鹵水分析方法+第4部分：硫酸根的測定+重量法編制說明

3《鹵水分析方法第4部分硫酸根的測定重量法》編制說明資源標(biāo)準(zhǔn)制修訂工作計劃的通知批準(zhǔn)了關(guān)于《鹵水分析方法第4部本文件由青海省地質(zhì)礦產(chǎn)測試應(yīng)用中心、國家地質(zhì)實驗測試中4湖鹵水分析測試機構(gòu)采用的是上個世紀(jì)八十年代青海地礦實驗室編5根據(jù)項目來源，2022年3月由青海省地質(zhì)礦產(chǎn)測試應(yīng)用中心抽62019年開始，由青海省地質(zhì)礦產(chǎn)測試應(yīng)用中心聯(lián)合青海省柴達(dá)木綜合地質(zhì)勘察院一共投入120萬元進行了《鹵水分析標(biāo)準(zhǔn)方法研原子發(fā)射光譜法》（202313013）、《鹵項，詳見自然資源部辦公廳關(guān)于印發(fā)2023年度自確度與精密度)第1部分：總則與定義》（GB/T6379.1-2004）、《測量方法與結(jié)果的準(zhǔn)確度(正確度與精密度)第2部分：確定標(biāo)準(zhǔn)測量方法重復(fù)性與再現(xiàn)性的基本方法》（GB/T6379.2-2004）、《測量方法與結(jié)果的準(zhǔn)確度(正確度與精密度)第3部分：標(biāo)準(zhǔn)測量方法7精密度的中間度量》（GB/T6379.3-2012）和《測量方法與結(jié)果的準(zhǔn)編號地名類型采集數(shù)量1-XZ-BGCN31.690781°E89.455490°西藏那曲市班戈縣班戈錯碳酸鹽型2-XJ-BLKHN43.617463°E92.776877°新疆哈密市巴里坤縣巴里坤湖硫酸鈉型3-XJ-XCHN43.434253°E93.912150°新疆哈密市伊吾縣幻彩湖硫酸鎂型4-QH-MHN38.244572°E94.314511°青海海西州馬海氯化物型5-QH-HTGN38.33157°E91.467103°青海海西州茫崖市花土溝硫酸鎂型6-QH-DCDN37.485975°E95.101957°青海海西州大柴旦行委硫酸鎂型7-QH-CEHN37.024499°E994.919759°青海海西州格爾木市察爾汗硫酸鎂型8分析編號1234567硫酸根g/L24.829.30.5153.027.82.93塑料大桶中，再稱取37.50kg的二次去離子水，混合均勻，放置109制備好的樣品都按照國家一級標(biāo)準(zhǔn)物質(zhì)的要求進行了均勻性檢中華人民共和國國家計量技術(shù)規(guī)范（國家一級標(biāo)準(zhǔn)物質(zhì)）JJG參照ISO導(dǎo)則35《標(biāo)準(zhǔn)物質(zhì)/標(biāo)準(zhǔn)樣品的定值——通用原則和測試參數(shù)1-XZ-BGC2-XJ-BLK3-XJ-XCH4-QH-MH5-QH-HTG6-QH-DCD7-QH-CEH項目（單位）SO42-（g/L）平均值(X)24.9028.254.440.2315.036.736.73單元數(shù)最小值(min)24.927.94.410.226.676.67最大值(max)25.028.74.470.246.816.81標(biāo)準(zhǔn)偏差(S)0.010.210.010.000.110.030.03相對偏差(RSD%)0.060.760.322.070.80.470.47單元間方差S120.000.020.002.220.010.000.00單元內(nèi)方差S220.000.050.002.220.010.000.00F實測值10.372.0110.800.810.81F0.01(v1,v2)2.742.742.742.742.742.742.74F0.05(v1,v2)2.042.042.042.042.042.042.04Ubb4.6E0.070.000.000.030.000.00表1.4項目成員一覽表專業(yè)職稱專業(yè)工作對標(biāo)準(zhǔn)的具體貢獻魏振宏巖礦測試本科高級工程師項目總負(fù)責(zé)霍成玉化學(xué)工程與工藝本科高級工程師21文本及編制說明編寫石華化學(xué)工程與工藝本科正高級工程師20方法研究、協(xié)作實驗數(shù)據(jù)統(tǒng)計材料化學(xué)本科高級工程師23方法研究、協(xié)作實驗數(shù)據(jù)統(tǒng)計張?？品治龌瘜W(xué)本科高級工程師方法研究、協(xié)作實驗數(shù)據(jù)統(tǒng)計孫紅賓分析化學(xué)本科工程師方法研究、協(xié)作實驗數(shù)據(jù)統(tǒng)計郭心瑋環(huán)境工程研究生工程師3方法研究、協(xié)作實驗數(shù)據(jù)統(tǒng)計劉彬材料化學(xué)本科程師方法研究、協(xié)作實驗數(shù)據(jù)統(tǒng)計杜作朋應(yīng)用化學(xué)研究生高級工程師方法試驗巖礦測試本科正高級工程師29方法試驗陳秀娜材料學(xué)研究生工程師7方法試驗孔曉彥應(yīng)用化學(xué)本科工程師方法試驗張國龍應(yīng)用化學(xué)本科高級工程師樣品采集制備朱琳化學(xué)工程與工藝本科高級工程師數(shù)據(jù)統(tǒng)計何媛媛化學(xué)工程與工藝本科工程師方法研究賴秋祥化學(xué)本科高級工程師參與標(biāo)準(zhǔn)方法驗證丘麗珍///22參與標(biāo)準(zhǔn)方法驗證鄭建業(yè)巖礦分析研究生高級工程師標(biāo)準(zhǔn)方法精密度協(xié)作實驗張偉化學(xué)工程研究高級工程標(biāo)準(zhǔn)方法精密度協(xié)作實驗生師序號實驗室名稱聯(lián)系人地址1國家地質(zhì)實驗測試中心北京市西城區(qū)百萬莊大街26號2青海省地質(zhì)礦產(chǎn)測試應(yīng)用中心杜作朋青海省西寧市城中區(qū)新城北路9號3中國地質(zhì)科學(xué)院地球物理地球化學(xué)勘查研究所徐進力河北省廊坊市廣陽區(qū)金光道84號4山東省地質(zhì)科學(xué)研究院山東省濟南市歷下區(qū)歷山路52號5湖北省地質(zhì)實驗測試中心武漢市硚口區(qū)古田五路9號地質(zhì)大樓6安徽省地質(zhì)實驗研究所安徽省合肥市廬陽區(qū)阜陽北路318號7湖南省地質(zhì)實驗測試中心湖南省長沙市雨花區(qū)城南中路290號8黑龍江省地質(zhì)礦產(chǎn)實驗測試研究中心張振華黑龍江省哈爾濱市香坊區(qū)新鄉(xiāng)里9中國地質(zhì)科學(xué)院礦產(chǎn)綜合利用研究所成都市武侯區(qū)二環(huán)路南三段5號人南大廈A座420房間長沙礦冶院檢測技術(shù)有限責(zé)任公司楊炳紅湖南省長沙市岳麓區(qū)麓山南路966號研究大樓中國冶金地質(zhì)總局山東局測試中心李艷香濟南市歷下區(qū)山師東路14號福建紫金礦冶測試技術(shù)有限公司林翠芳福建省龍巖市上杭縣南崗工業(yè)園區(qū)興杭路43號2標(biāo)準(zhǔn)編制原則和確定主要內(nèi)容的論據(jù)）；《測量方法與結(jié)果的準(zhǔn)確度(正確度與精密度)第2部分：確定）；《測量方法與結(jié)果的準(zhǔn)確度(正確度與精密度)第3部分：標(biāo)準(zhǔn)）；是某特定分析方法在給定置信度內(nèi)能夠從試樣中檢出待測組分是某特定分析方法在給定置信度和允許誤差范圍內(nèi)能夠從試樣中定量檢出待測組分的最小濃度或最小量。本方法取3倍的檢出限加標(biāo)回收以回收率判定。試樣中待測組分的加標(biāo)回收率控制在采用重復(fù)分析的方法進行控制:每一批試樣隨機抽取20%的試樣作為檢查分析樣。一批少于10重復(fù)分析結(jié)果的相對偏差依據(jù)相應(yīng)的重復(fù)分析相對偏差允許限3試驗驗證的分析、綜述報告，技術(shù)經(jīng)濟論證，預(yù)期的經(jīng)濟效益、社會效益和生態(tài)效益）：3.1.2.1溫控電熱板：0℃~300℃;3.1.2.3馬弗爐：0℃~1000℃。繼續(xù)煮沸并保溫30min，將燒杯置于水浴中蓋表面皿靜置4小時或室溫放置過夜。用慢速定量濾紙過濾沉淀,將沉淀全部移于濾紙上,無氯離子為止。將沉淀及濾紙移于預(yù)先灼燒至恒重的瓷坩堝中,于馬弗爐中低溫灰化后，逐漸升溫至800℃~850℃灼燒1h。取出，稍冷試樣中按照公式（1）計算SO42-的含量，結(jié)果數(shù)字修約規(guī)則按p（SO42-)=m×0.4116×106p(SO42-)—鹵水中硫酸根的含量，單位為毫克每升（mg/Lm—稱取沉淀的質(zhì)量，單位為克（gV—試樣溶液的體積,單位為豪升（燒溫度在800℃~850℃之間對結(jié)果最佳。沉淀于水浴中蓋表面皿靜置4小時已經(jīng)沉淀完全，或室溫放置過夜也能沉淀完全。10%氯化鋇2023年組織十二家實驗室采用本標(biāo)準(zhǔn)與我中心進行比對驗證，表3.1硫酸根檢出限數(shù)據(jù)統(tǒng)計表（mg/L）平行樣品編號試樣備注測定結(jié)果（g/L）173.62273.15373.32472.52573.67673.12773.88872.25974.3373.2272.8674.21標(biāo)準(zhǔn)偏差S12（mg/L）0.633計算的方法檢出限（mg/L）定量限（mg/L）5.7檢測值226.8225.7224.5226.3223.9224.7224.5224.5227.6226.3加標(biāo)量250\250\加標(biāo)后474.7476.899.1%101.3精密度0.55%檢測值4425445444714426444244094428442644194425加標(biāo)量5000\5000\加標(biāo)后9362938998.3%98.8%精密度0.41%檢測值14988149651502515153152171504615096151531502414966加標(biāo)量15000\15000\加標(biāo)后298352987698.997.8精密度0.58%實驗室名稱1-XZ-BGC2-XJ-BLKH3-XJ-XCH4-QH-MH5-QH-HTG6-QH-DCD7-QH-CEHSO42-（水平）國家地質(zhì)實驗測試中心124.6527.964.2650.20615.076.6691.153224.3927.864.3470.19814.726.5041.153324.7528.294.2980.20614.926.57424.528.224.3470.20614.876.4881.136青海省地質(zhì)礦產(chǎn)測試應(yīng)用中心524.9428.674.4710.22915.486.804624.9328.434.5190.22415.346.784724.8828.544.4970.25215.526.871.329824.6828.44.5660.22115.326.8271.272中國地質(zhì)科學(xué)院地球物理地球化學(xué)926.128.94.860.2477.4126.34.860.2477.1626.129.54.820.2477.4926.1294.820.2477.49山東省地質(zhì)科學(xué)研究院24.8228.024.1740.21414.996.6431.09524.8827.964.1740.2315.046.6761.13624.8428.014.1320.22215.126.6931.12824.7928.054.0910.23914.976.7091.087湖北省地質(zhì)實驗測試中心24.828.324.5760.26815.196.9010.96524.8128.284.530.27715.176.8970.95824.7528.294.5420.2715.186.890.9892024.7728.334.5520.2696.8690.962安徽省地質(zhì)實驗研究所2125.1328.444.3790.27214.946.6881.2352224.8227.784.470.3615.026.9151.2592324.1423.714.2890.33115.176.6061.2222424.3327.174.3710.26815.046.7091.231南省地質(zhì)實驗測試中心2524.8627.954.4040.2226.7091.2042624.8227.914.4410.22114.836.6272724.928.034.4160.22214.826.7051.2072824.8227.994.4250.22414.856.6681.205黑龍江省地質(zhì)礦產(chǎn)實驗測試研究中2925.3428.24.3730.25715.336.821.22624.3327.754.5180.2776.8041.19732125.3228.034.4190.24715.266.9171.21624.0726.444.6410.27515.386.8221.224中國地質(zhì)科學(xué)院礦產(chǎn)綜24.2727.734.3960.2414.696.6021.18324.2427.814.40.23314.866.661.19824.3627.434.3010.226.66424.0427.824.3920.23914.826.5531.194長沙礦冶院檢測技術(shù)有限責(zé)任公司24.7928.074.3960.2146.5361.17224.7227.824.3230.21314.956.5341.16424.827.964.3450.21314.966.5431.1644024.7427.944.3690.2196.5391.181中國冶金地質(zhì)總局山東測試4124.3328.614.5360.22614.866.8041.2354224.4527.954.4560.2114.746.8161.2434324.5728.244.4860.21814.616.7911.2354424.3728.44.540.2314.786.7871.227福建紫金礦冶測試技術(shù)4525.1929.144.40.22215.766.981.2044625.0729.224.440.22115.596.944725.1929.314.420.22215.646.971.2074825.0329.264.420.22415.576.971.205實驗室1234567Lab_124.57228.0824.31420.204014.8956.55781.1405Lab_224.85828.5104.51320.231515.4156.82131.2603Lab_326.15029.3504.84000.247016.1507.38751.3200Lab_424.83328.0104.14280.226215.0306.68021.1115Lab_524.78228.3054.55000.271015.1856.88920.9685Lab_624.60526.7754.37720.307815.0426.72951.2368Lab_724.85027.9704.42150.222214.8256.67721.2040Lab_824.76527.6054.48780.264015.2926.84081.2158Lab_924.22827.6974.37220.233014.7686.61981.1788Lab_1024.76227.9474.35820.214814.9786.53801.1702Lab_1124.43028.3004.50450.221014.7486.79951.2350Lab_1225.12029.2324.42000.222215.6406.96501.2040實驗室1234567Lab_10.1590.2050.04010.00400.1440.08220.0158Lab_20.1210.1220.04030.01410.1000.03690.0545Lab_30.1000.5070.02310.00000.1910.15630.0000Lab_40.0380.0370.03980.01070.0670.02830.0241Lab_50.0280.0240.01950.00410.0130.01420.0140Lab_60.4522.1080.07400.04520.0950.13140.0158Lab_70.0380.0520.01560.00130.0210.03820.0029Lab_80.6610.7990.11870.01450.0790.05150.0132Lab_90.1350.1830.04760.00920.0850.05280.0266Lab_100.0390.1020.03140.00290.0260.00390.0081Lab_110.1060.2780.04060.00890.1040.01320.0065Lab_120.0820.0720.01630.00130.0850.01730.0029實驗室1234567Lab_1-0.543-0.096-0.768-1.188-0.654-1.024-0.530Lab_20.0600.5220.429-0.2470.6100.1270.832Lab_32.7821.7342.3950.2832.3962.6021.510Lab_40.007-0.200-1.799-0.429-0.325-0.489-0.859Lab_5-0.1000.2260.6511.1040.0510.424-2.484Lab_6-0.473-1.983-0.3892.363-0.296-0.2740.565Lab_70.043-0.258-0.122-0.565-0.824-0.5020.192Lab_8-0.136-0.7850.2770.8640.3110.2130.326Lab_9-1.267-0.652-0.419-0.196-0.962-0.753-0.094Lab_10-0.142-0.291-0.503-0.819-0.452-1.111-0.192Lab_11-0.8420.2180.377-0.606-1.0110.0320.544Lab_120.6121.564-0.131-0.5651.1570.7550.192h5%臨界值h1%臨界值2.252.252.252.252.252.252.25實驗室6水平2為歧離值。實驗室3水平1、水平3、水平5、水平6、實驗室5水平7、實驗室6水平4為離群值。實驗室1234567Lab_10.6430.3020.7930.2631.4781.1800.755Lab_20.4900.1800.7970.9271.0260.5302.605Lab_30.4050.7470.4570.0001.9602.2440.000Lab_40.1540.0550.7870.7040.6870.4061.152Lab_50.1130.0350.3850.2700.1330.2040.669Lab_61.8293.1061.4632.9720.9751.8870.755Lab_70.1540.0770.3080.0850.2150.5480.139Lab_82.6751.1772.3470.9540.8110.7390.631Lab_90.5460.2700.9410.6050.8720.7581.271Lab_100.1580.1500.6210.1910.2670.0560.387Lab_110.4290.4100.8030.5851.0670.1900.311Lab_120.3320.1060.3220.0850.8720.2480.139k5%臨界值k1%臨界值實驗室6水平1為歧離值。實驗室2水平7、實驗室3水平5、水平6、實驗室6水平2、水平4、水平6、實驗室8水平1、水平3為離群值。實驗室1234567Ci0.5960.8040.4590.7360.3200.4200.565C5%臨界值0.3260.3260.3260.3260.3260.3260.326C1%臨界值0.3920.3920.3920.3920.3920.3920.392實驗室1水平6、實驗室11水平2為歧離值。實驗室2水平7、實驗室3水平6、實驗室6水平2、水平4、實驗室8水平1、水平3為離群值。實驗室1234567Gl1.2671.9831.7991.1881.0111.1112.484Gp2.7821.7352.3952.3632.3962.6021.5102.4122.4122.4122.4122.4122.4122.4122.6362.6362.6362.6362.6362.6362.636實驗室3水平6、實驗室5水平7為歧離值。實驗室3水平1為離群值。實驗室1234567-0.5170.5920.7740.7880.7510.270-0.4050.3560.2720.2420.2300.680G2下5%點0.25370.25370.25370.25370.25370.25370.25370.17380.17380.17380.17380.17380.17380.1738樣品編號1-XZ-BGC2-XJ-BLKH3-XJ-XCH4-QH-MH5-QH-HTG6-QH-DCD7-QH-CEH認(rèn)定值： g/L實驗室123456724.6527.964.2650.20615.076.6691.15324.3927.864.3470.19814.726.5041.15324.7528.294.2980.20614.926.5724.528.224.3470.20614.876.4881.1362―124.9428.674.4710.22915.486.8042―224.9328.434.5190.22415.346.7842―324.8828.544.4970.25215.526.871.3292―424.6828.44.5660.22115.326.8271.2723―126.128.94.860.2477.413―226.34.860.2477.163―326.129.54.820.2477.493―426.1294.820.2477.494―124.8228.024.1740.21414.996.6431.0954―224.8827.964.1740.2315.046.6761.1364―324.8428.014.1320.22215.126.6931.1284―424.7928.054.0910.23914.976.7091.0875―124.828.324.5760.26815.196.9010.9655―224.8128.284.530.27715.176.8970.9585―324.7528.294.5420.2715.186.890.9895―424.7728.334.5520.2696.8690.9626―125.1328.444.3790.27214.946.6881.2356―224.8227.784.470.3615.026.9151.2596―324.1423.714.2890.33115.176.6061.2226―424.3327.174.3710.26815.046.7091.2317―124.8627.954.4040.2226.7091.2047―224.8227.914.4410.22114.836.6277―324.928.034.4160.22214.826.7051.2077―424.8227.994.4250.22414.856.6681.2058―125.3428.24.3730.25715.336.821.2268―224.3327.754.5180.2776.8041.1978―325.3228.034.4190.24715.266.9171.2168―424.0726.444.6410.27515.386.8221.2249―124.2727.734.3960.2414.696.6021.1839―224.2427.814.40.23314.866.661.1989―324.3627.434.30