lab. manual by y. matsushi - 京都大学 · 2012-05-10 · chemistry for in-situ 10be and 26al...

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Chemistry for in-situ 10 Be and 26 Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

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Page 1: Lab. manual by Y. Matsushi - 京都大学 · 2012-05-10 · Chemistry for in-situ 10Be and 26Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

Chemistry for in-situ 10Be and 26Al measurement

for terrestrial quartz by AMS at MALT

Lab. manual by Y. Matsushi

Ver. 2.0

Page 2: Lab. manual by Y. Matsushi - 京都大学 · 2012-05-10 · Chemistry for in-situ 10Be and 26Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

Qtz 10

Be 26

Al chemistry

Ver. 2.0

1

in-situ 10Be26Al

Y. Matsushi

10Be 26

Al !AMS"#$%&'()*+(,-./0123456#7,%89:%,(;<#Kohl and Nishiizumi (1992)=9HeimsathStone>?@#(ABCD;#E$D56F/034CDGHI'()#Kohl and Nishiizumi (1992)JK'(G;

LMNO%/0PQRSTUVWXYZ[\]^X#_`abcdG;

efFghijkl<mnop)qrksFktefuvwF+(;ef#xyz|G$%,(G~C#D$%k@k,;d)hPE pUp#7!Uzq,z= ,"¡\¢K;£#/0\¤Xo¥¦#K,(§1¨©!HF"PQ,#7,%ªC,«G_`ab¬'(;­#7kz(ik®DMSDS t¯°ef±?²#PQ%+( HF§³\UV´µ¶· ¸V?¹º»¼~C%tG;½¾¿ÀoÁ¿ÃÄÅÆ\U#7,%ÇÈÉ#G(Ê|ËÌ!ÍÈ3ÎÏÐÄ"&C%tG;ef/ÑÒ'(ÓFº»Ô#Õ7AÖ8o12´×4ef#(ØÙÚkvwÛ4pJ#ÜHhz+(;

ÝKohl, C.P., Nishiizumi, K., 1992. Chemical isolation of quartz for measurement of

in-situ–produced cosmogenic nuclides. Geochimica et Cosmochimica Acta 56,

3583–3587.

Heimsath, A.M. Dartmouth Univ. Lab Procedures (http://www.public.asu.edu/~aheimsat/)

Stone, J.O. Washington Univ. Lab Procedures

(http://depts.washington.edu/cosmolab/chem.html) Þßàá !âã12ä å" æ12FçdèéGHêë ìí2002;ÝîïðØ æ×4efuD 13ñë òói2ôõä1976;

R.J. ö¶÷X !øùú ûü" æý2þ¶· eCDi2D#ë 121998; 12å å æõ efvw#ËdD#ë 121993; 12å å æõ efvw#ËdD#ë 121987;

J.R. Y¶\ ! ´ ü" æÑÒ#(¦ ë òó122000;

Page 3: Lab. manual by Y. Matsushi - 京都大学 · 2012-05-10 · Chemistry for in-situ 10Be and 26Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

Qtz 10

Be 26

Al chemistry

Ver. 2.0

2

T°®×ÄH C!"#'!w%ç$»Ø[¶%&XGC%'("; U)¶*\o+]F,-×PQ.t; */X\F<4 cm0#1|2(!3G;U¡\4p¢KG;5À7k,d"; ~400 gM6zº¬;

×oÄH C!"#'!w%ç$»Ø[¶%&XGC%'("; P$p|78 5 L PP9\:\#~500 g+(; ¨;¨F<-,-×=,>C%PQ.t!_×z>:%,$%h?#Ck,;@¨ÛA@Bk,G!!"; ÓC°z+QD@ktk(FEQ#=F'(!º¬k@GH3I=FC%h,"; /0JKL#MC110 °CFNOPrB(;

!"#$%&'()*+,-

UYXZF+(,pÌF/0QR'(!3G;Up¢KG"; 1–0.25 mm STUFV$GWCQXKT\VÜ#YVCDZ*#D%,t; 1 mm[Óh\6QRCU]^Q_'; 1–0.25 mm§]^Xz 150~200 g ¼'F|:G OK; >1 mm G <0.25 mm§]^X½:`:Z*#&X IDHaC%'Û; ]µY÷\µbUY\FUZcd;

TUWXYZ#ab!!

1 mm

0.25 mm

1 mm

0.25 mm

Page 4: Lab. manual by Y. Matsushi - 京都大学 · 2012-05-10 · Chemistry for in-situ 10Be and 26Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

Qtz 10

Be 26

Al chemistry

Ver. 2.0

3

!

6M HCl + 0.03% H2O2./01234 5

: QRef°/02Lg9X500 mlhÑH2O2Ki9XHCl!TXj"H2O2!£k" 2 L g9Xº¬lmn!9Xo1º»¤p"; /0qC9X ID GGh#Hr!100 g/L acid: Øã#7|~180 g"; MQ 0.9 LS(; 500 mlhÑFTXj HCl 0.9 LS(; !st×uvwx+(/0¬ab: »y HCl:zC%K|, ¼~'(G"; 30% H2O2 1.8 mlS¨75~#rB%tz;§Y+Q#|7t]k,G;

\YiH3I¨#VYVC¨;¨V?h#Ø'(rF:(; 6H3I&¶YVC80 °CF>12 h\]^X;

(>12 cycles of 50 min U-sonic with 10 min pause);

p¡p7%PQôC·§V?F¿ÀCk,M6#'; !÷\K"mnPQ(; ·§V?FÓC°hYX#; ~200 ml MQF 2Gd=FC=F¨hYX#; MQF>3Gd=FC=F¨¨;]X#!¨>Ckz@ËdG";

80 °CFOP; OPqCZ*#'Û;

80 °C, 12 h for HCl treatment 95 °C, 8-9 h × 3~4 times for HF/HNO3 leaching

~180 g sample

0.9 L MQ

0.9 L 12M HCl

~1.8 ml 30% H2O2

2 L

bottle

Page 5: Lab. manual by Y. Matsushi - 京都大学 · 2012-05-10 · Chemistry for in-situ 10Be and 26Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

Qtz 10

Be 26

Al chemistry

Ver. 2.0

4

HF "#$%&HF

1% HF/HNO3.6789&Meteoric 10Be 5

: t34f°/02Lg9X100 mlhÑHFHNO3!£k" 2 L g9Xº¬lmn!9Xo1º»¤p"; /0qC9X ID GGh#Hr!7.5-9 g/L acid: Øã#7| ~15-18 g: 1 sample#7|V\Y>100 g"; MQ 1.92 LS(;

100 mlhÑFconc. HF43 mlconc. HNO333 mlS¨75~#rB%tz;§Y+Q#|7t]k,G;

H3I¨#YVC95 °CF 9 h \]^X

(9 cycles of 50 min U-sonic with 10 min pause);

p¡p7%PQôC·§V?F¿ÀCk,M6#'; !§K"mnCPQ(; ÓC°YX#; ~200 ml MQF 2Gd=FC=F¨hYX#; Ó~|=F9Xç$%&XV 1ã#G(; MQF>3Gd=FC=F¨¨;]X#!¨>Ckz@ËdG";

Ø34Ø'ÛC%th 80 °CFOP;

#\¤X 3^Q_'!2 Y\X9@ 1 sample#7|V 1ã"; !º¬#ÍO% ?¡¢¸X"; ~4 Y\X\¤Xz$$D@80 °CFOP; OPq;Z*#'(;

~15-18 g sample

1.92 L MQ

43 ml conc. HF

33 ml conc. HNO3

2 L

bottle

Page 6: Lab. manual by Y. Matsushi - 京都大学 · 2012-05-10 · Chemistry for in-situ 10Be and 26Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

Qtz 10

Be 26

Al chemistry

Ver. 2.0

5

'(")*+,-HF

Be :;<=>?&HF .67@ABC#DDEFGHIJKLMNOPQR-

: \¤Xf° /0200 ml PTFE 9\:\PTFEÉÑL5 ml ¢£VBeKh9X\XhѤV)\VHFHNO3!¥¦ K or¤i©&K"HClO4Wako Be 100ppm AAS-STDWako Al 1000ppm AAS-STD

PTFE 9\:\#öX!/0+X"; *§%P$D Be-STDVq; ¢£V¤Gh=,;h BeKh9X§; ¨9\:\ /0q!<60 g";©qª#/0«@rk,d#;/0w%ç$»Ø#'; 100ppm Be-STD 3 ml!0.3 mgBe"¬Cq; ­i|,Q/0#®°¯B(G#k(F°K#(±1#ab;q²a³C%v&gi²¯°P(;!ÆZ:X# Be¸´=9¢£V¤º»±S1000ppm Al-STD 2 ml!2

mgAl"¬";l<$$D9\:\#ÉÑL B%t; w%¸´¬z$$D@Be- Al-STD V\6qCµ¶;

PTFE 9\:\#100 mlhÑF conc. HNO3 20 mlconc. HF 100 ml S(; 9\:\~200·¤V)\VÓ#¸Î!©¹6º»6ÑF¼~"; ɼ ¥¦½¾¼~;ÉÑL¿#CGCGi§1×z ô'(Fab;¤V)\VÓ#rk,G; zÀw#¥¦CÁÂzktk(F HFÃÄaÅ';aG|¤V)\V9@9\:\'G JKOÁCD@9\:\8¤V)\V©¹#YC%²hÆÇG';

conc. HNO3 10 mlÈ# conc. HF 10 ml Sr@#JKOÁ; conc. HNO3 10 mlÈ# conc. HClO4 10 ml Sr@#JKOÁ; conc. HNO3 1 mlÈ# conc. HF 3 ml Sr@#JKOÁ; conc. HNO3 3 mlÈ# conc. HClO4 3 ml Sr@#JKOÁ; gl< 3^Q_';

Ék,CÊÉ#ËzOÁCD@C%Z*#¦¶C%t;

3 ml 100 ppm

Be carrier sol.

(0.3 mgBe)

20~60 g quartz

Page 7: Lab. manual by Y. Matsushi - 京都大学 · 2012-05-10 · Chemistry for in-situ 10Be and 26Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

Qtz 10

Be 26

Al chemistry

Ver. 2.0

6

Sample ID

Procedure

Note

~1 ml conc. HNO3/g qtz (~20 ml)~5 ml conc. HF/g qtz (~100 ml)

Additional conc. HNO3 & HFDry up

~10 ml conc. HNO3 & HF

Dry up

~10 ml conc. HNO3 & HClO4

Dry up

~1 ml conc. HNO3

~3 ml conc. HFDry up

~3 ml conc. HNO3 & HClO4

Dry up

Repeat 3 times

~1 ml conc. HNO3/g qtz (~20 ml)~5 ml conc. HF/g qtz (~100 ml)

Additional conc. HNO3 & HFDry up

~10 ml conc. HNO3 & HF

Dry up

~10 ml conc. HNO3 & HClO4

Dry up

~1 ml conc. HNO3

~3 ml conc. HFDry up

~3 ml conc. HNO3 & HClO4

Dry up

Repeat 3 times

~200

Page 8: Lab. manual by Y. Matsushi - 京都大学 · 2012-05-10 · Chemistry for in-situ 10Be and 26Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

Qtz 10

Be 26

Al chemistry

Ver. 2.0

7

Al.)"/#012304256% 67S AlTUVW$XBY

: OÁ/05 ml ¢£VhѤV)\VBe Kh9XHNO3!¥¦ K[Ó"10 ml ÌÍÛÌÍÛÕ%ÌÍÛqK9X

\XhÑ# conc. HNO3ÃGQ¢£V¤GØÎ#Gh=,; ¶T¢£VFOÁ/0#conc. HNO33.7 ml»7S(; MQ 6.3 ml»7S(; º¬k@ÏtH3I#9(ksC%/0Àw#¥9'!wxk@lÉиÎ'(G,"; hÑFMQ 90 mlS(;

ÌÍÛöX!/0l+X";

¥hQ9\:\q; ÌÍÛ§YGQÌÍÛÑ#ÏtÒB%§Yu°¨q; /0¥h 2.5 ml MCÌÍÛG¢£V¤Gh=,;hBeKh9X§;hÆz»Ó#7,D@Ô|P(; /0¥h 2.5 mlÕ3!~7.5 ml"ÌÍÛ#M'; ¢£V¤/0ÖG#×Ø'(G; ÌÍÛ#§YÒBÙq; ÌÍÛ§Y%*§%Fµ¶;

¤V)\V!~150°C"F/0JKOÁrB(; OÁC%Z*#¦¶'(;

~100 g sol.

7.5 mlaliquot

3.7 ml conc. HNO3

6.3 ml MQ

Leave for hours

90 ml MQ

Page 9: Lab. manual by Y. Matsushi - 京都大学 · 2012-05-10 · Chemistry for in-situ 10Be and 26Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

Qtz 10

Be 26

Al chemistry

Ver. 2.0

8

789%:;

FeMnNPPZ[\.]^_M`abcde(R )

: OÁ/0DOWEX 1-X8 100–200 mesh i\ :!25 ml":Õ%hT\VÏÚÛÜV100 ml PTFE 9\:\5 ml ¢£VMQ=9XUg¶VhÑPFAV¤V)\VHCÝ!¥¦ K[Ó"H2O2!¥¦ K[Ó" : Þ¶ßX×Øàá!DOWEX 1-X8 100–200 mesh"=FK¹#çK'(QyCâ#![25

ml × (:lã1)]M6"PQô'; MQ St9|äåCG@t¸ÎC%ÓC°æ%(;KçoDQzktk(F=F^Q_';àá#Éèk(Âz+(¾Ug¶VÄFPQ.t; ::Õ%#º¬lYVC:Ü#héÜVYV'(; i\ÃPQôC:Ó#B(;MQ FÇGC¯êëF7@#C%\6 MQ>C%ìk¹­®#C%t; 25 ml hÑFÑQPQôÑí,ê:#>C¯FhéÎ#î7(; :# MQ :D'GotàᢣVFaC:#¸9#Í­rB%,t;àá?#ï:Dðño?çzk,d#;DàáÓz¨7#k(d#; hT\VÏÚÛYV;:GT\V#òêöXC%t; !"#$ : :Ü#héÜVYV;ÏÚÛ¨?TOT\VW(; T\V# conc. (12M) HCÝ 25 ml!1:":(;¨?TóôC%Wõ$tQóhÆFàáÓïrk,d#>';àáÉzöÊɧG±1; [Ü:#¥¡h>'G|w%Op÷; 0.5M HCݺ¬<!øùØúAB"; 0.5M HCÝ 50 ml!2:">';àáÉzöÊÉ9@ûüÉ#; 9M HCÝ!with 0.1% H2O2"º¬<!øùØúAB"; 9M HCl 30 ml!1.2:">';àáÉz\6öÊɧG±1;

Conditioning 12M HCl (1 column ) 0.5M HCl (2 column ) 9M HCl w 0.1% H2O2 (1.2 column ) Sample loading SMP sol. (2+1+1 ml 9M HCl w 0.1% H2O2 ) Elution 9M HCl w 0.1% H2O2 (1.2 column )

25 ml column DOWEX 1-X8 100–200 mesh

Page 10: Lab. manual by Y. Matsushi - 京都大学 · 2012-05-10 · Chemistry for in-situ 10Be and 26Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

Qtz 10

Be 26

Al chemistry

Ver. 2.0

9

!"#$ %&''' OÁ/0$D 200 ml PTFE9\:\#¶T¢£VF 9 M HCÝ!with 0.1% H2O2" 2 mlS¥¦rB(!¥hý!III"TTþÂ[FeClx](x−3)−#$%É+(,XXþÂ#$%ß)XÉ#"; /0lUg¶V 9M HCl!0.1% H2O2"FGh=,; 100 ml PTFE 9\:\#öX;

()*+" ,-.:ÜhéÜVöXCD PTFE 9\:\#PQS(; Ug¶VF 200 ml PTFE 9\:\?/0¥ht9|äå:ÏÚÛ»C%/0¥hàáÓ#¸9#B(; 200 ml PTFE 9\:\# 9M HCl!with 0.1% H2O2" 1 ml:Ug¶VGGh#'',F#:#>';l<hdØ6^Q_';

Ug¶V/0ÖG#S(G; \6ÏÚÛPQ9M HCl!with 0.1% H2O2" 30 ml!1.2:">';

·§V?#¤V)\VYV; ¥¡h$D 100 ml PTFE 9\:\~150·FJKOÁrB(;

:Ü#héÜVYVCMQ 50 mlM6>'; hhYX§; àá·§V?FOPrB%9@efU¤×GC%æ%(;

/0123.hÑK,%PFAV#¥¦ K[Ó conc. HCl!12M">18.2 MΩ MQFøùC%<;Gh=,ksÖC%#7t(G;ÈLMFh;

456789:;/0<

HCl : MQ Øã+DQX !:" º¬!25 ml: 8ãG|; HCl + MQ"

12 M HCl =conc.HCl 1 200 ml

0.5 M HCl 1 : 23 2 >400 ml!20 + 460 ml" 9 M HCl

† 3 : 1 2.6 >520 ml !450 + 150 ml"!+ ~2.0 ml H2O2"

† ~0.1%6#k(dconc.(30%)H2O2¬;

Page 11: Lab. manual by Y. Matsushi - 京都大学 · 2012-05-10 · Chemistry for in-situ 10Be and 26Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

Qtz 10

Be 26

Al chemistry

Ver. 2.0

10

<89%:; f^_M`abcgde!Bhij. Be, Al kh

: OÁ/0DOWEX 50W-X8 100–200 mesh i\ :!25 ml":Õ%hT\VÏÚÛÜV100 ml & 200 ml PTFE 9\:\50 mli9X5

ml ¢£VMQ =9XUg¶VhÑPFA V¤V)\VHCÝ!¥¦ K[Ó"H2O2!¥¦ K[Ó" LMG#¶ßX×Øàá!DOWEX 50W-X8":#AYV'(; øù<p÷¾Ð#!p÷¥¡h>C%,(Ð#"; !"#$ . :Ü#hé9XYV; 6M HCÝ 100 ml!4:":#>'; àá­zy'(; MQ 50 ml!2:":#>'; àá­zû#(;

!"#$ %&... OÁ/0$D 200 ml PTFE 9\:\#¶T¢£VF0.5M HCÝ!with 0.1% H2O2"2 mlS¥¦rB(; Ug¶V 0.5M HCl!0.1% H2O2"FGh=,; 100 ml & 200 ml PTFE 9\:\(:lÕ2 )#öX;/0 ID¾Be/AlW8tG; 50 mli9X(:lÕ2 )#öX;/0ID¾Be/AlW8tG;

()*+" .:ÜhÜVF,; Ug¶VF200 ml PTFE9\:\?/0¥ht9|äå:ÏÚÛ»C%/0¥hàáÓ#¸9#B(; 200 ml PTFE 9\:\# 0.5 M HCl!with 0.1% H2O2" 1 ml:Ug¶VGGh#'',F#:#>';l<hdØ6^Q_';Ug¶V/0ÖG#S(G; ,-.0.5M HCl!with 0.1% H2O2" 96 ml :!Sample sol.G+$B% 4:">';

Conditioning 6M HCl (4 column ) MQ (2 column ) Sample loading SMP sol. (2+1+1 ml 0.5M HCl w 0.1% H2O2 ) Elution 0.5M HCl w 0.1% H2O2 (total 4 column) 1.2M HCl (1.8+4 column) The latter 4 frac. for Be 3M HCl (1+2+0.8 column) The middle 2 frac. for Al

25 ml column DOWEX 50-X8 100–200 mesh

Page 12: Lab. manual by Y. Matsushi - 京都大学 · 2012-05-10 · Chemistry for in-situ 10Be and 26Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

Qtz 10

Be 26

Al chemistry

Ver. 2.0

11

:ÜhéÜVöXCD 50 ml i9X!Be"#PQS(; 1.2M HCl 45 ml!1.8:">';ÆÜi9X§YC%'Û; :Üi9X!Be"öXCD 200 ml PTFE 9\:\!Be"#PQS(; 1.2M HCl 100 ml!4:">'; ÆÜ¥¡h$DPTFE9\:\!Be"¤V)\V!·§V?; ~150·"FJKOÁrB(;

:Ü#öXCD 50 ml i9X!Al"YV; 3M HCl 25 ml!1:">'; :Üi9X!Al"öXCD 100 ml PTFE 9\:\!Al"#PQS(; 3M HCl 50 ml!2:">'; ÆÜ¥¡h$D PTFE 9\:\!Al"¤V)\V!·§V?; ~150 ·"FJKOÁrB(; :Ü#=s 50 ml i9X!Al"\6YV; 3M HCl 20 ml!0.8:">'; ÆÜi9X§YC%'Û;

:Ü#héÜVYVCMQ 50 mlM6>'; hhYX§; àá·§V?FOPrB%9@efU¤×GC%æ%(; hT\VÏÚÛMQF,FZ*#:%t;

=5678>?@Conditioning Elution

6M

HCl × 4 column

0.5M HCl

w 0.1% H2O2

× 4 column (Total)

× 1.8 column MQ × 2 column

1.2M HCl

× 4 column Be frac.

Sample loading & linsing × 1 column

× 2 column Al frac. 2+1+1 ml 0.5M HCl

w 0.1% H2O2

3M HCl

× 0.8 column

=56789:;/0<

HCl : MQ Øã+DQX !:" º¬!25 ml: 8ãG|;

HCl + MQ" 6 M HCl 1 : 1 4 >800 ml!420 + 420 ml"

0.5 M HCl† 1 : 23 4 >800 ml!40 + 920 ml"!+ ~3.2 ml H2O2"

1.2 M HCl 1 : 9 5.8 >1200 ml!30 + 270 & 100 + 900 ml" 3 M HCl 1 : 3 3.8 >800 ml!200 + 600 ml"

† ~0.1%6#k(dconc.(30%)H2O2¬'(;

Page 13: Lab. manual by Y. Matsushi - 京都大学 · 2012-05-10 · Chemistry for in-situ 10Be and 26Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

Qtz 10

Be 26

Al chemistry

Ver. 2.0

12

=>?@

BeOHlm(RnoBCplmqrDs.tuv 5

: OÁBeCl2/0]XPTFE§%Y\10 mlÌÍÛÌÍÛÕ%Z¸&\5 ml ¢£VUg¶V!/0l×2"Be Kh9X MQ Ki9XK PFA VHNO3!¤i©&K"NH4OH!¥¦ K" K PFAV# 3M NH4OH3M HNO3øùhdØã#=FK<; ]X§%Y\=FKF=F; =,CD¢£VFOÁ/0!BeCl2"$D 50 ml PTFE 9\:\# 3M HNO3 2

ml:/0t¥9'; ÌÍÛ#öX

50 ml PTFE 9\:\/0¥hUg¶VF]X#MC#§%YXC%ÌÍÛ#M'; ¢£VF 50 ml PTFE9\:\#MQ 1 ml:Ug¶VGGh#'',F#ÌÍÛ#M';l<hdØ6^Q_';Ug¶V]X/0ÖG#S(G;

¢£VFÌÍÛ# 3M NH4OH 4 ml:Z¸&\FGd'(;Be(OH)2zÍ; Ì`¡!2500 RPM; 10 min"; ÓC° Beh9X§;

M¢£VFÌÍÛ# 3M HNO3 2 ml:Z¸&\FGdC% Be(OH)2¥9'; ÓHæÍÌ`¡ÓC°ël<^Q_';

Be(OH)2

Precipitation

Dissolve

Be(OH)2

4 ml

3 M

NH4OH

Be(OH)2

Precipitation

SMP sol.

2 ml 3 M

HNO3 &

1 ml MQA2

4 ml

3 M

NH4OH

2 ml

3 M

HNO3

Centrifuge &

decantation

Final Be(OH)2

Precipitation

Centrifuge &

decantation

Page 14: Lab. manual by Y. Matsushi - 京都大学 · 2012-05-10 · Chemistry for in-situ 10Be and 26Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

Qtz 10

Be 26

Al chemistry

Ver. 2.0

13

!A

Be, Al wxyxz|&~0

: AlOÁ/0BeÍ/0¢XYVUg¶V1 ml M¢£VMQ9X 9\:\ ¹¤V)\V:Ü\Â)Xi9X

BeBCDE3·§V?tcdCDBe OÁK¤V)\VGÅFµY÷\FÔ,D:Ü\YV; Ug¶VFt=FCDMQFqt''; Z 9\:\¤V)\VÓ#Ê/0Î%÷\V#Hr'(; ÌÍÛ9@ Be(OH)2Ug¶VF 9\:\#MC%,t;º¬k@Ì`¡FÌÍÛ8#­rB% ,ô'<!^Q_';Ø6# 9\:\#Q|@k,¾¨yC"GCD+G\¬^Q_'; 80·F%¨"G';#$#ab!%&F6Ó']k,G"; O,%|D@ 150·M6#F6Ó'%N#¨z"G'; /0zOÁCD@Â)XÜL!æp\ëéμ~´HrG"#MC(# ¹F§Y'(;§Y(#9)BÂ)X?#YV; 6-7ÐCBeO§G1rB(; zSD@*§%F¦¶´Á&C%'Û;F|(ê'#)UËd;

AlBCDE3OÁ AlCl3/0$D 50 ml PTFE 9\:\#¶T¢£VF 0.5 ml MQ¬; Be#÷\V#Î8,%:Ü\|¤V)\VÓFOPrB(; /0zOÁCD@§KZ*¹Ó#Ê!æp\ëéμ~´HrG" ¹F§YCD(#§#:(; 900·F 1 h CAl2O3§G1rB(; zSD@*§%F¦¶´Á&C%'Û;F|(ê'#)UËd;

~80 °C

Be: >400 °C ~7 min with a microwave Al: ~900 °C, 1 h with a muffle kiln

Page 15: Lab. manual by Y. Matsushi - 京都大学 · 2012-05-10 · Chemistry for in-situ 10Be and 26Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

Qtz 10

Be 26

Al chemistry

Ver. 2.0

14

BC3

Be, Al wxyxAMSQtJQ#IQ-X

: BeO/0Al2O3/0)UU*\+,:-\·¢XYVZ§.¶\XpßQX/QX )UU*\:-\·#0&=FC%OP;

UpU¢)U-\XöX¤µY÷\Fcd; Z§.¶w#1t;.ÂYV; ¢XYVç$%)U2°Õ%Ê%,t; Z*#öX; /0Kß+(,/QXKU*\mn; Z§.¶ 10 cm35!Õ/0l"#jQ/0 W<!]\V<$%t;

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\XpPQS%<!/0ÖG#^Q_';

w%/0)UC$$D@\XöX¤?=>?rB;½@=FC%OPrB(;

!! 10Be-26

Al-AMS

Al Be

Al2O3 : Ag

= 1 : 1~0.8

BeO : Nb

= 2 : 1

Page 16: Lab. manual by Y. Matsushi - 京都大学 · 2012-05-10 · Chemistry for in-situ 10Be and 26Al measurement for terrestrial quartz by AMS at MALT Lab. manual by Y. Matsushi Ver. 2.0

Qtz 10

Be 26

Al chemistry

Ver. 2.0

15

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ISJOPPTUVOWX: MQA:-H3I=FAMQAOP

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[\: §TX9\:\?F!ÖtG,"-MQ!>18.2 MΩ"H3I=FAYVXH3I=FÕ2AOP

)]^X : *\H¦!¢XIz$DhJ:zP:k,h"A§´DÇUgXCQ=,AK-U*\þLTFCQ=,A¨;¨AMQ AMQH3I=FAYVXH3I=FÕ2AOP