闅ㄨ憲宸ユキ(y猫)鐨勭櫦(f膩)灞曪紝姹炴薄鏌撹秺渚嗚秺鍤撮噸銆傜敱浜庢睘鐨勬薄鏌撶壒鎬�锛屼笉鏄撳垎瑙e強杞�(zhu菐n)绉�銆傞€犳垚浜嗛鍝佷腑瀵岄泦浜嗗悇绋惈姹炲寲鍚堢墿锛屽緸鑰屽皫(d菐o)鑷村悇绋參鎬�銆佹€ユ€ф睘涓瘨浜嬩欢闋诲嚭銆傜洰鍓�锛岄鍝佷腑姹炵殑涓昏瀛樺湪褰㈠紡鍙垎鐐虹劇姗熸睘鍜屾湁姗熸睘鍏╁ぇ椤烇紝鍏朵腑鏈夋姹炵殑姣掓€ч仩澶т簬鐒℃姹�锛岀劇姗熸睘涓昏鏄皪鑵庤嚐鏈夋瘨鎬т綔鐢紝鑰屾湁姗熸睘涓昏灏嶈叇绲勭箶鍌峰姣旇純澶�銆傚洜姝ゅ皪姹炲舰鎱�(t脿i)鐨勭洠(ji膩n)娓’寰楀挨鐐洪噸瑕併€�
鏈枃鍙冭€冨湅瀹惰(w猫i)鐢熷拰瑷堝妰鐢熻偛濮斿摗鏈冪櫦(f膩)甯冪殑銆奊B 5009.17-2014 椋熷搧涓敳鍩烘睘鐨勬脯瀹氥€�锛岄€氶亷HPLC-ICPMS鑱�(li谩n)鐢紝閲囩敤C18鏌�锛屽埄鐢ㄧ瓑搴︽礂鑴殑鏂瑰紡灏嶇█閰告蹈鎻愬悗鐨勫ぇ绫抽€茶浜嗗垎鏋�锛屽悓鏅傚皪妯e搧閲囧彇浜嗗姞妯欒檿鐞�锛屼笖鍔犳鍥炴敹鐜囪壇濂�銆傛脯瑭︾祼(ji茅)鏋滆〃鏄�锛岃┎鏂规硶鑳藉蹇€熸簴纰哄湴閫茶澶х背妯e搧涓睘褰㈡厠(t脿i)鐨勫垎鏋�銆�
1.鍎€鍣ㄧ啊浠�
鏈柟娉曢噰鐢⊿kyray Instrument LC-310E鑸嘔CP-MS 2000E鑱�(li谩n)鐢紝閲囩敤涓€閸靛紡鏁�(sh霉)鎿�(j霉)閲囬泦銆佺簿婧栧紡璀滃湒瀹氫綅鍙婂挤澶х殑杌熶欢璀滃湒铏曠悊鍔熻兘锛屽彲婊胯冻涓嶅悓鐨勫舰鎱�(t脿i)娓│闇€姹傦紙濡傚湒1锛�銆�
鍦�1.HPLC-ICPMS鑱�(li谩n)鐢ㄦ脯姹炲舰鎱�(t脿i)鐨勫垎鏋愬剙
2.娓│鍘熺悊
妯e搧婧舵恫缍�(j墨ng)閬庡墠铏曠悊锛岀敱HPLC閫叉ǎ鍙i€叉ǎ锛岀稉(j墨ng)鑹茶瓬鏌卞垎闆�锛岄€氶亷闇у寲鍣ㄩ湩鍖栧悗閫佸叆楂樻韩绛夐洟瀛愰珨涓�锛屽共鐕ャ€佸師瀛愬寲銆侀浕闆紝鍏冪礌闆㈠瓙缍�(j墨ng)鎺ュ彛瀹ら€插叆璩�(zh矛)璀滃剙锛岄€氶亷闆㈠瓙閫忛彙绯荤当(t菕ng)銆佽唱(zh矛)閲忓垎鏋愬櫒鍙婃娓櫒锛屾娓櫒灏嶇浉鎳�(y墨ng)鍏冪礌闆㈠瓙鍋氬嚭闊挎噳(y墨ng)锛堟瘡绉掗洟瀛愯▓鏁�(sh霉)cps锛坈ounts
per second锛�锛岀稉(j墨ng)杌熶欢铏曠悊锛岄熆鎳�(y墨ng)寮峰害鍜屾檪闁撶祫鎴愮殑宄伴潰绌嶈垏鐩告噳(y墨ng)绲勫垎闆㈠瓙婵冨害鎴愭姣旈棞(gu膩n)绯婚€茶瀹氭€у畾閲忓垎鏋�銆�
3.瀵﹂閮ㄥ垎
3.1瀵﹂瑷�(sh猫)鍌欏強瑭﹀姂
娑茬浉鑹茶瓬-闆绘劅鑰﹀悎绛夐洟瀛愰珨璩�(zh矛)璀滆伅(li谩n)鐢ㄥ剙锛堟睙铇囧ぉ鐟炲剙鍣ㄨ偂浠芥湁闄愬叕鍙革級锛�
闆诲瓙澶╁钩锛圔SA224S锛岃辰澶氬埄鏂級锛�
鑹茶瓬鏌憋紙Ultimate XB-C18锛�4.6脳150mm锛�5渭m锛�锛�
瓒呯磾姘寸郴绲�(t菕ng)锛圡illipore锛岄浕闃荤巼鐐�18.25M惟路cm锛�锛�
楣介吀锛堝劒(y艒u)绱氱磾锛孲charlau锛�锛�
姘ㄦ按锛堝劒(y艒u)绱氱磾锛屼笂娴锋櫠绱旇│鍔戞湁闄愬叕鍙革級锛�
涔欓吀閵紙鍎�(y艒u)绱氱磾锛岄樋鎷変竵鍖栧(xu茅)瑭﹀姂锛�锛�
L锛嶅崐鑳辨皑閰革紙鐢熺墿绱旓紝闃挎媺涓佸寲瀛�(xu茅)瑭﹀姂锛�锛�
鐢查唶锛堣壊璀滅磾锛孫ceanpak 鑹茶瓬绱旇│鍔戯級锛�
姹炲舰鎱�(t脿i)妯欐簴婧舵恫锛堟按涓睘GBW锛圗锛�083186銆佺敳鍩烘睘GBW锛圗锛�083364銆佷箼鍩烘睘GBW锛圗锛�081524锛屼腑鍦嬭▓閲忕瀛�(xu茅)闄級锛�
瓒呰伈娉紙KH-500E,鏄嗗北绂惧壍(chu脿ng)锛�锛�
闆欏姛鑳芥按娴存亽婧尟钑╁櫒锛圫HA-B,姹熻槆鍦嬭彲锛�锛�
楂橀€熼洟蹇冩锛圱G16G,鍑辩壒锛�銆�
3.2妯e搧鍓嶈檿鐞�
绋卞彇澶х背妯e搧1.0g锛堢簿纰鸿嚦0.001g锛�锛岀疆浜�15mL鐨勯洟蹇冪涓�锛屽姞鍏�10mL鐨勯菇閰告憾娑诧紙5mol/L锛夐潨缃亷澶�銆傚悗缍�(j墨ng)甯告韩姘存荡鎸暕60min锛屼簬4鈩冧笅浠�8000r/min鐨勮綁(zhu菐n)閫熼€茶闆㈠績15min銆傚彇涓婂堡娓呮恫2mL鑷�5mL鐨勫閲忕摱涓�锛岀敤绋€姘ㄦ按瑾�(di脿o)绡€(ji茅)PH鍒�7.0锛屽啀鍔犲叆0.1mL鐨凩锛嶅崐鑳辨皑閰革紙10g/L锛�锛屾渶鍚庣敤瓒呯磾姘村畾瀹硅嚦鍒诲害骞舵悥鍕�銆傜敤0.45渭m鐨勬湁姗熺郴婵捐啘閬庢烤鍚�锛屽緟娓€�
3.3娴佸嫊鐩稿強姹炲舰鎱�(t脿i)妯欐簴婧舵恫閰嶅埗
3.3.1娴佸嫊鐩哥殑閰嶅埗
60mmol/L涔欓吀閵紜0.1%L-鍗婅儽姘ㄩ吀锛�5%鐢查唶锛氱ū鍙�4.627g涔欓吀閵�锛�1.21gL-鍗婅儽姘ㄩ吀浜�100mL瀹归噺鐡朵腑锛屽姞鍏ュ皯閲忕殑瓒呯磾姘村苟浜庨浕鐔辨澘涓婂姞鐔变娇鍏跺畬鍏ㄦ憾瑙�锛屽喎鍗诲悗瀹氬鑷�100mL銆傚皣瀹氬濂界殑婧舵恫绉诲叆1000mL鐨勬穻娲楁恫鐡朵腑锛屽悓鏅傚姞鍏�50mL鐨勭敳閱囷紝瀹氬鑷�1L銆傜稉(j墨ng)0.45渭m鐨勬湁姗熺郴婵捐啘閬庢烤鍚庯紝浜庤秴鑱叉尝瓒呰伈鑴埃30min锛岀従(xi脿n)鐢ㄧ従(xi脿n)閰�銆�
3.3.2姹炲舰鎱�(t脿i)妯欐簴婧舵恫锛�
涓夌ó姹炴婧栨憾娑查噰鐢ㄦ穻娲楁恫鎸夌収姊害婵冨害鐨勬柟寮忎緷娆¤绋€閲嬬偤1.0渭g/L銆�2.0.渭g/L銆�4.0渭g/L銆�8.0渭g/L銆�10.0渭g/L 娣峰悎妯欐簴婧舵恫锛屽悓鏅傞厤鍒�5渭g/L涓夌ó姹炲舰鎱�(t脿i)鐨勫柈妯欐憾娑�锛岀敤渚嗗垽鍒ユ瘡绋睘褰㈡厠(t脿i)鐨勫嚭宄版檪闁�銆�
3.4瀵﹂姊濅欢
3.4.1鑹茶瓬姊濅欢
鑹茶瓬姊濅欢瑭宠琛�1銆�
琛�1. HPLC鍒嗘瀽姊濅欢
鍙冩暩(sh霉)
|
鍙冩暩(sh霉)瑷�(sh猫)瀹�
|
鑹茶瓬鏌�
|
Ultimate XB锛�C18锛�5渭m锛�150脳4.6mm銆�
|
娴佸嫊鐩�
|
60mmol/L涔欓吀閵�锛�0.1%L-鍗婅儽姘ㄩ吀锛�5%鐢查唶锛�pH=7.0锛�銆�
|
娴� 閫�
|
1.0mL/min
|
鏌� 婧�
|
25鈩�
|
閫叉ǎ閲�
|
100渭L
|
娲楄劔绋嬪簭
|
绛夊害娲楄劔
|
3.4.2璩�(zh矛)璀滄浠�
ICP-MS鍒嗘瀽姊濅欢瑕嬭〃2銆�
琛�2.ICP-MS鍒嗘瀽姊濅欢
鍙冩暩(sh霉)
|
鍙冩暩(sh霉)瑷�(sh猫)瀹�
|
鍙冩暩(sh霉)
|
鍙冩暩(sh霉)瑷�(sh猫)瀹�
|
鍔� 鐜�
|
1300W
|
绛夐洟瀛愭埃
|
13L/min
|
杓斿姪姘�
|
1.06L/min
|
杓� 姘�
|
1.2L/min
|
閲囨ǎ娣卞害
|
16
|
鍒嗘瀽妯″紡
|
妯欐簴妯″紡
|
寰呮脯璩�(zh矛)閲忔暩(sh霉)
|
202
|
椐愮暀鏅傞枔
|
10ms
|
3.5瀵﹂绲�(ji茅)鏋�
3.5.1妯欐簴鏇茬窔
鎸夌収娣峰悎妯欐簴婧舵恫婵冨害1.0渭g/L銆�2.0.渭g/L銆�4.0渭g/L銆�8.0渭g/L銆�10.0渭g/L 閫叉ǎ寰楀埌鑹茶瓬鍦栵紝瑷堢畻鍏跺嘲闈㈢⿳锛屼互婵冨害鍜屽嘲闈㈢⿳绻埗妯欐簴鏇茬窔锛岀窔鎬х浉闂�(gu膩n)绯绘暩(sh霉)鍧囧ぇ浜�0.999锛岀祼(ji茅)鏋滆┏瑕嬪湒2-1~2-3銆�
鍦�2-1.Hg2+妯欐簴鏇茬窔
鍦�2-2.MetHg妯欐簴
鍦�2-3.EtHg妯欐簴鏇茬窔
3.5.2鑹茶瓬鍒嗛洟鍦�
1.0渭g/L銆�2.0.渭g/L銆�4.0渭g/L銆�8.0渭g/L銆�10.0渭g/L 姹炲舰鎱�(t脿i)娣峰悎妯欐簴婧舵恫鍒嗛洟鑹插湒璀滃鍦�3鎵€绀�锛屽叾涓劇姗熸睘锛圚g2+锛�銆佺敳鍩烘睘锛圡etHg锛�銆佷箼鍩烘睘锛圗tHg)鐩稿皪淇濈暀鏅傞枔鍒嗗垾鐐�118s銆�185s銆�379s锛屽緸璀滃湒鐤婂姞鍦栦笂鍙互鐪嬪嚭锛屼笁绋睘褰㈡厠(t脿i)鍑哄嘲鏅傞枔绌�(w臎n)瀹氾紝涓斿垎闆㈠害杓冨ソ銆�
鍦�3. 姹炲舰鎱�(t脿i)娣峰悎妯欐簴婧舵恫鍒嗛洟鍦栬瓬
3.5.3 妾㈠嚭闄�
濡傚湒4鎵€绀虹偤1.0渭g/L姹炲舰鎱�(t脿i)娣峰拰妯欐簴婧舵恫鍒嗛洟鍦栬瓬锛屼互鍚勫舰鎱�(t脿i)宄伴檮杩戝熀绶氳檿鐨�3鍊嶄俊鍣瘮锛圫/N)宄伴珮灏嶆噳(y墨ng)鐨勬績搴︿綔鐐烘鍑洪檺锛屾憾娑蹭腑Hg2+銆丮etHg銆丒tHg鍒嗗垾鐐�0.112渭g/L銆�0.0718渭g/L銆�0.0698渭g/L銆�
鍦�4. 1.0渭g/L姹炲舰鎱�(t脿i)娣峰悎妯欐簴婧舵恫鍦栬瓬
3.5.4 娓│绲�(ji茅)鏋�
浠ュぇ绫虫ǎ鍝佺偤瑭︽ǎ锛岄€茶绋€閰告蹈鎻�锛屽悓鏅傜偤浜嗚€冨療鏂规硶鐨勬簴纰烘€э紝骞跺皪澶х背瑭︽ǎ閲囧彇浜嗗姞妯欑殑鏂瑰紡锛屾脯瑭︾祼(ji茅)鏋滆┏瑕嬭〃3銆�
琛�3 澶х背妯e搧鍙婃ǎ鍝佸姞妯欑祼(ji茅)鏋�
绲勫垎鍚嶇ū
|
绋€閲嬪悗婵冨害
|
鍘熸恫婵冨害
|
鍔犳鍚庢績搴�
|
鍔犳鍥炴敹鐜�
|
锛�渭g/L锛�
|
锛�渭g/kg锛�
|
锛�渭g/L锛�
|
锛�%锛�
|
鐒℃姹�
|
0.227
|
5.68
|
5.84
|
112
|
鐢插熀姹�
|
鏈鍑�
|
ND
|
4.50
|
90
|
涔欏熀姹�
|
鏈鍑�
|
ND
|
4.67
|
93
|
鍦�5. 澶х背妯e搧鍙婃ǎ鍝佸姞妯�5.0渭g/L鍦栬瓬
4. 绲�(ji茅)璜�
鏈枃寤虹珛浜哃C-ICPMS娓│澶х背涓睘褰㈡厠(t脿i)鐨勫垎鏋愭柟娉�锛岀祼(ji茅)鏋滆〃鏄庤┎鏂规硶妾㈠嚭闄愪綆銆佹脯瑭︾祼(ji茅)鏋滄簴纰�锛屽叾鍔犳鍥炴敹鐜囧湪90%~112%涔嬮枔锛岀窔鎬х浉闂�(gu膩n)绯绘暩(sh霉)鍧囧湪0.999浠ヤ笂锛涘悓鏅傛睘鐨勪笁绋舰鎱�(t脿i)鑳藉鍦�8min宸﹀彸瀹屾垚锛屼笖鍒嗛洟搴﹁純濂�锛岃┎鏂规硶鍙豢瓒抽鍝佷腑澶х背妯e搧姹炲舰鎱�(t脿i)鍒嗘瀽鐨勮姹�銆�
5.鍙冭€冩枃鐛�
[1] 鍦嬪琛�(w猫i)鐢熷拰瑷堝妰鐢熻偛濮斿摗鏈冪櫦(f膩)甯� GB 5009.17-2014椋熷搧瀹夊叏鍦嬪妯欐簴 椋熷搧涓敳鍩烘睘鐨勬脯瀹� 娑茬浉鑹茶瓬-鍘熷瓙鐔掑厜鍏夎瓬鑱�(li谩n)鐢ㄦ柟娉曪紝2015銆�