卤水分析方法+第4部分：硫酸根的测定+重量法编制说明

3《卤水分析方法第4部分硫酸根的测定重量法》编制说明资源标准制修订工作计划的通知批准了关于《卤水分析方法第4部本文件由青海省地质矿产测试应用中心、国家地质实验测试中4湖卤水分析测试机构采用的是上个世纪八十年代青海地矿实验室编5根据项目来源，2022年3月由青海省地质矿产测试应用中心抽62019年开始，由青海省地质矿产测试应用中心联合青海省柴达木综合地质勘察院一共投入120万元进行了《卤水分析标准方法研原子发射光谱法》（202313013）、《卤项，详见自然资源部办公厅关于印发2023年度自确度与精密度)第1部分：总则与定义》（GB/T6379.1-2004）、《测量方法与结果的准确度(正确度与精密度)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/T6379.2-2004）、《测量方法与结果的准确度(正确度与精密度)第3部分：标准测量方法7精密度的中间度量》（GB/T6379.3-2012）和《测量方法与结果的准编号地名类型采集数量1-XZ-BGCN31.690781°E89.455490°西藏那曲市班戈县班戈错碳酸盐型2-XJ-BLKHN43.617463°E92.776877°新疆哈密市巴里坤县巴里坤湖硫酸钠型3-XJ-XCHN43.434253°E93.912150°新疆哈密市伊吾县幻彩湖硫酸镁型4-QH-MHN38.244572°E94.314511°青海海西州马海氯化物型5-QH-HTGN38.33157°E91.467103°青海海西州茫崖市花土沟硫酸镁型6-QH-DCDN37.485975°E95.101957°青海海西州大柴旦行委硫酸镁型7-QH-CEHN37.024499°E994.919759°青海海西州格尔木市察尔汗硫酸镁型8分析编号1234567硫酸根g/L24.829.30.5153.027.82.93塑料大桶中，再称取37.50kg的二次去离子水，混合均匀，放置109制备好的样品都按照国家一级标准物质的要求进行了均匀性检中华人民共和国国家计量技术规范（国家一级标准物质）JJG参照ISO导则35《标准物质/标准样品的定值——通用原则和测试参数1-XZ-BGC2-XJ-BLK3-XJ-XCH4-QH-MH5-QH-HTG6-QH-DCD7-QH-CEH项目（单位）SO42-（g/L）平均值(X)24.9028.254.440.2315.036.736.73单元数最小值(min)24.927.94.410.226.676.67最大值(max)25.028.74.470.246.816.81标准偏差(S)0.010.210.010.000.110.030.03相对偏差(RSD%)0.060.760.322.070.80.470.47单元间方差S120.000.020.002.220.010.000.00单元内方差S220.000.050.002.220.010.000.00F实测值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项目成员一览表专业职称专业工作对标准的具体贡献魏振宏岩矿测试本科高级工程师项目总负责霍成玉化学工程与工艺本科高级工程师21文本及编制说明编写石华化学工程与工艺本科正高级工程师20方法研究、协作实验数据统计材料化学本科高级工程师23方法研究、协作实验数据统计张保科分析化学本科高级工程师方法研究、协作实验数据统计孙红宾分析化学本科工程师方法研究、协作实验数据统计郭心玮环境工程研究生工程师3方法研究、协作实验数据统计刘彬材料化学本科程师方法研究、协作实验数据统计杜作朋应用化学研究生高级工程师方法试验岩矿测试本科正高级工程师29方法试验陈秀娜材料学研究生工程师7方法试验孔晓彦应用化学本科工程师方法试验张国龙应用化学本科高级工程师样品采集制备朱琳化学工程与工艺本科高级工程师数据统计何媛媛化学工程与工艺本科工程师方法研究赖秋祥化学本科高级工程师参与标准方法验证丘丽珍///22参与标准方法验证郑建业岩矿分析研究生高级工程师标准方法精密度协作实验张伟化学工程研究高级工程标准方法精密度协作实验生师序号实验室名称联系人地址1国家地质实验测试中心北京市西城区百万庄大街26号2青海省地质矿产测试应用中心杜作朋青海省西宁市城中区新城北路9号3中国地质科学院地球物理地球化学勘查研究所徐进力河北省廊坊市广阳区金光道84号4山东省地质科学研究院山东省济南市历下区历山路52号5湖北省地质实验测试中心武汉市硚口区古田五路9号地质大楼6安徽省地质实验研究所安徽省合肥市庐阳区阜阳北路318号7湖南省地质实验测试中心湖南省长沙市雨花区城南中路290号8黑龙江省地质矿产实验测试研究中心张振华黑龙江省哈尔滨市香坊区新乡里9中国地质科学院矿产综合利用研究所成都市武侯区二环路南三段5号人南大厦A座420房间长沙矿冶院检测技术有限责任公司杨炳红湖南省长沙市岳麓区麓山南路966号研究大楼中国冶金地质总局山东局测试中心李艳香济南市历下区山师东路14号福建紫金矿冶测试技术有限公司林翠芳福建省龙岩市上杭县南岗工业园区兴杭路43号2标准编制原则和确定主要内容的论据）；《测量方法与结果的准确度(正确度与精密度)第2部分：确定）；《测量方法与结果的准确度(正确度与精密度)第3部分：标准）；是某特定分析方法在给定置信度内能够从试样中检出待测组分是某特定分析方法在给定置信度和允许误差范围内能够从试样中定量检出待测组分的最小浓度或最小量。本方法取3倍的检出限加标回收以回收率判定。试样中待测组分的加标回收率控制在采用重复分析的方法进行控制:每一批试样随机抽取20%的试样作为检查分析样。一批少于10重复分析结果的相对偏差依据相应的重复分析相对偏差允许限3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）：3.1.2.1温控电热板：0℃~300℃;3.1.2.3马弗炉：0℃~1000℃。继续煮沸并保温30min，将烧杯置于水浴中盖表面皿静置4小时或室温放置过夜。用慢速定量滤纸过滤沉淀,将沉淀全部移于滤纸上,无氯离子为止。将沉淀及滤纸移于预先灼烧至恒重的瓷坩埚中,于马弗炉中低温灰化后，逐渐升温至800℃~850℃灼烧1h。取出，稍冷试样中按照公式（1）计算SO42-的含量，结果数字修约规则按p（SO42-)=m×0.4116×106p(SO42-)—卤水中硫酸根的含量，单位为毫克每升（mg/Lm—称取沉淀的质量，单位为克（gV—试样溶液的体积,单位为豪升（烧温度在800℃~850℃之间对结果最佳。沉淀于水浴中盖表面皿静置4小时已经沉淀完全，或室温放置过夜也能沉淀完全。10%氯化钡2023年组织十二家实验室采用本标准与我中心进行比对验证，表3.1硫酸根检出限数据统计表（mg/L）平行样品编号试样备注测定结果（g/L）173.62273.15373.32472.52573.67673.12773.88872.25974.3373.2272.8674.21标准偏差S12（mg/L）0.633计算的方法检出限（mg/L）定量限（mg/L）5.7检测值226.8225.7224.5226.3223.9224.7224.5224.5227.6226.3加标量250\250\加标后474.7476.899.1%101.3精密度0.55%检测值4425445444714426444244094428442644194425加标量5000\5000\加标后9362938998.3%98.8%精密度0.41%检测值14988149651502515153152171504615096151531502414966加标量15000\15000\加标后298352987698.997.8精密度0.58%实验室名称1-XZ-BGC2-XJ-BLKH3-XJ-XCH4-QH-MH5-QH-HTG6-QH-DCD7-QH-CEHSO42-（水平）国家地质实验测试中心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青海省地质矿产测试应用中心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中国地质科学院地球物理地球化学926.128.94.860.2477.4126.34.860.2477.1626.129.54.820.2477.4926.1294.820.2477.49山东省地质科学研究院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湖北省地质实验测试中心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安徽省地质实验研究所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南省地质实验测试中心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黑龙江省地质矿产实验测试研究中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中国地质科学院矿产综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长沙矿冶院检测技术有限责任公司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中国冶金地质总局山东测试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福建紫金矿冶测试技术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实验室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实验室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实验室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%临界值h1%临界值2.252.252.252.252.252.252.25实验室6水平2为歧离值。实验室3水平1、水平3、水平5、水平6、实验室5水平7、实验室6水平4为离群值。实验室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%临界值k1%临界值实验室6水平1为歧离值。实验室2水平7、实验室3水平5、水平6、实验室6水平2、水平4、水平6、实验室8水平1、水平3为离群值。实验室1234567Ci0.5960.8040.4590.7360.3200.4200.565C5%临界值0.3260.3260.3260.3260.3260.3260.326C1%临界值0.3920.3920.3920.3920.3920.3920.392实验室1水平6、实验室11水平2为歧离值。实验室2水平7、实验室3水平6、实验室6水平2、水平4、实验室8水平1、水平3为离群值。实验室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实验室3水平6、实验室5水平7为歧离值。实验室3水平1为离群值。实验室1234567-0.5170.5920.7740.7880.7510.270-0.4050.3560.2720.2420.2300.680G2下5%点0.25370.25370.25370.25370.25370.25370.25370.17380.17380.17380.17380.17380.17380.1738样品编号1-XZ-BGC2-XJ-BLKH3-XJ-XCH4-QH-MH5-QH-HTG6-QH-DCD7-QH-CEH认定值： g/L实验室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