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3第一章工作簡(jiǎn)況1243456789目前各實(shí)驗(yàn)室鹵水分析測(cè)試多采用的是內(nèi)部參考資料材料《鹽湖鹵5測(cè)定鹵水費(fèi)時(shí)費(fèi)力的局面,為鹵水分析獲取準(zhǔn)確可靠的數(shù)據(jù)提供保6DB63/T1849-2020《鹵水中鋰的測(cè)定電感耦合等離子體質(zhì)譜法》、DB63/T1848-2020《鹵水中鉀、鈉、鈣、鎂的測(cè)定電7序號(hào)專(zhuān)業(yè)工1234567898第二章標(biāo)準(zhǔn)編制原則和確定標(biāo)準(zhǔn)主要內(nèi)容的依據(jù)標(biāo)準(zhǔn)方法的整體結(jié)構(gòu)和內(nèi)容編寫(xiě)方法國(guó)家標(biāo)準(zhǔn)有統(tǒng)一要求和規(guī)本標(biāo)準(zhǔn)的主要技術(shù)指標(biāo)包括方法檢出限、測(cè)定范圍(方法定量1、方法檢出限是指特定分析方法中,分析物能夠被識(shí)93、方法測(cè)定范圍上限一般是通過(guò)用相當(dāng)于樣品數(shù)的計(jì)數(shù)-濃度校準(zhǔn)曲線,測(cè)定該實(shí)驗(yàn)條件下被測(cè)物質(zhì)的濃度范圍,第三章試驗(yàn)驗(yàn)證的分析、綜述報(bào)告,技術(shù)經(jīng)濟(jì)論證,預(yù)期的經(jīng)濟(jì)效益、社會(huì)效益和生態(tài)效益目前各實(shí)驗(yàn)室鹵水分析測(cè)試多采用的是上個(gè)世紀(jì)八十年代青海地礦包含全部三種鹵水類(lèi)型(碳酸鹽型、硫酸鹽型、氯化物型各成分湖型湖型型型型XZ-BGC湖XJ-BLKH型鹵水類(lèi)型BXZ-BGC碳酸鹽型5XJ-BLKH5氯化物型5B樣品編號(hào)LiBRbCs1-XZ-BGC-17.53746.0800.2750.0630.2177.63246.0150.2690.0920.2307.61946.4780.2590.0740.2138.10548.4030.2680.0790.2287.78646.7800.2620.0770.2277.70548.3570.2580.0760.2207.94848.5290.2690.0720.2238.26248.9100.2780.0750.2328.19349.3860.2790.0750.2287.69747.0100.2710.0760.2257.94151.2530.2730.0790.230AVE/(μg/L)7.85747.9270.2690.0760.225SD(N=11)0.2481.6200.0070.0070.006RSD(N=11)3.1613.3812.6748.8572.6522-XJ-BLKH-20.35716.9520.0304.7520.6010.36617.9300.0284.6690.5960.35117.6510.0274.7990.5820.35918.8720.0284.8080.5990.36418.1890.0294.6460.5840.34916.9800.0274.7460.5900.37118.3290.0284.6980.6000.37718.1550.0285.0730.6220.33717.2810.0264.6760.5740.35116.2410.0274.6710.5750.35017.3180.0274.6460.575AVE/(μg/L)0.35717.6270.0284.7440.591SD(N=11)0.0110.7580.0010.1230.015RSD(N=11)3.1964.3003.8072.6002.4863-XJ-XCH-60.3945.1260.0321.2572.1380.3935.0270.0331.2522.1530.4285.3260.0301.3562.1800.4475.6960.0321.2952.1750.4635.3260.0311.4002.2160.4085.2880.0321.2842.1340.4485.4560.0321.3212.2680.3954.9530.0291.2392.1050.4715.8390.0351.4782.4050.3914.9370.0301.2252.0360.4135.0990.0301.2582.055AVE/(μg/L)0.4235.2790.0311.3062.170SD(N=11)0.0300.2940.0020.0780.102RSD(N=11)7.1225.5775.2075.9514.7234-QH-MH-101.3098.0120.08137.9540.8211.2858.5850.08036.8280.8281.4219.3900.08541.2750.8921.4859.8920.08843.6690.9061.4799.6610.08641.8250.9381.4149.4360.08641.1950.8681.4489.0720.08641.1700.9051.5239.6910.09042.6120.9221.4059.1260.08640.4720.8701.3859.0270.08338.9830.8951.4029.3780.09040.8890.899AVE/(μg/L)1.4149.2060.08640.6250.886SD(N=11)0.0710.5380.0032.0010.036RSD(N=11)5.0515.8473.9274.9264.0915-QH-HTG-116.30516.7360.6290.9044.3526.03115.6530.6170.8644.2906.43016.8650.6550.9144.2276.15316.4770.6170.9014.1326.24017.6510.6300.9234.1945.88316.2080.6240.8864.0926.29717.1220.6330.8884.3626.42216.3400.6430.9324.1936.41016.2890.6550.9214.3776.03716.3200.6160.8764.1816.33617.4400.6340.9084.387AVE/(μg/L)6.23116.6460.6320.9024.253SD(N=11)0.1830.5880.0140.0210.105RSD(N=11)2.9353.5332.2482.3542.4646-QH-DCD-330.987137.5960.1492.4421.02330.173141.5490.1422.3690.96632.478146.2940.1452.5911.06532.835150.1050.1522.6221.02432.793144.1690.1542.5901.07532.219146.7980.1502.6121.07232.841147.7480.1482.5731.05033.794145.1590.1552.6411.06131.805143.2150.1442.4801.00032.590148.0690.1482.5951.01533.676158.2060.1512.5561.032AVE/(μg/L)32.381146.2640.1492.5521.035SD(N=11)1.0725.2480.0040.0850.034RSD(N=11)3.3113.5882.7763.3323.2667-QH-CEH-319.61625.4210.4726.8390.12421.30827.3630.5067.4770.12921.21428.0640.5097.3750.13020.79827.8960.4997.4020.12421.68826.9740.5217.3760.12721.59627.5140.5157.6860.13321.30027.6910.5217.8390.12921.85128.5220.5107.8560.13020.68627.4140.4947.4150.12621.16127.6820.5007.2550.12720.82727.5790.5127.3900.128AVE/(μg/L)21.09527.4650.5057.4460.128SD(N=11)0.6160.7880.0140.2830.003RSD(N=11)2.9202.8682.7623.8032.0359Be24Mg238U~1.5%~3.5%功率(W)BeMgInUCeO/CeCe++/Ce800164822689931672076793079.92.8990011082181274125534872613.18845913011694734799763.902.67688711635373347707522.932.0750567960156126626272.53功率與元素計(jì)數(shù)變化圖元素計(jì)數(shù)CPS300000.0250000.0200000.0150000.0100000.0 50000.00.0Be9(cps)(cps)(cps)U238(cps)800900100011001200功率W改變霧化氣流量后檢測(cè)各元素的計(jì)數(shù)變化,檢測(cè)結(jié)果見(jiàn)表11,載氣流速L/minBe(cps)Mg(cps)In(cps)U(cps)CeO/Ce(%)Ce++/Ce(%)0.9026364191933359415472.270.9235555544842190507012.370.9443996393550118587602.430.9659748548364375695452.510.98810912074083139807192.992.45Be9(cps)Mg24(cps)(cps)U238(cps)CeO/CeCe++/Ce737711835576637788592.5855169045560980657122.4545167422350429586962.4541097283646900539092.44輔助氣流速L/minBe(cps)Mg(cps)In(cps)U(cps)CeO/Ce(%)Ce++/Ce2.222.352.432.542.802.0912000000.010000000.08000000.06000000.04000000.02000000.00.0y=-通用格式0100200300400500600BBK-1鹵水樣品作為方法精密度協(xié)作試驗(yàn)樣品樣品信息見(jiàn)表16。樣品全部第2部分:確定標(biāo)準(zhǔn)測(cè)量方法重復(fù)性與再現(xiàn)性的基本方法(GB/T湖型湖型型型型XZ-BGC湖XJ-BLKH型1343-2022《標(biāo)準(zhǔn)物質(zhì)的定值及均勻性、穩(wěn)定性評(píng)估》中對(duì)于均勻性協(xié)作實(shí)驗(yàn)鹵水樣品嚴(yán)格執(zhí)行國(guó)家一級(jí)標(biāo)準(zhǔn)物質(zhì)研制技術(shù)規(guī)范的21,22,……,x2平均值2;設(shè)組內(nèi)平方和Q2=11(j-)…(3.4)組間自由度v1=m-1…(3.5)組內(nèi)自由度2=N-m…(3.6)根據(jù)自由度(ν1,ν2)及給定的顯著性水平α,可由F表查得臨界α值。若F<Fα,則認(rèn)為組內(nèi)與組間無(wú)明顯差異,樣品是均勻的,若F≥Fα,則懷疑各組間有系統(tǒng)差異,即樣品之間存在差異,若記這sn——組內(nèi)測(cè)量次數(shù)。bb=sbb…………………樣品編號(hào)XZ-BGCXJ-XCH總平均值(X)7.8338871.356.067.4260單元數(shù)最小值(min)7.4537469.25264.6251最大值(max)8.140873.559.870.8269標(biāo)準(zhǔn)偏差(S)0.1319.8600.90922.4752.3411.7184.737組間方差s120.01893.5080.926483.8416.3253.67332.276組內(nèi)方差s220.01798.9560.781515.0445.0852.61717.844F實(shí)測(cè)值0.940.94F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不確定度(ubb)0.0142.840.226.450.640.592.19樣品編號(hào)XZ-BGCXJ-XCH總平均值(X)5064276478522472單元數(shù)最小值(min)4924196368152374最大值(max)5174346618722523標(biāo)準(zhǔn)偏差(S)6.4783.6775.03715.69935.43025.27016.787組間方差s1264.65113.24833.975248.9751356.651818.057381.390組內(nèi)方差s2231.37813.64421.356245.2891208.022554.800235.311F實(shí)測(cè)值2.060.97F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不確定度(ubb)3.332.057.049.376.98樣品編號(hào)XZ-BGCXJ-XCH總平均值(X)32.8307642884014647447449923單元數(shù)最小值(min)29.6294541953907626145359619最大值(max)36.33140437341596669497010240標(biāo)準(zhǔn)偏差(S)1.51836.12042.33253.062120.326108.018175.200組間方差s122.3101522.3561790.2703408.18417983.210987.135894.1組內(nèi)方差s222.3001203.0221792.8222539.06712842.611985.528268.7F實(shí)測(cè)值0.92F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不確定度(ubb)0.05841.430.850.4樣品編號(hào)XZ-BGCXJ-XCH總平均值(X)14407255671673423288246362330814464單元數(shù)最小值(min)14068234301592021845232752212013900最大值(max)14865263001727324255254752461114726標(biāo)準(zhǔn)偏差(S)207.888456.749379.180508.222474.988389.668214.012組間方差s12465894299934.8176661.-245591.6355450.1236707.373540.4組內(nèi)方差s2241643.6166005.8128431.7264214.9165022.8112237.132856.4F實(shí)測(cè)值0.932.152.112.24F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不確定度(ubb)40.6211252204樣品編號(hào)XZ-BGCXJ-XCH總平均值(X)2.7126.533.649.049.244.451.2單元數(shù)最小值(min)2.726.433.448.848.944.251.1最大值(max)2.7326.633.749.349.444.751.4標(biāo)準(zhǔn)偏差(S)0.0110.0620.0860.1170.1930.1840.125組間方差s120.0000.0030.0090.0160.0380.0330.019組內(nèi)方差s220.0000.0040.0070.0130.0370.0340.014F實(shí)測(cè)值0.860.97F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不確定度(ubb)0.0030.0170.0290.0320.0120.0530.043樣品編號(hào)XZ-BGCXJ-XCH總平均值(X)24.928.34.440.236.73單元數(shù)最小值(min)24.927.94.410.226.67最大值(max)2528.74.470.246.81標(biāo)準(zhǔn)偏差(S)0.0150.2160.0140.0050.1200.0320.006組間方差s120.000220.0600.000210.0000170.0140.00110.000046組內(nèi)方差s220.000220.0400.000200.0000240.0140.00100.000040F實(shí)測(cè)值0.710.98F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不確定度(ubb)0.0000.0820.0010.0010.0350.0070.001樣品編號(hào)XZ-BGCXJ-XCH總平均值(X)42.684.561.383.584.282.4單元數(shù)最小值(min)42.384.361.283.284.182.3最大值(max)42.984.661.483.984.382.5標(biāo)準(zhǔn)偏差(S)0.1780.0870.0550.2021.9140.0830.054組間方差s120.0290.0100.0030.0483.8510.0090.004組內(nèi)方差s220.0330.0060.0030.0373.5780.0060.002F實(shí)測(cè)值0.860.89F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不確定度(ubb)0.0500.0340.0150.0600.300.0310.023樣品編號(hào)XZ-BGCXJ-XCH總平均值(X)45.04.958.0923.5單元數(shù)最小值(min)43.34.777.6822最大值(max)47.35.338.4524.4標(biāo)準(zhǔn)偏差(S)0.9050.4080.1050.2070.4383.7970.504組間方差s120.9150.1930.0110.0580.24315.5460.330組內(nèi)方差s220.7730.1540.0110.0360.16813.8890.219F實(shí)測(cè)值F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不確定度(ubb)0.220.110.0130.0860.160.740.19樣品編號(hào)XZ-BGCXJ-XCH總平均值(X)45.34.988.0923.7單元數(shù)最小值(min)43.94.898.0323.1最大值(max)46.45.088.1424.3標(biāo)準(zhǔn)偏差(S)0.7680.2240.0550.0350.5170.7570.357組間方差s120.6730.0630.0050.0020.2910.5620.116組內(nèi)方差s220.5510.0440.0020.0010.2560.5780.132F實(shí)測(cè)值2.490.970.88F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不確定度(ubb)0.200.0790.0320.0120.110.220.100樣品編號(hào)XZ-BGCXJ-XCH總平均值(X)7.790.380.386.0830.3單元數(shù)最小值(min)7.510.330.355.8728.4最大值(max)8.180.416.3932.4標(biāo)準(zhǔn)偏差(S)0.1330.1070.0110.0570.1120.9400.516組間方差s120.0220.0110.0000.0040.0121.1820.379組內(nèi)方差s220.0160.0120.0000.0030.0130.7440.214F實(shí)測(cè)值0.990.92F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不確定度(ubb)0.0470.0310.0040.0220.0320.380.23樣品編號(hào)XZ-BGCXJ-XCH總平均值(X)7.630.350.365.8630.6單元數(shù)最小值(min)7.360.330.335.7730.3最大值(max)7.910.380.385.9531.1標(biāo)準(zhǔn)偏差(S)0.1950.0150.0170.0190.0590.2460.254組間方差s120.0390.000340.000270.000400.0050.0550.081組內(nèi)方差s220.0380.000190.000280.000330.0030.0640.057F實(shí)測(cè)值0.970.86F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不確定度(ubb)0.0240.0070.0050.0050.0270.0690.088樣品編號(hào)XZ-BGCXJ-XCH總平均值(X)0.0874.0334.00.762.096.21單元數(shù)最小值(min)0.0763.6533.10.732.046.04最大值(max)0.0944.1834.90.792.236.45標(biāo)準(zhǔn)偏差(S)0.0050.0860.0930.4820.0180.0410.093組間方差s120.0000290.0110.0090.3020.00040.00180.0088組內(nèi)方差s220.0000260.0050.0080.2000.00030.00160.0087F實(shí)測(cè)值2.11F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不確定度(ubb)0.0010.0450.0210.180.0080.0080.007樣品編號(hào)XZ-BGCXJ-XCH總平均值(X)0.0834.1440.30.792.586.99單元數(shù)最小值(min)0.0814.0539.60.752.556.85最大值(max)0.0864.23410.832.617.11標(biāo)準(zhǔn)偏差(S)0.0020.0800.0180.4270.0250.0190.084組間方差s120.0000030.0080.00040.2360.00080.000380.009組內(nèi)方差s220.0000020.0060.00030.1580.00050.000360.006F實(shí)測(cè)值F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不確定度(ubb)0.0000.0300.0040.160.0090.0020.031樣品編號(hào)XZ-BGCXJ-XCH總平均值(X)0.250.0310.0310.0780.600.150.48單元數(shù)最小值(min)0.240.0240.0250.0760.580.140.47最大值(max)0.270.0390.0390.080.630.160.49標(biāo)準(zhǔn)偏差(S)0.0110.0050.0040.0010.0150.0070.008組間方差s120.000120.000020.000020.000000.000280.000060.00007組內(nèi)方差s220.000130.000020.000020.000000.000180.000050.00007F實(shí)測(cè)值0.950.94F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不確定度(ubb)0.0030.0000.0010.0000.0060.0020.001樣品編號(hào)XZ-BGCXJ-XCH總平均值(X)0.220.520.814.040.910.12單元數(shù)最小值(min)0.20.50.793.960.880.11最大值(max)0.240.540.824.140.940.14標(biāo)準(zhǔn)偏差(S)0.0100.0140.0210.0110.0560.0210.010組間方差s120.000110.000240.00040.00020.0040.00040.00010組內(nèi)方差s220.000090.000180.00050.00010.0030.00050.00009F實(shí)測(cè)值0.940.90F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不確定度(ubb)0.0030.0040.0060.0050.0220.0060.002于F分布臨界值(F“表明單元間方差與單LiBRbCsXZ-BGC7.5446.10.250.0630.22XJ-BLKH0.360.0274.750.60X
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