GB-T 11066.12-2024 金化學(xué)分析方法 第12部分

CCSH15電感耦合等離子體原子發(fā)射光譜法國(guó)家市場(chǎng)監(jiān)督管理總局國(guó)家標(biāo)準(zhǔn)化管理委員會(huì)I Ⅲ 12規(guī)范性引用文件 1 2 25試劑或材料 2 57樣品 57.1試樣 57.2試料 5 58.1空白試驗(yàn) 58.2測(cè)定次數(shù) 5 58.4工作曲線的繪制 69試驗(yàn)數(shù)據(jù)處理 610精密度 710.1重復(fù)性 7 附錄A(資料性)推薦的電感耦合等離子體原子發(fā)射光譜儀工作條件參數(shù) 附錄B(資料性)電感耦合等離子體原子發(fā)射光譜法中多譜線擬合法使用示例 附錄C(資料性)精密度試驗(yàn)原始數(shù)據(jù) ⅢGB/T11066.12—2024本文件按照GB/T1.1—2020《標(biāo)準(zhǔn)化工作導(dǎo)則第1部分：標(biāo)準(zhǔn)化文件的結(jié)構(gòu)和起草規(guī)則》的規(guī)定起草。本文件是GB/T11066《金化學(xué)分析方法》的第12部分。GB/T11066已經(jīng)發(fā)布了以下部分：-—銀量的測(cè)定火試金法；火焰原子吸收光譜法；火焰原子吸收光譜法；——銅、鉛和鉍量的測(cè)定火焰原子吸收光譜法；火花原子發(fā)射光譜法；乙酸乙酯萃取-電感耦合等離子體原子發(fā)射光譜法；——硅量的測(cè)定鉬藍(lán)分光光度法；電感耦合等離子體質(zhì)譜法；電感耦合等離子體原子發(fā)射光譜法。請(qǐng)注意本文件的某些內(nèi)容可能涉及專利。本文件的發(fā)布機(jī)構(gòu)不承擔(dān)識(shí)別專利的責(zé)任。本文件由中國(guó)有色金屬工業(yè)協(xié)會(huì)提出。本文件由全國(guó)有色金屬標(biāo)準(zhǔn)化技術(shù)委員會(huì)(SAC/TC243)歸口。本文件起草單位：紫金礦業(yè)集團(tuán)股份有限公司、福建紫金礦冶測(cè)試技術(shù)有限公司廈門分公司、北礦檢測(cè)技術(shù)股份有限公司、大冶有色設(shè)計(jì)研究院有限公司、深圳市中金嶺南有色金屬股份有限公司、有色金屬技術(shù)經(jīng)濟(jì)研究院有限責(zé)任公司、山東恒邦冶煉股份有限公司、華津國(guó)檢(深圳)金銀珠寶檢驗(yàn)中心有GB/T11066.12—2024確檢測(cè)金的化學(xué)成分顯得尤為重要。GB/T11066根據(jù)檢測(cè)對(duì)象和檢測(cè)手段的不同，由12個(gè)部分構(gòu)成。-—第1部分：金量的測(cè)定火試金法。目的在于規(guī)定金中金含量的火試金法及適用的測(cè)定范圍?！?部分：銀量的測(cè)定火焰原子吸收光譜法。目的在于規(guī)定金中銀含量的火焰原子吸收光譜法及適用的測(cè)定范圍?！?部分：鐵量的測(cè)定火焰原子吸收光譜法。目的在于規(guī)定金中鐵含量的火焰原子吸收光譜法及適用的測(cè)定范圍?！?部分：銅、鉛和鉍量的測(cè)定火焰原子吸收光譜法。目的在于規(guī)定金中銅、鉛和鉍含量的火焰原子吸收光譜法及適用的測(cè)定范圍。 —第6部分：鎂、鎳、錳和鈀量的測(cè)定火焰原子吸收光譜法。目的在于規(guī)定金中鎂、鎳、錳和鈀含量的火焰原子吸收光譜法及適用的測(cè)定范圍?；鸹ㄔ影l(fā)射光譜法。目的 乙酸乙酯萃取-電感耦合等離子酯萃取-電感耦合等離子體原子發(fā)射光譜法及適用的測(cè)定范圍。——第9部分：砷和錫量的測(cè)定氫化物發(fā)生-原子熒光光譜法。目的在于規(guī)定金中砷和錫含量的氫化物發(fā)生-原子熒光光譜法及適用的測(cè)定范圍?！?0部分：硅量的測(cè)定鉬藍(lán)分光光度法。目的在于規(guī)定金中硅含量的鉬藍(lán)分光光度法及適用的測(cè)定范圍。電感耦合等離子體質(zhì)譜譜法及適用的測(cè)定范圍。電感耦合等離子體原子發(fā)射光譜法。目的在于采用基體匹配-標(biāo)準(zhǔn)曲線法及多譜線擬合法等校正方法，使用電感耦合等離子體原子發(fā)射光譜儀測(cè)定金質(zhì)量。GB/T11066.12—2024電感耦合等離子體原子發(fā)射光譜法警告——使用本文件的人員應(yīng)有正規(guī)實(shí)驗(yàn)室工作的實(shí)踐經(jīng)驗(yàn)。本文件并未指出所有可能的安全問(wèn)題。使用者有責(zé)任采取適當(dāng)?shù)陌踩徒】荡胧⒈ＷC符合國(guó)家有關(guān)法規(guī)規(guī)定的條件。1范圍表1測(cè)定范圍元素測(cè)定范圍(質(zhì)量分?jǐn)?shù))%元素測(cè)定范圍(質(zhì)量分?jǐn)?shù))%元素測(cè)定范圍(質(zhì)量分?jǐn)?shù))%AgKPtFeNaPbBiVAsMgNiMoMnPdAl2規(guī)范性引用文件下列文件中的內(nèi)容通過(guò)文中的規(guī)范性引用而構(gòu)成本文件必不可少的條款。其中，注日期的引用文件，僅該日期對(duì)應(yīng)的版本適用于本文件；不注日期的引用文件，其最新版本(包括所有的修改單)適用于本文件。12GB/T11066.12—2024GB/T6682分析實(shí)驗(yàn)室用水規(guī)格和試驗(yàn)方法GB/T17433—2014冶金產(chǎn)品化學(xué)分析基礎(chǔ)術(shù)語(yǔ)3術(shù)語(yǔ)和定義GB/T17433—2014界定的術(shù)語(yǔ)和定義適用于本文件。4原理5試劑或材料5.230%過(guò)氧化氫。5.3鹽酸(p=1.19g/mL)。5.4硝酸(p=1.42g/mL)。5.5鹽酸(1+1)。5.6鹽酸(1+9)。5.7硝酸(1+1)。5.8混合酸：以1體積硝酸(5.4)、3體積鹽酸(5.3)和4體積的水混合均勻。5.9乙醇(1+1)。5.10金(wAu≥99.999%,單個(gè)雜質(zhì)元素含量不大于0.0002%,雜質(zhì)總和不大于0.0010%)。5.11銀標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬銀(wAg≥99.99%),置于100mL聚四氟乙烯燒杯中，加入5.12銅標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬銅(wcu≥99.99%),置于100mL聚四氟乙烯燒杯中，加入5.13鐵標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬鐵(Wre≥99.99%),置于100mL聚四氟乙烯燒杯中，加入5.14鉛標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬鉛(wpb≥99.99%),置于100mL聚四氟乙烯燒杯中，加入5.15鉍標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬鉍(wgi≥99.99%),置于100mL聚四氟乙烯燒杯中，加入5.16鎂標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬鎂(wmg≥99.99%),置于100mL聚四氟乙烯燒杯中，加入35.17鎳標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬鎳(wni≥99.99%),置于100mL聚四氟乙烯燒杯中，加入5.18錳標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬錳(wMn≥99.99%),置于100mL聚四氟乙烯燒杯中，加入5.19鉻標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬鉻(wc≥99.99%),置于100mL聚四氟乙烯燒杯中，加入5.20鋅標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬鋅(wzn≥99.99%),置于100mL聚四氟乙烯燒杯中，加入5.23鈷標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬鈷(wc?≥99.99%),置于100mL聚四氟乙烯燒杯中，加5.24鈣標(biāo)準(zhǔn)貯存溶液：稱取0.2497g碳酸鈣(基準(zhǔn)試劑，預(yù)先在105℃烘2h,置于干燥器中冷卻至室5.25鉀標(biāo)準(zhǔn)貯存溶液：稱取0.1907g于500℃~600℃烘至恒重的氯化鉀，置于100mL聚四氟乙烯5.27釩標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬釩(wv≥99.99%),5.28鎘標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬鎘(wca≥99.99%),置于100mL聚四氟乙烯燒杯中，加入5.29錸標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬錸(Wre≥99.99%),置于100mL3mL鹽酸(5.3),1mL硝酸(5.4),低溫加熱溶解完全，移入100mL塑料容量瓶中，加入10mL鹽酸5.30鋁標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬鋁(wai≥99.99%),置于100mL聚四氟乙烯燒杯中，加入20mL鹽酸(5.5),低溫加熱溶解，冷卻至室溫，用鹽酸(5.5)移入100mL塑料容量瓶中并稀釋至刻4GB/T11066.12—20245.31銻標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬銻(wsb≥99.99%),置于100mL聚四氟乙烯燒杯中，加入5.32鈀標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬鈀(wpa≥99.99%),置于100mL聚四氟乙烯燒杯中，加入5.33鉑標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬鉑(wp≥99鹽酸(5.3)和4mL30%過(guò)氧化氫(5.2),于160℃~180℃烘箱中溶解48h以上至溶解完全。取出溶樣5.36錫標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬錫(wsm≥99.99%),置于100mL聚四氟乙烯燒杯中，加入5.37硅標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬硅(wsi≥99.99%),置于聚四氟乙烯燒杯中，加少量水潤(rùn)5.39鋯標(biāo)準(zhǔn)貯存溶液：稱取0.1000g金屬鋯(wz≥99.99%),5mL氫氟酸溶液(1+1),再滴加硝酸(5.4)加熱，溶解完全后，冷卻至室溫，移入100mL塑料容5.40鉬標(biāo)準(zhǔn)貯存溶液：稱取0.1500g三氧化鉬(WwMoo?≥99.95%),置于100mL聚四氟乙烯燒杯5GB/T11066.12—2024100mL混合酸(5.8),低溫加熱至溶液清亮，用水轉(zhuǎn)入500mL塑料容量瓶中，補(bǔ)加100mL混合酸5.46氬氣(體積分?jǐn)?shù)≥99.99%)。的銅標(biāo)準(zhǔn)溶液測(cè)量11次，其發(fā)射強(qiáng)度的相對(duì)標(biāo)準(zhǔn)偏差不超過(guò)推薦的電感耦合等離子體原子發(fā)射光譜儀工作條件參數(shù)見(jiàn)附錄A。7樣品(5.9),于電熱板上加熱煮沸5min后取下，將乙醇傾去，再用水洗滌試樣3次。加入20mL鹽酸(5.5),加熱煮沸5min,傾去鹽酸，再用水洗滌試樣3次。將試樣用無(wú)塵紙包裹，于105℃烘干后取出冷卻。稱取1.000g試樣(7.1),精確到0.08試驗(yàn)步驟隨同試料做基體匹配空白試驗(yàn)。應(yīng)獨(dú)立進(jìn)行不少于2次的測(cè)定，結(jié)果取其平均值。8.3.1將試料(7.2)置于100mL聚四氟乙烯燒杯中，加入20mL混合酸(5.8),蓋上聚四氟乙烯杯8.3.2于電感耦合等離子體原子發(fā)射光譜儀上，在選定的儀器工作條件下，測(cè)量試液及隨同試料空白6GB/T11066.12—20248.4工作曲線的繪制8.4.1系列標(biāo)準(zhǔn)溶液的配制分別于8個(gè)100mL塑料容量瓶中，加入2.5mL混合酸(5.8),20.00mL金基體標(biāo)準(zhǔn)溶液(5.45),再分別加入混合標(biāo)準(zhǔn)溶液A?(5.41)0mL、1.00mL、2.00mL、5.00mL、10.00mL、25.00mL,混合標(biāo)準(zhǔn)溶液A?(5.43)25.00mL、50.00mL,以鹽酸(5.6)稀釋至刻度，混勻。系列標(biāo)準(zhǔn)溶液質(zhì)量濃度見(jiàn)分別于8個(gè)100mL塑料容量瓶中，加入2.5mL混合酸(5.8),20.00mL金基體標(biāo)準(zhǔn)溶液(5.45),再分別加入混合標(biāo)準(zhǔn)溶液B?(5.42)0mL、1.00mL、2.00mL、5.00mL、10.00mL、25.00mL,混合標(biāo)準(zhǔn)溶液B?(5.44)25.00mL、50.00mL,以鹽酸(5.6)稀釋至刻度，混勻。系列標(biāo)準(zhǔn)溶液質(zhì)量濃度見(jiàn)注：可使用市售有證標(biāo)準(zhǔn)溶液。表2系列標(biāo)準(zhǔn)溶液濃度單位為微克每毫升序號(hào)元素STD-1STD-2STD-3STD-4STD-5STD-6STD-7STD-8A組Ag、Cu、Fe、Pb、Bi、Mg、Ni、Mn、Cr、Zn、As、Na、Co、Ca、K、Li、V、Cd、Re、Al00.100.200.502.507.50B組Sb、Pd、Pt、Rh、Ti、Sn、Si、Te、Zr、Mo00.100.200.502.507.508.4.2工作曲線繪制與測(cè)試試液測(cè)定相同條件下，測(cè)量系列標(biāo)準(zhǔn)溶液中各元素的強(qiáng)度，以被測(cè)元素的濃度為橫坐標(biāo)、信號(hào)強(qiáng)度為縱坐標(biāo)，繪制工作曲線。9試驗(yàn)數(shù)據(jù)處理按式(1)計(jì)算被測(cè)元素的質(zhì)量分?jǐn)?shù)w,數(shù)值以%表示：式中：V——試料溶液的體積，單位為毫升(mL);m——試料質(zhì)量，單位為克(g);計(jì)算結(jié)果保留至小數(shù)點(diǎn)后四位?！?GB/T11066.12—202410精密度在重復(fù)性條件下獲得的兩次獨(dú)立測(cè)試結(jié)果的測(cè)定值，在以下給出的平均值范圍內(nèi)，這兩個(gè)測(cè)試結(jié)果的絕對(duì)值不超過(guò)重復(fù)性限(r),超過(guò)重復(fù)性限(r)的情況不超過(guò)5%,重復(fù)性限(r)按表3數(shù)據(jù)采用線性內(nèi)插法求得。精密度試驗(yàn)原始數(shù)據(jù)見(jiàn)附錄C。元素質(zhì)量分?jǐn)?shù)%重復(fù)性限(r)%Ag0.00100.00020.00940.00130.05040.00410.00110.00020.00960.00100.06160.0030Fe0.00170.00030.01630.00160.06380.0032Pb0.00090.00020.00910.00110.05430.0027Bi0.00080.00020.00810.00110.05140.00380.00070.00020.00720.00100.05360.0029Mg0.00020.00010.00990.00060.04740.0029Ni0.00090.00020.00940.00070.04990.0022Mn0.00090.00020.00920.00060.05370.00228GB/T11066.12—2024表3重復(fù)性限(續(xù))元素質(zhì)量分?jǐn)?shù)%重復(fù)性限(r)%Pd0.00080.00020.00830.00080.05370.00320.00030.00020.00940.00050.05670.0029Pt0.00080.00020.00820.00080.06170.00230.00080.00010.00830.00080.0430.00320.00030.00010.00980.00080.04860.0020.00090.00020.00850.00050.05450.0038As0.00060.00020.00990.00120.04990.00230.00080.00020.00730.00090.05380.00310.00030.00010.00910.00080.04810.00280.00080.00010.00820.00060.05410.00250.00030.00010.01040.00140.04850.00429GB/T11066.12—2024表3重復(fù)性限(續(xù))元素質(zhì)量分?jǐn)?shù)%重復(fù)性限(r)%K0.00030.00010.01010.00140.04940.0040.00080.00010.01020.00110.04940.0021Na0.00030.00010.01030.00140.0530.00350.00070.00010.00770.00050.04840.0035V0.00020.00010.01020.0010.05020.00260.00030.00010.00990.00070.04870.00210.00070.00010.0080.00050.0630.0024Mo0.00030.00010.010.00070.04290.00290.00020.00010.01040.00080.04920.0025Al0.00030.00010.010.00110.05020.0034GB/T11066.12—2024在再現(xiàn)性條件下獲得的兩次獨(dú)立測(cè)試結(jié)果的測(cè)定值，在表4給出的平均值范圍內(nèi)，這兩個(gè)測(cè)試結(jié)果的絕對(duì)值不超過(guò)再現(xiàn)性限(R),超過(guò)再現(xiàn)性限(R)的情況不超過(guò)5%,再現(xiàn)性限(R)按表4數(shù)據(jù)采用線性內(nèi)插法求得。精密度試驗(yàn)原始數(shù)據(jù)見(jiàn)附錄C。表4再現(xiàn)性限元素質(zhì)量分?jǐn)?shù)%再現(xiàn)性限(R)%Ag0.0010.00030.00940.0020.05040.0050.00110.00030.00960.00130.06160.0052Fe0.00170.00040.01630.00280.06380.0041Pb0.00090.00020.00910.00130.05430.0042Bi0.00080.00040.00810.00170.05140.00410.00070.00030.00720.00150.05360.0031Mg0.00020.00010.00990.00150.04740.0056Ni0.00090.00020.00940.00150.04990.0027Mn0.00090.00030.00920.00150.05370.0043GB/T11066.12—2024表4再現(xiàn)性限(續(xù))元素質(zhì)量分?jǐn)?shù)%再現(xiàn)性限(R)%Pd0.00080.00030.00830.0010.05370.0050.00030.00030.00940.00180.05670.0044Pt0.00080.00030.00820.0010.06170.00360.00080.00010.00830.00120.0430.00470.00030.00010.00980.00120.04860.00360.00090.00020.00850.00130.05450.004As0.00060.00030.00990.00150.04990.00480.00080.00020.00730.00140.05380.00370.00030.00020.00910.00180.04810.0040.00080.00020.00820.00120.05410.00350.00030.00020.01040.00150.04850.0044GB/T11066.12—2024表4再現(xiàn)性限(續(xù))元素質(zhì)量分?jǐn)?shù)%再現(xiàn)性限(R)%K0.00030.00030.01010.00260.04940.00490.00080.00030.01020.00130.04940.0035Na0.00030.00020.01030.00160.0530.00520.00070.00030.00770.00110.04840.0044V0.00020.00010.01020.00130.05020.00340.00030.00010.00990.00090.04870.00310.00070.00020.0080.00180.0630.0047Mo0.00030.00020.010.00140.04290.00370.00020.00020.01040.0010.04920.0032Al0.00030.00020.010.00170.05020.0035GB/T11066.12—202411試驗(yàn)報(bào)告試驗(yàn)報(bào)告至少應(yīng)給出以下內(nèi)容： 本文件編號(hào)； 分析結(jié)果及其表示： 式驗(yàn)中觀察到的異?，F(xiàn)象； GB/T11066.12—2024(資料性)推薦的電感耦合等離子體原子發(fā)射光譜儀工作條件參數(shù)推薦的電感耦合等離子體原子發(fā)射光譜儀工作條件參數(shù)見(jiàn)表A.1,分析譜線推薦表及干擾元素見(jiàn)表A.1電感耦合等離子體原子發(fā)射光譜儀工作條件參數(shù)推薦表功率霧化室氣流觀測(cè)高度泵流量等離子體流量輔助體流量時(shí)間觀測(cè)WL/minL/minL/minL/mins方式0.700.705軸向表A.2電感耦合等離子體原子發(fā)射光譜儀分析譜線推薦表及干擾元素元素波長(zhǎng)干擾元素元素波長(zhǎng)干擾元素元素波長(zhǎng)干擾元素Ag328.068267.716K766.490324.752Pt265.945V670.784Fe259.939343.489Na589.592Pb220.353336.121214.281Bi213.857V292.402217.582AsPd343.823Mg285.213228.616226.502Ni231.604317.933Mo202.031PtMn259.372Pd340.458251.611Al394.401注：表格空白指該譜線在試驗(yàn)條件下(或設(shè)備本身)未發(fā)現(xiàn)干擾元素。GB/T11066.12—2024(資料性)電感耦合等離子體原子發(fā)射光譜法中多譜線擬合法使用示例以某一型號(hào)電感耦合等離子體原子發(fā)射光譜儀采用多譜線擬合法消除Pd對(duì)As188.979nm的干擾為例。a)譜線選擇：選擇188.979nm作為As分析譜線，按標(biāo)準(zhǔn)曲線法建立分析方法。b)待測(cè)溶液：空白溶液(kb)、As標(biāo)準(zhǔn)溶液(a)20mg/L、Pd標(biāo)準(zhǔn)溶液(i)10mg/L,均含2%金基體。根據(jù)多譜線擬合原理，分析元素和干擾元素濃度能采集到干擾峰即可，但從實(shí)際出發(fā)，所用溶液濃度宜接近實(shí)際樣品的濃度。c)檢測(cè)：在與樣品檢測(cè)相同的儀器條件下，將空白溶液(kb)、As標(biāo)準(zhǔn)溶液(a)、Pd標(biāo)準(zhǔn)溶液(i)作為待測(cè)試樣檢測(cè)。d)建立多譜線擬合(MSF)模型：在結(jié)果數(shù)據(jù)(Results)的檢查光譜窗口(ExamineSpectra),將“檢查”(Examine)調(diào)整為“檢查多譜線擬合”(ExamineMSF)。在數(shù)據(jù)選擇窗口(SelectData)將空白溶液(kb)設(shè)為“空白b”(Blank)、As標(biāo)準(zhǔn)溶液(a)設(shè)為“分析物a”(Analyte)、Pd標(biāo)準(zhǔn)溶e)在方法中帶入多譜擬合(MSF)模型：選擇相應(yīng)的方法，在程序窗口(Process)將“峰值處理”選擇步驟d)所建立的模型，更新并保存方法。f)采用帶入多譜線擬合(MSF)模型的方法處理數(shù)據(jù)或檢測(cè)樣品。GB/T11066.12—2024(資料性)精密度試驗(yàn)原始數(shù)據(jù)表C.1銀的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)12345671123212331234123512361237123表C.2銅的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)Wcu/%1234567110.00110.00110.00110.00110.00110.00110.001120.00990.00940.01020.01010.00990.01010.010030.06410.06200.06130.06440.06430.06270.0616210.00110.00100.00130.00120.00120.00130.001220.00920.00990.00940.00980.01020.01050.010330.06280.06420.06370.06490.06020.06070.0632310.00110.00120.00120.00110.000980.00100.001120.00970.00930.00860.00880.00970.00970.009930.06370.06120.06120.06270.06090.06060.0616410.000970.000940.000960.000950.000970.000920.0009420.00930.00900.00920.00930.00940.00930.009430.05900.05920.05890.05950.05860.05910.0589510.00120.00120.00110.00120.00120.00120.001220.00880.00940.00930.00900.00940.00950.009530.06030.06090.06050.06070.06070.06010.0599610.000920.00120.00100.00100.00100.00110.001120.00910.00960.00890.00980.00920.00850.009530.06200.06130.05910.06160.05990.06170.0599710.00110.00110.00110.00110.00110.00110.001120.00990.00980.00980.00980.01020.00990.009930.06290.06350.06300.06330.06300.06310.0641GB/T11066.12—2024表C.3鐵的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)WFe/%1234567Fe110.00170.00160.00150.00190.00170.00200.001720.01580.01690.01700.01590.01640.01650.017230.06090.06390.06290.06010.06490.06300.0619210.00180.00160.00150.00150.00160.00150.001720.01560.01670.01730.01690.01650.01700.015930.06150.06420.06180.06200.06430.06390.0631310.00180.00190.00170.00180.00180.00180.001720.01740.01590.01650.01630.01500.01600.017730.06540.06430.06620.06730.06300.06600.0648410.00170.00160.00160.00170.00160.00150.001820.01640.01620.01540.01680.01700.01580.016630.06430.06260.06380.06630.06540.06380.0649510.00190.00180.00170.00180.00180.00180.001820.01590.01490.01520.01580.01490.01500.015130.06450.06330.06510.06510.06450.06460.0640610.00140.00180.00150.00170.00160.00160.001720.01570.01540.01570.01450.01460.01570.015230.06470.06360.06210.06380.06490.06350.0636710.00180.00180.00180.00180.00180.00180.001820.01770.01760.01760.01760.01780.01750.017830.06350.06350.06300.06300.06320.06300.0630表C.4鉛的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)Wpb/%1234567Pb110.000950.000930.000990.000970.000930.000930.0009120.00880.00900.00880.00920.00920.00900.009130.05490.05490.05630.05540.05560.05610.0553210.000800.000920.00110.000970.000900.000930.0008020.00910.00870.00890.00910.00860.00880.008930.05370.05470.05530.05690.05580.05720.0536310.000850.000870.000960.000950.000970.00100.0008420.00920.00870.00840.00820.00890.00890.008430.05670.05660.05500.05480.05310.05520.0524410.000890.000820.000760.000850.000830.000940.0009320.00960.00980.00930.00950.00960.00950.009530.05250.05270.05350.05260.05280.05300.0528510.000810.000830.000980.000920.00100.00110.001120.00830.00840.00820.00830.00830.00840.008830.05330.05340.05320.05340.05250.05290.0520610.000820.000910.000860.000820.000900.000930.0008820.00890.00890.00910.00880.00880.00870.009330.05340.05270.05320.05300.05330.05370.0537710.00100.000910.000900.000900.000910.00100.0009020.01030.01040.01040.01050.01040.01040.010430.05580.05500.05530.05680.05350.05470.0557表C.5鉍的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)WB/%1234567Bi110.00100.000940.000830.000830.000880.000870.0009320.00800.00820.00840.00800.00780.00840.008530.05110.04750.05150.05300.04960.05000.0534210.000800.000900.000840.00100.000940.000820.001020.00820.00770.00790.00870.00740.00860.007630.05360.05270.04950.04890.05160.05240.0494310.000820.000810.000870.000800.000700.000710.0007720.00880.00870.00760.00740.00740.00810.008030.05110.05110.05280.05340.05240.05110.0514410.000750.000770.000790.000770.000810.000840.0007420.00750.00750.00730.00750.00730.00780.007630.05250.05130.05220.05180.05140.05080.0519510.000820.000640.000510.000570.000580.000600.0005220.00750.00780.00770.00760.00760.00760.007630.05250.04940.05230.05260.05260.05270.0520610.000920.000980.000720.000980.000830.000970.0009120.00720.00900.00800.00780.00900.00760.008530.04900.05000.05040.05240.05300.05150.05247l0.000910.000900.000910.000910.000920.000900.0008920.00890.00900.00900.00890.00900.00900.009130.05200.05110.05190.05150.05040.05060.0506表C.6銻的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)Wsb/%1234567110.000630.000660.000620.000640.000690.000730.0007920.00740.00750.00750.00700.00710.00720.007330.05290.05300.05490.05290.05170.05430.0539210.000700.000800.000880.000700.000800.000700.0008520.00670.00750.00720.00730.00660.00700.007330.05320.05510.05460.05390.05270.05370.0530310.000720.000610.000670.000690.000700.000620.0006320.00710.00680.00710.00630.00710.00650.007130.05100.05250.05560.05280.05320.05530.0547410.000610.000570.000550.000580.000620.000630.0005720.00760.00770.00710.00740.00750.00760.007630.05330.05460.05550.05520.05460.05340.0543510.000710.000740.000770.000740.000690.000700.0006820.00740.00750.00750.00760.00690.00720.006930.05080.05210.05390.05390.05320.05260.0529610.000660.000710.000620.000640.000610.000760.0006420.00770.00770.00780.00740.00730.00720.007530.05470.05400.05420.05250.05380.05280.0547710.000670.000890.000750.000710.000750.000740.0007520.00690.00730.00720.00710.00720.00710.007130.05400.05340.05330.05340.05410.05410.0540表C.7鎂的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)WMg/%1234567Mg110.000210.000210.000180.000190.000240.000230.0001820.00990.00990.00990.00990.00950.01050.009730.04420.04700.04620.04500.04680.04770.0480210.000300.000200.000300.000200.000300.000300.0003020.00990.01020.01040.00990.00990.01010.009930.04510.04550.04600.04710.04690.04590.0466310.000220.000180.000210.000160.000260.000200.0002120.00970.00990.010-00.00970.010-00.00970.009330.04700.04890.05070.05020.04800.04920.0503410.000280.000240.000250.000290.000280.000290.0002620.01010.01020.00980.01040.01010.01030.010330.05010.05090.05020.05000.05020.05030.0501510.000190.000200.000190.000180.000180.000180.0001820.01070.01060.01080.01070.01080.01080.010630.04570.04500.04630.04690.04560.04620.0462610.000310.000220.000230.000210.000220.000230.0003420.00990.00980.00930.00920.00950.01000.009930.04740.04610.04700.04350.04530.04750.0455710.000230.000250.000240.000250.000230.000220.0002420.00920.00910.00910.00920.00930.00920.009230.04800.04700.04720.04770.04710.04730.0485表C.8鎳的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)12345671123212331234123512361237123表C.9錳的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)WMn/%1234567Mn110.00110.00110.00100.00100.00110.00100.001020.00960.00970.00980.00960.00960.00950.009030.05550.05530.05410.05440.05420.05520.0541210.00100.00100.000960.00110.00110.00100.0009720.00920.00940.01000.00970.00960.00970.009230.05350.05450.05610.05520.05360.05500.0538310.00110.00100.000940.000980.00100.00100.0009920.00900.00950.00920.00950.00920.00930.009130.05690.05540.05380.05280.05520.05480.0552410.000930.000870.000890.000940.000910.000970.0009120.00860.00860.00840.00870.00860.00910.008630.05150.05150.05130.05140.05210.05190.0521510.000780.000920.000880.000870.000870.000870.0008720.00860.00840.00840.00840.00840.00850.008530.05260.05310.05330.05350.05270.05270.0532610.000820.000810.000830.000810.000910.000900.0008920.00900.00920.00900.00950.00910.00910.009230.05290.05140.05320.05140.05230.05380.0523710.000810.000840.000810.000800.000830.000800.0008020.00980.00970.00970.00970.00990.00990.009930.05480.05530.05450.05520.05460.05530.0550GB/T11066.12—2024表C.10鈀的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)Wpa/%1234567Pd110.000840.000900.000820.000880.000830.000920.0008320.00830.00840.00780.00810.00820.00830.008530.05310.05180.05600.05370.05090.05490.0538210.000900.000870.000860.000850.000910.000940.0009220.00840.00890.00930.00870.00840.00850.008730.05260.04990.05330.05380.05510.05490.0531310.000780.000810.000780.000780.000810.000770.0007220.00830.00820.00820.00810.00840.00810.008130.05490.05510.05460.05350.05350.05270.0534410.000920.000950.000860.000910.000860.000880.0008920.00860.00850.00860.00880.00860.00850.008530.05510.05570.05480.05380.05520.05420.0535510.000900.000860.000910.000890.000860.000850.0008420.00840.00810.00850.00860.00810.00820.008030.05270.05480.05440.05560.05500.05530.0546610.000860.000810.000840.000820.000810.000910.0008320.00840.00810.00790.00840.00810.00820.007930.05330.05290.05270.05190.05370.05350.0536710.000810.000770.000670.000760.000690.000700.0007120.00820.00820.00800.00810.00820.00810.008230.05300.05290.05290.05350.05290.05320.0527表C.11鉻的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)Wcr/%1234567110.000230.000260.000230.000260.000210.000280.0002220.00950.00940.00950.00960.00900.00930.009430.05700.05900.05750.05690.05690.05600.0580210.000380.000350.000360.000390.000410.000430.0004020.00980.00950.00960.00970.00980.00970.009730.05430.05730.05610.05650.05860.05780.0591310.000220.000260.000280.000290.000250.000240.0002920.00930.00910.00870.00860.00930.00920.009030.05730.05900.05870.05820.05810.05770.0573410.000330.000350.000310.000290.000340.000330.0003320.00890.00880.00870.00910.00870.00890.008730.05600.05660.05580.05540.05620.05580.0558510.000310.000310.000310.000330.000320.000330.0003220.00890.00870.00900.00890.00880.00890.008930.05890.05490.05730.05720.05590.05610.0555610.000220.000230.000240.000170.000180.000190.0002920.00940.00940.00920.00930.00940.00970.009630.05460.05530.05490.05510.05300.05460.0526710.000410.000410.000520.000510.000500.000450.0004220.01060.01050.01040.01050.01070.010-50.010730.05760.05720.05770.05750.05750.05800.0572GB/T11066.12—2024表C.12鉑的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)Wp/%1234567Pt110.000920.000920.000920.000930.000870.000930.0009120.00850.00860.00860.00840.00820.00800.007930.06160.06170.06250.06270.06380.06000.0638210.000900.00100.00100.000900.000900.00110.0009020.00860.00910.00790.00860.00850.00810.008730.06340.06290.06220.06410.06130.06270.0623310.00100.000980.000700.000780.000790.000800.0007820.00870.00850.00790.00830.00760.00770.007930.06390.06370.06180.06140.06210.06360.0639410.000700.000680.000720.000730.000710.000720.0007120.00770.00760.00770.00800.00790.00790.007930.06150.06160.06120.06110.06130.06160.0613510.000810.000830.000910.000800.000840.000790.0007020.00840.00860.00850.00870.00800.00830.008030.05980.06000.06040.05970.06010.05960.0600610.000710.000720.000740.000840.000710.000810.0007820.00780.00800.00790.00820.00830.00800.008230.06210.06140.060-00.06120.06110.06080.0608710.000890.00100.00110.000920.000890.000890.0008920.00840.00860.00830.00820.00810.00830.008330.06140.06190.06320.06090.06160.06180.0617GB/T11066.12—2024表C.13銠的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)WRb/%1234567110.000840.000880.000820.000830.000810.000800.0007920.00820.00830.00830.00790.00790.00830.008030.04250.04340.04400.04270.04350.04380.0448210.000850.000870.000880.000840.000890.000840.0008620.00880.00890.00890.00900.00900.00890.008930.04360.04220.04320.04370.04480.04190.0439310.000940.000810.000800.000800.000820.000840.0007920.00880.00850.00770.00750.00850.00820.007430.04110.04270.04540.04540.04150.04170.0411410.000930.000910.000860.000880.000890.000870.0008620.00830.00850.00830.00850.00820.00850.008330.04050.04020.03970.04030.04080.04040.0407510.000850.000800.000770.000830.000830.000790.0007620.00810.00810.00800.00820.00770.00790.007630.04230.04320.04230.04210.04200.04200.0453610.000820.000810.000840.000820.000770.000820.0008120.00890.00830.00870.00800.00800.00810.008730.04460.04480.04500.04290.04270.04200.0456710.000810.000800.000810.000810.000810.000800.0008320.00840.00850.00840.00850.00850.00840.008530.04430.04400.04470.04470.04490.04450.0442GB/T11066.12—2024表C.14鈦的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)Wπi/%1234567110.000240.000240.000250.000260.000220.000200.0002420.00980.00990.01040.00930.00980.00990.009630.04720.04890.04790.04950.04900.05030.0486210.000200.000200.000290.000290.000200.000200.0003020.01090.01040.00960.00990.00990.01010.009730.04880.04790.04750.04910.04890.04920.0478310.000270.000250.000300.000320.000300.000310.0003120.00990.01040.00990.00980.01020.00990.010130.04930.04950.04760.04850.04960.04950.0496410.000310.000320.000330.000340.000330.000350.0003420.01020.01010.01020.00990.01000.01020.010230.05050.05010.05070.05020.05040.05020.0501510.000280.000270.000270.000270.000270.000270.0002720.00970.00950.00940.00940.00950.00940.009630.04870.04600.04780.04710.04780.04810.0475610.000250.000310.000220.000340.000210.000230.0002620.00890.00880.00920.00980.00880.00920.009330.04660.04680.04730.04730.04680.04700.0478710.000280.000260.000250.000280.000270.000240.0002820.00940.00960.00950.00970.00970.00980.009830.04920.04900.04990.04990.04830.04990.0486GB/T11066.12—2024表C.15鋅的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)Wz/%1234567110.000930.000940.000900.000970.000930.000880.0008720.00870.00870.00890.00820.00840.00860.008530.05360.05180.05560.05410.05380.05620.0582210.000850.000900.000870.000930.000890.000950.0009420.00880.00880.00890.00860.00860.00870.008730.05190.05710.05380.05500.05620.05480.0560310.000960.000930.000940.000880.000880.000880.0009220.00880.00860.00910.00920.00840.00840.009030.05200.05490.05520.05330.05370.05510.0568410.000750.000810.000770.000840.000810.000860.0007420.00800.00800.00780.00820.00830.00820.007930.05430.05350.05380.05380.05400.05320.0529510.000840.000790.000790.000800.000790.000790.0008320.00790.00790.00780.00780.00790.00790.007930.05280.05460.05480.05470.05470.05400.0537610.000850.000820.000810.000770.000710.000790.0008220.00880.00820.00830.00860.00860.00830.008230.05370.05400.05180.05240.05570.05350.0548710.000910.000910.000930.000910.000900.000910.0009020.00900.00900.00900.00900.00910.00890.009030.05570.05580.05550.05520.05550.05570.0554GB/T11066.12—2024表C.16砷的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)WAs/%1234567As110.000600.000560.000620.000600.000540.000450.0006620.01080.01050.01070.00950.00920.00980.009530.05160.05080.04900.05160.05100.04860.0506210.000800.000600.000520.000700.000600.000500.0007020.00960.00860.01030.00980.01040.00930.010230.04990.04960.05020.05050.05060.04950.0506310.000580.000600.000600.000540.000560.000550.0005420.01040.01050.01000.01010.00990.01000.011030.05050.05290.04980.05100.05060.05110.0508410.000560.000540.000550.000580.000610.000580.0005520.01010.00990.01000.01020.00980.00990.010130.04700.04570.04720.04700.04750.04710.0468510.000640.000520.000580.000430.000470.000470.0005920.01000.01010.01010.00990.01010.01010.010030.04910.04990.05000.05110.04990.05100.0501610.000710.000720.000450.000630.000540.000510.0005520.01030.01020.00920.01010.01020.01070.010730.04870.04980.04750.04780.05060.04960.0483710.000410.000400.000410.000420.000410.000400.0004020.00920.00920.00910.00930.00940.00920.009330.05170.05150.05110.05110.05150.05190.0520GB/T11066.12—2024表C.17錫的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)Ws,/%1234567110.000820.000780.000790.000830.000760.000730.0007320.00760.00760.00760.00730.00680.00690.007330.05310.05160.05390.05320.05260.05190.0519210.000800.000800.000800.000800.000800.000700.0007020.00780.00750.00650.00710.00700.00630.007030.05450.05260.05180.05540.05530.05340.0543310.000740.000680.000670.000730.000710.000680.0007220.00800.00750.00700.00770.00720.00740.008230.05200.05400.05430.05160.05290.05560.0556410.000880.000850.000810.000870.000850.000910.0008320.00730.00760.00750.00760.00770.00770.007530.05550.05490.05550.05500.05340.05390.0531510.000800.000730.000780.000760.000720.000720.0008420.00740.00750.00760.00760.00700.00710.007230.05310.05670.05570.05510.05540.05500.0547610.000720.000710.000820.000750.000710.000770.0008820.00720.00700.00680.00670.00730.00720.007230.05220.05500.05460.05270.05340.05280.0529710.000810.000800.000800.000800.000810.000810.0008020.00700.00730.00770.00710.00700.00710.007730.05370.05370.05350.05310.05360.05310.0534GB/T11066.12—2024表C.18硅的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)Wsi/%1234567110.000300.000380.000220.000270.000230.000360.0002420.00840.00850.00940.00940.00870.00890.009030.04680.04800.05020.04950.04790.04620.0486210.000300.000300.000210.000410.000300.000300.0002020.00920.00950.00870.00960.00870.00870.008930.04880.04790.04740.04900.04710.04800.0469310.000450.000500.000440.000330.000310.000290.0004220.00900.00900.00960.00930.00910.00920.008630.04850.04650.04710.05120.04820.04880.0476410.000330.000320.000300.000340.000310.000350.0003420.01040.01010.01010.00990.01040.01010.010230.05050.05010.05030.05010.05090.05040.0501510.000270.000310.000310.000280.000330.000310.0003220.00880.00870.00880.00880.00870.00890.008530.04710.04690.04800.04700.04660.04690.0466610.000210.000330.000320.000240.000310.000350.0003220.00930.00930.00930.00870.00920.00960.008630.04840.04770.04680.04810.04860.04560.0472710.000300.000320.000300.000310.000280.000300.0002920.00880.00800.00820.00830.00830.00840.008430.04740.04620.04760.04700.04810.04810.0479GB/T11066.12—2024表C.19鈷的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)Wc。/%1234567110.000920.000880.000900.000870.000860.000920.0009620.00880.00870.00860.00800.00880.00840.008230.05420.05290.05580.05430.05360.05490.0545210.000800.000790.000760.000870.000810.000850.0008220.00840.00810.00850.00880.00840.00860.008330.05610.05530.05400.05370.05350.05520.0524310.000750.000790.000820.000820.000850.000870.0007520.00850.00820.00820.00810.00860.00860.008430.05490.05380.05480.05220.05380.05520.0535410.000730.000750.000770.000750.000820.000740.0007320.00760.00790.00840.00790.00790.00780.007930.05290.05470.05470.05350.05280.05410.0537510.000790.000840.000790.000780.000790.000790.0007920.00790.00790.00800.00790.00800.00800.008130.05410.05300.05480.05500.05510.05510.0546610.000710.000680.000720.000710.000660.000720.0007920.00740.00740.00740.00790.00760.00760.007630.05380.05420.05370.05250.05470.05340.0527710.000830.000840.000830.000780.000790.000790.0007920.00870.00870.00870.00810.00880.00870.008730.05510.05410.05450.05440.05370.05400.0545GB/T11066.12—2024表C.20鈣的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)Wc./%12345671123212331234123512361237123GB/T11066.12—2024表C.21鉀的精密度試驗(yàn)原始數(shù)據(jù)元素實(shí)驗(yàn)室水平數(shù)Wk/%1234567K110.000220.000220.000270.000330.000320.000270.0002920.01080.00950.01160.01010.01050.01060.009630.05000.04760.05330.04940.04700.04800.0510210.000300.000400.000300.000500.000300.000400.0004020.01220.01170.01110.01130