GB-T 43901-2024 鎳鐵 砷、錫、銻、鉛和鉍含量 電感耦合等離子體質(zhì)譜法（ICP-MS）

ICS77.100CCSH11中華人民共和國(guó)國(guó)家標(biāo)準(zhǔn)GB/T43901—2024電感耦合等離子體質(zhì)譜法(ICP-MS)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)ⅠGB/T43901—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。請(qǐng)注意本文件的某些內(nèi)容可能涉及專(zhuān)利。本文件的發(fā)布機(jī)構(gòu)不承擔(dān)識(shí)別專(zhuān)利的責(zé)任。本文件由中國(guó)鋼鐵工業(yè)協(xié)會(huì)提出。本文件由全國(guó)生鐵及鐵合金標(biāo)準(zhǔn)化技術(shù)委員會(huì)(SAC/TC318)歸口。本文件起草單位:山西太鋼不銹鋼股份有限公司、廣東邦普循環(huán)科技有限公司、青島博正檢驗(yàn)技術(shù)有限公司、廣東中南鋼鐵股份有限公司、內(nèi)蒙古新太實(shí)業(yè)集團(tuán)有限公司、石家莊創(chuàng)譜科技有限公司、青島德泓謹(jǐn)信科技有限公司、吉鐵鐵合金有限責(zé)任公司、河北津西國(guó)際貿(mào)易有限公司、冶金工業(yè)信息標(biāo)準(zhǔn)研究院。1GB/T43901—2024電感耦合等離子體質(zhì)譜法(ICP-MS)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?并保證符合國(guó)家有關(guān)法規(guī)規(guī)定的條件。1范圍本文件描述了鎳鐵中砷、錫、銻、鉛和鉍含量的電感耦合等離子體質(zhì)譜法分析方法。本文件適用于鎳鐵中砷、錫、銻、鉛和鉍含量的測(cè)定。各元素的測(cè)定范圍見(jiàn)表1。表1元素及測(cè)定范圍元素測(cè)定范圍(質(zhì)量分?jǐn)?shù))/%As0.0005~0.01Sn0.0002~0.009Sb0.0002~0.01Pb0.0001~0.008Bi0.00004~0.00352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。GB/T6379.1測(cè)量方法與結(jié)果的準(zhǔn)確度(正確度與精密度)第1部分:總則與定義GB/T6379.2測(cè)量方法與結(jié)果的準(zhǔn)確度(正確度與精密度)第2部分:確定標(biāo)準(zhǔn)測(cè)量方法重復(fù)性與再現(xiàn)性的基本方法GB/T6682分析實(shí)驗(yàn)室用水規(guī)格和試驗(yàn)方法GB/T8170數(shù)值修約規(guī)則與極限數(shù)值的表示和判定GB/T12806實(shí)驗(yàn)室玻璃儀器單標(biāo)線(xiàn)容量瓶GB/T12808實(shí)驗(yàn)室玻璃儀器單標(biāo)線(xiàn)吸量管GB/T25050鎳鐵錠或塊成分分析用樣品的采取GB/T25051鎳鐵顆粒成分分析用樣品的采取3術(shù)語(yǔ)和定義本文件沒(méi)有需要界定的術(shù)語(yǔ)和定義。2GB/T43901—20244原理試料用稀硝酸分解,以氬等離子體為離子化源,使用電感耦合等離子體質(zhì)譜儀測(cè)定砷、錫、銻、鉛和鉍,測(cè)定時(shí)以釔作為內(nèi)標(biāo)元素(亦可采用其他合適的內(nèi)標(biāo)元素或混合內(nèi)標(biāo))進(jìn)行校正。5試劑除非另有說(shuō)明,在分析中僅使用各待測(cè)元素質(zhì)量分?jǐn)?shù)均低于0.0001%的高純?cè)噭┖透呒兯?符合GB/T6682中實(shí)驗(yàn)室用水一級(jí)水規(guī)格,同時(shí)電阻率不小于18MΩ/cm)。在分析中使用的標(biāo)準(zhǔn)溶液可以按本文件規(guī)定的方法配制,也可采用市售的有證溶液標(biāo)準(zhǔn)物質(zhì)/標(biāo)準(zhǔn)樣品。5.1高純鎳。砷、錫、銻和鉛元素質(zhì)量分?jǐn)?shù)均小于0.0001%,鉍元素質(zhì)量分?jǐn)?shù)小于0.00004%。5.2高純鐵。砷、錫、銻和鉛元素質(zhì)量分?jǐn)?shù)均小于0.0001%,鉍元素質(zhì)量分?jǐn)?shù)小于0.00004%。5.3鹽酸,ρ≈1.19g/mL。5.4硝酸,ρ≈1.42g/mL。5.5氫氟酸,ρ≈1.15g/mL。5.6鹽酸溶液(1+1)。5.7硝酸溶液(1+1)。5.8硝酸溶液(1+3)。5.9鹽酸溶液(1+9)。5.10硝酸溶液(1+9)。5.11砷標(biāo)準(zhǔn)儲(chǔ)備溶液,1mg/mL。稱(chēng)取1.0000g單質(zhì)砷(質(zhì)量分?jǐn)?shù)不小于99.99%),置于300mL燒杯中,慢慢加入50mL硝酸溶液(5.7),低溫加熱溶解后,轉(zhuǎn)至1000mL容量瓶中,以水稀至刻度,混勻。此溶液1mL含1mg砷。5.12錫標(biāo)準(zhǔn)儲(chǔ)備溶液,1mg/mL。稱(chēng)1.0000g金屬錫(質(zhì)量分?jǐn)?shù)不小于99.99%),移入一個(gè)300mL燒杯中,加入50mL鹽酸溶液(5.6),加熱溶解,冷至室溫,轉(zhuǎn)移入1000mL容量瓶中,用鹽酸溶液(5.9)稀釋至刻度,混勻。用水稀釋至刻度,混勻。此溶液1mL含1mg錫。5.13銻標(biāo)準(zhǔn)儲(chǔ)備溶液,1mg/mL。稱(chēng)取1.0000g金屬銻(質(zhì)量分?jǐn)?shù)不小于99.99%),加50mL鹽酸(5.3)微熱溶解后,轉(zhuǎn)至1000mL容量瓶中,以水稀至刻度,混勻。此溶液1mL含1mg銻。5.14鉛標(biāo)準(zhǔn)儲(chǔ)備溶液,1mg/mL。稱(chēng)取1.0000g金屬鉛(質(zhì)量分?jǐn)?shù)不小于99.99%),置于300mL燒杯中,慢慢加入50mL硝酸溶液(5.7),煮沸,趕盡氮氧化物,冷卻后移入1000mL容量瓶中,用水稀釋至刻度,混勻。此溶液1mL含1mg鉛。5.15鉍標(biāo)準(zhǔn)儲(chǔ)備溶液,1mg/mL。稱(chēng)取1.0000g金屬鉍(質(zhì)量分?jǐn)?shù)不小于99.99%),置于300mL燒杯中,慢慢加入50mL硝酸溶液(5.7),加熱溶解,取下稍冷,移入1000mL容量瓶中,用硝酸溶液(5.10)稀釋至刻度,混勻。此溶液1mL含1mg鉍。5.16混合標(biāo)準(zhǔn)溶液A,砷、錫、銻和鉛元素各10μg/mL,鉍元素5μg/mL。分別移取10.00mL砷標(biāo)準(zhǔn)儲(chǔ)備溶液(5.11)、錫標(biāo)準(zhǔn)儲(chǔ)備溶液(5.12)、銻標(biāo)準(zhǔn)儲(chǔ)備溶液(5.13)、鉛標(biāo)準(zhǔn)儲(chǔ)備溶液(5.14);移取5.00mL鉍標(biāo)準(zhǔn)儲(chǔ)備溶液(5.15)于一個(gè)1000mL容量瓶中。加入20mL硝酸(5.4),用水稀釋至刻度,混勻。此溶液1mL含砷、錫、銻、鉛元素各10μg,含鉍元素為5μg。3GB/T43901—20245.17混合標(biāo)準(zhǔn)溶液B,砷、錫、銻、鉛元素各1μg/mL,鉍元素0.5μg/mL。分別移取10.00mL混合標(biāo)準(zhǔn)溶液A(5.16)于一個(gè)100mL容量瓶中,加入2mL硝酸(5.4),用水稀釋至刻度,混勻。此溶液1mL含砷、錫、銻和鉛元素各1μg,含鉍元素為0.5μg。5.18釔標(biāo)準(zhǔn)溶液。a)釔標(biāo)準(zhǔn)儲(chǔ)備溶液,1mg/mL。稱(chēng)取0.1270g純氧化釔(Y2O3質(zhì)量分?jǐn)?shù)不小于99.99%),置于300mL燒杯中,加入20mL硝酸溶液(5.7),待完全溶解后,冷卻,移入100mL容量瓶中,用水稀釋至刻度,混勻。此溶液1mL含1mg釔。b)釔標(biāo)準(zhǔn)溶液,100μg/mL。移取10.00mL釔標(biāo)準(zhǔn)儲(chǔ)備溶液[5.18a)]于一個(gè)100mL容量瓶中,加入2mL硝酸(5.4),用水稀釋至刻度,混勻。此溶液1mL含釔100μg。c)釔標(biāo)準(zhǔn)溶液,1μg/mL。移取10.00mL釔標(biāo)準(zhǔn)溶液[5.18b)]于一個(gè)1000mL容量瓶中,加入20mL硝酸(5.4),用水稀釋至刻度,混勻。此溶液1mL含釔1μg。5.19釔內(nèi)標(biāo)溶液,50ng/mL。移取50.00mL釔標(biāo)準(zhǔn)溶液[5.18c)]于一個(gè)1000mL容量瓶中,用水稀釋至刻度,加入20mL硝酸(5.4),混勻。此溶液1mL含釔50ng。5.20鎳基體溶液,10mg/mL。稱(chēng)取1.0g高純鎳(5.1),精確至0.001g,置于300mL燒杯中,加入50mL硝酸溶液(5.7),待完全溶解后,冷卻,移入100mL容量瓶中,用水稀釋至刻度,混勻。此溶液1mL含10mg鎳。5.21鐵基體溶液,10mg/mL。稱(chēng)取1.0g高純鐵粉(5.2),精確至0.001g,置于300mL燒杯中,加入50mL硝酸溶液(5.7),待完全溶解后,冷卻,移入100mL容量瓶中,用水稀釋至刻度,混勻。此溶液1mL含10mg鐵。5.22氬氣,純度大于99.99%。6儀器和設(shè)備6.1實(shí)驗(yàn)室玻璃儀器GB/T12808規(guī)定的A級(jí)。所有玻璃器皿應(yīng)用鹽酸溶液(5.9)清洗,然后再用水洗凈。6.2電感耦合等離子體質(zhì)譜儀6.2.1測(cè)定同位素的推薦參數(shù)配備有磁扇式電感耦合等離子質(zhì)譜儀(高分辨電感耦合等離子質(zhì)譜儀)或四極桿電感耦合等離子質(zhì)譜儀(低分辨電感耦合等離子質(zhì)譜儀)或飛行時(shí)間電感耦合等離子質(zhì)譜儀。依據(jù)儀器使用說(shuō)明書(shū)建立分析程序,按照表2選擇待測(cè)元素和內(nèi)標(biāo)元素的測(cè)定同位素。砷、錫、銻、鉛和鉍的同位素豐度及干擾見(jiàn)附錄C。4GB/T43901—2024表2各元素測(cè)定同位素的推薦質(zhì)量數(shù)、內(nèi)標(biāo)元素的同位素質(zhì)量數(shù)、豐度元素測(cè)定同位素及質(zhì)量數(shù)豐度%As75As100Sn118Sn24.3120Sn32.4Sb121SbPb208PbBi209Bi100Y(內(nèi)標(biāo))89Y100在儀器最佳工作條件下,凡能達(dá)到6.2.2和6.2.3指標(biāo)者均可使用。6.2.2最小精度(RSD)測(cè)量濃度為10ng/mL或5ng/mL的待測(cè)元素的基體匹配標(biāo)準(zhǔn)溶液,計(jì)算連續(xù)10次測(cè)量結(jié)果的相對(duì)標(biāo)準(zhǔn)偏差,最小精度(RSD)應(yīng)不超過(guò)5%。6.2.3檢出限(LOD)和定量限(LOQ)檢出限(LOD)和定量限(LOQ)定義分別如式(1)和式(2)。LOD=4.65×σ×…………(1)LOQ=14.1×σ×…………(2)式中:σ—測(cè)量10次空白溶液強(qiáng)度的標(biāo)準(zhǔn)偏差;Cs—標(biāo)準(zhǔn)溶液的濃度,單位納克每毫升(ng/mL);Xs—測(cè)量10次標(biāo)準(zhǔn)溶液的平均強(qiáng)度;Xb—測(cè)量10次空白溶液的平均強(qiáng)度。測(cè)量基體和酸度與試液一致的空白溶液10次,計(jì)算各元素檢出限和定量限。砷元素的檢出限應(yīng)小于0.8ng/mL,定量限應(yīng)小于2.4ng/mL。錫、銻、鉛元素的檢出限應(yīng)小于0.3ng/mL,定量限應(yīng)小于0.9ng/mL。鉍元素的檢出限應(yīng)小于0.1ng/mL,定量限應(yīng)小于0.3ng/mL。7取樣和樣品制備7.1按照GB/T25050或GB/T25051的規(guī)定取樣。7.2實(shí)驗(yàn)室樣品通常以鉆、銑或磨加工而成,屑、粉或顆粒狀樣品不需再加工。注1:如懷疑在鉆、銑或磨過(guò)程中樣品沾上油或油脂,用高純度丙酮清洗后晾干。注2:如實(shí)驗(yàn)室樣品粒度不均勻,測(cè)試樣品采用分樣器縮分出來(lái)。5GB/T43901—20248分析步驟8.1試料稱(chēng)取0.10g試樣(7.2),精確至0.0001g,置于150mL錐形瓶中。8.2測(cè)定次數(shù)對(duì)同一個(gè)試樣至少進(jìn)行兩次獨(dú)立分析。8.3空白試驗(yàn)隨同試料做空白試驗(yàn)?？瞻自囼?yàn)應(yīng)使用相當(dāng)于試料中的鎳和鐵量的高純鎳(5.1)和高純鐵(5.2)的代替試料。8.4試液的制備將稱(chēng)有試料(8.1)的錐形瓶中加入10mL硝酸溶液(5.8),低溫加熱至完全溶解,冷卻至室溫,轉(zhuǎn)移至100mL的容量瓶中,用水稀釋至刻度,混勻。此溶液為待測(cè)試液。注1:高硅試樣可加3滴~5滴氫氟酸(5.5)助溶。有些高碳樣品可能會(huì)有殘余碳不溶,定容100mL后用快速濾紙干過(guò)濾。注2:如使用離線(xiàn)內(nèi)標(biāo)校正法,則在空白和試樣溶液稀釋至刻度前加入5.00mL的釔標(biāo)準(zhǔn)溶液[5.18c)]。8.5校準(zhǔn)系列溶液的配制按照樣品含鎳量的高低分別配置不同鎳和鐵比例的三組標(biāo)準(zhǔn)系列,每組制備1份校準(zhǔn)空白溶液和5份校準(zhǔn)標(biāo)準(zhǔn)溶液。每組分別將約50mL水加入6個(gè)100mL容量瓶中,按表3加入鎳基體溶液、鐵基體溶液、多元素混合標(biāo)準(zhǔn)溶液,加入硝酸(5.4)2.0mL,用水稀釋至刻度,混勻。表3多元素混合校準(zhǔn)空白溶液和校準(zhǔn)溶液鎳鐵牌號(hào)(含鎳量)加入鎳基體溶液量(5.20)mL加入鐵基體溶液量(5.21)mL加入多元素混合標(biāo)準(zhǔn)溶液B(5.17)mL校準(zhǔn)系列溶液中元素濃度ng/mL校準(zhǔn)系列溶液中鉍元素濃度ng/mLFeNi20、FeNi30(含鎳量15%~35%)2.57.50002.57.50.5052.52.57.51.001052.57.52.50252.57.55.0050252.57.510.00100506GB/T43901—2024表3多元素混合校準(zhǔn)空白溶液和校準(zhǔn)溶液(續(xù))鎳鐵牌號(hào)(含鎳量)加入鎳基體溶液量(5.20)mL加入鐵基體溶液量(5.21)mL加入多元素混合標(biāo)準(zhǔn)溶液B(5.17)mL校準(zhǔn)系列溶液中元素濃度ng/mL校準(zhǔn)系列溶液中鉍元素濃度ng/mLFeNi40、FeNi50(含鎳量35%~60%)5.05.00005.05.00.5052.55.05.01.001055.05.02.50255.05.05.0050255.05.010.0010050FeNi70(含鎳量60%~80%)7.03.00007.03.00.5052.57.03.01.001057.03.02.50257.03.05.0050257.03.010.00100508.6測(cè)定根據(jù)待測(cè)鎳鐵樣品的含鎳量,選擇合適鎳和鐵比例的校準(zhǔn)系列溶液(見(jiàn)表3)。待電感耦合等離子體質(zhì)譜儀運(yùn)行穩(wěn)定后,于待測(cè)元素和內(nèi)標(biāo)元素質(zhì)量數(shù)處(見(jiàn)表2),依次測(cè)定標(biāo)準(zhǔn)系列溶液(按8.5配制)、空白試液(按8.3制備)、分析試液(按8.4制備)中待測(cè)元素和內(nèi)標(biāo)元素的離子流信號(hào)強(qiáng)度。以標(biāo)準(zhǔn)溶液中待測(cè)元素的質(zhì)量濃度為橫坐標(biāo),待測(cè)元素與內(nèi)標(biāo)元素的離子流信號(hào)強(qiáng)度比值為縱坐標(biāo),繪制校準(zhǔn)曲線(xiàn)。各元素校準(zhǔn)曲線(xiàn)相關(guān)系數(shù)應(yīng)在0.9990以上,否則需重新進(jìn)行校準(zhǔn)或重新配制標(biāo)準(zhǔn)溶液進(jìn)行標(biāo)準(zhǔn)化。測(cè)量試液中的待測(cè)元素的信號(hào)強(qiáng)度,減去空白試驗(yàn)溶液的強(qiáng)度即為凈強(qiáng)度,由工作曲線(xiàn)查得待測(cè)元素的濃度,以ng/mL計(jì)。9分析結(jié)果計(jì)算及表示9.1分析結(jié)果的計(jì)算按式(3)計(jì)算待測(cè)元素含量(ωM),以質(zhì)量分?jǐn)?shù)(%)表示。ωM=×100…………(3)式中:ρ—由校準(zhǔn)曲線(xiàn)得到的元素質(zhì)量濃度,單位為納克每毫升(ng/mL);V—試液體積,單位為毫升(mL);m—試料質(zhì)量,單位為克(g)。7GB/T43901—20249.2分析結(jié)果的確定與表示同一試樣兩次獨(dú)立分析結(jié)果差值的絕對(duì)值不大于重復(fù)性限,則取算術(shù)平均值作為分析結(jié)果。如果兩次獨(dú)立分析結(jié)果差值的絕對(duì)值大于重復(fù)性限,則按照附錄A的規(guī)定追加測(cè)量次數(shù)并確定分析結(jié)果。分析結(jié)果按GB/T8170修約,保留兩位有效數(shù)字。10精密度精密度試驗(yàn)是2022年由10個(gè)實(shí)驗(yàn)室對(duì)11個(gè)鎳鐵樣品中的砷、錫、銻、鉛和鉍5個(gè)元素進(jìn)行測(cè)定。樣品信息參見(jiàn)附錄B中的表B.1。精密度試驗(yàn)原始數(shù)據(jù)見(jiàn)附錄B的表B.2~表B.6。各實(shí)驗(yàn)室對(duì)每個(gè)樣品測(cè)試3次。在GB/T6379.1定義的可重復(fù)性條件下進(jìn)行兩次測(cè)定,第3次測(cè)定是使用同一臺(tái)儀器在不同時(shí)間,在新的校準(zhǔn)之后進(jìn)行的。按照GB/T6379.2的規(guī)則對(duì)共同精密度試驗(yàn)得到的結(jié)果數(shù)據(jù)進(jìn)行統(tǒng)計(jì)處理。各元素含量與試驗(yàn)結(jié)果的重復(fù)性限、室內(nèi)再現(xiàn)性和再現(xiàn)性限的函數(shù)關(guān)系式見(jiàn)表4。表4精密度函數(shù)關(guān)系式元素水平范圍/%重復(fù)性/%室內(nèi)再現(xiàn)性/%再現(xiàn)性/%As0.0005~0.01lgr=0.7373lgm-1.8188lgRw=0.6250lgm-1.9201lgR=0.7764lgm-1.1591Sn0.0002~0.009lgr=0.7114lgm-2.1515lgRw=0.7500lgm-1.8152lgR=0.7366lgm-1.3063Sb0.0002~0.01lgr=0.6713lgm-2.0387lgRw=0.7960lgm-1.4395lgR=0.5474lgm-1.7219Pb0.0001~0.008lgr=0.7461lgm-1.9415lgRw=0.8185lgm-1.5183lgR=0.7215lgm-1.2785Bi0.00004~0.0035lgr=0.6947lgm-1.9802R=0.1029m+0.000015lgR=0.7360lgm-1.3256由精密度函數(shù)關(guān)系式計(jì)算得出的各元素均勻分布含量的重復(fù)性限、再現(xiàn)性限值見(jiàn)表5。表5均勻分布含量的重復(fù)性限(r)和再現(xiàn)性限(Rw和R)元素m/%r/%Rw/%R/%As0.00050.0000560.000100.000190.00100.0000930.000160.000320.00300.000210.000320.000760.00500.000310.000440.00110.00700.000390.000540.00150.00900.000470.000630.00180.0100.000510.000680.0019Sn0.00020.0000160.0000260.0000930.00050.0000320.0000510.0001830.00100.0000520.0000860.0003050.00300.000110.000200.000680.00500.000160.000290.00100.00700.000210.000370.00130.00900.000250.000450.00158GB/T43901—2024表5均勻分布含量的重復(fù)性限(r)和再現(xiàn)性限(Rw和R)(續(xù))元素m/%r/%Rw/%R/%Sb0.00020.000030.000040.000180.00050.000060.000090.000300.00100.000090.000150.000430.00300.000190.000360.000790.00500.000260.000540.001040.00700.000330.000700.001250.00900.000390.000860.001440.0100.000420.000930.00153Pb0.00010.0000120.0000120.000070.00050.0000390.0000480.000220.00100.0000660.0000860.000360.00200.000110.000160.000590.00400.000190.000280.000980.00600.000250.000390.00130.00800.000310.000500.0016Bi0.000040.0000090.0000190.0000270.000100.0000170.0000250.0000540.000500.0000530.0000660.000180.00100.0000860.000120.000290.00200.000140.000220.000490.00300.000180.000320.000660.00350.000210.000380.00074在重復(fù)性限(r)條件下,獲得的兩次獨(dú)立測(cè)試結(jié)果的絕對(duì)差值不大于重復(fù)性限(r),以大于重復(fù)性限(r)的情況不超過(guò)5%為前提。在室內(nèi)再現(xiàn)性限(Rw)條件下,獲得的兩次獨(dú)立測(cè)試結(jié)果的絕對(duì)差值不大于室內(nèi)再現(xiàn)性(Rw),以大于室內(nèi)再現(xiàn)性(Rw)的情況不超過(guò)5%為前提。在再現(xiàn)性限(R)條件下,獲得的兩次獨(dú)立測(cè)試結(jié)果的絕對(duì)差值不大于再現(xiàn)性限(R),以大于再現(xiàn)性限(R)的情況不超過(guò)5%為前提。11試驗(yàn)報(bào)告試驗(yàn)報(bào)告應(yīng)包括下列內(nèi)容:a)實(shí)驗(yàn)室的名稱(chēng)和地址;b)試驗(yàn)報(bào)告的簽發(fā)日期;c)本文件編號(hào);d)識(shí)別試樣必要的細(xì)節(jié);9GB/T43901—2024e)分析結(jié)果;f)結(jié)果的編號(hào);g)在測(cè)定過(guò)程中觀察到的異常現(xiàn)象和本文件中沒(méi)有規(guī)定的可能對(duì)試樣和認(rèn)證標(biāo)準(zhǔn)物質(zhì)的結(jié)果產(chǎn)生影響的任何操作。10GB/T43901—2024附錄A(規(guī)范性)試驗(yàn)結(jié)果接受程序流程圖試驗(yàn)結(jié)果接受程序流程圖如圖A.1所示。標(biāo)引符號(hào)說(shuō)明:r—重復(fù)性限;X—分析值。圖A.1試驗(yàn)結(jié)果接受程序流程圖2424附錄B(資料性)精密度試驗(yàn)原始數(shù)據(jù)共同精密度樣品信息如表B.1所示。精密度試驗(yàn)原始數(shù)據(jù)見(jiàn)表B.2~表B.6。表B.1共同精密度試驗(yàn)樣品信息%(質(zhì)量分?jǐn)?shù))試樣編號(hào)牌號(hào)NiAssnsbPbBiCsiPsCrCoCuNiFe-1FeNi2014.350.00240.00120.00030.00400.00351.731.390.0230.0732.291.940.094NiFe-216.810.00200.000730.00970.000140.000440.02060.01460.00490.02090.04690.3790.040NiFe-320.00.000560.000120.000220.000190.000220.00150.00170.00070.00090.00020.00020.0005NiFe-423.570.000930.00250.00340.00330.00301.4561.9030.00660.05050.750.7150.003NiFe-5FeNi3025.680.00290.00090.00090.000420.000221.162.900.0240.2651.171.560.094NiFe-634.090.00960.00610.00970.00610.00230.1680.4810.01620.00650.300.6250.04NiFe-735.80.00600.00510.00560.00220.00240.02080.02250.00490.1090.0320.800.088NiFe-8FeNi4041.60.01070.00650.000750.00540.00140.01110.01850.01480.06850.02510.8060.112NiFe-942.980.00250.00060.00170.00060.000040.0530.740.00940.0180.520.530.019NiFe-10FeNi5061.340.01040.00870.001480.00790.00110.0050.0030.0070.100.010.900.19NiFe-11FeNi7079.970.002240.000490.000880.000740.000850.0020.00250.00270.00050.00010.00070.001411GB11GB/T43901—20GBGB/T43901—202412表B.2砷(As)元素精密度試驗(yàn)原始數(shù)據(jù)12%(質(zhì)量分?jǐn)?shù))水平j(luò)測(cè)定次數(shù)n實(shí)驗(yàn)室i1234567891011230.001720.001710.001730.003590.003730.003890.003110.003110.003050.002320.002280.000530.003790.003860.003930.003370.003430.003540.002760.002700.002680.002340.002350.002460.002170.002210.0021121230.002050.002070.001950.002110.002090.002470.001910.001970.001760.001770.001830.001350.002220.002270.002200.001920.001860.001750.002050.002100.002210.001770.001980.001980.001820.001850.001760.001860.001790.0018231230.0004880.0004550.0005180.000878b0.000920b0.000797b0.0005310.0004950.0005440.0005700.0005460.0005720.0005980.0006060.0006000.0005750.0005820.0005930.000895b0.000909b0.000888b0.0006010.0005770.0006780.0005300.0005450.0005000.0005430.0005900.00054541230.0005020.0004890.0004930.001480.001340.001510.0009150.0009140.0009840.001260.001240.001110.0004350.0004300.0004260.001120.001000.001060.001440.001380.001310.0007890.0007630.0008360.0008660.0009120.0009810.0006670.0006490.00068451230.002900.002840.002860.003940.003870.003860.003280.003260.003280.004080.004050.003610.002480.002420.002430.003220.003380.003310.003950.003900.003810.003050.003140.002910.00281a0.002560.002610.0025961230.009210.009270.009030.009220.009390.009820.009770.009470.009640.009890.009770.00990.01010.01040.01030.009220.009190.008920.009570.009490.009720.009980.009730.01000.008640.008510.008850.009840.009960.0098871230.005940.005930.005820.006240.006500.006560.005590.005930.005740.005880.005820.006010.005880.005790.005700.006350.006450.006390.006380.006460.006550.006090.005730.005880.005670.005680.005370.005730.005680.005762424表B.2砷(As)元素精密度試驗(yàn)原始數(shù)據(jù)(續(xù))%(質(zhì)量分?jǐn)?shù))水平j(luò)測(cè)定次數(shù)n實(shí)驗(yàn)室i1234567891081230.008470.008370.008260.01190.01210.01250.01130.01120.01100.01120.01040.01070.01170.01150.01150.01150.01090.01160.01080.01100.01160.01160.01160.01080.01000.01010.01040.009030.009120.0090591230.002840.002890.002710.003630.003560.003480.002630.002590.002590.00221b0.00184b0.00268b0.002430.002300.002250.003110.002930.003090.003490.003560.003610.003160.002880.002940.002620.002710.002570.003020.003170.00321101230.01050.01040.01030.01110.01120.01090.01010.01050.01020.01010.01020.01010.01040.01020.01020.01080.01090.01010.01060.01080.01010.01020.01070.01020.009640.009650.009890.01030.01040.0107111230.001930.001920.002150.002460.002440.002680.002070.002140.002260.002190.002160.002240.002130.002250.002070.001930.002070.002040.002430.002390.002510.002380.002410.002210.002340.002450.002560.002410.002370.00244a數(shù)據(jù)為歧離值。b數(shù)據(jù)為離群值。13GB13GB/T43901—20GBGB/T43901—202414表B.3錫(sn)元素精密度試驗(yàn)原始數(shù)據(jù)14%(質(zhì)量分?jǐn)?shù))水平j(luò)測(cè)定次數(shù)n實(shí)驗(yàn)室i1234567891011230.001060.001120.001080.001280.001260.001250.001180.001170.001130.001290.001340.001480.0009860.0009970.0009910.001050.001150.001010.001130.001080.001160.001290.001280.001240.001360.001330.001220.001450.001460.0013421230.001010.0009930.001050.0006890.0006920.0007040.0007400.0007540.0007070.0008040.0007900.0008190.0007280.0007270.0007270.0002650.0002860.0002760.0007070.0006980.0006890.0007390.0007410.0007430.0008770.0008930.0008460.00101b31230.0001420.0001310.0001520.0001540.0001560.0001510.0001300.0001250.0001300.0001920.0001970.0001920.0001100.0001190.0001090.0001470.0001580.0001620.0001600.0001560.0001450.0001350.0001250.0001050.0002050.0002100.0001780.0001850.0001600.00016641230.002230.002180.002210.002520.002510.002580.002490.002460.002340.002670.002750.002670.002960.002910.002870.002060.002080.001970.002570.002510.002400.002370.002470.002460.002760.002890.003020.002480.002450.0024451230.0009240.0009210.0009590.0009410.0009430.0009630.0009190.0009120.0008580.001110.001080.001090.000289b0.000277b0.000273b0.0008770.0008960.0009020.0009620.0009490.0009650.0009830.0009710.0009180.00102b0.00109b0.0008630.0008500.00084361230.005980.006130.006210.005970.006010.005900.006230.006270.006080.006250.006230.006390.006090.006150.006130.006110.006240.006160.005790.005880.005970.005620.005660.006050.006330.006420.006590.006370.006410.0063871230.004890.004990.005070.005310.005330.005540.005170.005330.004840.005020.005120.005190.005230.005110.005050.004860.005010.004960.005230.005180.005350.004600.004630.004780.005660.005690.005370.004990.004950.005012424表B.3錫(sn)元素精密度試驗(yàn)原始數(shù)據(jù)(續(xù))%(質(zhì)量分?jǐn)?shù))水平j(luò)測(cè)定次數(shù)n實(shí)驗(yàn)室i1234567891081230.006880.006870.006730.006070.005990.006160.006960.006940.006980.006680.006470.006430.007100.007010.006980.00444a0.00620b0.00624b0.00531b0.006800.006700.006950.007140.007210.007000.006220.006310.0063791230.0006810.0006810.0006450.0006790.0007010.0007270.0005830.0006020.0006160.0006640.0006390.0006400.0005170.0005020.0004950.0005710.0005810.0005950.0007110.0007060.0006920.0007080.0006560.0006760.0006440.0006510.0006870.0005920.0005800.000579101230.009080.009100.009260.008690.008620.008590.008550.008510.008820.008270.008290.008480.008950.009050.008870.009190.008990.009060.008980.008860.008840.008670.008720.008790.009470.009230.009690.007580.007500.00747111230.0005110.0005080.0005140.0005800.0005880.0005690.0004960.0004900.0005010.0005420.0005360.0005520.0004840.0005030.0004900.0005010.0005230.0004990.0005720.0005610.0005890.0005210.0005110.0004940.000586b0.000623b0.000692b0.0004730.0004780.000487a數(shù)據(jù)為歧離值。b數(shù)據(jù)為離群值。15GB15GB/T43901—20GBGB/T43901—202416表B.4銻(sb)元素精密度試驗(yàn)原始數(shù)據(jù)16%(質(zhì)量分?jǐn)?shù))水平j(luò)測(cè)定次數(shù)n實(shí)驗(yàn)室i1234567891011230.0004230.0003960.0004090.000733b0.000728b0.000570b0.0004240.0004070.0003750.0004090.0004270.0004800.0002200.0002310.0002260.0004650.0004540.0004460.0006330.0006410.0006530.0006010.0006140.0006030.0003920.0003880.0003530.0003530.0003460.00034921230.01030.01020.01000.009910.009910.009900.009580.009690.009080.01000.009880.009860.0122b0.0124b0.01000.009860.009890.009800.009720.009870.009070.009330.009630.009350.009210.009140.009510.009690.0097231230.0002560.0002430.0002240.000303b0.000355b0.000493b0.0002490.0002320.0002610.0002450.0002180.0002340.0001380.0001450.0001330.0001790.0001960.0001930.0003330.0003450.0003630.0002550.0002640.0002840.0001910.0002210.0002410.0002290.0002380.00022941230.003020.002910.003180.003710.003620.003310.003550.003560.003410.003750.003930.003750.004100.004020.003960.003170.003270.003380.003380.003490.003550.002690.003090.002780.003050.003220.003450.003130.003060.0030551230.0009870.0009710.0009930.001090.001160.001210.0009670.0009470.0008580.001020.0009710.001030.000273b0.000282b0.000277b0.0008280.0008250.0007990.001050.001120.001180.001230.001100.001140.0008570.0008470.0008960.0008610.0008710.00084661230.009830.01000.01010.009130.009060.009570.01090.01080.01010.00586b0.0114b0.01050.01080.01060.008770.008670.008560.009230.009360.009410.008490.008630.009560.009730.009780.009460.01020.01030.010271230.005090.004920.005070.005660.005690.005530.00453b0.00557b0.005750.005860.005690.005790.005860.005910.005420.005540.005690.005760.005770.006580.005260.005410.005630.005280.005240.005362424表B.4銻(sb)元素精密度試驗(yàn)原始數(shù)據(jù)(續(xù))%(質(zhì)量分?jǐn)?shù))水平j(luò)測(cè)定次數(shù)n實(shí)驗(yàn)室i1234567891081230.0007210.0007040.0007310.001000.001020.0009430.0007920.0007870.0008000.0006940.0006050.0007350.0007050.0006920.0006890.001000.001090.0009890.0007690.0007430.0009670.0007710.0007590.0007890.0007180.0007030.00070791230.002010.002080.002110.002290.002210.002090.001710.001850.001860.001430.001210.001800.001450.001510.001360.001790.001860.001710.002240.002170.002250.001580.001630.002090.001770.001730.001680.001830.001820.00178101230.001770.001740.001810.001550.001530.001320.001580.001620.001660.001550.001570.001550.001080.001140.001010.001510.001670.001640.001280.001370.001450.001260.001390.001680.001560.001540.001620.001300.001390.00132111230.0009750.0009430.0009240.001100.001070.001030.0008920.0009040.0009300.0008960.0008460.0008800.000332b0.000344b0.000327b0.0009050.0008970.0009140.001040.001010.001080.0009290.0009360.0009270.0009040.0009130.0009740.0009530.0009380.000949a數(shù)據(jù)為歧離值。b數(shù)據(jù)為離群值。17GB17GB/T43901—20GBGB/T43901—202418表B.5鉛(pb)元素精密度試驗(yàn)原始數(shù)據(jù)18%(質(zhì)量分?jǐn)?shù))水平j(luò)測(cè)定次數(shù)n實(shí)驗(yàn)室i1234567891011230.004120.004240.004130.003890.003840.004120.003930.003890.004000.00487b0.00529b0.00559b0.004480.004410.004450.003950.004210.004160.003750.003680.003890.004130.003990.004390.004020.003970.003840.003890.003900.0038621230.0001780.0001840.0001560.0001660.0001680.0001750.0001130.0000970.0001110.0001410.0001430.0001470.0000820.0000850.0000830.0000960.0000980.0001020.0001780.0001690.0001800.0001300.0001080.0001000.0000950.0001130.0001340.0002310.0002600.00024131230.0002720.0003100.0002860.0003540.0003440.0003660.0002000.0001880.0001970.0003150.0003100.0003140.0002410.0002470.0002370.0001900.0001760.0001810.0003650.0003620.0003560.0001960.0002210.0001970.0002470.0022500.0002350.0002620.0002780.00026941230.003310.003380.003270.002910.002920.002850.003380.003230.003160.003130.003190.003250.002880.002890.002920.002980.003170.003400.003110.003110.003340.003330.003410.0032951230.0004470.0004540.0004320.0004730.0004790.0005110.0004000.0003980.0003700.000698b0.000615b0.000652b0.0002650.0002750.0002710.0004320.0004250.0004190.0004790.0004720.0004880.0003260.0003190.0003280.000532b0.000497b0.000424b0.0004580.0004440.00043561230.006090.006280.006150.005500.005460.005190.006160.006490.006610.007190.007170.007470.006050.005940.006010.006390.006150.006260.005470.005530.005390.005290.005270.006140.005470.005670.005990.006460.006510.0064971230.001980.002070.002160.002040.002040.001980.002260.002380.002170.002630.002500.002610.001880.001980.001910.002260.002160.002310.002140.002110.002250.001780.001920.002130.002170.002060.001860.002270.002320.002202424表B.5鉛(pb)元素精密度試驗(yàn)原始數(shù)據(jù)(續(xù))%(質(zhì)量分?jǐn)?shù))水平j(luò)測(cè)定次數(shù)n實(shí)驗(yàn)室i1234567891081230.005260.004980.005110.005080.005130.005340.006130.006120.006030.005580.005490.005300.005930.006010.005890.005420.005210.005340.005080.005010.005150.00623b0.00606b0.00721b0.004930.004960.005120.005550.005470.0055791230.0007150.0007250.0006910.0006050.0006110.0005880.0005610.0005510.0005630.0006570.0006490.0006450.0005870.0005990.0005820.0005960.0006050.0005830.0006010.0005960.0006110.0006470.0006270.0006760.000711b0.000678b0.000614b0.001490.001380.00135101230.00807b0.008770.008770.009160.007850.007730.008090.007310.007430.007450.008050.008160.008000.008860.008690.008790.008650.008710.008770.007970.008110.008170.006350.006450.006540.006430.006500.00658111230.0007000.0006930.0007570.0007010.0007140.0006770.0007330.0007340.0007430.0007320.0007060.0007240.0006240.0006330.0006240.0007370.0007470.0007360.0007010.0006920.0007090.0008680.0008380.0007520.0006640.0006680.0007150.0007630.0007520.000764a數(shù)據(jù)為歧離值。b數(shù)據(jù)為離群值。19GB19GB/T43901—20GBGB/T43901—202420表B.6鉍(Bi)元素精密度試驗(yàn)原始數(shù)據(jù)20%(質(zhì)量分?jǐn)?shù))水平j(luò)測(cè)定次數(shù)n實(shí)驗(yàn)室i1234567891011230.003210.003330.003180.003480.003440.003660.003340.003310.003440.00400b0.00441b0.00450b0.003830.003760.003710.00406a0.003530.003600.003720.003430.003320.003620.003260.003340.003490.003420.003400.0033921230.0004730.0005280.0004560.0004630.0004640.0005010.0004220.0004390.0004150.0004850.0004840.0005140.0003870.0003750.0003700.0004090.0004080.0003920.0005100.0005020.0004970.0005010.0004640.0004610.0003640.0003620.0003700.0004550.0004410.00044031230.0002000.0001780.0002200.0002440.0002410.0002570.0002280.0002160.0002250.0002400.0002360.0002420.0001840.0001960.0001810.0002580.0002450.0002350.0002650.0002540.0002430.0002300.0002470.0002300.0001920.0001830.0001680.0002330.0002230.00022341230.003060.003020.003160.002950.002960.003030.002940.0