鐪炬墍鍛ㄧ煡锛岀牱琚獚(r猫n)鐐烘槸涓€绋嚧鐧岀墿锛屽唬娉涘瓨鍦ㄤ簬鑷劧鐣屼腑锛岄暦(zh菐ng)鏈熸帴瑙告渻(hu矛)灏�(du矛)浜洪珨閫犳垚鍗卞銆傜牱鐨勬瘨鎬ц垏鍏跺寲瀛�(xu茅)褰㈡厠(t脿i)鏈夐棞(gu膩n)锛屼笉鍚屽児(ji脿)鎱�(t脿i)銆佷笉鍚屽舰鎱�(t脿i)鐨勭牱鍏舵瘨鎬у樊鐣板緢澶�銆備竴鑸締(l谩i)瑾�(shu艒)锛岀劇(w煤)姗�(j墨)鐮风殑姣掓€ч仩(yu菐n)閬�(yu菐n)澶т簬鏈夋(j墨)鐮枫€�

鏈枃鍙冭€冨湅(gu贸)瀹惰(w猫i)鐢熷拰瑷�(j矛)鍔冪敓鑲插鍝℃渻(hu矛)鐧�(f膩)甯冪殑銆奊B 5009.11-2014 椋熷搧涓劇(w煤)姗�(j墨)鐮风殑娓�(c猫)瀹氥€�锛岄€氶亷(gu貌)HPLC-ICPMS鑱�(li谩n)鐢�锛岄噰鐢℉amilton PRP-X-100锛�250脳4.1mm锛夐櫚闆㈠瓙鑹茶瓬鏌憋紝鐢�15mmol/L纾烽吀浜屾矮閵ㄥ強25mmol/L纾烽吀浜屾矮閵紙pH=8.0锛変綔娣嬫礂娑诧紝鐢ㄦ搴︽礂鑴殑鏂瑰紡娓�(c猫)瀹氫簡娌虫按妯ｅ搧涓殑浜旂ó鐮峰舰鎱�(t脿i)锛屼笖鍔犳(bi膩o)鍥炴敹鐜囪壇濂�锛岀祼(ji茅)鏋滆〃鏄�锛岃┎鏂规硶鑳藉蹇€熸簴(zh菙n)纰哄湴閫�(j矛n)琛屾按璩�(zh矛)妯ｅ搧涓殑鐮峰舰鎱�(t脿i)鐨勫垎鏋�銆�

1.鍎€鍣ㄧ啊(ji菐n)浠�

HPLC-310E鏄ぉ鐟炲剙鍣ㄨ嚜涓荤爺鐧�(f膩)鐨勬柊涓€浠ｆ恫鐩歌壊璀滃剙锛岃┎瑷�(sh猫)鍌欓噰鐢ㄥ井铏曠悊鍣ㄦ櫤鑳芥帶鍒跺線寰�(f霉)寮忛洐鏍撳骞惰伅(li谩n)娉�锛屽叿鏈夊伐浣滆€愬鍊奸珮銆佺┅(w臎n)瀹氬彲闈�銆佹搷浣滄柟渚跨瓑鐗归粸(di菐n)?锛熻摢?sh铆)鐝�(xi脿n)绛夊害娲楄劔鍜屾搴︽礂鑴叐绋柟寮�锛屼笖鍏锋湁杓冮珮鐨勯潏鏁忓害銆佸垎闆㈠害鍜屽彲闈犳€�銆�

ICP-MS 2000E閲囩敤閫�(j矛n)鍙ｅ皠闋婚浕婧愶紝淇濊瓑鍎€鍣ㄥ彲澶氱ó妯″紡绌�(w臎n)瀹氶亱(y霉n)琛�锛屽悓鏅�(sh铆)鍒╃敤鍏堥€�(j矛n)鐨勭瓑闆㈠瓙楂斿睆钄芥妧琛�(sh霉)锛屾サ澶х殑鎻愰珮浜嗗剙鍣ㄧ殑闈堟晱搴�銆傝┎瑷�(sh猫)鍌欏叿鏈夋鍑洪檺浣庛€侀潏鏁忓害楂�銆佸垎鏋愰€熷害蹇€佺董璀�(h霉)鏂逛究銆侀珮鑰愰菇鎬у強楂樻€�?x煤n)r(ji脿)姣旂瓑鐗归粸(di菐n)銆�

HPLC-ICPMS鑱�(li谩n)鐢ㄥ剙閲囩敤涓€閸靛紡鏁�(sh霉)鎿�(j霉)閲囬泦銆佺簿婧�(zh菙n)寮忚瓬鍦栧畾浣嶅強寮�(qi谩ng)澶х殑杌熶欢璀滃湒铏曠悊鍔熻兘锛屽彲婊�(m菐n)瓒充笉鍚岀殑褰㈡厠(t脿i)娓�(c猫)瑭﹂渶姹傦紙濡傚湒1锛�銆�

鍦�1.HPLC-ICPMS鑱�(li谩n)鐢ㄦ脯(c猫)鐮峰舰鎱�(t脿i)鐨勫垎鏋愬剙

2.娓�(c猫)瑭﹀師鐞�

妯ｅ搧婧舵恫缍�(j墨ng)閬�(gu貌)鍓嶈檿鐞�锛岀敱HPLC閫�(j矛n)妯ｅ彛閫�(j矛n)妯�锛岀稉(j墨ng)鑹茶瓬鏌卞垎闆紝閫氶亷(gu貌)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�銆佸師瀛愬寲銆侀浕闆�锛屽厓绱犻洟瀛愮稉(j墨ng)鎺ュ彛瀹ら€�(j矛n)鍏ヨ唱(zh矛)璀滃剙锛岄€氶亷(gu貌)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�(c猫)鍣�锛屾娓�(c猫)鍣ㄥ皪(du矛)鐩告噳(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▓(j矛)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�(qi谩ng)搴﹀拰鏅�(sh铆)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€�(j矛n)琛屽畾鎬у畾閲忓垎鏋愩€�

3.瀵�(sh铆)椹�(y脿n)閮ㄥ垎

3.1瀵�(sh铆)椹�(y脿n)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Hamilton PRP-X100锛�4.1脳250mm锛�10渭m锛�锛�

瓒呯磾姘寸郴绲�(t菕ng)锛圡illipore锛岄浕闃荤巼鐐�18.2M惟路cm锛�锛�

姘ㄦ按锛堝劒(y艒u)绱�(j铆)绱�锛屼笂娴锋櫠绱�?c猫)鍣敮閭㈣柊顐堣崋顮€?

纾烽吀浜屾矮閵紙鍎�(y艒u)绱�(j铆)绱旓紝鍦�(gu贸)钘ラ泦鍦�(tu谩n)鍖栧(xu茅)瑭﹀姂鏈夐檺鍏徃锛�锛�

涔欎簩鑳哄洓涔欓吀浜岄垑锛堝劒(y艒u)绱�(j铆)绱�锛岄樋鎷変竵鍖栧(xu茅)瑭﹀姂锛�

5绋牱褰㈡厠(t脿i)妯�(bi膩o)婧�(zh菙n)婧舵恫锛堜簽鐮烽吀鏍癸紙GBW08666锛�銆佺牱閰告牴锛圙BW08667锛�銆佺牱鑶藉牽锛圙BW08671锛夈€佷竴鐢插熀鐮凤紙GBW08668锛�銆佷簩鐢插熀鐮凤紙GBW08669锛夛紝涓湅(gu贸)瑷�(j矛)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�銆�

3.2妯ｅ搧鍓嶈檿鐞�

娌虫按妯ｅ搧缍�(j墨ng)0.45渭m鐨勬按绯绘烤鑶滅洿鎺ラ亷(gu貌)婵�銆�

3.3娴佸嫊(d貌ng)鐩稿強鐮峰舰鎱�(t脿i)妯�(bi膩o)婧�(zh菙n)婧舵恫閰嶅埗

15mmol/L NH₄H₂PO₄婧舵恫锛氭簴(zh菙n)纰虹ū(ch膿ng)鍙�1.726g纾烽吀浜屾矮閵紝婧朵簬1000 mL瓒呯磾姘翠腑锛岀稉(j墨ng)0.45渭m鐨勬按绯绘烤鑶滈亷(gu貌)婵惧悗锛屼簬瓒呰伈姘存荡涓秴鑱茶劔姘�30min銆�

25mmol/L NH₄H₂PO₄婧舵恫锛氭簴(zh菙n)纰虹ū(ch膿ng)鍙�2.876g纾烽吀浜屾矮閵�锛屾憾浜�1000 mL瓒呯磾姘翠腑锛岀敤姘ㄦ按瑾�(di脿o)绡€(ji茅)PH鑷�8.0锛岀稉(j墨ng)0.45渭m鐨勬按绯绘烤鑶滈亷(gu貌)婵惧悗锛屼簬瓒呰伈姘存荡涓秴鑱茶劔姘�30min銆�

20mmol/L EDTA-2Na婧舵恫锛氭簴(zh菙n)纰虹ū(ch膿ng)鍙�0.745g涔欎簩鑳哄洓涔欓吀浜岄垑锛屽姞鍏ュ皯閲忚秴绱旀按锛屼簬150鈩冪殑闆荤啽鏉夸笂鍔犵啽鑷充箼浜岃兒鍥涗箼閰镐簩閳夊畬鍏ㄦ憾瑙�锛屽喎鍗诲悗瀹氬鑷�100 mL鐨勫閲忕摱涓互寰呭倷鐢ㄣ€�

鐮峰舰鎱�(t脿i)妯�(bi膩o)婧�(zh菙n)婧舵恫锛�

5绋牱妯�(bi膩o)婧�(zh菙n)婧舵恫閲囩敤20mmol/L EDTA-2Na鎸夌収姊害婵冨害鐨勬柟寮忎緷娆¤绋€閲嬬偤0.5渭g/L銆�1.0渭g/L銆�2.0渭g/L銆�5.0渭g/L銆�10.0渭g/L銆�20.0渭g/L 娣峰悎妯�(bi膩o)婧�(zh菙n)婧舵恫锛屽悓鏅�(sh铆)閰嶅埗浜旂ó鐮峰舰鎱�(t脿i)鐨�5渭g/L鐨勫柈妯�(bi膩o)婧舵恫浠ユ渚�(l谩i)鍒ゅ垾姣忕ó鐮峰舰鎱�(t脿i)鍑哄嘲鏅�(sh铆)闁�銆�

3.4瀵�(sh铆)椹�(y脿n)姊濅欢

3.4.1鑹茶瓬姊濅欢

     鑹茶瓬姊濅欢瑭宠(ji脿n)琛�1鍜岃〃2銆�

琛�1. HPLC鍒嗘瀽姊濅欢

琛�2. 姊害娲楄劔姊濅欢

3.4.2璩�(zh矛)璀滄浠�

     ICP-MS鍒嗘瀽姊濅欢瑕�(ji脿n)琛�3銆�

琛�3. ICP-MS鍒嗘瀽姊濅欢

3.5瀵�(sh铆)椹�(y脿n)绲�(ji茅)鏋�

3.5.1鑹茶瓬鍒嗛洟鍦�

鎸夎〃2鐨勬礂鑴浠�锛岄€�(j矛n)妯�20.0渭g/L鐮峰舰鎱�(t脿i)娣峰悎妯�(bi膩o)婧�(zh菙n)婧舵恫锛屽緱鍒颁簲绋牱鍒嗛洟鑹茶瓬鍦�锛屽鍦�2銆侫sC銆丄s³⁺銆丏MA銆丮MA銆丄s⁵⁺鐩稿皪(du矛)淇濈暀鏅�(sh铆)闁撳垎鍒ョ偤120s銆�155s銆�247s銆�329s銆�583s锛岀附鍒嗛洟鏅�(sh铆)闁撶磩鐐�600s銆�

鍦�2. 5绋牱褰㈡厠(t脿i)鐨勬贩鍚堟(bi膩o)婧�(zh菙n)婧舵恫鑹茶瓬鍦�

3.5.2妯�(bi膩o)婧�(zh菙n)鏇茬窔

鎸夌収娣峰悎妯�(bi膩o)婧�(zh菙n)婧舵恫婵冨害0.5渭g/L銆�1.0渭g/L銆�2.0渭g/L銆�5.0渭g/L銆�10.0渭g/L銆�20.0渭g/L閫�(j矛n)妯ｅ緱鍒拌壊璀滃湒锛岃▓(j矛)绠楀叾宄伴潰绌嶏紝浠ユ績搴﹀拰宄伴潰绌嶇躬鍒舵(bi膩o)婧�(zh菙n)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�(ji脿n)鍦�3-1~3-5銆�

鍦�3-3.DMA妯�(bi膩o)婧�(zh菙n)鏇茬窔                               鍦�3-4.MMA妯�(bi膩o)婧�(zh菙n)鏇茬窔

3.5.3 妾㈠嚭闄�

鍦�4鐐�5.0渭g/L娣峰拰妯�(bi膩o)婧�(zh菙n)婧舵恫鑹茶瓬鍦�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�(du矛)鎳�(y墨ng)鐨勬績搴︿綔鐐烘鍑洪檺锛孉sC銆丄s³⁺銆丏MA銆丮MA銆丄s⁵⁺鍒嗗垾鐐�0.078渭g/L銆�0.10渭g/L銆�0.11渭g/L銆�0.13渭g/L銆�0.16渭g/L銆�

鍦�4. 5.0渭g/L浜旂ó鐮峰舰鎱�(t脿i)鐨勬贩鍚堟(bi膩o)婧�(zh菙n)婧舵恫鑹茶瓬鍦�

3.5.4 娓�(c猫)瑭︾祼(ji茅)鏋�

娌虫按妯ｅ搧鍙婂姞妯�(bi膩o)1渭g/L鐨勬脯(c猫)瑭︾祼(ji茅)鏋滆┏瑕�(ji脿n)琛�4锛屾ǎ鍝佸強鍔犳(bi膩o)鍚庣牱褰㈡厠(t脿i)鐤婂姞璀滃湒濡傚湒5鎵€绀�銆�

琛�4   妯ｅ搧涓悇鐮峰舰鎱�(t脿i)鐨勬脯(c猫)瑭︾祼(ji茅)鏋�

鍦�5. 娌虫按妯ｅ強娌虫按妯ｅ姞妯�(bi膩o)1.0渭g/L鑹茶瓬鍦�

4. 绲�(ji茅)璜�

鍒╃敤LC-ICPMS鑱�(li谩n)鐢ㄦ脯(c猫)瑭︽渤姘存ǎ鍝佷腑鐨勪簲绋牱褰㈡厠(t脿i)锛屾脯(c猫)瑭︾祼(ji茅)鏋滆〃鏄�锛岃┎鏂规硶妾㈠嚭闄愪綆銆佺窔鎬х浉闂�(gu膩n)绯绘暩(sh霉)鍧囧湪0.999浠ヤ笂锛屾ǎ鍝佸姞妯�(bi膩o)鍥炴敹鐜囧湪87.8%-112.7%涔嬮枔锛涘悓鏅�(sh铆)浜旂ó鐮峰舰鎱�(t脿i)鑳藉鍦�600s鍏�(n猫i)瀹屾垚鍒嗘瀽锛屼笖鍒嗛洟搴﹁純濂�锛屾鏂规硶鍙豢(m菐n)瓒虫按璩�(zh矛)妯ｅ搧涓牱鐨勫舰鎱�(t脿i)鍒嗘瀽銆�

5.鍙冭€冩枃鐛�(xi脿n)

 [1] 鍦�(gu贸)瀹惰(w猫i)鐢熷拰瑷�(j矛)鍔冪敓鑲插鍝℃渻(hu矛)鐧�(f膩)甯� GB 5009.11-2014椋熷搧瀹夊叏鍦�(gu贸)瀹舵(bi膩o)婧�(zh菙n) 椋熷搧涓劇(w煤)姗�(j墨)鐮风殑娓�(c猫)瀹� 娑茬浉鑹茶瓬-鍘熷瓙鐔掑厜鍏夎瓬娉�锛�2015銆�