ed mccurdy, icp-ms product marketing, agilent uk
TRANSCRIPT
å³ 1. Agilent 8900 åå°äœä»æ§ã®ããªãã«åé極 ICP-MS ããã³ I-AS ã«ããŒä»ããªãŒããµã³ãã©
Agilent ICP-MS ãžã£ãŒãã«
2018 幎 4 æ - 第 72 å·
åå°äœæ¥çã®èŠä»¶ã«å¿ããŠé²åãã ã¢ãžã¬ã³ãã® ICP-MS æè¡ Ed McCurdy, ICP-MS Product Marketing, Agilent UK
æ¬å·ã® ICP-MS ãžã£ãŒãã«ã§ã¯ãåå°äœæ¥çã«ããã ICP-MS ãš ICP-QQQ ã®åœ¹å²ã«ã€ããŠè©³ãã説æããŸããã¢ãžã¬ã³ã㯠1990 幎以æ¥ã倧æåå°äœã¡ãŒã«ãŒãååŠè£œåäŸçµŠæ¥è ãšç·å¯ã«é£æºã㊠ICP-MS ã·ã¹ãã ããã³ã¢ããªã±ãŒã·ã§ã³ãéçºããå€åã®æ¿ããåæ¥çã®èª²é¡ã«å¯Ÿå¿ããŠããŸãããã¢ãžã¬ã³ãã¯ããªãã¢ã¯ã·ã¹ã€ãªã³ãšã¯ãŒã«ãã©ãºããç¬èªã®é«æ床 8900 ICP-QQQ ãš MS/MS ã¢ãŒããªã©ããã®æ¥çã«æ¬ ãããªãéèŠãª ICP-MS æè¡ã®é©æ°ãäž»å°ããŠããŸããã
1 ããŒãžåå°äœæ¥çã®èŠä»¶ã«å¿ããŠé²åããã¢ãžã¬ã³ãã® ICP-MS æè¡
2-3 ããŒãžåå°äœæ¥çã«ããã ICP-MS ãš ICP-QQQ
4-5 ããŒãžåå°äœè£œé ã§äœ¿çšãããé«çŽåºŠé žã®åæ
6 ããŒãžé»åã¿ãã³ã«å«ãŸãã埮ééå±ã® 枬å®
7 ããŒãžUS Winter Plasma Conference ã®ææ
8 ããŒãžåå°äœæ¥çåãã®åãçµã¿: ã¢ãžã¬ã³ãã®æè¡é©æ°ãAgilent ICP-MS é¢é£è³æ
2
2018 幎 4 æ - 第 72 å·Agilent ICP-MS ãžã£ãŒãã«
åå°äœæ¥çã«ããã ICP-MS ãš ICP-QQQKatsuo Mizobuchi, Abe Gutierrez, Bert Woods, and Ed McCurdy, Agilent Technologies
å³ 1 ã«ãŠãšã補é ããã»ã¹ã®æŠèŠã瀺ããŸããå°é»å±€ã絶çžå±€ãããããæ²çããã¹ãã³ã°ããšããã³ã°ããŸããè€éãªæ©æ§ãã¿ãŒã³ã®ç·å¹ 㯠10 ããã¡ãŒãã« (nm) ãšããå°ããã§ãã10 nm ã¯çŽ 40 åã® Si ååãšåçã§ããããŒãé åãè¿œå ããŸããããã«ã¯ãã·ãªã³ã³ã®äŒå°æ§ãå€ããç¹æ®ãªååãæ²çãŸãã¯åã蟌ãŸããŸãã
Si ããŒã¹ã®éç©åè·¯ (IC) ã«ã¯ãæ°çŸäžåã®ç¬ç«ãããã©ã³ãžã¹ã¿ãæèŒãããŠããŸãããã©ã³ãžã¹ã¿ã¯é žåç©ãããªã·ãªã³ã³ãçªåã±ã€çŽ ã®èªé»äœã®ãã¿ãŒã³å±€ã§æ§æãããéå±çžäºæ¥ç¶ã®åœ¹ç®ãæãããŸããå±€ã¯ããã€ã¢ã¹ãã§æ¥ç¶ããã 3D æ§é ã§ãã
çŸåšã®ã10 nmã圢ç¶ã«ã¯ã1970 幎代åœæã®åè·¯ã®æ©èœãçŽ 1000 åã® 1 ã«çž®å°ãããŠæèŒãããŠããŸãããã®ãããªå°ååãé«å¯åºŠåã«äŒŽããæ±æç©è³ªã®ç®¡çã®æ¹åãå¿ èŠãšãªããŸãããã®ããé«çŽåºŠååŠè¬åãžã®ããŒãºãé«ãŸããICP-MS ã®æ§èœã«å¯ŸããèŠæ±ãéåžžã«é«ããªã£ãŠããŸãã
åå°äœã®æŠèŠåå°äœæ©åšã®è£œé ã§ã¯ãæ±ææºãå³å¯ã«ç®¡çããå¿ èŠããããŸããæ¥çã®èŠç©ãã«ããã°ãæ©çãŸãæ倱ã®åå ã®çŽ 50 % ã¯æ±æã§ãã
æ±æ管çã§ãŸãéèŠãªã®ã¯ãé«çŽåºŠã®ãŠãšãåºæ¿ã§ããåºæ¿ã¯éåžžã¯ã·ãªã³ã³è£œã§ãããçåã±ã€çŽ ãçªåã±ã€çŽ ãã¬ãªãŠã ãçŽ ãªã©ã®ãã®ä»ã®ææã䜿çšãããŸããé«çŽåºŠã®é»åã°ã¬ãŒãã®ã·ãªã³ã³ã®çŽåºŠã¯ã9Nïœ 11N (99.9999999 %ïœ99.999999999 %) ã§ããå¿ èŠããããŸããæ±æã«ã€ã㊠9N ã®çŽåºŠãšã¯ãåºäœ Si ã«å«ãŸããäžçŽç©å çŽ ã®åèšã 1 ppb 以äžãšããããšã§ãã
æ±æç©è³ªãå¢ããªãããã«ããã«ã¯ããŠãšãåºæ¿ã®é«çŽåºŠãç¶æããã ãã§ãªãããŠãšã補é ããã»ã¹ã§äœ¿çšããååŠè¬åã®çŽåºŠãæ éã«ç®¡çããå¿ èŠããããŸããéå±æ±æãåé¡ãªã®ã¯ã絶çžç Žå£é»å§ã®äœäžãªã©ã«ãã£ãŠãæçµè£œåã®é»æ°çç¹æ§ã«åœ±é¿ãäžããå¯èœæ§ãããããã§ãã
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åå°äœè£œé ã«ããã ICP-MSICP-MS æè¡ã®éçº: 1980 幎代㫠ICP-MS ãç»å Žãããšãåå°äœã¡ãŒã«ãŒãååŠè£œåäŸçµŠæ¥è ããã®é«æ床ãäœãæ€åºéçãå€å çŽ åæåææ©èœã«å€§ããªé¢å¿ãå¯ããŸãããICP-MS ã®äœ¿çšã¯ã1990 幎代㮠HP 4500 ã®ãã¯ãŒã«ãã©ãºããã®éçºã«äŒŽã£ãŠæ¥éã«å¢å ããŸãããICP-MS ã®ã¯ãŒã«ãã©ãºãã«ãã£ãŠåŸ®éæ¿åºŠã® NaãKãCaãããã³ Fe ã枬å®ã§ãããããåå°äœã¡ãŒã«ãŒãååŠè£œåäŸçµŠæ¥è ã¯ã°ã©ãã¡ã€ããã¡ãŒãã¹ AAS ãçšããŠãããã®å çŽ ã枬å®ããå¿ èŠããªããªããŸããã
ICP-MS ã®æ©åšã¡ãŒã«ãŒã¯æè¡é©æ°ãç¶ããè¿å¹Žã§ã¯ããªãã«åé極 ICP-MS (ICP-QQQ) ããªãªãŒã¹ããŸããã2012 幎ã«ãªãªãŒã¹ãããã¢ãžã¬ã³ãã® 8800 ICP-QQQ ã¯ãã·ã³ã°ã«åé極 ICP-MS ãšæ¯ã¹ãŠé«æ床ãäœããã¯ã°ã©ãŠã³ããå¹²æžæå¶ãªã©ã®ç¹ãåªããŠããŸãããã®ãããSiãPãSãCl ãªã©ã®åçš®å çŽ ãå«ãããŸããŸãªæ±æå çŽ ããäœæ¿åºŠã§ãã¢ãã¿ãªã³ã°ã§ããŸããã¢ãžã¬ã³ã㯠8900 ICP-QQQ ã®ãªãªãŒã¹ã«ãããæ©åšæ§é ã®å°ååãæ©çãŸãããã³æ©åšæ§èœã®åäžãç®æããŠãåå°äœæ¥çãç¶ç¶çã«ãµããŒãããŸãã
ææ: ã·ãªã³ã³ãŠãšãåºæ¿ãšãé¢é£ããå±€ããã³ã³ãŒãã£ã³ã°ã®éå±æ±æã¯ãè¡šé¢éå±æœåº (SME) ãæ°çžå解 (VPD) ã«ãã£ãŠã¢ãã¿ãªã³ã°ã§ããŸããVPD ã§ã¯ãè¡šé¢å±€ (æªå 工㮠SiããŸãã¯èªç¶ãŸãã¯ç±çã«é žåãã SiO2) ã HF èžæ°ã§æº¶è§£ããŸãã溶解ããéå±ãéããŠãH2SiF6 ã®æ¶²æ»Žã§ ICP-MS åæãå®è¡ããŸããããã補é ã§äœ¿çšããããã®ä»ã®ææãäŸãã°ããªã¡ãã«ã¬ãªãŠã (TMG)ãããªã¡ãã«ã¢ã«ã (TMA)ããžã¡ãã«äºé (DMZ)ãããã©ãšããã·ã·ã©ã³ (TEOS)ãããªã¯ããã·ã©ã³ (TCS) ãªã©ã®éå±ææ©ååç©ã¯ãICP-MS ã«ããåæã«é©ããŠããŸãããã®ãããªååç©ã¯ãææ©éå±ååŠæ°çžæé·æ³ (MOCVD) ãååå±€æé·æ³ã«ãããŠèéå±èããšãã¿ãã·ã£ã«çµæ¶å±€ãå¢ããããã«äœ¿çšãããããªã«ãŒãµã§ããAlãCuãTiãCoãNiãTaãWãHf ãªã©ã®çŽéå±ã¯ãç©çæ°çžæé·æ³ (PVD) ã§ãŠãšãè¡šé¢ã«èéå±èãäœãããã®ã¹ããã¿ãªã³ã°ã¿ãŒã²ãããšããŠäœ¿çšãããŸããHigh-k èªé»äœã«ã¯ãZrãHfãSrãTaãããã³ã¬ã¢ã¢ãŒã¹å çŽ (REE) ã®å¡©åç©ãšã¢ã«ã³ãã·ããå«ãŸããŸãããããã®ææã«ã¯ããããæ±æç©è³ªã®èš±å®¹é床ããããããICP-MS ã«ããåæãå¿ èŠã§ãã
ããã»ã¹ååŠè¬å: å³ 1 ã®ãšãããIC 補é ã«ã¯å€ãã®ãŠãšãåŠçã¹ãããããããŸãã䜿çšããååŠè¬åã¯ãŠãšãè¡šé¢ã«æ¥è§Šãããããæ±æ管çãäžå¯æ¬ ã§ããè¡š 1 ã«ãäžè¬çã«äœ¿çšãããååŠè¬åã®äŸã瀺ããŸãã
æ±æ管çã«ãããŠæãéèŠãªããã»ã¹ååŠè¬åãšããŠãè¶ çŽæ°Ž (UPW) ãš RCA æšæºã¯ãªãŒãã³ã° (SC) 溶液ã§ãã SC-1 ããã³ SC-2 ããããŸããRCA ã¯ãªãŒãã³ã°æé ã«ãã£ãŠãããããå·ããã«ããŠãšãè¡šé¢ããååŠæ±æç©è³ªã埮ç²åäžçŽç©ãé€å»ã§ããŸããSC-1 (è±ã€ãªã³æ°Ž (DIW) ã«å«ãŸãã NH4OH ãš H2O2) ã«ãã£ãŠããŠãšãè¡šé¢ããææ©æ®çç©ãèãç²åãé€å»ãããŸãã次ã«ãSC-2 (DIW ã«å«ãŸãã HCl ãš H2O2) ã«ãã£ãŠã€ãªã³æ±æç©è³ªãé€å»ãããŸãã
SEMI ä»æ§: åå°äœè£œé è£ çœ®ææåäŒ (SEMI) ã¯ãç¹ã«ããã»ã¹ååŠè¬åãšã¬ã¹ã®èŠæ Œããã³ä»æ§ãçå®ããäžççãªåå°äœæ¥çå£äœã§ããå€ãã®åå°äœã¡ãŒã«ãŒã¯çŸåšãGrade 3 ãŸã㯠4 ã®ååŠè¬å (800ïœ 90 nm ã®åœ¢ç¶ã«é©ãã Tier-B ãŸã㯠Tier-C ä»æ§) ã䜿çšããŠããŸãããã ãæ§é ã®å°ååã«äŒŽããTier-D ã Tier-E ã®ååŠè£œåä»æ§ãžã®å¯Ÿå¿ãå¿ èŠãšãªããŸããTier-E ã§ã¯ 0.1 ppt æªæºã® DL ãšã0.5 ppt ã§ã®ã¿ãŒã²ããå çŽ ã®æ£ç¢ºãªæ·»å ååçãæ±ããããŸãããã®ãããICP-QQQ ã®æ§èœåäžãå¿ èŠã§ãã
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åŠç äžè¬çã«äœ¿çšãããååŠè¬å
ã¯ãªãŒãã³ã° çŽæ°ŽãSC-1 (NH4OH ãš H2O2)ãSC-2 (HCl ãš H2O2)ãSPM (éé žåç¡«é»æ··åç©ãH2SO4 ãš H2O2 ã®æ··åç©)ãDHF (åžé HF)ãIPA (ã€ãœãããã«ã¢ã«ã³ãŒã«)ãã¡ã¿ããŒã«
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3
Agilent ICP-MS ãžã£ãŒãã«2018 幎 4 æ - 第 72 å·
å³ 1. 68 % ã®é«çŽåºŠ HNO3 ã«å«ãŸããè€æ°ã® SEMI ä»æ§å çŽ ã®æ€éç·
å³ 2. 20 % ã®é«çŽåºŠ HCl ã«å«ãŸãã 39Kã51Vã52Crãããã³ 74Ge ã®æšæºæ·»å æ³ã®æ€éç·ãäœã BEC ãšåªããçŽç·æ§ã瀺ããŠããŸãã
4
Agilent ICP-MS ãžã£ãŒãã« 2018 幎 4 æ - 第 72 å·
åå°äœè£œé ã§äœ¿çšãããé«çŽåºŠé žã®åæKazuo Yamanaka and Kazuhiro Sakai, Agilent Technologies Japan
å¡©é ž: (ãã®å®éšã§äœ¿çšããŠãããããª) åžè²©ã°ã¬ãŒãã® HCl 㯠20 % ãŸã㯠36 % ã§ããã®ã«å¯Ÿããåå°äœã°ã¬ãŒãã® HCl 㯠37ïœ 38 % ã§ãããã¹ãŠã®ã°ã¬ãŒãã«ãããŠãå¡©åãããªãã¯ã¹ãéåžžã«é«ããšè€æ°ã®å€ååã€ãªã³ã圢æãããäžéšã®äž»èŠå çŽ ãžã®é倧ãªã¹ãã¯ãã«å¹²æžã®åå ãšãªããŸããäŸãã° H2
37Cl+ 㯠39K+ã35Cl16O+ 㯠51V+ã35Cl16OH+ 㯠52Cr+ ã«ã37Cl16O+ 㯠53Cr+ã35Cl37Cl+ 㯠72Ge+ã37Cl2+ 㯠74Ge+ã40Ar35Cl+ 㯠75As+ ã«å¹²æžããŸããåèš 50 çš®é¡ã®å çŽ (SEMI èŠæ Œ C27-0708 Tier-C ä»æ§ã®å šæåãå«ã) ããè€æ°ã®èª¿æŽã¢ãŒãã§åäœãã 8900 ICP-QQQ ã§æž¬å®ããŸãããåã¢ãŒãã®ããŒã¿ã¯ããµã³ãã«ããšã«èªåçã« 1 ã€ã®ã¬ããŒãã«ãŸãšããããŸããã
DL ããã³ MDL: 20 % ã® HCl ã«å«ãŸãã 50 çš®é¡ã®å çŽ ãã¹ãŠã§ã1 æ¡ã® ppt ãŸãã¯ãµã ppt ã® DL ããã³ BEC ãéæããŸããã
å®éçµæ: è¡š 1 ã«ã20 % ã®é«çŽåºŠ HCl ãš 36 % ã®äœçŽåºŠ HCl ã§ãæšæºæ·»å æ³ (MSA) ã§æž¬å®ãããã¹ãŠã® SEMI ä»æ§å çŽ ã®å®éããŒã¿ã瀺ããŸãã
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ç¡é ž: Agilent 8900 ICP-QQQ ã䜿çšããŠãåžéããŠããªãåžè²©ã°ã¬ãŒã (61ïœ 68 %) ã® HNO3 ãçŽæ¥åæããŸãããçŽæ¥åæã«ãã£ãŠãµã³ãã«ååŠçãç°¡çŽ åãããåžéäžã®æ±æç©è³ªã®æ··å ¥ãé²ãããšãã§ããŸãã
DL ãš BEC: 8900 ICP-QQQ ã䜿çšããŠåèš 49 çš®é¡ã®å çŽ ã枬å®ããŸããã8900 ICP-QQQ ã¯è€æ°ã®èª¿æŽã¢ãŒãã§åäœãã1 åã®åæã§åãµã³ãã«ãã€ã¢ã«ã«èªåçã«åãæ¿ããããŸãããã¹ãŠã® SEMI ã¿ãŒã²ããå çŽ ã«ã€ããŠãåªããçŽç·æ§ãšãµã ppt ã®æ€åºéç (DL) ãåŸãããŸãããNaãKãCaãFe ã§ã¯ãå žåçãªæšæºæ·»å ã®æ€éç·ã瀺ããŸãã (å³ 1)ã49 çš®é¡ã®å çŽ ãã¹ãŠ ããSEMI èŠæ Œ C35-0708 Tier-B [1] 㧠69ïœ 70 % ã® HNO3 ã«ã€ããŠèŠå®ãããŠãã 1 ÎŒg/L (ppb) æªæºãšããæ倧é床ããå€§å¹ ã«äœãæ¿åºŠã§æž¬å®ãããŸããã
è¡š 1. é«çŽåºŠ HCl ã® SEMI ä»æ§å çŽ ã®å®éçµæ
å çŽ ãµã³ãã« 120% HCl
ãµã³ãã« 236% HCl
DL
ng/L
Li <DL <DL 0.032
B 4.1 15 0.55
Na 0.15 6.4 0.064
Mg <DL 6.5 0.077
Al <DL 23 0.20
K 0.17 1.5 0.087
Ca 0.68 13 0.44
Ti 0.074 1.4 0.051
V 0.19 4.6 0.11
Cr <DL 0.55 0.18
Mn <DL 0.071 0.016
åå°äœé¢é£ã®ã¢ããªã±ãŒã·ã§ã³ããŒã:
⢠Analysis of Trace Metal Impurities in High Purity Hydrochloric Acid Using ICP-QQQã5991-8675EN
⢠Direct Analysis of Trace Metal Impurities in High Purity Nitric Acid Using ICP-QQQã5991-8798EN
⢠Determination of Ultratrace Elements in High Purity H2O2 with Agilent 8900 ICP-QQQã5991-7701EN
⢠MS/MS ã¢ãŒãã® Agilent 8900 ICP-QQQ ã«ããã è¶ é«çŽåºŠã®åå°äœã°ã¬ãŒãã®ç¡«é žã«å«ãŸãã埮éå çŽ ã® æž¬å®ã5991-7008JAJP
⢠Agilent 8900 ICP-QQQ ãçšãã極埮éæ¿åºŠã¬ãã«ã®ãªã³ã ç¡«é»ãã±ã€çŽ ãå¡©çŽ ã®åæã5991-6852JAJP
⢠Agilent 8800 ããªãã«åé極 ICP-MS ãçšãããè¶ çŽæ°Žäžã® ã«ã«ã·ãŠã ã®è¶ 埮éåæã5991-1693JAJP
⢠Direct Analysis of Trace Metallic Impurities in High Purity HCl by ICP-MSã5990-7354EN
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DL
ng/L
Fe 0.27 7.6 0.24
Ni <DL <DL 0.66
Cu 0.12 0.57 0.10
Zn <DL 1.1 0.14
As* 48 39 0.73
Cd 0.10 0.34 0.090
Sn 3.3 2.3 0.57
Sb 1.5 0.95 0.66
Ba 0.005 <DL 0.005
Pb 0.023 0.13 0.028
5
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1Johns Hopkins Bloomberg School of Public Health, Baltimore, Maryland, USA; 2Columbia Mailman School of Public Health, New York, New York, USA; 3Institute of Chemistry, University of Graz, Graz, Austria
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