΢Á¿ÔªËØ £¬ÊÇÏà¶ÔÖ÷Á¿ÔªËØ»®·ÖµÄ £¬Æ¾¾Ý¼Ä´æ¹¤¾ß²î±ð £¬¿ÉÒÔ·ÖΪ¶àÖÖÀàÐÍ¡£Ä¿Ç° £¬±È½ÏÊܹØ×¢µÄÖ÷ÒªÓÐÁ½Àà £¬Ò»ÖÖÊÇÉúÎïÌåÖеÄ΢Á¿ÔªËØ £¬ÁíÒ»ÖÖÊÇ·ÇÉúÎïÌåÖУ¨ÈçÑÒʯÖУ©µÄ΢Á¿ÔªËØ¡£Õë¶Ô¿óʯ΢Á¿ÔªËصļì²âÒªÁìÖ÷Òª°üÀ¨µç×Ó̽ÕëÆÊÎö·¨¡¢ÖÐ×ӻÆÊÎö·¨¡¢µÈÀë×ÓÌå¹âÆ×·¨¼°ÖÊÆ×·¨¡£Í¨Ì«¹ýÎöÑо¿Î¢Á¿ÔªËØ £¬¿ÉÒԵóö¿ó´²ÖеÄÏ¡ÓÐÔªËØ¿óÎïµÄÂþÑܼÍÂÉ¡£
±¾ÎIJο¼¹ú¼ÒÊг¡¼à¶½ÖÎÀí×ܾ֡¢¹ú¼Ò±ê×¼»¯ÖÎÀíίԱ»áÐû²¼µÄ¡¶GB/T 6730.81-2020Ìú¿óʯ ¶àÖÖ΢Á¿ÔªËغ¬Á¿µÄ²â¶¨ µç¸ÐñîºÏµÈÀë×ÓÌåÖÊÆ×·¨¡· £¬½ÓÄÉ7mLHCL+1mLHF+2.5mLHNO3¶ÔǦ¿óʯ±ê×¼ÎïÖÊ£¨GBW07236£©½øÐÐ΢²¨Ïû½â £¬Ñ¡È¡Ge¡¢Rh¡¢In¡¢Tb¡¢Lu×÷ÄÚ±ê £¬Ð£ÕýÒÇÆ÷ƯÒƼ°ÑùÆ·»ùÌåËù´øÀ´µÄÓ°ÏìºÍ²¨¶¯¡£ÀûÓÃICP-MS 2000E½øÐвⶨ £¬½á¹û±êÃ÷¸ÃÒªÁìÄܹ»¿ìËÙ¡¢×¼È·µØÆÊÎö¿óʯÑùÆ·ÖеĶàÖÖ΢Á¿ÔªËØ¡£
1.ÒÇÆ÷¼ò½é
ICP-MS 2000EÊÇÃÀʨ¹ó±ö»á×ÔÖ÷Ñз¢µÄµç¸ÐñîºÏµÈÀë×ÓÌåÖÊÆ×ÒÇ£¨Èçͼ1£© £¬½ÓÄÉPRCÅöײ·´Ó¦³Ø¼¼Êõ £¬ÓÐЧÏû³ý¶àÔ×ÓÀë×Ó×ÌÈÅ £¬¸Ã¿îÒÇÆ÷¾ßÓÐÁéÃô¶È¸ß¡¢¼ì³öÏ޵͡¢Îȶ¨ÐԺõÈÓŵ㡣
ͼ1. ICP-MS 2000Eµç¸ÐñîºÏµÈÀë×ÓÌåÖÊÆ×ÒÇÍâ¹Ûͼ
2.²âÊÔÔÀí
ÑùÆ·¾Î¢²¨Ïû½â´¦Àí £¬Í¨¹ýÎí»¯Æ÷Îí»¯ºóËÍÈë¸ßεÈÀë×ÓÌåÖÐ £¬¸ÉÔï¡¢Ô×Ó»¯¡¢µçÀë £¬ÔªËØÀë×Ó¾½Ó¿ÚÊÒ½øÈëÖÊÆ×ÒÇ £¬Í¨¹ýÀë×Ó͸¾µÏµÍ³¡¢ÖÊÁ¿ÆÊÎöÆ÷¼°¼ì²âÆ÷ £¬¼ì²âÆ÷¶ÔÏàÓ¦ÔªËØÀë×Ó×ö³öÏìÓ¦£¨Ã¿ÃëÀë×Ó¼ÆÊýcps£¨counts per second£©£© £¬ÀûÓÃÏìӦǿ¶ÈÓë´ý²âÔªËØÀë×ÓŨ¶È³ÉÕý±È¹Øϵ½øÐж¨Á¿ÆÊÎö¡£
3.ʵÑ鲿·Ö
3.1 ʵÑéËùÓÃÉ豸¼°ÊÔ¼Á
ICP-MS 2000E(´øÅöײ·´Ó¦³Ø £¬ÃÀʨ¹ó±ö»á)£»
΢²¨Ïû½âÒÇ(WX-8000 £¬ÉϺ£ÒÙÒ¢)£»
ʵÑéËùÓó¬´¿Ë®(µç×èÂÊ´ï18.25M¦¸¡¤cm,
Ĭ¿ËÃÜÀí²© £¬µÂ¹ú£©£»
ÏõËᣨÖÊÁ¿±ÈΪ65%,G.R £¬ÈøÀÍ £¬Î÷°àÑÀ£©£»
ÑÎËᣨÖÊÁ¿±ÈΪ37%,G.R £¬ÈøÀÍ £¬Î÷°àÑÀ£©£»
Çâ·úËᣨÖÊÁ¿±ÈΪ40% £¬G.R £¬¹úÒ©¼¯ÍÅ£©£»
ÔªËرê×¼ÈÜÒº(10?g/mL £¬Inorganic
Ventures £¬ÃÀ¹ú)£»
ë²Æø£¨´¿¶È99.999% £¬Air Products £¬ÃÀ¹ú£©¡£
3.2 ÑùÆ·Ç°´¦Àí
³ÆÈ¡Á½¸öƽÐÐÊÔÑù£¨GBW07236£©¸÷0.1g£¨¾«È·ÖÁ0.0001g£©ÓÚÊÂÏÈÏ´ºÃµÄ΢²¨Ïû½â¹ÞÖÐ £¬»®·Ö¼ÓÈë7mLHCL+1mLHF+2.5mLHNO3 £¬Ô¤·´Ó¦20·ÖÖÓºó £¬¸ÇÉÏÏû½â¸Ç £¬Í¬Ê±×öÊÔÑù¿Õ°×¡£½«Ô¤´¦ÀíºÃµÄÏû½â¹ÞÖÃÓÚ΢²¨Ïû½âÒÇÖнøÐÐÏû½â£¨±í1£©¡£´ýÏû½âÍê³É¡¢ÀäÈ´ºó £¬·¿ªÏû½â¹Þ £¬²¢Óó¬´¿Ë®³åÏ´¸Ç×ÓÖÁÉÙÁ½´Î £¬ÔÚ¸ÏËáÒÇÉÏ80¡æ½øÐиÏËá´¦Àí £¬´ý»ÆÑÌ𾡠£¬È¡ÏÂÀäÈ´ÖÁÊÒΠ£¬¶¨ÈÝÖÁ100mLËÜÁÏÈÝÁ¿Æ¿ÖУ¨ËùÓÐʵÑéÓÃÆ÷Ãó¾ùÓÃËá½þÅÝÁôËÞ£© £¬³åÏ´Ïû½â¹Þ2~3´Î £¬Í¬Ê±»®·Ö¼ÓÈë50¦Ìg/L Ge¡¢10¦Ìg/L£¨In¡¢Rh¡¢Tb¡¢Lu£©»ìÏýÄÚ±ê £¬ÓÃ2%ÏõËᶨÈÝÖÁ¿Ì¶ÈÒ¡ÔÈ¡£
±í1. ΢²¨Ïû½âÒÇÊÂÇé²ÎÊý
|
°ì·¨
|
ζÈ/¡æ
|
ѹÁ¦/atm
|
¼á³Öʱ¼ä/min
|
|
1
|
120
|
10
|
3
|
|
2
|
150
|
12
|
10
|
|
3
|
180
|
18
|
10
|
|
4
|
200
|
25
|
30
|
3.3 ±ê×¼ÈÜÒºÅäÖÆ
ÅäÖƲî±ðŨ¶ÈÌݶÈCo¡¢Cu¡¢Y¡¢Cd¡¢Sb¡¢La¡¢Ce¡¢Pr¡¢Nd¡¢Sm¡¢Dy¡¢Ho¡¢Tm¡¢Yb¡¢W¶àÔªËØ»ìÏý±ê×¼ÈÜÒº £¬ÓÚһϵÁÐ100mLµÄÈÝÁ¿Æ¿ÖÐ £¬Í¬Ê±»®·Ö¼ÓÈë50¦Ìg/L Ge¡¢10¦Ìg/L£¨In¡¢Rh¡¢Tb¡¢Lu£©»ìÏýÄÚ±ê £¬ÓÃ2%ÏõËᶨÈÝÖÁ¿Ì¶ÈÒ¡ÔÈÒÔ´ý±¸Ó㨱í2£©¡£
±í2. ¸÷ÔªËرê×¼ÈÜҺŨ¶È£¨?g/L£©
|
ÔªËØ
|
±êÒº1
|
±êÒº2
|
±êÒº3
|
±êÒº4
|
±êÒº5
|
±êÒº6
|
|
Co¡¢La¡¢Ce¡¢Ho
|
1.0
|
2.0
|
5.0
|
10.0
|
20.0
|
50.0
|
|
Cu¡¢Y¡¢Cd¡¢Sb¡¢Nd¡¢Dy¡¢Tm¡¢W
|
5.0
|
10.0
|
20.0
|
50.0
|
100
|
200
|
|
Pr¡¢Sm
|
0.50
|
1.0
|
2.0
|
3.0
|
4.0
|
5.0
|
3.4 ÒÇÆ÷²ÎÊýÓÅ»¯
½ÓÄÉ10¦Ìg/L Li¡¢Co¡¢In¡¢Ce
¡¢Uµ÷гҺ¶ÔÒÇÆ÷½øÐÐÓÅ»¯£¨±í3£©¡£
±í3. ÒÇÆ÷ÊÂÇé²ÎÊý
|
ÒÇÆ÷²ÎÊý
|
ÊÂÇéÌõ¼þ
|
ÒÇÆ÷²ÎÊý
|
ÊÂÇéÌõ¼þ
|
|
RFµçÔ´¹¦ÂÊ
|
1300W
|
µÈÀë×ÓÆø
|
13L/min
|
|
¸¨ÖúÆø
|
1.06
L/min
|
ÔØ Æø
|
1.2L/min
|
|
²ÉÑùÉî¶È
|
16
|
ɨÃè·½·¨
|
Ìø ·å
|
3.5 ʵÑéÊý¾Ý
´ýÒÇÆ÷ÈÈ»úÍê³Éºó £¬ÔÚ±ê׼ģʽ϶ÔÊÔÑù½øÐÐƽÐвⶨ6´Î¡£½«6´Î²â¶¨½á¹ûÈ¡Æäƽ¾ù×÷ΪÊÔÑù²â¶¨Öµ £¬Í¬Ê±ÅÌËãÆ侫Ãܶȣ¨±í4£©¡£
±í4. Ǧ¿óʯ±ê×¼ÎïÖÊ£¨GBW07236£©²â¶¨Öµ¼°¾«Ãܶȣ¨n=6£©
|
ÔªËØ
|
ͬλËØ
|
±ê×¼Öµ
mg/kg
|
²â¶¨Öµ
mg/kg
|
¾«ÃÜ¶È £¨%£©
|
|
Co
|
59
|
15.7¡À2.3
|
17.25
|
1.45
|
|
Cu
|
65
|
350¡À20
|
337.61
|
0.48
|
|
Y
|
89
|
16.2¡À2.1
|
15.44
|
2.64
|
|
Cd
|
111
|
2.6¡À0.4
|
2.85
|
1.60
|
|
Sb
|
121
|
12¡À1.3
|
11.88
|
1.09
|
|
La
|
139
|
31.2¡À1.5
|
31.00
|
1.30
|
|
Ce
|
140
|
66.8¡À1.8
|
67.43
|
1.23
|
|
Pr
|
141
|
6.2¡À0.7
|
6.88
|
1.08
|
|
Nd
|
146
|
23.4¡À1.2
|
24.23
|
1.55
|
|
Sm
|
147
|
4.6¡À0.3
|
4.58
|
1.92
|
|
Dy
|
163
|
3.1¡À0.4
|
3.45
|
2.47
|
|
Ho
|
165
|
0.65¡À0.08
|
0.63
|
2.90
|
|
Tm
|
169
|
0.26¡À0.02
|
0.25
|
2.88
|
|
Yb
|
172
|
1.7¡À0.3
|
1.99
|
2.01
|
|
W
|
182
|
30.6¡À2.6
|
31.37
|
0.88
|
4. ½áÂÛ
ÀûÓÃ΢²¨Ïû½â·¨ £¬½ÓÄÉHCL-HF-HNO3ÈýËáÌåϵ¶ÔÑùÆ·½øÐÐÇ°´¦Àí £¬ÒÔGe¡¢Rh¡¢In¡¢Tb¡¢Lu×÷ÄÚ±ê £¬Ð£ÕýÒÇÆ÷ƯÒƺͻùÌåµÄÓ°Ïì £¬Ê¹Óõç¸ÐñîºÏµÈÀë×ÓÌåÖÊÆ×ÒÇICP-MS 2000E²â¶¨Á˹ú¼ÒÒ»¼¶±ê×¼ÎïÖÊǦ¿óʯ£¨GBW07236£©ÖÐ15ÖÖ΢Á¿ÔªËØ £¬Æä²â¶¨ÖµÓë±ê×¼ÖµÍêÈ«ÎÇºÏ £¬¾«ÃܶÈÔÚ0.46%~2.90%Ö®¼ä¡£×ÛÉÏËùÊö £¬¸ÃÒªÁì¿ÉÒÔÂú×ã¿óʯÑùÆ·µÄ΢Á¿ÔªËؼì²â £¬°üÀ¨Ï¡ÍÁÔªËØ¡£
5.²Î¿¼ÎÄÏ×
[1]
¹ú¼ÒÊг¡¼à¶½ÖÎÀí×ܾÖ/¹ú¼Ò±ê×¼»¯ÖÎÀíίԱ»á GB/T
6730.81-2020Ìú¿óʯ ¶àÖÖ΢Á¿ÔªËغ¬Á¿µÄ²â¶¨ £¬µç¸ÐñîºÏµÈÀë×ÓÖÊÆ×·¨ £¬È«¹úÌú¿óʯÓ뻹ÔÌú±ê×¼»¯¼¼ÊõίԱ»á £¬2020¡£
