ÍÁÈÀ×÷ΪũҵÉú²ú»î¶¯µÄÖ÷ÒªÔØÌåºÍÇéÐÎÎÛȾÎïµÄÖ÷ÒªÊÜÌå £¬ÆäÎÛȾˮƽÓëÈËÃǵÄÉúÑÄϢϢÏà¹Ø ¡£Í¨¹ýÑо¿Ë®ÏµµÄÖ÷Òª×é³É²¿·Ö--³Á»ýÎï £¬¿ÉÒÔÏàʶÎÛȾÏÖ×´ £¬×·ËݸÃÇøÓòÖؽðÊôÎÛȾÀúÊ· £¬Ñо¿ÎÛȾÎïµÄ³Á»ý¼°×ª±ä¼ÍÂÉ ¡£Ëæ׏¤Òµ»¯µÄÉú³¤ £¬ÍÁÈÀºÍˮϵ³Á»ýÎïÖеÄÖؽðÊôÎÛȾ £¬ÒѾÑÏÖØÓ°ÏìÁËÉú̬ƽºâ ¡£Òò´Ë £¬¶ÔÍÁÈÀºÍˮϵ³Á»ýÎïÖеÄÖؽðÊô¼à²âÒѳÉΪÇéÐμà²âµÄÖ÷ÒªÊÖ¶ÎÖ®Ò» ¡£
±¾ÎIJο¼Éú̬ÇéÐβ¿³õ¸å¡¶ÍÁÈÀºÍ³Á»ýÎï½ðÊôÔªËØ×ÜÁ¿ µç¸ÐñîºÏµÈÀë×ÓÌåÖÊÆ×·¨¡· £¬½ÓÄɲî±ð±ÈÀýµÄ»ìÏýËᣨ9mL HNO3+3mL HCl+3mLHF+1.5mLHClO4)¶ÔÍÁÈÀºÍˮϵ³Á»ýÎï±ê×¼ÎïÖʾÙÐÐÏû½â £¬½ÓÄÉRh¡¢Re×÷ÄÚ±ê £¬ÓÃICP-MS¾ÙÐвⶨ £¬Ð§¹ûÅú×¢¸ÃÒªÁìÄܹ»¿ìËÙ¡¢×¼È·µØÆÊÎöÍÁÈÀºÍ³Á»ýÎïÖеÄÖؽðÊôÔªËØ ¡£
1. ÒÇÆ÷¼ò½é
ICP-MS 2000BÊÇ×ðÁú¿Ê±ÖйúÕ¾×ÔÖ÷Ñз¢µÄµç¸ÐñîºÏµÈÀë×ÓÌåÖÊÆ×ÒÇ £¬¸ÃÒÇÓþßÓÐѸËٶȸߡ¢¼ì³öÏ޵͡¢ÎȹÌÐԺá¢ÏßÐÔ¹æÄ£¹ã¡¢ÖÊÆ××ÌÈÅСµÈÌص㠣¬¿ÉÓÃÓÚÇéÐμà²â¡¢Ê³ÎïÇå¾²¡¢Ò½Ò©¼°ÐÄÀíÆÊÎö¡¢Ê¯ÓÍ»¯¹¤µÈÖÚ¶àÁìÓò ¡£
ͼ1. ICP-MS2000Bµç¸ÐñîºÏµÈÀë×ÓÌåÖÊÆ×ÒÇÍâ¹Ûͼ
2. ²âÊÔÔÀí
ÍÁÈÀºÍ³Á»ýÎïÑùÆ·¾Ïû½âºó £¬ÊÔÑùÓÉÔØÆø´øÈëÎí»¯ÏµÍ³Îí»¯ £¬ÒÔÆøÈܽºÐÎʽ½øÈë¸ßεÈÀë×ÓÌå £¬³ä·ÖÕô·¢¡¢½âÀë¡¢Ô×Ó»¯ºÍµçÀë £¬×ª»¯³ÉµÄ´øµçºÉÀë×Ó¾Àë×Ó´«Êäϵͳ½øÈëÖÊÆ×ÒÇ £¬Æ¾Ö¤Àë×ÓµÄÖʺɱȾÙÐÐÊèÉ¢²¢¶¨ÐÔ¡¢¶¨Á¿ÆÊÎö ¡£
3. ʵÑ鲿·Ö
3.1ʵÑéËùÓÃ×°±¸¼°ÊÔ¼Á
ICP-MS2000B(×ðÁú¿Ê±ÖйúÕ¾)£»
΢²¨Ïû½âÒÇ(WX-8000 £¬ÉϺ£ÒÙÒ¢)£»
¸ÏËáÒÇ£¨ÉϺ£ÒÙÒ¢£©£»
ʵÑéÓó¬´¿Ë®µç×èÂÊ´ï18.25M¦¸¡¤cm£¨Merck Millipore£©£»
65%ÏõËá £¬37%ÑÎËᣨG.R £¬Scharlau£©£»
Çâ·úËá¼°¸ßÂÈËᣨG.R £¬¹úÒ©¼¯ÍÅ£©£»
ÔªËرê×¼ÈÜÒº(10mg/L £¬Inorganic Ventures) ¡£
3.2 ÑùÆ·Ç°´¦Öóͷ£
¸÷³ÆÈ¡0.1gÍÁÈÀ¼°Ë®Ïµ³Á»ýÎï±êÑùÖÁ¾ÛËÄ·úÒÒϩ΢²¨Ïû½â¹ÞÖÐ £¬¼ÓÉÙÁ¿µÄ³¬´¿Ë®Èóʪºó £¬¼ÓÈë9mLÏõËáºÍ3mLÑÎËá ¡£Ô¤·´Ó¦20·ÖÖÓºó £¬¼Ó¸ÇÅ¡½ôÏû½â¹Þ £¬Í¬Ê±×öÑùÆ·¿Õȱ ¡£Æ¾Ö¤±í1µÄÉýγÌÐò¾ÙÐÐÏû½â £¬´ýÏû½âÍê³ÉºóÀäÈ´ÖÁÊÒΠ£¬¼ÓÈë3mLÇâ·úËá £¬ÔÚµçÈÈ°åÉÏ200¡æ¾ÙÐÐ·É¹è ¡£·´Ó¦Ô¼40minºó £¬ÔÙ¼ÓÈë1.5mL¸ßÂÈËá £¬ÔÚ¸ÏËáÒÇÉÏ180¡æ¾ÙÐиÏËá´¦Öóͷ£ £¬Ö±ÖÁ°×ÑÌ £¬ÄÚÈÜÎï³Ê²»Á÷¶¯×´Ì¬ £¬È¡ÏÂÉÔÀä £¬ÓÃÉÙÁ¿ÏõËá³åÏ´Ïû½â¹ÞÄÚ±Ú £¬Ê¹ÓÃÓàÎÂÏûÈÚ¸½ÔÚÏû½â¹ÞÄڱڵIJÐÔü ¡£Ó󬴿ˮϴåªÏû½â¹ÞÄÚ±ÚÖÁÉÙÈý´Î £¬½«Ïû½âҺתÒÆÖÁ 100 mL ÈÝÁ¿Æ¿ÖÐ £¬Ñ¡ÓÃîî¡¢ïª×öÄÚ±ê £¬Í¬Ê±½«ÑùÆ·ºÍÑùÆ·¿ÕȱÖл®·Ö¼ÓÈë10?g/Lî請ìÏýÄÚ±ê £¬Óó¬´¿Ë®¶¨ÈÝÖÁ¿ÌÏß £¬Ò¡ÔÈÒÔ´ýÆÊÎö ¡£
±í1 . ΢²¨Ïû½âÉýγÌÐò
|
ÉýÎÂʱ¼ä/min
|
Ïû½âζÈ/¡æ
|
¼á³Öʱ¼ä/min
|
|
5
|
120
|
3
|
|
3
|
160
|
3
|
|
3
|
180
|
25
|
3.3 ±êÒºÉèÖÃ
½ÓÄÉÖð¼¶Ï¡Ê͵ķ½·¨ £¬ÅäÖƽéÖÊΪ2%ÏõËáµÄ¶àÔªËرê×¼»ìÏýÈÜÒºÓÚһϵÁÐ100 mL ÈÝÁ¿Æ¿ÖÐ £¬Ñ¡ÓÃîî¡¢ïª×öÄÚ±ê £¬ÄÚ±êŨ¶ÈΪ10?g/L £¬Óó¬´¿Ë®¶¨ÈÝÖÁ¿Ì¶È²¢Ò¡ÔÈ ¡£ÅäÖÆŨ¶ÈÈç±í2Ëùʾ ¡£
±í2. ¸÷ÔªËرê×¼ÇúÏßŨ¶È£¨?g/L£©
|
Ôª ËØ
|
±êÒº1
|
±êÒº2
|
±êÒº3
|
±êÒº4
|
±êÒº5
|
±êÒº6
|
|
9Be¡¢121Sb¡¢238U
|
0.5
|
1.0
|
5.0
|
10.0
|
20.0
|
50.0
|
|
52Cr¡¢59Co¡¢60Ni¡¢65Cu¡¢208Pb
|
5.0
|
10.0
|
20.0
|
50.0
|
100
|
200
|
|
114Cd
|
0.1
|
0.5
|
1.0
|
2.0
|
5.0
|
10.0
|
±¸×¢£ºÆäÖÐ114CdºÍ208Pb½ÓÄÉ×ÌÈÅ·½³Ì¾ÙÐÐУÕý £¬114Cd=114Cd×Ü-0.027*118Sn;208Pb=206Pb£«207Pb£«208Pb ¡£
3.4 ÒÇÆ÷²ÎÊý
½ÓÄÉ10¦Ìg/L Li ¡¢Co¡¢
In¡¢
Ce¡¢
Uµ÷гҺ¶ÔÒÇÆ÷¾ÙÐÐÓÅ»¯ £¬Ëù»ñµÃµÄÒÇÆ÷²ÎÊýÈçÏ£º
RFµçÔ´¹¦ÂÊ£º1300W µÈÀë×ÓÆø£º13L/min
¸¨ÖúÆøÁ÷ËÙ£º1.06 L/min ÔØ Æø£º 1.2L/min
²ÉÑùÉî¶È£º 20 ɨÃè·½·¨£º Ìø ·å
3.5 ʵÑéÊý¾Ý
´ýÒÇÆ÷ÎÈ¹Ìºó £¬¶ÔÑùÆ·¿ÕȱÈÜҺƽÐвⶨ8´Î £¬ÅÌËã8´Î²âÊÔЧ¹ûµÄ±ê×¼Îó²îSD £¬ÒÔ3*SD/K(KΪ±ê×¼ÇúÏßбÂÊ)¶ÔÓ¦µÄŨ¶ÈΪҪÁì¼ì³öÏÞ£»Í¬Ê±¶ÔÍÁÈÀ¼°³Á»ýÎï±êÑù¾ÙÐÐÈý´ÎƽÐвâÊÔ £¬ËùµÃЧ¹ûÈç±í3 ¡£
±í3. ¼ì³öÏÞ¡¢±ê×¼ÎïÖʲⶨֵ¼°Ï¸Ãܶȣ¨n=3£©
|
ÔªËØ
|
ÒªÁì¼ì³öÏÞ(ng/L)
|
GBW07407
(GSS-7)
|
ϸÃܶȣ¨%£©
|
GBW07312
(GSD-12)
|
ϸÃܶȣ¨%£©
|
|
±ê×¼Öµ£¨mg/kg£©
|
²â¶¨Öµ£¨mg/kg£©
|
±ê×¼Öµ£¨mg/kg£©
|
²â¶¨Öµ£¨mg/kg£©
|
|
9Be
|
8.9
|
2.8¡À0.6
|
2.92
|
4.42
|
8.2¡À0.7
|
8.28
|
1.44
|
|
52Cr
|
295.0
|
410¡À23
|
392.89
|
0.26
|
35¡À3
|
34.90
|
0.37
|
|
59Co
|
891.4
|
97¡À6
|
95.04
|
2.60
|
8.8¡À0.7
|
9.00
|
0.79
|
|
60Ni
|
40.3
|
276¡À15
|
287.76
|
0.25
|
12.8¡À1.3
|
12.48
|
0.42
|
|
65Cu
|
40.4
|
97¡À6
|
100.76
|
2.81
|
1230¡À33
|
1231.16
|
0.23
|
|
114Cd
|
7.8
|
0.08¡À0.02
|
0.070
|
8.32
|
4.0¡À0.3
|
4.23
|
0.36
|
|
121Sb
|
21.7
|
0.42¡À0.09
|
0.46
|
5.75
|
24¡À3
|
26.91
|
0.50
|
|
208Pb
|
25.1
|
14¡À3
|
12.31
|
1.87
|
285¡À1
|
275.33
|
0.49
|
|
238U
|
17.8
|
2.2¡À0.4
|
2.18
|
1.65
|
7.8¡À0.7
|
7.73
|
0.56
|
4. ½áÂÛ
½ÓÄÉ΢²¨Ïû½â·¨ £¬ÓÃICP-MS
2000B²â¶¨ÁËÍÁÈÀºÍˮϵ³Á»ýÎïÖÐBe¡¢Cr¡¢Co¡¢Ni¡¢Cu¡¢Cd¡¢Sb¡¢Pb¡¢U 9ÖÖÖؽðÊôÔªËØ £¬ÒªÁì¼ì³öÏÞÔÚ7.8ng/L-891.4ng/LÖ®¼ä £¬²â¶¨ÖµÓëÖ¤Êé±ê×¼ÖµÎÇºÏ £¬ÇÒÖظ´ÐÔÓÅÒì ¡£ÊµÑéЧ¹ûÅú×¢¸ÃÒªÁì¼ì³öÏÞµÍ £¬²âÊÔЧ¹û׼ȷ £¬¿ÉÒÔÖª×ãÍÁÈÀºÍˮϵ³Á»ýÎï¶àÔªËØ׼ȷ¡¢¿ìËÙÆÊÎöµÄÒªÇó ¡£
5.²Î¿¼ÎÄÏ×
[1]
ÁºÊçÐù¡¢ÍõÐÀ¡¢Îâºç¡¢ËﻪÎÄ £¬Î¢²¨Ïû½â/ICP-MS²â¶¨Ë®Ïµ³Á»ýÎïÖÐ9ÖÖÖؽðÊôÔªËØ[J];¹âÆ×ѧÓë¹âÆ×ÆÊÎö£»2012Äê03ÆÚ ¡£
[2] ÇéÐα£»¤²¿ £¬HJ 832-2017 ÍÁÈÀºÍ³Á»ýÎï½ðÊôÔªËØ×ÜÁ¿ £¬Î¢²¨Ïû½â·¨ £¬ÖйúÇéÐγöÊéÉç £¬2017 ¡£
