北美娱乐

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技术文章
XRF筛选方法若干问题
发布时间:2018-08-27   点击次数:447次

1.方法的范围、应用及概述

北美娱乐  ZHEIGEFANGFASHIYONGLAIDUIDIANZIDIANQICHANPINJIBENCAILIAOZHONGQIAN、GE、GONG、GE、XIUDESHAIXUANFENXI,YIBANLAISHUOXRFDECESHIJIEGUOSHISHANGSHUYUANSUDEZONGHANLIANG,ERBUNENGFENBIANYUANSUDEBUTONGJIATAIJIBUTONGHUAHEWUXINGTAI。YINCILIUJIAGE、DUOXIULIANBENHEDUOXIUERBENMIDESHIJIHANLIANGXUYAOYONGXIANGXIHUAXUEFENXIFANGFALAIJINXINGQUEREN。

北美娱乐  XRFSHIYIZHONGTONGGUOBIJIAOLAIJINXINGDINGLIANGDEYIQI,YINCITADEBIAOXIANYILAIYUXIAOZHUNFANGFA(XIAOZHUNQUXIAN)DEZHILIANG,JIYILAIYUXUANZEDEXIAOZHUNWUZHIHEXUANZEDEYIQIXIANGYINGMOSHI。XRFFENXIYISHOUJITIGANRAO(XISHOUHEJIAQIANG)HEGUANGPUGANRAO。BINGBUSHISUOYOULEIXINGDEXRFDOUNENGGOUSHIYONGYUGEZHONGDAXIAOJIXINGZHUANGDEYANGPIN。

  YOUYIZHONGTONGYONGDEXIAOZHUNFANGFA,JIJIBENCANSHUXIAOZHUNFA(FP)。FPFASHIZHIYONGCHUNDEYUANSU、CHUNDEHUAHEWUHUOJISHAOSHUDEJUYOUYIDINGJITIZUCHENGDEXIAOZHUNWUZHILAIJINXINGXIAOZHUNDEFANGFA。DUIYUSUOYOUDEXRFXIAOZHUNFANGFA,RUGUOXIAOZHUNWUZHIDEZUCHENGYUEJIEJINYANGPIN,CESHIDEZHUNQUEDUJIUYUEGAO。

北美娱乐  YOUYIZHONGJINGYANXIAOZHUNFANGFA,JISHIYONGXIAOZHUNWUZHI,BINGTONGGUOYUNSUANFANGFALAIXIAOZHENGJITIJIGUANGPUCHANSHENGDEGANRAO(XIAOZHENGXISHU)。DANSHIZHEIZHONGFANGFAYAOQIUXIAOZHUNWUZHIDEYUANSUZUCHENGHEYANGPINYIZHI。RUGUOXIAOZHUNWUZHIZHONGQUESHAOMOUYIKENENGCHANSHENGGANRAODEYUANSU,ERYANGPINZHONGYOUHANYOUGAIYUANSU,CESHIJIEGUOKENENGDAOZHIHENDADEPIANCHA。YOUYUXIANYOUDEXIAOZHUNWUZHISHULIANGYOUXIAN,YINCIZAIYIGEFANGFAZHONGJIJIEJUESUOYOUKENENGDEJITIGANRAOHEGUANGPUGANRAO,YOUBAOCHIHAODEDEZHUNQUEDU,SHIYIJIANFEICHANGFUZAHUOZHEKEYISHUOSHIBUKENENGDERENWU。

  DUIYUYOUTUCENGDECAILIAOHEDUOGETUCENGJIEGOUDECAILIAO,SHIXIANBUZHIDAOTUCENGDEJIEGOUSHIHENNANHUODEZHUNQUEJIEGUODE,YINWEIXIAOZHUNMOSHIDEXUANZEZHUYAOYILAIYUYANGPINZHONGTUCENGDEJIEGOU。DUIYUYIZHONGTUCENGHUOTUCENGJIAOBODEQINGKUANG,BIXUJINSHENCHULIYIBAOZHENGXRFJUYOUZUGOUDELINGMINDUKEYIJIANCECHUTUCENGZHONGHANLIANGHENDIDEWUZHI。

  XRFSHAIXUANFENXIYOUYIXIALIANGZHONGFANGSHI:FEIPOHUAIXING——DUIHUODEDEYANGPINZHIJIEJINXINGFENXI;POHUAIXING——ZAIFENXIQIANYUNYONGJIXIEDEHUOHUAXUEDEFANGFAJINXINGYANGPINQIANCHULI。

  ZHEIGECESHIFANGFADEMUDESHIDUIBUTONGCAILIAOZHONGSHIFOUCUNZAIXIANYONGWUZHIJINXINGSHAIXUAN。ZHEIGEFANGFATIGONGDESHIYIZHONGTONGCHANGBEICHENGWEIBANDINGLIANGDECESHISHOUDUAN,NEIJIUSHISHUO,JIEGUODEXIANGDUIBUQUEDINGDUYIBANZAI30%HUOGENGHAO,CISHIDEZHIXINDUWEI68%。GENJUYONGHUZIJIDEXUYAO,YIXIEYONGHUHAIKEYIJIESHOUGENGGAODEBUQUEDINGDU,TONGGUOZHEIZHONGBANDINGLIANGDECESHIKEYILINGYONGHUSHAIXUANCHUXUYAOJINXINGXIANGXIFENXIDECAILIAO。ZHEIZHONGCESHIDEZHUYAOMUDESHIWEIFENGXIANGUANLITIGONGXINXI。

  2.取样

北美娱乐  2.1DUIYUFEIPOHUAIFANGSHI:CAOZUOZHEYINGGAIJIANGYANGPINFANGZAIYIQIHESHIDEWEIZHISHANG,JIYAOBAOZHENGDAICESHIBUFENWEIZHIZHUNQUE,YOUYAOBAOZHENGQITAFEICESHIBUFENBUHUIBEIJIANCE。CAOZUOZHEBIXUBAOZHENGDAICESHIBUFENHEYIQIZHIJIANJULIHEJIHEWEIZHIDEKEZHONGXIANXING。CAOZUOZHEBIXUKAOLVDAICESHIBUFENJINKENENGJUYOUGUIZEWAIXING,RUMIANJI、BIAOMIANCUCAODU、YIZHIDEWULIJIEGOUDENG。RUGUOXUYAOCONGDADEWUTIZHONGHUODEDAICESHIBUFEN,CAOZUOZHEXUYAOJIANGQUYANGBUZHOUYIWENZIXINGSHIJILUXIALAI。

北美娱乐  2.2DUIYUPOHUAIFANGSHI:CAOZUOZHEXUJIANGZHENGGEQUYANGDEFANGFAHEGUOCHENGYIWENZIXINGSHIJILUXIALAI,YINWEIZHEIYANGZUODUIHOUXUZHENGQUEDEJIESHICESHIJIEGUOHENZHONGYAO。RUGUOYAOJIANGDAICESHIBUFENZHICHENGFENMO,YAOBAOZHENGCESHIDIANDELIJINGDAXIAOKEZHIHUOKEKONG;WEILEFANGZHIKELIYOUBUTONGDEHUAXUE、XINGTAIHUOKUANGWUZUCHENG,LIJINGBIXUJINKENENGDEXIAOYIJIANGDICHALIANGXISHOUXIAOYING。RUGUOYAOJIANGCAILIAORONGJIEDAOYETIJITIZHONG,YAOJILUBEIRONGJIECAILIAODEZHILIANGHEWULITEZHENG;ZHONGRONGYEYAOWANQUANJUNYUN,DUIBURONGBUFENSHIRUHECHULIDEBIXUSHUOMING,YIBAOZHENGHELIDEJIESHIZHONGCESHIJIEGUO;HAIYAOSHUOMINGRUHEKEZHONGXIANDEJIANGDAICESHIRONGYEYINRUYIQIJINXINGCESHI,LIRUSHIYONGYIGERONGJIHEJIEGOUYIDINGDEYETICHI。RUGUOYAOJIANGCAILIAOHEGUTIJITIHUNHE,YAOJILUGAICAILIAODEZHILIANGHEWULITEZHENG;ZHONGGUTI(RONGRONGZHUANGTAIHUOYAJINDEXIAOQIU)BIXUJUNYUNYIZHI;DUIBUNENGHUNHEDEBUFENSHIRUHECHULIDEBIXUSHUOMING,YIBAOZHENGHELIDEJIESHIZHONGCESHIJIEGUO。

  3.测试过程 测试过程包括仪器的准备、待测试样品的制备上机以及进行校准,必须有相应的操作说明。还要注意所使用仪器的局限性,例如有些型号的仪器对面积非常小或厚度较薄的样品不能检测或是不能准确定量,对这种情况就要求操作者小心处理并要详细记录,以保证合理的解释测试结果。测试前需要对仪器进行优化,仪器性能的确认:每种分析物的灵敏度、光谱分辨率、检出限、适用的面积大小、样品制备及测试的可重现性、校准方法的准确性。灵敏度是区别不同仪器的性能和确保采用的校准是否有意义的重要指标;光谱分辨率是确保数据收集和校准时被分析物和干扰谱线能被正确的区分并处理的重要指标;检出限即为三倍空白重复测试的标准偏差(不少于7次测量,置信区间为95%);适用的面积大小决定了实际的待测试部分是什么;样品制备及测试的可重现性是证明测试方法可控的一个重要参数。

  4.基体效应和谱线干扰 由于电子电气产品的多样性和材料、元器件的复杂性,X射线荧光光谱法快速筛选电子电气产品中限制使用物质铅、汞、铬、镉和溴不可避免地收到材料中各种基体的影响和材料中包括分析元素在内的其它多种元素谱线重叠的光谱干扰。分析元素特征谱线的干扰主要来自谱线的吸收效应和增强效应。

  4.1GEZHONGCAILIAOJITIDEYINGXIANG FENXIYUANSUTEZHENGPUXIANDEJITIYINGXIANGZHUYAOLAIZIPUXIANDEXISHOUXIAOYINGHEZENGQIANGXIAOYING。

  4.1.1JUHEWUCAILIAO FENXIYUANSUTEZHENGPUXIANSHOUYOUJIGAOFENZIJITICHANSHENGPUXIANBEIJINGDEYANZHONGYINGXIANG;PVCCAILIAOZHONGDEClYUANSU,TIANJIAJIZHONGDECa、Ti、SnDENGYUANSU,ZURANJIZHONGDEBrHESbDENGYUANSUDUIFENXIYUANSUTEZHENGPUXIANDEYINGGUANGQIANGDUYOUXISHOUXIAOYING;YANGPINZHONGDESb、SnHEBrDENGYUANSUDUIFENXIYUANSUTEZHENGPUXIANDEYINGGUANGQIANGDUYEYOUERCIZENGQIANGXIAOYING;DUIYUDAGONGLV(>500W)DEBOZHANGSESANDEXSHEXIANYINGGUANGGUANGPUYI(WDXRF),JUHEWUCAILIAODEYANGPINBIAOMIANKENENGYINZHANGSHIJIANSHIYONGGAOGONGLVDEXSHEXIANGUANGYUANZHAOSHEERSHIBIAOMIANBIANHEI,YINGXIANGCESHIJIEGUODEZHUNQUEXING,JIANYIMEICICEDINGSHISHIYONGXINZHIBEIDECESHIYANGPIN。

  4.1.2JINSHUCAILIAO BUTONGDEJINSHUJITIDUIFENXIYUANSUTEZHENGPUXIANCHANSHENGBUTONGDEXISHOUXIAOYINGHEERCIJIFAXIAOYING,RU:

北美娱乐  TIEHEJIN:Fe、Cr、Ni、Nb、Mo、WDENG;

北美娱乐  LVHEJIN:Al、Mg、Si、Cu、ZnDENG;

  TONGHEJIN:Cu、Zn、Sn、Pb、Mn、NiCoDENG;

北美娱乐  QIANXIHEJIN:Pb、Cu、Zn、Sn、Sb、Bi、AgDENG;

  XINHEJIN:Zn、AlDENG;

  GUIJINSHUHEJIN:Rh、Pd、Ag、Ir、Pt、Au、Cu、ZnDENG;

  QITAJINSHUJITI:Ti、MgDENG。

北美娱乐  DIANZIYUANQIJIANHEYINSHUAXIANLUBANCAILIAOKECANZHAOJINSHUCAILIAOHEJUHEWUCAILIAODEYINGXIANGYINSU。

北美娱乐  4.2 ZHONGDIEPUXIANDEGUANGPUGANRAO FENXIYUANSUTEZHENGPUXIANCUNZAIXIANGHUJIANPUXIANZHONGDIEGANRAO,YIJILAIZIYANGPINZHONGQITAYUANSUDEPUXIANZHONGDIEGANRAO。

北美娱乐  CdDEGANRAOYUANSUKENENGYOUBr、Pb、Sn、AgHESb;

  PbDEGANRAOYUANSUKENENGYOUBr、As、Bi;

  HgDEGANRAOYUANSUKENENGYOUBr、Pb、Bi、Au、GAOHANLIANGDECaHEFe;

  CrDEGANRAOYUANSUKENENGYOUCl;

北美娱乐  BrDEGANRAOYUANSUKENENGYOUFeHEPb。

北美娱乐  4.3 JITIXIAOYINGDUIFENXIYUANSUJIANCHUXIANDEYINGXIANG YIJUHEWUCAILIAOZHONGDAIFENXIYUANSUPbHECdWEILI:RUOCHUNJUHEWUCAILIAOZHONGCdDEJIANCHUXIANWEIA,YOUYUSHOUJITIXIAOYINGDEYINGXIANG,DANGJUHEWUCAILIAOZHONGHANYOU≥2%DESb,DANBUHANBrSHI,CISHICdDEJIANCHUXIANWEIA~2AZHIJIAN;DANGJUHEWUCAILIAOZHONGHANYOU≥2%DEBr,DANBUHANSbSHI,CISHICdDEJIANCHUXIANWEI≥2A。RUOCHUNJUHEWUCAILIAOZHONGPbDEJIANCHUXIANWEIB,YOUYUSHOUJITIXIAOYINGDEYINGXIANG,DANGJUHEWUCAILIAOZHONGHANYOU≥2%DESb,DANBUHANBrSHI,CISHIPbDEJIANCHUXIANWEI~2B;DANGJUHEWUCAILIAOZHONGHANYOU≥2%DEBr,DANBUHANSbSHI,CISHICdDEJIANCHUXIANWEI≥3B。

  5.结果的解释北美娱乐 根据欧盟RoHS指令要求,电子电气产品中限用物质铅、汞、铬、镉和溴的限量要求是,铅,汞,六价铬,多溴二苯醚(PBDE)或多溴联苯(PBB)小于、等于1000mg/kg,镉小于等于100mg/kg。XRF适用于电子电气产品中限用物质铅、汞、铬、镉和溴的快速筛选,即半定量分析,这样分析方式对测试结果的要求是在68%的置信度条件下允许结果误差为30%,对基体复杂的样品(如小的电子元器件等)其误差范围要求更宽,可以达到50%。

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