铁矿石 稀土总量的测定 偶氮胂Ш分光光度法 编制说明

《铁矿石稀土总量的测定偶氮胂Ⅲ分光光度法》铁标准化技术委员会组织起草单位成立了起草工作组，由包头成立了标准工作组，确定了标准修订的责任人和参与人，落实的进度安排和分工。工作组对国内外测定稀土总量的相关检验展情况进行全面调研，广泛搜集相关标准和国内外技术资料了试验研究报告，在此基础上编制出《铁矿石稀土总量的测定检测技术有限责任公司、核工业二0三研告，经工作组、验证实验室专家及有关专家研讨后，对标准本标准内容目前尚无国际标准，本次标准修订具体是根据中华人民共和国国家总则与定义》和GB/T6379.2《测量方法与结果的准部分：确定标准测量方法重复性与再现性的基本方法》确考虑分析方法的可操作性、科学性、节能环保、高效性，结合光度分析方法、重量分析方法和电感耦合等离子体发射光谱法国的企业和检验行业的实际情况，进行了方法的深入详细全国企业和检验实验室验证和征求意见，充分体现了标准锶、钡、铝及大量铁等。沉淀用盐酸溶解后，残余之钛、铁2.1样品溶解主要条件的选择矿物，这两种矿物无论采用硫酸冒烟-盐酸浸出还是盐酸-氢氟酸进行溶解，样品均分解不完全，需要采用焦硫酸钾处理残渣。根据包头稀土铁矿用刚玉坩埚熔融样品时，试液浑浊，测定结果偏高；采出现，试液澄清。因此，在保证样品消解完全和经济适2.3强碱分离和氟化分离条件的选择2.4稀土元素相互之间的比例（稀土配分）不同配制标准曲线的选择2.5偶氮胂Ⅲ的显色条件试验2.5.1波长的选择试验2.5.2显色酸度试验2.5.3缓存溶液的用量试验察不同量氯乙酸-氢氧化铵缓存溶液(体积比2:1)对吸光度的影响，试验结果表明，2.5.4显色剂的用量试验2.5.4显色温度和络合物稳定时间试验2.6共存元素干扰试验按铁矿石产品化学成分指标，试验主要考察了铝铁、镁、钠、镍等非稀土杂质含量不超过上述限量，对稀土2.7工作曲线的绘制与测定称样量及分取倍数计算方法测定下限，本方法根据偶氮胂Ⅲ分3.1标准样品的检测3.2方法比对123.3标加回收/%/mg/%据进行统计分析，得到的统计分析结果的重复性（r）和再现性标12345678水平j123456789试验室水平1水平2水平3水平4水平5水平6水平7水平8水平910.01300.03320.07350.1540.3540.4190.5350.8811.1520.01420.03280.07730.1440.3580.4030.5410.8951.1820.01390.03340.07520.1500.3700.4420.5520.8531.1250.01450.03150.07700.1370.3530.4320.5540.8891.1440.01270.03220.07410.1480.3460.4120.5630.9041.1870.01270.03150.07350.1420.3620.4160.5230.8551.09720.01150.02560.06990.1250.3440.3990.5460.9301.0940.01140.02870.07440.1310.3360.4010.5180.9211.0180.01160.02700.07210.1300.3450.4040.5320.8881.0710.01210.02840.06930.1240.3290.4040.5050.9651.0980.01050.02900.07060.1250.3270.4320.5650.8891.1210.01100.03020.07180.1270.3350.4220.5310.9581.05730.009800.02390.07380.1590.3330.4430.5730.8961.1300.009800.02460.07350.1590.3290.4450.5790.9041.1400.008900.02410.07310.1640.3270.4370.5670.8901.1260.009100.02440.07350.1630.3370.4470.5710.8861.1360.009300.02420.07310.1620.3350.4430.5670.8921.1320.009600.02410.07350.1630.3330.4450.5730.8961.13440.01100.02440.07180.1420.3230.4340.5170.8681.1330.01050.02560.07250.1350.3210.4250.5290.8491.0420.009280.02610.07240.1310.3270.4270.5170.8561.1010.009620.02640.07150.1350.3320.4140.5350.8680.01210.02720.07180.1270.330.4090.5260.8721.0220.009810.02710.07050.1150.3130.4180.5030.8661.00450.00970.02700.06670.1210.3150.4050.5040.8731.0420.01090.02670.06660.1410.3180.4160.5020.8571.0120.01150.02830.07020.1420.3280.4210.5090.8551.0530.01170.02710.07120.1350.3220.4190.5090.8671.0440.01100.02790.07020.1400.3250.4070.5100.8591.0370.01130.02750.06840.1320.3290.4130.5060.8831.05660.008200.02670.07210.1190.3550.4530.5750.9581.1730.007900.02670.07230.1190.3550.4520.5750.9581.1730.008400.02590.07220.1320.3460.4510.5820.9671.1030.008400.02670.07190.1190.3300.4520.5750.9591.1750.007800.02860.07420.1310.3550.4510.5980.9541.1050.008400.02780.07430.1310.3460.4510.5820.97370.01210.02500.07350.1470.3260.4210.5160.9331.0980.01180.02560.07230.1380.3310.4320.5590.9251.1000.01200.02430.07270.1440.3380.4290.5820.9151.0920.01250.02640.07310.1390.3280.4160.5130.8951.0990.01240.02420.07200.1420.3340.4290.5300.9061.0940.01220.02610.07280.1410.3220.4170.5230.9311.10080.01090.02690.07210.1070.3330.4120.5040.9131.0250.01140.02890.07040.1110.3260.4000.5470.9460.01250.02760.07110.1090.3420.4130.5200.9491.0790.01080.02630.06830.1210.3310.4250.5190.8781.0820.01000.02950.07060.1350.3410.4160.5340.8981.0460.01010.02720.07280.1130.3150.4290.5630.9591.032%%%y=0.0748x+0.0025y=0.0831x+0.005