鐵礦石 稀土總量的測定 偶氮胂Ш分光光度法 編制說明

《鐵礦石稀土總量的測定偶氮胂Ⅲ分光光度法》鐵標(biāo)準(zhǔn)化技術(shù)委員會組織起草單位成立了起草工作組，由包頭成立了標(biāo)準(zhǔn)工作組，確定了標(biāo)準(zhǔn)修訂的責(zé)任人和參與人，落實(shí)的進(jìn)度安排和分工。工作組對國內(nèi)外測定稀土總量的相關(guān)檢驗(yàn)展情況進(jìn)行全面調(diào)研，廣泛搜集相關(guān)標(biāo)準(zhǔn)和國內(nèi)外技術(shù)資料了試驗(yàn)研究報(bào)告，在此基礎(chǔ)上編制出《鐵礦石稀土總量的測定檢測技術(shù)有限責(zé)任公司、核工業(yè)二0三研告，經(jīng)工作組、驗(yàn)證實(shí)驗(yàn)室專家及有關(guān)專家研討后，對標(biāo)準(zhǔn)本標(biāo)準(zhǔn)內(nèi)容目前尚無國際標(biāo)準(zhǔn)，本次標(biāo)準(zhǔn)修訂具體是根據(jù)中華人民共和國國家總則與定義》和GB/T6379.2《測量方法與結(jié)果的準(zhǔn)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》確考慮分析方法的可操作性、科學(xué)性、節(jié)能環(huán)保、高效性，結(jié)合光度分析方法、重量分析方法和電感耦合等離子體發(fā)射光譜法國的企業(yè)和檢驗(yàn)行業(yè)的實(shí)際情況，進(jìn)行了方法的深入詳細(xì)全國企業(yè)和檢驗(yàn)實(shí)驗(yàn)室驗(yàn)證和征求意見，充分體現(xiàn)了標(biāo)準(zhǔn)鍶、鋇、鋁及大量鐵等。沉淀用鹽酸溶解后，殘余之鈦、鐵2.1樣品溶解主要條件的選擇礦物，這兩種礦物無論采用硫酸冒煙-鹽酸浸出還是鹽酸-氫氟酸進(jìn)行溶解，樣品均分解不完全，需要采用焦硫酸鉀處理殘?jiān)８鶕?jù)包頭稀土鐵礦用剛玉坩堝熔融樣品時(shí)，試液渾濁，測定結(jié)果偏高；采出現(xiàn)，試液澄清。因此，在保證樣品消解完全和經(jīng)濟(jì)適2.3強(qiáng)堿分離和氟化分離條件的選擇2.4稀土元素相互之間的比例（稀土配分）不同配制標(biāo)準(zhǔn)曲線的選擇2.5偶氮胂Ⅲ的顯色條件試驗(yàn)2.5.1波長的選擇試驗(yàn)2.5.2顯色酸度試驗(yàn)2.5.3緩存溶液的用量試驗(yàn)察不同量氯乙酸-氫氧化銨緩存溶液(體積比2:1)對吸光度的影響，試驗(yàn)結(jié)果表明，2.5.4顯色劑的用量試驗(yàn)2.5.4顯色溫度和絡(luò)合物穩(wěn)定時(shí)間試驗(yàn)2.6共存元素干擾試驗(yàn)按鐵礦石產(chǎn)品化學(xué)成分指標(biāo)，試驗(yàn)主要考察了鋁鐵、鎂、鈉、鎳等非稀土雜質(zhì)含量不超過上述限量，對稀土2.7工作曲線的繪制與測定稱樣量及分取倍數(shù)計(jì)算方法測定下限，本方法根據(jù)偶氮胂Ⅲ分3.1標(biāo)準(zhǔn)樣品的檢測3.2方法比對123.3標(biāo)加回收/%/mg/%據(jù)進(jìn)行統(tǒng)計(jì)分析，得到的統(tǒng)計(jì)分析結(jié)果的重復(fù)性（r）和再現(xiàn)性標(biāo)12345678水平j(luò)123456789試驗(yàn)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