½üÄêÀ´£¬Ëæ×ÅÖйú¾¼ÃµÄ¿ìËÙÉú³¤£¬Ðí¶àµØÇøÇéÐÎÖеĿÕÆø¡¢Ë®ºÍÍÁÈÀÊܵ½ÁËÒ»¶¨µÄÎÛȾ£¬¸øÈËÃǵÄÉíÌ念½¡´øÀ´ÁËΣº¦£¬ÓÈÆäÊÇijЩÖؽðÊôÔªËØ£¬ÉãÈë¹ýÁ¿»áÔì³É¸Î¡¢Éö¹¦Ð§ËðÉË£¬ÑÏÖØÕß¿ÉÄܻᵼÖÂÍíÄê³Õ´ô¡£Òò´Ë£¬ÖؽðÊôÎÛȾԽÀ´Ô½¶àµØÊܵ½ÎÀÉú²¿·ÖµÄÖØÊÓ¡£
ËäÈ»¿ÉÒÔÓÃÀ´¾ÙÐмì²âµÄÒÇÆ÷ÖÖÀàÐí¶à£¬¿ÉÊÇÓÉÓÚÈËÌåÖÐÐí¶àÖؽðÊôº¬Á¿½ÏµÍ£¨Àý ÈçWS/T113-1999Ö°Òµ½Ó´¥ïÓ¼°Æ仯ºÏÎïµÄÉúÎïÏÞÖµ£¬ÄòïÓΪ5¦Ìg/g ¼¡ôû£¬ÑªïÓ5¦Ìg/L£©£¬ÎªÏÖʵ¼ì²âÊÂÇéÌáÉýÁËÄѶȡ£Æ¾Ö¤¹ú¼ÒÎÀÉú¿µ½¡±ê×¼GBZ/T 308-2018£¬Ê¹Óõç¸ÐñîºÏµÈÀë×ÓÌåÖÊÆ×ÒÇ£¨ICP-MS£©£¬ÊµÏÖ¸ßЧ¡¢¿ìËٲⶨÈËÌåÄòÒºÖеÄÖؽðÊôÔªËØ¡£
1. ÒÇÆ÷¼ò½é
ICP-MS 2000EÊÇ9001cc½ðɳÒÔ³ÏΪ±¾ÒÇÆ÷×ÔÖ÷Ñз¢µÄµç¸ÐñîºÏµÈÀë×ÓÌåÖÊÆ×ÒÇ£¨Èçͼ1£©£¬½ÓÄÉÅöײ·´Ó¦³ØÊÖÒÕ£¬ÓÐÓõØÏû³ý¶àÔ×ÓÀë×Ó×ÌÈÅ£¬¾ßÓмì³öÏ޵͡¢Ñ¸Ëٶȸߡ¢ÏßÐÔ¶¯Ì¬¹æÄ£¿í¡¢ÖØÏÖÐÔºÍÖظ´ÐԸߵÈÌص㡣
ͼ1.ICP-MS
2000Eµç¸ÐñîºÏµÈÀë×ÓÌåÖÊÆ×ÒÇÍâ¹Ûͼ
2. ÊÔ¼ÁÒÇÆ÷
HNO3£¨A.R.£¬ÈøÀÍ£©£»
³¬´¿Ë®£¨18.25M¦¸?cm£¬ÃÜÀí²©£©£»
ÔªËرê×¼ÈÜÒº£¨10mg/L£¬Inorganic Ventures£©£»
ICP-MS2000E£¨9001cc½ðɳÒÔ³ÏΪ±¾£©¡£
3. ±ê×¼ÇúÏß»æÖÆ
3.1 ÅäÖÆ»ìºÍ±ê×¼ÈÜÒºÖÐÐÄÒº
»ìÏý±ê×¼ÈÜÒºA£º»®·ÖÒÆÈ¡0.5mL V¡¢Cr¡¢Co¡¢Cd¡¢Tl¡¢Pb£¨10mg/L£©µÄ±ê×¼ÈÜÒºÓÚ50mLµÄÈÝÁ¿Æ¿ÖУ¬¼ÓÈë1%ÏõËáÈÜÒº¶¨ÈÝÖÁ¿Ì¶È²¢Ò¡ÔÈ£»
»ìÏý±ê×¼ÈÜÒºB£º»®·ÖÒÆÈ¡2.5mL Y¡¢In¡¢Ho£¨10mg/L£©µÄ±ê×¼ÈÜÒºÓÚ25mLµÄÈÝÁ¿Æ¿ÖУ¬¼ÓÈë1%ÏõËáÈÜÒº¶¨ÈÝÖÁ¿Ì¶È²¢Ò¡ÔÈ¡£
3.2 ±ê×¼ÇúÏß»æÖÆ
½«ÅäÖƺõıê×¼»ìÏýÈÜÒºA»®·ÖÒÆÈ¡0¡¢0.05¡¢0.1¡¢0.5¡¢0.8ºÍ1mLÓÚһϵÁÐ100mLµÄÈÝÁ¿Æ¿ÖУ¬Í¬Ê±¼ÓÈë1mL±ê×¼ÈÜÒºB×÷ΪÄڱ꣨¶¨Èݺó×îÖÕŨ¶ÈΪ10¦Ìg/L£©£¬Ð£ÕýÒÇÆ÷ƯÒƺͻùÌåËù´øÀ´µÄÓ°Ïì¡£
4. Ç°´¦Öóͷ£
ÒÆÈ¡ÄòÒº2.4mLÓÚ50mLµÄÈÝÁ¿Æ¿ÖУ¬¼ÓÈë0.5 mLÏõËá¼°0.5 mL Y¡¢In¡¢HoµÄ»ìÏý±ê×¼B(1mg/L)£¬Ó󬴿ˮϡÊÍÖÁ¿Ì¶È²¢Ò¡ÔÈÒÔ´ýÆÊÎö£¬Í¬Ê±×öÑùÆ·¿Õȱ¡£
5. ÒÇÆ÷ÊÂÇé²ÎÊý
½ÓÄÉ10¦Ìg/L Li/Co/In/Ce/Uµ÷гҺÓÅ»¯ÒÇÆ÷²ÎÊý£¬Ê¹ÆäѸËÙ¶È×î¸ß£¬Í¬Ê±Ñõ»¯Îï²úÂʼ°Ë«µçºÉ²úÂʵÍÓÚ3%¡£ÆäÖÐ51VÊܵ½35Cl16O×ÌÈÅ£¬52CrÊܵ½40Ar12C×ÌÈÅ£¬¹Ê±ê׼ģʽÏÂÎÞ·¨¶Ô·°ºÍ¸õ¾ÙÐÐ׼ȷÕÉÁ¿¡£Òò´ËʹÓÃÁù¼«¸ËÅöײ·´Ó¦³ØÊÖÒÕ¶Ô·°ºÍ¸õÔªËØ»®·Ö¾ÙÐвâÊÔ¡£51V½ÓÄÉ1%ÑÎËá½éÖʵÄCo£¨10¦Ìg/L£©µÄ±ê×¼Òº¾ÙÐÐÒÇÆ÷²ÎÊýÓÅ»¯£¬Ê¹59Co/51VµÄ±ÈÖµ´óÓÚ18¡£ËùµÃÒÇÆ÷²ÎÊýΪ£ºRFµçÔ´¹¦ÂÊ1300w£¬µÈÀë×ÓÌåÆø13L/min£¬¸¨ÖúÆø1.06L/min£¬ÔØÆø1.2L/min£¬He/NH3Á÷Á¿Îª4.2 mL/min(NH3Õ¼1% V/V£©£»52Cr½ÓÄÉ10¦Ìg/L Li/Co/In/Ce/Uµ÷гҺÓÅ»¯59CoµÄÇ¿¶È£¬Ê¹ÆäÐźŵִï×î´ó£¬Í¬Ê±Ñõ»¯Îï¿ØÖÆÔÚ1.5%ÒÔÄÚ¡£ËùµÃÒÇÆ÷²ÎÊýΪ£ºRFµçÔ´¹¦ÂÊ1300w£¬µÈÀë×ÓÌåÆø13L/min£¬¸¨ÖúÆø1.06L/min£¬ÔØÆø1.2L/min£¬He/ H2Á÷Á¿Îª2 mL/min(H2Õ¼7% V/V£©¡£
6. ʵÑéÊý¾Ý
ÔÚÓÅ»¯ÒÇÆ÷µÄ²ÎÊýÌõ¼þÏ£¬Ò»Á¬²â¶¨ÑùÆ·¿Õȱ10´Î£¬ÓÃÈý±¶±ê×¼Îó²î³ýÒÔÇúÏßбÂÊËù¶ÔÓ¦µÄŨ¶ÈΪ¼ì³öÏÞ£»ÒÔ10±¶±ê×¼Îó²î³ýÒÔÇúÏßбÂÊËù¶ÔÓ¦µÄŨ¶ÈΪҪÁ춨Á¿ÏÂÏÞ¡£ÆäÖÐ59Co/111Cd/205Tl/208Pb½ÓÄÉÏ¡ÊͺóµÄÑùÆ·ÈÜÒº¼Ó±ê0.1¦Ìg/L¾ÙÐÐƽÐвⶨ7´Î£¬ÅÌËãÆäϸÃܶȣ¬51V½ÓÄÉÏ¡ÊͺóÑùÆ·ÈÜÒº¼Ó±ê0.050¦Ìg/L¾ÙÐÐƽÐвⶨ7´Î£¬ÅÌËãÆäϸÃܶȣ¬52Cr½ÓÄÉÑùÆ·ÈÜҺŨ¶ÈƽÐвⶨ7´Î£¬ÅÌËãÆäϸÃܶȣ»51V/59Co/111Cd/205Tl/208PbΪ¼Ó±êºó7´Î²âÊÔŨ¶ÈÈ¡Æäƽ¾ù£¬ÅÌËãÆä¼Ó±ê½ÓÄÉÂÊ£¬ÆäÖÐ52Cr½ÓÄɼӱê0.5¦Ìg/Lºó²âÊÔÆäŨ¶È£¬ËãÆä¼Ó±ê½ÓÄÉÂÊ£¨±í1£©¡£
±í1. ¼ì³öÏÞ¡¢½ÓÄÉÂʼ°Ï¸ÃܶÈÊý¾Ý
|
ͬλËØ
|
¼ì³öÏÞ
£¨ng/L£©
|
Ï¡ÊͺóÑùƷŨ¶È£¨¦Ìg/L£©
|
ÔҺŨ¶È
£¨¦Ìg/kg£©
|
¼Ó±ê0.1¦Ìg/LºóµÄÕÉÁ¿Öµ£¨¦Ìg/L£©
|
¼Ó±ê½ÓÄÉÂÊ£¨%£©
|
ϸÃܶÈ
£¨%£©
|
|
51V
|
2.83
|
0.0088
|
0.18
|
0.058
|
98.4
|
2.98
|
|
52Cr
|
14.30
|
0.13
|
2.71
|
0.72
|
118.8
|
7.26
|
|
59Co
|
1.79
|
0.14
|
3.03
|
0.24
|
95.2
|
1.93
|
|
111Cd
|
3.17
|
0.049
|
1.02
|
0.15
|
101.0
|
2.35
|
|
205Tl*
|
0.58
|
£¼0.019
|
£¼0.40
|
0.11
|
110.0
|
2.26
|
|
208Pb
|
0.47
|
0.0092
|
0.19
|
0.12
|
110.8
|
3.74
|
×¢£ºÓÉÓÚÑùÆ·ÖÐ205TlµÄº¬Á¿µÍÓÚ¼ì³öÏÞ£¬¹ÊÓö¨Á¿ÏÞÌåÏÖ¡£
7. ½áÂÛ
Óɱí1¿ÉÖª£¬µç¸ÐñîºÏµÈÀë×ÓÌåÖÊÆ×ÒÇICP-MS 2000E²â¶¨ÄòÒºÖÐ6ÖÖÖؽðÊô£¬³ýÁËҪ˼Á¿ÑùÆ·»ùÌåÒÖÖÆЧӦÍ⣬»¹ÒªÑ¡ÔñºÏÊʵÄÄÚ±êÔªËØÒÔУÕý»ùÌåºÍÒÇÆ÷ƯÒÆËù´øÀ´µÄÓ°Ïì¡£±¾ÊµÑéÊý¾ÝÅú×¢£¬¸ÃÒªÁì¼ì³öÏÞÔÚ0.47ng/L~14.30ng/LÖ®¼ä£¬¼Ó±ê½ÓÄÉÂÊÔÚ95.2%~118.8%Ö®¼ä£¬Ï¸ÃܶÈÔÚ1.93%~7.26%Ö®¼ä¡£½ÓÄÉICP-MS 2000E£¬¾ßÓмì³öÏ޵ͣ¬Ï¸Ãܶȸߣ¬ÆÊÎöËÙÂʿ죬²Ù×÷¼òÆÓ£¬ÍêÈ«¿ÉÒÔÖª×ã²â¶¨ÄòÒºÖеÄÖؽðÊôÔªËØ¡£
8. ²Î¿¼ÎÄÏ×
¹ú¼ÒÎÀÉú¿µ½¡Î¯Ô±»á£¬GBZ/T 308-2018ÄòÖжàÖÖ½ðÊôͬʱ²â¶¨£¬µç¸ÐñîºÏµÈÀë×ÓÖÊÆ×·¨£¬Öйú±ê×¼³öÊéÉ磬2018¡£
