卤水分析方法++第2部分：锂、铷、铯、锶和总硼含量的测定++电感耦合等离子体质谱法编制说明

3第一章工作简况1243456789目前各实验室卤水分析测试多采用的是内部参考资料材料《盐湖卤5测定卤水费时费力的局面，为卤水分析获取准确可靠的数据提供保6DB63/T1849-2020《卤水中锂的测定电感耦合等离子体质谱法》、DB63/T1848-2020《卤水中钾、钠、钙、镁的测定电7序号专业工1234567898第二章标准编制原则和确定标准主要内容的依据标准方法的整体结构和内容编写方法国家标准有统一要求和规本标准的主要技术指标包括方法检出限、测定范围（方法定量1、方法检出限是指特定分析方法中，分析物能够被识93、方法测定范围上限一般是通过用相当于样品数的计数-浓度校准曲线，测定该实验条件下被测物质的浓度范围，第三章试验验证的分析、综述报告，技术经济论证，预期的经济效益、社会效益和生态效益目前各实验室卤水分析测试多采用的是上个世纪八十年代青海地矿包含全部三种卤水类型（碳酸盐型、硫酸盐型、氯化物型各成分湖型湖型型型型XZ-BGC湖XJ-BLKH型卤水类型BXZ-BGC碳酸盐型5XJ-BLKH5氯化物型5B样品编号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功率与元素计数变化图元素计数CPS300000.0250000.0200000.0150000.0100000.0 50000.00.0Be9(cps)(cps)(cps)U238(cps)800900100011001200功率W改变雾化气流量后检测各元素的计数变化，检测结果见表11，载气流速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辅助气流速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卤水样品作为方法精密度协作试验样品样品信息见表16。样品全部第2部分：确定标准测量方法重复性与再现性的基本方法（GB/T湖型湖型型型型XZ-BGC湖XJ-BLKH型1343-2022《标准物质的定值及均匀性、稳定性评估》中对于均匀性协作实验卤水样品严格执行国家一级标准物质研制技术规范的21，22，……，x2平均值2；设组内平方和Q2=11(j-)…（3.4）组间自由度v1=m-1…（3.5）组内自由度2=N-m…（3.6）根据自由度(ν1,ν2）及给定的显著性水平α,可由F表查得临界α值。若F<Fα,则认为组内与组间无明显差异，样品是均匀的，若F≥Fα,则怀疑各组间有系统差异，即样品之间存在差异，若记这sn——组内测量次数。bb=sbb…………………样品编号XZ-BGCXJ-XCH总平均值(X)7.8338871.356.067.4260单元数最小值(min)7.4537469.25264.6251最大值(max)8.140873.559.870.8269标准偏差(S)0.1319.8600.90922.4752.3411.7184.737组间方差s120.01893.5080.926483.8416.3253.67332.276组内方差s220.01798.9560.781515.0445.0852.61717.844F实测值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不确定度(ubb)0.0142.840.226.450.640.592.19样品编号XZ-BGCXJ-XCH总平均值(X)5064276478522472单元数最小值(min)4924196368152374最大值(max)5174346618722523标准偏差(S)6.4783.6775.03715.69935.43025.27016.787组间方差s1264.65113.24833.975248.9751356.651818.057381.390组内方差s2231.37813.64421.356245.2891208.022554.800235.311F实测值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不确定度(ubb)3.332.057.049.376.98样品编号XZ-BGCXJ-XCH总平均值(X)32.8307642884014647447449923单元数最小值(min)29.6294541953907626145359619最大值(max)36.33140437341596669497010240标准偏差(S)1.51836.12042.33253.062120.326108.018175.200组间方差s122.3101522.3561790.2703408.18417983.210987.135894.1组内方差s222.3001203.0221792.8222539.06712842.611985.528268.7F实测值0.92F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不确定度(ubb)0.05841.430.850.4样品编号XZ-BGCXJ-XCH总平均值(X)14407255671673423288246362330814464单元数最小值(min)14068234301592021845232752212013900最大值(max)14865263001727324255254752461114726标准偏差(S)207.888456.749379.180508.222474.988389.668214.012组间方差s12465894299934.8176661.-245591.6355450.1236707.373540.4组内方差s2241643.6166005.8128431.7264214.9165022.8112237.132856.4F实测值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不确定度(ubb)40.6211252204样品编号XZ-BGCXJ-XCH总平均值(X)2.7126.533.649.049.244.451.2单元数最小值(min)2.726.433.448.848.944.251.1最大值(max)2.7326.633.749.349.444.751.4标准偏差(S)0.0110.0620.0860.1170.1930.1840.125组间方差s120.0000.0030.0090.0160.0380.0330.019组内方差s220.0000.0040.0070.0130.0370.0340.014F实测值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不确定度(ubb)0.0030.0170.0290.0320.0120.0530.043样品编号XZ-BGCXJ-XCH总平均值(X)24.928.34.440.236.73单元数最小值(min)24.927.94.410.226.67最大值(max)2528.74.470.246.81标准偏差(S)0.0150.2160.0140.0050.1200.0320.006组间方差s120.000220.0600.000210.0000170.0140.00110.000046组内方差s220.000220.0400.000200.0000240.0140.00100.000040F实测值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不确定度(ubb)0.0000.0820.0010.0010.0350.0070.001样品编号XZ-BGCXJ-XCH总平均值(X)42.684.561.383.584.282.4单元数最小值(min)42.384.361.283.284.182.3最大值(max)42.984.661.483.984.382.5标准偏差(S)0.1780.0870.0550.2021.9140.0830.054组间方差s120.0290.0100.0030.0483.8510.0090.004组内方差s220.0330.0060.0030.0373.5780.0060.002F实测值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不确定度(ubb)0.0500.0340.0150.0600.300.0310.023样品编号XZ-BGCXJ-XCH总平均值(X)45.04.958.0923.5单元数最小值(min)43.34.777.6822最大值(max)47.35.338.4524.4标准偏差(S)0.9050.4080.1050.2070.4383.7970.504组间方差s120.9150.1930.0110.0580.24315.5460.330组内方差s220.7730.1540.0110.0360.16813.8890.219F实测值F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不确定度(ubb)0.220.110.0130.0860.160.740.19样品编号XZ-BGCXJ-XCH总平均值(X)45.34.988.0923.7单元数最小值(min)43.94.898.0323.1最大值(max)46.45.088.1424.3标准偏差(S)0.7680.2240.0550.0350.5170.7570.357组间方差s120.6730.0630.0050.0020.2910.5620.116组内方差s220.5510.0440.0020.0010.2560.5780.132F实测值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不确定度(ubb)0.200.0790.0320.0120.110.220.100样品编号XZ-BGCXJ-XCH总平均值(X)7.790.380.386.0830.3单元数最小值(min)7.510.330.355.8728.4最大值(max)8.180.416.3932.4标准偏差(S)0.1330.1070.0110.0570.1120.9400.516组间方差s120.0220.0110.0000.0040.0121.1820.379组内方差s220.0160.0120.0000.0030.0130.7440.214F实测值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不确定度(ubb)0.0470.0310.0040.0220.0320.380.23样品编号XZ-BGCXJ-XCH总平均值(X)7.630.350.365.8630.6单元数最小值(min)7.360.330.335.7730.3最大值(max)7.910.380.385.9531.1标准偏差(S)0.1950.0150.0170.0190.0590.2460.254组间方差s120.0390.000340.000270.000400.0050.0550.081组内方差s220.0380.000190.000280.000330.0030.0640.057F实测值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不确定度(ubb)0.0240.0070.0050.0050.0270.0690.088样品编号XZ-BGCXJ-XCH总平均值(X)0.0874.0334.00.762.096.21单元数最小值(min)0.0763.6533.10.732.046.04最大值(max)0.0944.1834.90.792.236.45标准偏差(S)0.0050.0860.0930.4820.0180.0410.093组间方差s120.0000290.0110.0090.3020.00040.00180.0088组内方差s220.0000260.0050.0080.2000.00030.00160.0087F实测值2.11F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不确定度(ubb)0.0010.0450.0210.180.0080.0080.007样品编号XZ-BGCXJ-XCH总平均值(X)0.0834.1440.30.792.586.99单元数最小值(min)0.0814.0539.60.752.556.85最大值(max)0.0864.23410.832.617.11标准偏差(S)0.0020.0800.0180.4270.0250.0190.084组间方差s120.0000030.0080.00040.2360.00080.000380.009组内方差s220.0000020.0060.00030.1580.00050.000360.006F实测值F0.01(14,30)2.742.742.742.742.742.742.74F0.05(14,30)2.042.042.042.042.042.042.04不确定度(ubb)0.0000.0300.0040.160.0090.0020.031样品编号XZ-BGCXJ-XCH总平均值(X)0.250.0310.0310.0780.600.150.48单元数最小值(min)0.240.0240.0250.0760.580.140.47最大值(max)0.270.0390.0390.080.630.160.49标准偏差(S)0.0110.0050.0040.0010.0150.0070.008组间方差s120.000120.000020.000020.000000.000280.000060.00007组内方差s220.000130.000020.000020.000000.000180.000050.00007F实测值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不确定度(ubb)0.0030.0000.0010.0000.0060.0020.001样品编号XZ-BGCXJ-XCH总平均值(X)0.220.520.814.040.910.12单元数最小值(min)0.20.50.793.960.880.11最大值(max)0.240.540.824.140.940.14标准偏差(S)0.0100.0140.0210.0110.0560.0210.010组间方差s120.000110.000240.00040.00020.0040.00040.00010组内方差s220.000090.000180.00050.00010.0030.00050.00009F实测值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不确定度(ubb)0.0030.0040.0060.0050.0220.0060.002于F分布临界值（F“表明单元间方差与单LiBRbCsXZ-BGC7.5446.10.250.0630.22XJ-BLKH0.360.0274.750.60X