鹵水分析方法+第1部分：鈣、鎂、鉀和鈉含量的測定+電感耦合等離子體原子發(fā)射光譜法編制說明

一、工作簡況碩士計碩士胡夢穎地質(zhì)學碩士工程師5張鵬鵬礦床學碩士工程師5龍秀甲李雪花工程師趙偉無機化學碩士研究員夏傳波應用化學碩士高級工程師二、標準編制原則和確定標準主要內(nèi)容的論據(jù)等元素該方法在靈敏度以及分析效率上都優(yōu)于傳統(tǒng)的原子吸收爾默公司該儀器采用高分辨率中階梯光柵交叉色散光學系統(tǒng)（分23MDL=t(n?1,0.99)×S……（2.1）鈣鉀鎂鈉鋰鍶濟效益、社會效益和生態(tài)效益KNa型型型湖型型XZ-BGCXJ-BLKHXJ-XCH型湖湖湖水樣品放置到一個50kg的高密度聚乙烯的塑料大桶中，再稱取協(xié)作實驗鹵水樣品嚴格執(zhí)行國家一級標準物質(zhì)研制技術(shù)規(guī)范的 2n2平均值2； ;設s12=……（3.7）s22=……（3.8）s.s.根據(jù)自由度(ν1,ν2）及給定的顯著性水平α,可由F表查得臨界的Fα值。若F<Fα,則認為組內(nèi)與組間無明顯差異，樣品是均勻α22——組內(nèi)方差；ubb=sbb…………………（3.12）sbb=ubb=?……（3.13）樣品編號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標準偏差(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實測值0.940.942.742.742.742.742.742.742.742.042.042.042.042.042.042.04不確定度(ubb)0.0142.840.226.450.640.592.19樣品編號XZ-BGCXJ-XCH總平均值(X)5064276478522472單元數(shù)最小值(min)4924196368152374最大值(max)5174346618722523標準偏差(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實測值2.060.972.742.742.742.742.742.742.742.042.042.042.042.042.042.04不確定度(ubb)3.332.057.049.376.98樣品編號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標準偏差(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實測值0.922.742.742.742.742.742.742.742.042.042.042.042.042.042.04不確定度(ubb)0.05841.430.850.4樣品編號XZ-BGCXJ-XCH總平均值(X)14407255671673423288246362330814464單元數(shù)最小值(min)14068234301592021845232752212013900最大值(max)14865263001727324255254752461114726標準偏差(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實測值0.932.152.112.242.742.742.742.742.742.742.742.042.042.042.042.042.042.04不確定度(ubb)40.6211252204樣品編號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標準偏差(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實測值0.860.972.742.742.742.742.742.742.742.042.042.042.042.042.042.04不確定度(ubb)0.0030.0170.0290.0320.0120.0530.04342-均勻性檢驗統(tǒng)計結(jié)果樣品編號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標準偏差(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實測值0.710.982.742.742.742.742.742.742.742.042.042.042.042.042.042.04不確定度(ubb)0.0000.0820.0010.0010.0350.0070.001樣品編號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標準偏差(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實測值0.860.892.742.742.742.742.742.742.742.042.042.042.042.042.042.04不確定度(ubb)0.0500.0340.0150.0600.300.0310.023樣品編號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標準偏差(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實測值2.742.742.742.742.742.742.742.042.042.042.042.042.042.04不確定度(ubb)0.220.110.0130.0860.160.740.19樣品編號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標準偏差(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實測值2.490.970.882.742.742.742.742.742.742.742.042.042.042.042.042.042.04不確定度(ubb)0.200.0790.0320.0120.110.220.100樣品編號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標準偏差(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實測值0.990.922.742.742.742.742.742.742.742.042.042.042.042.042.042.04不確定度(ubb)0.0470.0310.0040.0220.0320.380.23樣品編號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標準偏差(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實測值0.970.862.742.742.742.742.742.742.742.042.042.042.042.042.042.04不確定度(ubb)0.0240.0070.0050.0050.0270.0690.088樣品編號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標準偏差(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實測值2.112.742.742.742.742.742.742.742.042.042.042.042.042.042.04不確定度(ubb)0.0010.0450.0210.180.0080.0080.007樣品編號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標準偏差(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實測值2.742.742.742.742.742.742.742.042.042.042.042.042.042.04不確定度(ubb)0.0000.0300.0040.160.0090.0020.031樣品編號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標準偏差(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實測值0.950.942.742.742.742.742.742.742.742.042.042.042.042.042.042.04不確定度(ubb)0.0030.0000.0010.0000.0060.0020.001樣品編號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標準偏差(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實測值0.940.902.742.742.742.742.742.742.742.042.042.042.042.042.042.04不確定度(ubb)0.0030.0040.0060.0050.0220.0060.002樣品編號CaKMgNaLiBXZ-BGC7.1350328.2142787.290.07244.93804202938248030.334.03XJ-XCH71.76544296166450.345.0686841952404636.67.7553.825816830266275.910.7974.250282426030.32.21279144726.5925.2樣品編號CaKMgNaLiBXZ-BGC6.9849926.8138637.830.07150.23704323011249620.344.18XJ-XCH76.26754467169090.384.2687342682378438.37.3856.526156643266025.880.8276.550052378731.22.27277145516.7021.6分析波長選擇的基本原則是盡可能地選擇靈敏度高而干擾少的766.490nm、766.490nmR，Mg初選279.553nm、279.553nmR、285.213nm、285.213nmR，Na初選589.592nmR、330.237nm、體情況見表22。試驗中觀察各元素的譜線的形狀和相互間的干擾情KMgNa大，增加輔助氣流速可幫助提高性能，試驗中多數(shù)元素譜線強度在本試驗考察了不同進樣速率下背景與兩個不同濃度水平各成分的譜大，影響溶液的霧化效率且浪費樣品。本方法進樣速率采用1.5考察了不同觀測高度下背景與兩個不同濃度水平各成分的譜線強度本試驗中對水介質(zhì)和5%硝酸介質(zhì)的校準曲線進行對比，用以確說明兩組樣本完全相關(guān)且相關(guān)性在0.01水平上顯著，p值0.430(>0.05)，說明兩組樣本差異不顯著，這代表相同濃度不同介質(zhì)的兩本試驗比較了水介質(zhì)和5%硝酸介質(zhì)下鹵水標準物質(zhì)和樣品的測KNaB水△酸△水酸水酸水酸水酸水酸水酸水酸水酸注：表中△,表示自吸現(xiàn)象嚴重譜線強度無法計算。說明兩組樣本完全相關(guān)且相關(guān)性在0.01水平上顯著，p值0.05412345601K00Na00124501245B015KNaBKNaB1Lab_123456789Lab_10Lab_11Lab_12由于個別實驗室或數(shù)據(jù)可能與其他實驗室或其他數(shù)據(jù)明顯不一XZ-BGCXJ-XCH1―11―21―31―42―12―22―32―43―13―23―33―44―14―24―34―45―15―25―35―46―1-6―2-6―3-6―4-7―17―27―37―48―18―28―38―49―19―29―39―410―110―210―310―411―111―211―311―412―112―212―312―4XZ-BGCXJ-XCH-XZ-BGCXJ-XCH-XZ-BGCXJ-XCH1―11―21―31―42―12―22―32―43―13―23―33―44―14―24―34―45―15―25―35―46―16―26―36―47―17―27―37―48―18―28―38―49―19―29―39―410―110―210―310―411―111―211―311―412―112―212―312―4XZ-BGCXJ-XCHXZ-BGCXJ-XCHXZ-BGCXJ-XCH1―11―21―31―42―12―22―32―43―13―23―33―44―14―24―34―45―15―25―35―46―16―26―36―47―17―27―37―48―18―28―38―49―19―29―39―410―110―210―310―411―111―211―311―412―112―212―312―4XZ-BGCXJ-XCHXZ-BGCXJ-XCHXZ-BGCXJ-XCH1―11―21―31―42―12―22―32―43―13―23―33―44―14―24―34―45―15―25―35―46―16―26―36―47―17―27―37―48―18―28―38―49―19―29―39―410―110―210―310―411―111―211―311―412―112―212―312―4XZ-BGCXJ-XCHXZ-BGCXJ-XCHXZ-BGCXJ-XCH1―11―21―31―42―12―22―32―43―13―23―33―44―14―24―34―45―15―25―35―46―16―26―36―47―17―27―37―48―18―28―38―4-9―19―29―39―410―110―210―310―411―111―211―311―412―112―212―312―4XZ-BGCXJ-XCHXZ-BGCXJ-XCHXZ-BGCXJ-XCH1―11―21―31―42―12―22―32―43―13―23―33―44―14―24―34―45―15―25―35―46―16―26―36―47―17―247―37―48―18―28―38―49―19―29―39―410―110―210―310―411―111―211―311―412―112―212―312―4XZ-BGCXJ-XCHXZ-BGCXJ-XCHXZ-BGCXJ-XCH1―11―21―31―42―12―22―32―43―13―23―33―44―14―24―34―45―15―25―35―46―16―26―36―47―17―27―37―48―18―28―38―49―19―29―39―410―110―210―310―411―111―211―311―412―112―212―312―4XZ-BGCXJ-XCHXZ-BGCXJ-XCH匯總數(shù)據(jù)分別采用檢驗一致性的圖方法和檢驗離群值的數(shù)值方XZ-BGCXJ-XCHXZ-BGCXJ-XCHXZ-BGCXJ-XCH--XZ-B