本文選題：標準加入法 + 氯離子選擇性電極��； 參考：《冶金分析》2017年04期

【摘要】：采用HNO_3(1+2)溶解樣品,氯則全部以Cl~-形式溶解于溶液中,通過測定溶液中Cl~-質(zhì)量濃度,即可計算出碳酸稀土中氯含量。試驗探討了在以硝酸鉀和檸檬酸三鈉為總離子強度調(diào)節(jié)緩沖溶液(TISAB)體系中,主要以EDTA溶液絡(luò)合稀土離子,采用氯離子選擇性電極-標準加入法測定碳酸稀土中氯含量的方法。結(jié)果表明:溶液中Cl~-質(zhì)量濃度在2.0~40.0mg/L范圍內(nèi),EDTA溶液和TISAB溶液用量均為10mL,Cl~-質(zhì)量濃度的負對數(shù)與相應(yīng)電極電位(E)呈良好線性關(guān)系,線性相關(guān)系數(shù)為0.999 9;為保證測試結(jié)果的準確性,樣品和電極響應(yīng)斜率S值的測定須在同一恒溫體系下進行;方法檢出限為0.947mg/L;對于5mg/L的Cl~-,大量K~+、Na~+、NO_3~—不干擾Cl~-的測定,RE~(3+)、Ca~(2+)、Fe~(2+)、Na~+最大允許量分別為10.0、4.0、5.5、23g/L。按照實驗方法測定碳酸鑭和混合碳酸稀土中氯,結(jié)果的相對標準偏差(RSD,n=5)均小于5%;測定值與氯化銀比濁法的測定值基本一致。
[Abstract]:HNO3 (12) was used to dissolve the sample, and chlorine was dissolved in the solution in the form of Cln-. The chlorine content in rare earth carbonate can be calculated by determining the concentration of Cln- in the solution. In the system of potassium nitrate and trisodium citrate as total ion intensity adjusting buffer solution (TISAB), the method of chloride-selective electrode and standard addition method was used to determine the chlorine content in rare earth carbonate by complexing rare earth ions with EDTA solution. The results show that the negative logarithm of the concentration of EDTA and TISAB in the range of 2.0 渭 g / L and 10 mL / L of TISAB has a good linear relationship with the corresponding electrode potential (E), and the linear correlation coefficient is 0.999, in order to ensure the accuracy of the test results, The detection limit of the method is 0.947 mg / L, and for the 5mg / L Cli, a large amount of K ~ + Na ~ no _ 3O _ 3N ~ (3) -no _ (2) Ca ~ (2) Fe ~ (2) Na ~ (2) Na ~ (2) Na ~ (2) Na ~ (2) Na ~ (2) N ~ (2) is 10.0 ~ (4. 0) ~ 5. 5 ~ (23) g 路L ~ (-1) 路L ~ (-1) for 5 mg 路L ~ (-1) Cl ~ (-1). The determination of chlorine in lanthanum carbonate and mixed rare earth carbonate by the experimental method shows that the relative standard deviation (RSD) of the results is less than 5, and the determination value is basically the same as that determined by the silver chloride turbidimetric method.
【作者單位】： 贛州有色冶金研究所;江西離子型稀土工程技術(shù)研究有限公司;
【分類號】：TQ133.3;O657.15

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