瀹為獙瀹ゅ杈婄牬紕庢満嫻嬪畾鐓よ川鍚搥鏂規(guī)硶鍜屾墍鐢ㄧ殑瀹為獙瀹よ澶?/span>

1涓婚鍐呭涓庨€傜敤鑼冨洿

鏈爣鍑嗚瀹氫簡鐓や腑閾€嫻嬪畾鐢ㄧ殑璇曞墏銆佹潗鏂欍€佷華鍣ㄣ€佽澶囥€佺叅鏍楓€佹祴瀹氭楠ゃ€佺粨鏋滆〃榪板拰鍏佽宸€傛湰鏍囧噯閫傜敤浜庤鐓ゃ€佺儫鐓ゅ拰鏃犵儫鐓ゃ€?/span>

2鏂規(guī)硶鎻愯鐓ゆ牱鐏板寲錛岀劧鍚庣敤娣峰悎閾電洂鐔旇瀺銆佸啀鐢ㄥ惈紜濋吀鐩愮殑紼€紜濋吀嫻稿彇銆傛蹈鍙栨恫閫氳繃紓烽吀涓変竵閰壊灞傛煴錛屼嬌騫叉壈鍏冪礌鍒嗙錛岀敤媧楄劚娑叉礂涓嬫煴涓婂惛闄勭殑閾€銆傚湪寮辯⒈鎬ф憾娑?/span>(pH=8)涓紝閾€涓?/span>2-(5-婧?/span>-2-鍚″暥鍋舵唉)-5-浜屼箼鑳哄熀鑻厷(Br-PADAP錛夊艦鎴愭湁鑹茬殑浜屽厓緇滃悎鐗╋紝鐒跺悗榪涜鍏夊害嫻嬮噺錛屾眰寰楅搥鍚噺銆?/span>

3寮曠敤鏍囧噯GB474鐓ゆ牱鐨勫埗澶囨柟娉?/span>

4璇曞墏鍜屾潗鏂?/span>

4.1 鑱氫笁姘熸隘涔欑儻錛氱矑搴?/span>0.125~0.175mm銆?/span>

4.2涓欓叜錛?/span>GB686錛夈€?/span>

4.3 娣峰悎閾電洂錛氭盁鍖栭摰(GB1276)銆佹隘鍖栭摰(GB 658)銆佺～閰擱摰(GB1396)鍜岀閰擱摰(GB 659)浠?/span>3+2+2+3鐨勮川閲忔瘮娣峰寑銆佺爺緇嗐€佽鐡跺鐢ㄣ€?/span>

4.4 紓烽吀涓変竵閰?/span>(TBP錛?/span>-涔欓啔婧舵恫錛氬彇40mLTBP(HG3鈥?/span>1304)娉ㄥ叆100mL瀹歸噺鐡朵腑錛岀敤涔欓啔(HG3-1002錛夌█閲婂埌鍒誨害銆?/span>TBP搴旇繘琛屽涓嬮澶勭悊錛氬彇涓€瀹氶噺鐨?/span>TBP娉ㄥ叆鍒嗘恫婕忔枟涓紝鐢ㄧ瓑浣撶Н鐨?/span>50g/L紕抽吀閽犳按婧舵恫媧楁釘3嬈★紝鍐嶇敤絳変綋縐殑姘存礂娑?/span>3嬈★紝鍒嗙鍚庤鐡跺鐢ㄣ€?/span>

4.5 娣峰悎鎺╄斀娑詫細縐板彇12g鐜凡浜岃兒鍥涗箼閰?/span>(CYDTA)錛岀敤姘㈡哀鍖栭挔(GB 629)婧舵恫(c(NaOH)=1mol/L]婧惰В錛屽姞鍏?/span>3g姘熷寲閽?/span>(GB 1264)錛?/span>32g紓峰熀姘存潹閰?/span>(HG3-991)鍜?/span>400mL姘淬€傚緟鍏ㄩ儴婧惰В鍚庯紝鐢?/span>400g/L姘㈡哀鍖栭挔(GB629)婧舵恫鍜?/span>(1+1錛夌洂閰?/span>(GB622錛夎皟鏁存憾娑茬殑閰稿害鑷?/span>pH=8(鐢ㄧ簿瀵?/span>pH璇曠焊媯€楠岋級錛屽啀鐢ㄦ按紼€閲婂埌500mL銆?/span>

4.6涓変箼閱囪兒緙撳啿婧舵恫錛氬彇100mL涓変箼閱囪兒婧朵簬300mL姘翠腑錛岀敤(1+1錛夌洂閰稿拰姘㈡哀鍖栭挔婧舵恫[c(NaOH)=1mol/L]璋冩暣婧舵恫鐨勯吀搴﹀埌pH=8(鐢ㄧ簿瀵?/span>pH璇曠焊媯€楠岋級錛屽啀鐢ㄦ按紼€閲婂埌500mL銆?/span>

4.7 娣嬫礂娑詫細縐板彇200g紜濋吀閾?/span>(GB659)錛屽姞姘存憾瑙ｅ悗錛屽姞鍏?/span>130mL紜濋吀(GB626錛夛紝縐誨叆2L鐨勫閲忕摱涓紝鍔犳按紼€閲婂埌鍒誨害錛堟婧舵恫姣忓崌鍚?/span>100g紜濋吀閾靛拰1mol紜濋吀錛夈€?/span>

4.8媧楄劚娑詫細紜濋吀婧舵恫(c(HNO3)=1mol/L]銆?/span>

4.9 Br-PADAP涔欓唶婧舵恫錛氱О鍙?/span>0.25g 2-(5-婧?/span>-2-鍚″暥鍋舵愛)-5-浜屼箼鑳跺熀鑻厷(Br-PADAP錛夋憾浜?/span>500mL 鏃犳按涔欓唶(GB 678)涓€?/span>

4.10 閾€鏍囧噯婧舵恫錛氱О鍙?0.2109g紜濋吀閾€閰?/span>[UO2(NO3)26H20]錛屾憾浜庡皯閲忔按涓紝灝嗘憾娑茬Щ鍏?/span>1L瀹歸噺鐡朵腑錛岀敤姘寸█閲婂埌鍒誨害錛堟婧舵恫1mL鍚?/span>100渭g閾€錛夈€傚彇涓婅堪婧舵恫50.0mL浜?/span>g00mL瀹歸噺鐡朵腑錛岀敤姘寸█閲婂埌鍒誨害(姝ゆ憾娑?/span>1mL鍚?/span>10p渭g閾€錛夈€?/span>

4.11 閰氶厼(HGB 3039錛夋寚紺哄墏錛?/span>0.1g/L涔欓唶婧舵恫銆?/span>

5浠櫒銆佽澶?/span>

5.1 椹紬鐐夛細闄勬湁鐑數(shù)鍋跺拰楂樻俯璁★紝鑳芥帶娓╁湪600鹵10鈩冦€?/span>

5.2 鍒嗗厜鍏夊害璁★細鍚?/span>580nm娉㈤暱銆?/span>

5.3 鐡峰潻鍩氾細瀹歸噺50mL銆?/span>

5.4 鑹插眰鍒嗙鏌憋細濡傚浘鎵€紺恒€?/span>

6璇曢獙鍑嗗

6.1鑹插眰鏌辯殑鍒跺

6.1.1 TBP-鑱氫笁姘熸隘涔欑儻鐨勫埗澶囷細

縐板彇2g鑱氫笁姘熸隘涔欑儻(4.1)鏀懼叆50mL鐑ф澂涓紝閫愭淮鍔犲叆2mLTBP-涔欓啔婧舵恫(4.4)錛岃竟鍔犺竟鎼呮媽錛岀劧鍚庣疆浜庢按嫻翠笂鍔犵儹錛屽皢涔欓啔鍩烘湰闄ゅ幓銆傚啀鎸夊悓鏍鋒柟娉曞厛鍚庢淮鍔?/span>1mL鍜?/span>0.5mLTBP-涔欓啔婧舵恫騫跺垎鍒捀騫詫紝鏈€鍚庡皢涔欓啔瀹屽叏闄ゅ幓錛屽緱鍒版箍鐩愮姸棰楃矑錛岀◢鍐鳳紝娌挎澂澹佸姞鍏ュ皯閲忔按錛屽緱鍒伴洩鑺辯姸鐗╋紝鍗充負鍚擱檮鏈?TBP鐨勮仛涓夋盁姘箼鐑€?/span>

6.1.2 瑁呮煴

鍦ㄨ壊灞傚垎紱繪煴(5.4錛夊簳閮ㄦ斁鍏ュ皯閲忕幓鐠冩錛岀劧鍚庡瀭鐩存斁濂姐€傚湪鍒跺濂界殑2g TBP-鑱氫笁姘熸隘涔欑儻涓姞鍏ヨ繃閲忕殑姘達紝鎼呮媽錛屽垎鏁版鍊掑叆鑹插眰鍒嗙鏌辯殑璐恫鏉腑錛屼嬌TBP-鑱氫笁姘熸隘涔欑儻鍧囧寑娌夐檷錛屽茍灝嗘祦閫熸帶鍒跺湪1~2mL/min銆傚緟姘存祦灝藉悗錛屽姞鍏?/span>20mL娣嬫礂娑?/span>(4.7)澶囩敤銆備竴嬈¤鏌卞悗錛屽彲浣跨敤12嬈″乏鍙熾€?/span>

7鐓ゆ牱

嫻嬪畾鐢ㄧ殑鐓ゆ牱涓烘寜GB474鍒跺鐨勩€佺矑搴﹀皬浜?/span>0.2mm鐨勭┖姘斿共鐕ョ叅鏍楓€?/span>

8嫻嬪畾姝ラ

8.1 宸ヤ綔鏇茬嚎鐨勭粯鍒?/span>

8.1.1 鍚稿彇 0,0.5錛?/span>1.0,2.0,3.0,4.0鍜?5.0mL嫻撳害涓?/span>10渭g/mL鐨勯搥鏍囧噯婧舵恫(4.10)錛屽垎鍒敞鍏ヨ壊灞傚垎紱繪煴鐨勮串娑叉澂涓紝浣挎憾娑查€氳繃鑹插眰鍒嗙鏌便€傚緟婧舵恫嫻佸敖鍚庯紝鐢?/span>12mL娣嬫礂娑?/span>(4.7)鍒?/span>6嬈℃礂娑ゆ澂澹佸拰鑹插眰鍒嗙鏌憋紝鍐嶇敤4ml姘存穻媧椼€傛瘡嬈″姞娣嬫礂娑叉椂錛屽簲絳夋煴涓憾娑叉祦灝藉悗鍐嶅姞(浠ヤ笅鍑″嬈℃穻媧楅兘搴旈伒瀹堟鍘熷垯)銆傚皢浠ヤ笂娣嬫礂娑插純鍘伙紝閾€琚惛闄勩€傜劧鍚庡厛鐢?/span>2mL姘存穻媧?/span>1嬈★紝鍐嶇敤14mL媧楄劚娑?/span>(4.8)鍒?/span>4~6嬈℃穻媧楋紝鏈€鍚庣敤2mL姘存穻媧楋紝浣塊搥媧楄劚銆傚皢鍏ㄩ儴18mL宸﹀彸婧舵恫鏀墮泦浜?/span>50mL瀹歸噺鐡朵腑銆?/span>

8.1.2寰€瀹歸噺鐡朵腑鍔?/span>2mL娣峰悎鎺╄斀娑?/span>(4.5)銆?/span>1撮厷閰炴寚紺哄墏(4.11錛夛紝鐢?/span>150g/L鐨勬阿姘у寲閽狅紙GB629)婧舵恫璋冭嚦綺夌孩鑹詫紝鍐嶇敤鐩愰吀(GB 622)(c(HCl錛?/span>=1mol/L]璋冭嚦鏃犺壊錛屽姞2mL涓変箼閱囪兒緙撳啿娑?/span>(4.6)銆?/span>8mL涓欓叜(4.2錛夊拰2mLBr-PADAP 涔欓唶婧舵恫(4.9)錛屾憞鍖€錛堝娣鋒祳鍙鍔?/span>1mL涓欓叜錛夛紝鐢ㄦ按紼€閲婂埌鍒誨害錛屾憞鍖€銆?/span>

8.1.3 鏀劇疆30~60min錛岀劧鍚庣敤1cm姣旇壊鐨匡紝浜?/span>580nm娉㈤暱涓嬶紝浠ョ┖鐧芥憾娑蹭負鍙傛瘮錛屾祴閲忓悇鏍囧噯婧舵恫鐨勫惛鍏夊害銆傜┖鐧芥憾娑插簲鍏堢粡鑹插眰鍒嗙鏌卞惛闄勫拰媧楄劚澶勭悊銆?/span>

8.1.4 浠ュ惛鍏夊害涓虹旱鍧愭爣錛岄搥鍚噺涓烘í鍧愭爣緇樺埗宸ヤ綔鏇茬嚎銆?/span>

8.2鐓ゆ牱嫻嬪畾

8.2.1鐓ゆ牱鐨勭伆鍖栫О鍙栫害1g(綺劇‘鑷?/span>0.0002g)鐓ゆ牱錛堟牴鎹搥鐨勫惈閲忓彲閫傚綋澧炲噺錛変簬鐡峰潻鍩?/span>(5.3錛変腑錛屾斁鍏ラ┈寮楃倝(5.1)錛岀敱瀹ゆ俯閫愭笎鍔犵儹鍒?/span>600澹?/span>10鈩冿紝騫跺湪姝ゆ俯搴︿笅淇濇寔1h錛屽彇鍑哄潻鍩氬茍鍐峰嵈銆?/span>

8.2.2鐏版牱鐨勫鐞嗗湪鐩涙湁鐏版牱鐨勭摲鍧╁煔涓姞鍏?/span>3g娣峰悎閾電洂(4.3錛夊茍娣峰寑錛屽啀瑕嗙洊1~2g銆傚皢鍧╁煔緗簬鑳芥帶娓╃殑鐢電倝涓婏紝鍏堝湪浣庢俯涓嬬啍铻?/span>15~20min錛岀劧鍚庣◢紼嶅崌楂樻俯搴︿嬌鍏跺啋鐧界儫錛屽啀鍗囬珮娓╁害錛岀洿鑷崇櫧鐑熷啋灝斤紝紼嶅喎錛屽姞鍏?/span>20mL娣嬫礂娑?/span>(4.7)錛屽姞鐑紝浣跨洂綾繪憾瑙ｃ€?/span>

8.2.3閾€鐨勫垎紱誨皢鐏版牱澶勭悊娑插喎鍗達紝鐢ㄥ皬婕忔枟灝嗘憾娑茬洿鎺ユ護鍏ヨ壊灞傚垎紱繪煴鐨勮串娑叉澂鍐咃紝浣挎護娑查€氳繃鑹插眰鍒嗙鏌便€傚緟ゆ恫嫻佸敖鍚庯紝鐢?/span>6mL 娣嬫礂娑?/span>(4.7)鍒?/span>3嬈″拰4mL姘村垎2嬈℃穻媧楄壊灞傚垎紱繪煴錛屽皢浠ヤ笂娣嬫礂娑插純鍘伙紝閾€琚惛闄勩€傜敤2mL姘存穻媧楁煴1嬈★紝鍐嶇敤14mL媧楄劚娑?/span>(4.8)鍒?/span>4~6嬈℃穻媧楋紝鏈€鍚庣敤2mL姘存穻媧楋紝閾€琚礂鑴便€傚皢鍏ㄩ儴18mL宸﹀彸鐨勬穻媧楁恫鏀墮泦鍦?/span>50mL瀹歸噺鐡朵腑銆?/span>

8.2.4 閾€鐨勬祴瀹氫簬瀹歸噺鐡朵腑鍔犲叆2mL娣峰悎鎺╄斀娑?/span>(4.5)銆備互鍚庢祴瀹氭楠ゆ寜鏈爣鍑?/span>8.1.2鍜?/span>8.1.3鏉¤繘琛屻€備粠宸ヤ綔鏇茬嚎涓婃煡鍑虹浉搴旂殑閾€鍚噺銆?/span>

8.3絀虹櫧璇曢獙絀虹櫧璇曢獙闄や笉鍔犵叅鏍峰錛屽叾浣欐楠や笌鐓ゆ牱嫻嬪畾(7.2錛夊畬鍏ㄧ浉鍚屻€傚彇閲嶅嫻嬪畾緇撴灉鐨勭畻鏈鉤鍧囧€間綔涓虹┖鐧藉€箋€?/span>

9嫻嬪畾緇撴灉鐨勮〃榪伴搥鍚噺鎸変笅榪板叕寮忚綆楋細

鐓ょ偔鍚搥閲忚綆楀叕寮忎負錛?/span>Uad絀烘皵騫茬嚗鐓ゆ牱鍚噺絳変簬M1鍑忓幓M2錛屽湪闄や互M銆?/span>

寮忎腑錛?/span>Uad鈥旂┖姘斿共鐕ョ叅鏍蜂腑閾€鍚噺錛?/span>ug/g錛?/span>

M1鈥斺€旂叅鏍鋒憾娑蹭腑閾€鍚噺錛?/span>ug

m2鈥斺€旂┖鐧芥憾娑蹭腑閾€鍚噺錛屛?/span>g

M---絀烘皵騫茬嚗鐓ゆ牱璐ㄩ噺錛?/span>g銆?/span>

璁＄畻緇撴灉鍙栧埌灝忔暟鍚?/span>1浣嶏紝淇害鍒頒釜浣嶅茍鎶ュ嚭銆?/span>