本文選題：鎢精礦 + 焙燒鉬精礦　； 參考：《北京有色金屬研究總院》2017年碩士論文

【摘要】：本文研究制備了一個黑鎢精礦內(nèi)控標樣和一個焙燒鉬精礦內(nèi)控標樣,并建立了使用微波輔助酸消解-電感耦合等離子體原子發(fā)射光譜法同時測定鎢精礦樣品中的七種共存元素的方法。本文對鎢精礦、焙燒鉬精礦的用途、前景以及主要分析方法進行了調(diào)研。鎢礦、鉬礦的主要分析方法有重量法、滴定法等經(jīng)典化學分析方法,是礦物主量、常量元素分析的主要方法;電感耦合等離子體發(fā)射光譜法(ICP-AES)和電感耦合等離子體質(zhì)譜法(ICP-MS),由于其具有可進行多元素同時分析、方法簡便、靈敏度和準確度高等優(yōu)點,逐漸成為礦物雜質(zhì)分析的優(yōu)選方法。本文研究建立了微波輔助酸消解-ICP-AES法同時測定鎢精礦樣品中錳、砷、銅、磷、鉬、鋇、硅等七種主要共存元素的新方法。研究表明:(1)采用鹽酸、硝酸、氫氟酸(5+3+2)混酸作為微波消解酸,微波消解升溫到160℃C后保持1Omin,可將樣品完全溶解,溶液清亮,可用于直接測定,不需要分離鎢基體。(2)儀器最優(yōu)測試條件為射頻功率1200W,霧化氣流量0.75L/min,輔助氣流量1.5L/min,冷卻氣流量15L/min,觀察高度10mm,泵流量2.0L/min。(3)綜合信噪比,譜線干擾等因素,選擇的最佳分析線分別為 Mn(257.61 0nm),As(193.696nm),Cu(324.754nm),P(178.222nm),Mo(202.032nm),Ba(455.403nm),Si(250.690nm)。(4)本法的檢出限為6×10-4μg/mL～7×10-2μg/mL,加標回收率在95.7%～110%之間,相對標準偏差為1%～7%。(5)用本法分析了美國國家標準與技術(shù)研究院(NIST)的黑鎢精礦標樣(SRM277)和白鎢精礦標樣(SRM2430),測定結(jié)果在標準值土擴展不確定度內(nèi)。制備了黑鎢精礦和焙燒鉬精礦內(nèi)控標樣,具體步驟為:選取原料,成分設(shè)計、摻加、研磨、混勻、均勻性檢驗、穩(wěn)定性檢驗、定值等。獲得了粒度小于74μm,通過了均勻性檢驗的標準物質(zhì)候選物料。
[Abstract]:In this paper, an internal standard sample of wolframite concentrate and an internal control standard sample of calcined molybdenum concentrate have been prepared. A method for simultaneous determination of seven coexisting elements in tungsten concentrate samples by microwave assisted acid digestion and inductively coupled plasma atomic emission spectrometry was established. In this paper, the application, prospect and main analytical methods of tungsten concentrate and roasted molybdenum concentrate are investigated. The main analytical methods of tungsten and molybdenum are gravimetric method, titration method and other classical chemical analysis methods. Inductively coupled plasma emission spectrometry (ICP-AESS) and inductively coupled plasma-mass spectrometry (ICP-MS) have become the best methods for mineral impurity analysis due to their advantages of multielement simultaneous analysis, simplicity, high sensitivity and accuracy. A new microwave assisted acid digestion ICP-AES method for simultaneous determination of manganese, arsenic, copper, phosphorus, molybdenum, barium and silicon in tungsten concentrate has been developed. The results showed that the mixture of hydrochloric acid, nitric acid and hydrofluoric acid was used as microwave digestion acid. The sample could be completely dissolved by microwave digestion at 160 鈩，

本文編號：1898517