½üÄêÀ´ £¬Ëæ×ÅÖйú¾¼ÃµÄ¿ìËÙÉú³¤ £¬Ðí¶àµØÇøÇé¿öÖеĿÕÆø¡¢Ë®ºÍÍÁÈÀÊܵ½ÁËÒ»¶¨µÄÎÛȾ £¬¸øÈËÃǵÄÉíÌ彡¿µ´øÀ´ÁËΣº¦ £¬ÓÈÆäÊÇijЩÖؽðÊôÔªËØ £¬ÉãÈë¹ýÁ¿»áÔì³É¸Î¡¢Éö¹¦Ð§ËðÉË £¬ÑÏÖØÕß¿ÉÄܻᵼÖÂÀÏÄê³Õ´ô ¡£Òò´Ë £¬ÖؽðÊôÎÛȾԽÀ´Ô½¶àµØÊܵ½ÎÀÉú²¿·ÖµÄÖØÊÓ ¡£
ËäÈ»¿ÉÒÔÓÃÀ´½øÐмì²âµÄÒÇÆ÷ÖÖÀàÐí¶à £¬¿ÉÊÇÓÉÓÚÈËÌåÖÐÐí¶àÖؽðÊôº¬Á¿½ÏµÍ£¨Àý ÈçWS/T113-1999Ö°Òµ½Ó´¥ïÓ¼°Æ仯ºÏÎïµÄÉúÎïÏÞÖµ £¬ÄòïÓΪ5¦Ìg/g ¼¡ôû £¬ÑªïÓ5¦Ìg/L£© £¬ÎªÊµ¼Ê¼ì²âÊÂÇéÌáÉýÁËÄÑ¶È ¡£Æ¾¾Ý¹ú¼ÒÎÀÉú½¡¿µ±ê×¼GBZ/T 308-2018 £¬ÀûÓõç¸ÐñîºÏµÈÀë×ÓÌåÖÊÆ×ÒÇ£¨ICP-MS£© £¬ÊµÏÖ¸ßЧ¡¢¿ìËٲⶨÈËÌåÄòÒºÖеÄÖؽðÊôÔªËØ ¡£
1. ÒÇÆ÷¼ò½é
ICP-MS 2000EÊÇÃÀʨ¹ó±ö»áÒÇÆ÷×ÔÖ÷Ñз¢µÄµç¸ÐñîºÏµÈÀë×ÓÌåÖÊÆ×ÒÇ£¨Èçͼ1£© £¬½ÓÄÉÅöײ·´Ó¦³Ø¼¼Êõ £¬ÓÐЧµØÏû³ý¶àÔ×ÓÀë×Ó×ÌÈÅ £¬¾ßÓмì³öÏ޵͡¢ÁéÃô¶È¸ß¡¢ÏßÐÔ¶¯Ì¬¹æÄ£¿í¡¢ÖØÏÖÐÔºÍÖظ´ÐԸߵÈÌص㠡£
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£¨ÃÀʨ¹ó±ö»á£© ¡£
3. ±ê×¼ÇúÏß»æÖÆ
3.1 ÅäÖÆ»ìºÍ±ê×¼ÈÜÒºÖмäÒº
»ìÏý±ê×¼ÈÜÒºA£º»®·ÖÒÆÈ¡0.5mL V¡¢Cr¡¢Co¡¢Cd¡¢Tl¡¢Pb£¨10mg/L£©µÄ±ê×¼ÈÜÒºÓÚ50mLµÄÈÝÁ¿Æ¿ÖÐ £¬¼ÓÈë1%ÏõËáÈÜÒº¶¨ÈÝÖÁ¿Ì¶È²¢Ò¡ÔÈ £»
»ìÏý±ê×¼ÈÜÒºB£º»®·ÖÒÆÈ¡2.5mL Y¡¢In¡¢Ho£¨10mg/L£©µÄ±ê×¼ÈÜÒºÓÚ25mLµÄÈÝÁ¿Æ¿ÖÐ £¬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¿ÖÐ £¬Í¬Ê±¼ÓÈë1mL±ê×¼ÈÜÒºB×÷ΪÄڱ꣨¶¨Èݺó×îÖÕŨ¶ÈΪ10¦Ìg/L£© £¬Ð£ÕýÒÇÆ÷ƯÒƺͻùÌåËù´øÀ´µÄÓ°Ïì ¡£
4. Ç°´¦Àí
ÒÆÈ¡ÄòÒº2.4mLÓÚ50mLµÄÈÝÁ¿Æ¿ÖÐ £¬¼ÓÈë0.5 mLÏõËá¼°0.5 mL Y¡¢In¡¢HoµÄ»ìÏý±ê×¼B(1mg/L) £¬Ó󬴿ˮϡÊÍÖÁ¿Ì¶È²¢Ò¡ÔÈÒÔ´ýÆÊÎö £¬Í¬Ê±×öÑùÆ·¿Õ°× ¡£
5. ÒÇÆ÷ÊÂÇé²ÎÊý
½ÓÄÉ10¦Ìg/L Li/Co/In/Ce/Uµ÷гҺÓÅ»¯ÒÇÆ÷²ÎÊý £¬Ê¹ÆäÁéÃô¶È×î¸ß £¬Í¬Ê±Ñõ»¯Îï²úÂʼ°Ë«µçºÉ²úÂʵÍÓÚ3% ¡£ÆäÖÐ51VÊܵ½35Cl16O×ÌÈÅ £¬52CrÊܵ½40Ar12C×ÌÈÅ £¬¹Ê±ê׼ģʽÏÂÎÞ·¨¶Ô·°ºÍ¸õ½øÐÐ׼ȷÕÉÁ¿ ¡£Òò´ËÀûÓÃÁù¼«¸ËÅöײ·´Ó¦³Ø¼¼Êõ¶Ô·°ºÍ¸õÔªËØ»®·Ö½øÐвâÊÔ ¡£51V½ÓÄÉ1%ÑÎËá½éÖʵÄCo£¨10¦Ìg/L£©µÄ±ê×¼Òº½øÐÐÒÇÆ÷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 £¬Á¬Ðø²â¶¨ÑùÆ·¿Õ°×10´Î £¬ÓÃÈý±¶±ê׼ƫ²î³ýÒÔÇúÏßбÂÊËù¶ÔÓ¦µÄŨ¶ÈΪ¼ì³öÏÞ £»ÒÔ10±¶±ê׼ƫ²î³ýÒÔÇúÏßбÂÊËù¶ÔÓ¦µÄŨ¶ÈΪҪÁ춨Á¿ÏÂÏÞ ¡£ÆäÖÐ59Co/111Cd/205Tl/208Pb½ÓÄÉÏ¡ÊͺóµÄÑùÆ·ÈÜÒº¼Ó±ê0.1¦Ìg/L½øÐÐƽÐвⶨ7´Î £¬ÅÌËãÆ侫ÃÜ¶È £¬51V½ÓÄÉÏ¡ÊͺóÑùÆ·ÈÜÒº¼Ó±ê0.050¦Ìg/L½øÐÐƽÐвⶨ7´Î £¬ÅÌËãÆ侫ÃÜ¶È £¬52Cr½ÓÄÉÑùÆ·ÈÜҺŨ¶ÈƽÐвⶨ7´Î £¬ÅÌËãÆ侫ÃÜ¶È £»51V/59Co/111Cd/205Tl/208PbΪ¼Ó±êºó7´Î²âÊÔŨ¶ÈÈ¡Æäƽ¾ù £¬ÅÌËãÆä¼Ó±ê½ÓÄÉÂÊ £¬ÆäÖÐ52Cr½ÓÄɼӱê0.5¦Ìg/Lºó²âÊÔÆäŨ¶È £¬ËãÆä¼Ó±ê½ÓÄÉÂÊ£¨±í1£© ¡£
±í1. ¼ì³öÏÞ¡¢½ÓÄÉÂʼ°¾«ÃܶÈÊý¾Ý
|
ͬλËØ
|
¼ì³öÏÞ
£¨ng/L£©
|
Ï¡ÊͺóÑùƷŨ¶È£¨¦Ìg/L£©
|
ÔҺŨ¶È
£¨¦Ìg/kg£©
|
¼Ó±ê0.1¦Ìg/LºóµÄÕÉÁ¿Öµ£¨¦Ìg/L£©
|
¼Ó±ê½ÓÄÉÂÊ£¨%£©
|
¾«ÃܶÈ
£¨%£©
|
|
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 £¬³ýÁËÒª¿¼ÂÇÑùÆ·»ùÌåÒÖÖÆЧӦÍâ £¬»¹ÒªÑ¡ÔñºÏÊʵÄÄÚ±êÔªËØÒÔУÕý»ùÌåºÍÒÇÆ÷ƯÒÆËù´øÀ´µÄÓ°Ïì ¡£±¾ÊµÑéÊý¾Ý±êÃ÷ £¬¸ÃÒªÁì¼ì³öÏÞÔÚ0.47ng/L~14.30ng/LÖ®¼ä £¬¼Ó±ê½ÓÄÉÂÊÔÚ95.2%~118.8%Ö®¼ä £¬¾«ÃܶÈÔÚ1.93%~7.26%Ö®¼ä ¡£½ÓÄÉICP-MS 2000E £¬¾ßÓмì³öÏÞµÍ £¬¾«ÃÜ¶È¸ß £¬ÆÊÎöËÙ¶È¿ì £¬²Ù×÷¼òµ¥ £¬ÍêÈ«¿ÉÒÔÂú×ã²â¶¨ÄòÒºÖеÄÖؽðÊôÔªËØ ¡£
8. ²Î¿¼ÎÄÏ×
¹ú¼ÒÎÀÉú½¡¿µÎ¯Ô±»á £¬GBZ/T 308-2018ÄòÖжàÖÖ½ðÊôͬʱ²â¶¨ £¬µç¸ÐñîºÏµÈÀë×ÓÖÊÆ×·¨ £¬Öйú±ê×¼³öÊéÉç £¬2018 ¡£
