方法檢出限(MDL)昭/L15銥Ir0.0310.0030.0120.0030.0010.0030.0310.0110

21、.0316鑭La8.7808.2607.9887.6137.3547.0616.7500.3471.0917镥Lu9.3088.9838.6778.4148.1477.8947.5680.3100.9818釹Nd9.0278.5938.1888.0767.6017.3986.9540.3541.1119磷P5.8745.6355.6175.7165.5455.7765.8740.1090.3420鈧Sc8.3337.9357.6347.2636.9056.4576.0090.3871.2221釤Sm9.1168.6558.3418.1137.7907.4447.1560.3160.9922鈦T

22、i0.8670.8960.9440.6580.7620.7200.7250.0990.3123錫Sn5.8575.9825.7685.4335.5945.2155.8570.2600.8224鋱Tb9.1248.6658.4218.2017.8617.5717.2340.2960.9325碲Te3.9574.8674.8213.9114.1844.6853.4560.4971.5626釷Th9.0678.8128.5858.2758.0527.7409.0670.2920.9227銩Tm9.1668.8618.5758.3308.0097.7187.4380.3140.9928鈾U5.9985

23、.7625.9465.6545.9985.7625.2450.2460.7729鎢W14.86514.13513.62013.19712.80012.41614.8650.8212.5830釔Y8.6158.0637.7047.3596.9336.6616.2820.4181.3131鐿Yb9.1968.8658.6648.3147.9737.6547.4000.3401.0732鈀Pd0.6170.6080.5900.6170.6080.5900.6170.0110.0433鐠Pr8.7778.3168.0547.7797.3787.1216.8390.3471.0934錸Re0.1260.

24、1180.1190.1140.1040.1050.0930.0100.0335釘Ru2.4142.1512.0982.0251.9081.9372.1660.1580.5036銠Rh1.1121.0430.9840.9510.9170.9540.9430.0630.2037鉑Pt0.0430.0000.0000.0080.0160.0000.0190.0140.0438鋯Zr8.4597.8747.5137.0778.4597.8747.5130.5061.5939鐵Fe153.730153.37915&179159.109153.730155.615153.9252.3587.41表2.2-

25、2方法檢出限元素檢出濃度(mg/L)標(biāo)準(zhǔn)偏差(SD)方法檢出限(MDL)mg/L1鋰Li1.4501.4671.4061.4501.4671.4061.3420.0260.082鋁Al2.3072.3172.2122.2402.1482.2392.3980.0760.24元素檢出濃度(mg/L)標(biāo)準(zhǔn)偏差(SD)方法檢出限(MDL)mg/L3銣Rb0.5090.5500.5280.5390.5550.5570.6000.0260.084鍶Sr5.4785.6115.5605.6375.4665.5275.8360.1170.373、方法精密度3.1、固體廢物分解法稱取0.10000.2000g樣

26、品，置于聚四氟乙烯坩堝中，用少量水沖洗內(nèi)壁潤(rùn)濕試樣后，加入硝酸4.0m1、鹽酸1.0m1、氫氟酸1.0m1、雙氧水1.0ml,在石墨消解儀上進(jìn)行消解，消解后冷卻至室溫，打開(kāi)蓋子，進(jìn)行趕酸，直至盡干，用去離子水定容至50.0ml,加水至標(biāo)線，分別測(cè)定，結(jié)果見(jiàn)表3.1-1、表3.1-2。表3.1-1方法精密度元素土壤樣品溶液檢出濃度(mg/kg)平均值(mg/kg)相對(duì)標(biāo)準(zhǔn)偏差(RSD%)銀Ag0.2820.2860.2900.2880.2920.2970.2840.2881.68金Au0.1050.0970.1050.0810.1260.0810.0990.09914.4硼B(yǎng)0.1700.119

27、0.1440.1990.1830.165-0.16317.4鉍Bi0.1210.1050.0940.0890.0890.098-0.09912.3鈰Ce14.37215.15215.46015.59615.69515.86715.90915.4363.21銫Cs1.6031.6181.6381.6481.6611.7051.6451.6461.83鏑Dy0.9831.0001.0391.0281.0441.0441.0651.0292.54鉺Er0.7530.7990.7970.8160.8070.8130.8260.8022.74銪Eu0.1930.1970.2040.2010.2060.2

28、090.2040.2022.51鎵Ga3.8053.9283.8714.0013.9974.2354.0653.9863.26釓Gd1.1631.2321.2531.2521.2361.2821.2781.2422.97鍺Ge1.4101.3971.4151.4951.5341.5191.5541.4754.12鉿Hf3.0713.0223.1843.2803.9243.9253.7823.45510.9欽Ho0.2100.2150.2230.2220.2250.2230.2270.2212.56銦In0.0200.0100.0110.0100.0110.0120.0100.0114.72銥I

29、r0.0160.0150.0150.0160.0180.017-0.0167.23元素土壤樣品溶液檢出濃度（mg/kg）平均值（mg/kg）相對(duì)標(biāo)準(zhǔn)偏差（RSD%）鑭La6.2346.5876.7236.7586.8366.9046.9066.7073.26鋰Li9.7799.7019.94510.16910.20710.63410.08910.0752.87镥Lu0.1670.1780.1810.1780.1810.1820.1840.1792.87鈮Nb1.4171.3541.4471.6091.5811.5381.5181.4955.70釹Nd5.5645.8596.0015.9616.

30、0376.0626.1235.9442.91鈧Sc1.1391.1571.1461.1621.1841.1801.1841.1651.48釤Sm1.1161.1881.1981.1961.2281.2251.2281.1973.06鍶Sr4.2204.1954.2044.2144.1914.3354.1844.2201.14錫Sn16.02017.72017.70117.11417.10517.12616.58217.0533.52鋱Tb0.1720.1790.1860.1830.1870.1850.1840.1822.74碲Te0.2660.3990.3210.2550.3150.302-0

31、.31016.5釷Th8.1598.7728.8528.8168.7988.8018.8168.7162.62銩Tm0.1300.1370.1370.1360.1360.1410.1410.1372.67鈾U5.0085.3255.3575.5885.4735.6715.3695.3993.68鎢W0.5420.5360.5260.5100.5000.507-0.5203.00釔Y4.6504.8764.9694.9745.0515.0675.0934.9542.86鐿Yb1.0011.0411.0801.0561.0701.0971.0691.0592.72鈀Pd6.0725.8155.63

32、95.5805.4775.5405.7825.7013.33鐠Pr1.5161.5981.6341.6231.6571.6591.6571.6212.94銣Rb78.39280.22580.89582.55181.23479.365-80.4441.82錸Re0.0010.0010.0010.0010.0010.001-0.00117.6釘Ru0.0300.0360.0390.0380.0380.026-0.03414.1銠Rh0.0050.0050.0040.0040.0040.004-0.00410.6鉑Pt0.0480.0420.0430.0460.0340.048-0.04411.3鋯

33、Zr11.47112.76012.52212.31112.18012.251-12.2493.56表3.1-2方法精密度元素土壤樣品溶液檢出濃度（g/kg）平均值（g/kg）相對(duì)標(biāo)準(zhǔn)偏差（RSD）鋁Al5.1594.9154.9204.8684.8144.9614.7564.9132.43鐵Fe6.7176.6796.4296.6336.7646.3736.7006.6142.12鈦Ti0.5430.5430.5670.5810.5850.5910.5890.5713.40元素土壤樣品溶液檢出濃度（g/kg）平均值（g/kg）相對(duì)標(biāo)準(zhǔn)偏差(RSD)磷P0.7180.7220.7030.7180

34、.7140.718-0.7150.92鈣Ca41.87440.18842.21339.70143.18141.874-41.4313.133.2、固體廢物浸出液稱取150200g樣品，按固液比1：10的比例加入浸提劑，于翻轉(zhuǎn)振蕩器上，在溫度23C下振蕩18h,過(guò)濾，取固體廢物浸出液50.0m1,置于消解罐中，加入4.0m1硝酸和1.0ml鹽酸，將消解罐放入裝置內(nèi)進(jìn)行消解，消解后冷卻至室溫，打開(kāi)蓋子進(jìn)行趕酸，溶液定容至50.0ml容量瓶中。分別測(cè)定，結(jié)果見(jiàn)表3.2-1、表3.2-2。表3.2-1方法精密度元素土壤樣品溶液檢出濃度（gg/L）平均值（gg/L）相對(duì)標(biāo)準(zhǔn)偏差（RSD%）金Au1.42

35、51.2341.0111.4251.2341.0111.4251.22313.83硼B(yǎng)6.4695.5624.7186.4695.5624.7185.58312.8鉍Bi0.0690.1410.1010.0690.0740.0570.07621.5鈰Ce8.8538.1597.9587.6097.2986.9736.6597.7564.25銫Cs17.31617.80917.85018.43219.04618.06818.0873.00鏑Dy9.1258.7408.4318.2597.9687.6717.3808.3503.35鉺Er9.2258.9428.6258.3807.9977.707

36、7.4438.4864.07銪Eu10.51210.1069.8489.5499.2748.9068.6179.6943.22鎵Ga14.16915.18914.47414.74916.39614.16915.0124.73釓Gd9.0328.7058.4938.2078.0057.6877.2778.3523.20鍺Ge0.2320.2140.2340.1410.1740.1450.1320.17322.1鉿Hf6.5236.3135.9795.8605.8296.5236.1014.46欽Ho9.1618.8018.4888.2857.9877.6547.3488.3903.53銦In0.

37、0080.0070.0050.0040.0050.0040.6051.82銥Ir0.0310.0030.0120.0030.0010.0030.0310.00224.7鑭La8.7808.2607.9887.6137.3547.0616.7507.8044.44镥Lu9.3088.9838.6778.4148.1477.8947.5688.5553.62元素土壤樣品溶液檢出濃度（Rg/L）平均值（Rg/L）相對(duì)標(biāo)準(zhǔn)偏差（RSD%）釹Nd9.0278.5938.1888.0767.6017.3986.9548.1144.36磷P5.8745.6355.6175.7165.5455.7765.87

38、45.6941.91鈧Sc8.3337.9357.6347.2636.9056.4576.0097.4345.21釤Sm9.1168.6558.3418.1137.7907.4447.1568.2253.84鈦Ti0.8670.8960.9440.6580.7620.7200.7250.79612.4錫Sn5.8575.9825.7685.4335.5945.2155.8575.6424.61鋱Tb9.1248.6658.4218.2017.8617.5717.2348.2873.57碲Te3.9574.8674.8213.9114.1844.6853.4564.26911.6釷Th9.067

39、8.8128.5858.2758.0527.7409.0678.6853.36銩Tm9.1668.8618.5758.3308.0097.7187.4388.4443.72鈾U5.9985.7625.9465.6545.9985.7625.8402.38鎢W14.86514.13513.62013.19712.80012.41614.86513.5066.10釔Y8.6158.0637.7047.3596.9336.6616.2827.5155.56鐿Yb9.1968.8658.6648.3147.9737.6547.4008.4544.03鈀Pd0.6170.6080.5900.6170.6

40、080.5900.6170.6051.82鐠Pr8.7778.3168.0547.7797.3787.1216.8397.8824.41錸Re0.1260.1180.1190.1140.1040.1050.0930.1119.40釘Ru2.4142.1512.0982.0251.9081.9372.1662.1007.52銠Rh1.1121.0430.9840.9510.9170.9540.9430.9866.41鉑Pt0.0430.0000.0000.0080.0160.0000.0190.01711.1鋯Zr8.4597.8747.5137.0778.4597.8747.5137.7316

41、.5鐵Fe153.730153.379158.179159.109153.730155.615155.6241.60表3.2-2方法精密度元素土壤樣品溶液檢出濃度（mg/L）平均值（g/kg）相對(duì)標(biāo)準(zhǔn)偏差（RSD）鋰Li1.4501.4671.4061.4501.4671.4061.4411.80鋁Al2.3072.3172.2122.2402.2691.96銣Rb0.5090.5500.5280.5390.5550.5363.08鍶Sr5.4785.6115.5605.6375.4665.5501.244、方法準(zhǔn)確度4.1、固體廢物準(zhǔn)確度測(cè)定分析方法同前面相同，分別測(cè)定，計(jì)算方法準(zhǔn)確度，準(zhǔn)確

42、度測(cè)定結(jié)果見(jiàn)表4.1-1、加標(biāo)回收率結(jié)果見(jiàn)4.1-2。表4.1-1土壤標(biāo)樣GBW07408計(jì)算方法準(zhǔn)確度元素標(biāo)準(zhǔn)值(mg/kg)取樣量(g)樣品濃度(mg/kg)平均值(mg/kg)相對(duì)誤差(%)Sc11.70.70.113411.431-11.431-2.30Y2620.113423.958-23.958-7.86Ho0.970.080.11341.088-1.08812.21Tm0.460.070.11340.464-0.4640.78Yb2.80.20.11343.046-3.0468.80Lu0.430.040.11340.457-0.4576.19La3630.158633.031-

43、33.031-8.25Ce6670.158666.042-66.0420.06Pr8.30.80.15867.708-7.708-7.14Nd3220.158629.632-29.632-7.40Sm5.90.40.15865.799-5.799-1.72Tb0.890.080.15860.834-0.834-6.24Dy4.80.40.15864.647-4.647-3.18Er2.80.20.15862.756-2.756-1.56Eu1.20.10.18861.346-1.34612.2Gd5.40.50.18865.296-5.296-1.93Th11.80.70.188611.111

44、-11.111-5.84Ge1.270.200.42151.341-1.3415.60Nb1520.123514.290-14.290-4.73W1.70.20.20151.5431.5521.543-9.20Ti38001200.20153683.923-3683.923-3.05Zr229120.1395222.436-222.436-2.87In0.0440.0130.17150.0460.0440.0451.95Hf7.00.80.33157.563-7.5638.04Bi0.300.040.17150.3390.2640.3144.65結(jié)果表明，相對(duì)誤差在-9.20%12.2%之間。

45、表4.1-2加標(biāo)回收率計(jì)算方法準(zhǔn)確度元素加標(biāo)前測(cè)定值(gg/L)加標(biāo)后測(cè)定值(gg/L)加標(biāo)量(gg/L)平均加標(biāo)回收率()Li41.38888.06589.086-50.094.4Al17.15938.48438.484-20.091.5Fe27.59440.28440.284-15.087.4Ga16.37422.12221.462一一5.0108Rb329.554419.515412.631一一10086.5Sr17.33743.41144.097-30.088.1Cs6.76011.64711.942-5.0101U22.17727.26926.116一一5.090.3B0.6704.6954.856一一一4.0103Re0.0033.2803.244-