發(fā)布時間：2018-05-08 11:16

  本文選題：火焰原子吸收光譜法(FAAS) + 錫鉛焊料(焊錫)　； 參考：《冶金分析》2016年12期

【摘要】：在采用火焰原子吸收光譜(FAAS)法對錫鉛焊料(簡稱焊錫)中Ag進行測定時,Sn的存在會產(chǎn)生干擾。實驗探討了用FAAS測定時Sn對Ag的干擾,結果表明測定不大于2μg/mL的Ag時,Sn最大允許量為5mg/mL。據(jù)此,根據(jù)試樣中Ag含量的高低,分別建立了分離Sn基體和不分離Sn基體后在1.8mol/L HCl介質(zhì)中用FAAS測定焊錫中Ag的方法。利用Ag+可與過量Cl-反應生成[AgCl4]3-可溶絡合物的特點,當試樣中Ag質(zhì)量分數(shù)大于0.02%時,采用HCl(3+1)-H_2O_2溶樣或HCl-HBr-H_2O_2溶樣及排Br后可直接用FAAS對試液進行測定;當Ag質(zhì)量分數(shù)不大于0.02%時,采用HCl-HBr-H_2O_2體系溶樣、排Br及揮發(fā)分離Sn基體后,再利用FAAS進行測定。實驗表明,Ag質(zhì)量濃度在0.2~2.5μg/mL范圍內(nèi)呈線性關系,相關系數(shù)為0.999 96,檢出限為0.004μg/mL。干擾試驗表明:在70~100℃低溫下以HCl-H_2O_2排盡引入的Br和揮發(fā)分離Sn基體可防止Pb沉淀的濺跳;70%~90%Pb基體在HCl介質(zhì)中可沉淀為PbCl2,此時,需靜置至澄清后再測定以防止Pb沉淀對待測試液抽吸產(chǎn)生影響。將實驗方法用于焊錫代表樣及標樣中0.002 3%~1.1%中Ag的測定,測定結果與其他方法(萃取光度法或電位滴定法)或認定值基本一致,相對標準偏差(RSD,n=9~11)為0.88%~4.8%。方法應用于實際樣品分析,回收率為95%~106%。
[Abstract]:The existence of Sn will interfere with the presence of Sn in the determination of Ag in tin lead solder (FAAS) by flame atomic absorption spectrometry. The interference of Sn to Ag at FAAS determination is investigated. The result shows that the maximum allowable amount of Sn is 5mg/mL. when the Ag is not more than 2 u g/mL, and the separation S is established according to the Ag content in the sample. The n matrix and the Sn matrix are not separated from the matrix in the 1.8mol/L HCl medium by FAAS. The Ag+ can be used to react with the excess Cl- to produce the [AgCl4]3- soluble complex. When the Ag mass fraction of the sample is greater than 0.02%, the test solution is directly measured by HCl (3+1) dissolution sample or dissolution sample. When the mass fraction of Ag is not more than 0.02%, HCl-HBr-H_2O_2 system is used to dissolve samples, Br and volatilization Sn matrix, then FAAS is used for the determination. The experiment shows that the Ag mass concentration is linear in the range of 0.2~2.5 mu g/mL, the correlation coefficient is 0.99996, the detection limit is 0.004 u g/mL. interference test, which shows the HCl-H_2O_2 row at 70~100 C low temperature. The Br and volatilization Sn matrix can prevent the splash of Pb precipitation; 70%~90%Pb matrix can be precipitated in HCl medium and PbCl2. At this time, it is required to be static and then determined to prevent Pb precipitation from treating test liquid. The experimental method is applied to the determination of Ag in the representative sample of solder and the 0.002 3%~1.1% in the standard sample, and the results are determined with the others. The method (extraction photometric method or potentiometric titration) is basically the same, and the relative standard deviation (RSD, n=9~11) is applied to the actual sample analysis by the 0.88%~4.8%. method, and the recovery rate is 95%~106%.

【作者單位】： 云南錫業(yè)集團公司研究設計院;
【基金】：國家質(zhì)量監(jiān)督檢驗檢疫總局國家標準修訂項目(2001-19A)
【分類號】：TG42;O657.31

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本文編號：1861175