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

ICS77.100CCSH11中華人民共和國國家標準GB/T43901—2024電感耦合等離子體質譜法(ICP-MS)國家市場監(jiān)督管理總局國家標準化管理委員會ⅠGB/T43901—2024本文件按照GB/T1.1—2020《標準化工作導則第1部分:標準化文件的結構和起草規(guī)則》的規(guī)定起草。請注意本文件的某些內容可能涉及專利。本文件的發(fā)布機構不承擔識別專利的責任。本文件由中國鋼鐵工業(yè)協(xié)會提出。本文件由全國生鐵及鐵合金標準化技術委員會(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、青島博正檢驗技術有限公司、廣東中南鋼鐵股份有限公司、內蒙古新太實業(yè)集團有限公司、石家莊創(chuàng)譜科技有限公司、青島德泓謹信科技有限公司、吉鐵鐵合金有限責任公司、河北津西國際貿易有限公司、冶金工業(yè)信息標準研究院。1GB/T43901—2024電感耦合等離子體質譜法(ICP-MS)警告—使用本文件的人員應有正規(guī)實驗室工作的實踐經(jīng)驗。本文件并未指出所有可能的安全問題。使用者有責任采取適當?shù)陌踩徒】荡胧?并保證符合國家有關法規(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、鉛和鉍含量的測定。各元素的測定范圍見表1。表1元素及測定范圍元素測定范圍(質量分數(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容通過文中的規(guī)范性引用而構成本文件必不可少的條款。其中,注日期的引用文件,僅該日期對應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測量方法與結果的準確度(正確度與精密度)第1部分:總則與定義GB/T6379.2測量方法與結果的準確度(正確度與精密度)第2部分:確定標準測量方法重復性與再現(xiàn)性的基本方法GB/T6682分析實驗室用水規(guī)格和試驗方法GB/T8170數(shù)值修約規(guī)則與極限數(shù)值的表示和判定GB/T12806實驗室玻璃儀器單標線容量瓶GB/T12808實驗室玻璃儀器單標線吸量管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術語和定義本文件沒有需要界定的術語和定義。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譜儀測定砷、錫、銻、鉛和鉍,測定時以釔作為內標元素(亦可采用其他合適的內標元素或混合內標)進行校正。5試劑除非另有說明,在分析中僅使用各待測元素質量分數(shù)均低于0.0001%的高純試劑和高純水(符合GB/T6682中實驗室用水一級水規(guī)格,同時電阻率不小于18MΩ/cm)。在分析中使用的標準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準物質/標準樣品。5.1高純鎳。砷、錫、銻和鉛元素質量分數(shù)均小于0.0001%,鉍元素質量分數(shù)小于0.00004%。5.2高純鐵。砷、錫、銻和鉛元素質量分數(shù)均小于0.0001%,鉍元素質量分數(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砷標準儲備溶液,1mg/mL。稱取1.0000g單質砷(質量分數(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錫標準儲備溶液,1mg/mL。稱1.0000g金屬錫(質量分數(shù)不小于99.99%),移入一個300mL燒杯中,加入50mL鹽酸溶液(5.6),加熱溶解,冷至室溫,轉移入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銻標準儲備溶液,1mg/mL。稱取1.0000g金屬銻(質量分數(shù)不小于99.99%),加50mL鹽酸(5.3)微熱溶解后,轉至1000mL容量瓶中,以水稀至刻度,混勻。此溶液1mL含1mg銻。5.14鉛標準儲備溶液,1mg/mL。稱取1.0000g金屬鉛(質量分數(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鉍標準儲備溶液,1mg/mL。稱取1.0000g金屬鉍(質量分數(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混合標準溶液A,砷、錫、銻和鉛元素各10μg/mL,鉍元素5μg/mL。分別移取10.00mL砷標準儲備溶液(5.11)、錫標準儲備溶液(5.12)、銻標準儲備溶液(5.13)、鉛標準儲備溶液(5.14);移取5.00mL鉍標準儲備溶液(5.15)于一個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混合標準溶液B,砷、錫、銻、鉛元素各1μg/mL,鉍元素0.5μg/mL。分別移取10.00mL混合標準溶液A(5.16)于一個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釔標準溶液。a)釔標準儲備溶液,1mg/mL。稱取0.1270g純氧化釔(Y2O3質量分數(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)釔標準溶液,100μg/mL。移取10.00mL釔標準儲備溶液[5.18a)]于一個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)釔標準溶液,1μg/mL。移取10.00mL釔標準溶液[5.18b)]于一個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釔內標溶液,50ng/mL。移取50.00mL釔標準溶液[5.18c)]于一個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儀器和設備6.1實驗室玻璃儀器GB/T12808規(guī)定的A級。所有玻璃器皿應用鹽酸溶液(5.9)清洗,然后再用水洗凈。6.2電感耦合等離子體質譜儀6.2.1測定同位素的推薦參數(shù)配備有磁扇式電感耦合等離子質譜儀(高分辨電感耦合等離子質譜儀)或四極桿電感耦合等離子質譜儀(低分辨電感耦合等離子質譜儀)或飛行時間電感耦合等離子質譜儀。依據(jù)儀器使用說明書建立分析程序,按照表2選擇待測元素和內標元素的測定同位素。砷、錫、銻、鉛和鉍的同位素豐度及干擾見附錄C。4GB/T43901—2024表2各元素測定同位素的推薦質量數(shù)、內標元素的同位素質量數(shù)、豐度元素測定同位素及質量數(shù)豐度%As75As100Sn118Sn24.3120Sn32.4Sb121SbPb208PbBi209Bi100Y(內標)89Y100在儀器最佳工作條件下,凡能達到6.2.2和6.2.3指標者均可使用。6.2.2最小精度(RSD)測量濃度為10ng/mL或5ng/mL的待測元素的基體匹配標準溶液,計算連續(xù)10次測量結果的相對標準偏差,最小精度(RSD)應不超過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—測量10次空白溶液強度的標準偏差;Cs—標準溶液的濃度,單位納克每毫升(ng/mL);Xs—測量10次標準溶液的平均強度;Xb—測量10次空白溶液的平均強度。測量基體和酸度與試液一致的空白溶液10次,計算各元素檢出限和定量限。砷元素的檢出限應小于0.8ng/mL,定量限應小于2.4ng/mL。錫、銻、鉛元素的檢出限應小于0.3ng/mL,定量限應小于0.9ng/mL。鉍元素的檢出限應小于0.1ng/mL,定量限應小于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實驗室樣品通常以鉆、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:如實驗室樣品粒度不均勻,測試樣品采用分樣器縮分出來。5GB/T43901—20248分析步驟8.1試料稱取0.10g試樣(7.2),精確至0.0001g,置于150mL錐形瓶中。8.2測定次數(shù)對同一個試樣至少進行兩次獨立分析。8.3空白試驗隨同試料做空白試驗?？瞻自囼瀾褂孟喈斢谠嚵现械逆嚭丸F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,轉移至100mL的容量瓶中,用水稀釋至刻度,混勻。此溶液為待測試液。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有殘余碳不溶,定容100mL后用快速濾紙干過濾。注2:如使用離線內標校正法,則在空白和試樣溶液稀釋至刻度前加入5.00mL的釔標準溶液[5.18c)]。8.5校準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準系列,每組制備1份校準空白溶液和5份校準標準溶液。每組分別將約50mL水加入6個100mL容量瓶中,按表3加入鎳基體溶液、鐵基體溶液、多元素混合標準溶液,加入硝酸(5.4)2.0mL,用水稀釋至刻度,混勻。表3多元素混合校準空白溶液和校準溶液鎳鐵牌號(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加入多元素混合標準溶液B(5.17)mL校準系列溶液中元素濃度ng/mL校準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多元素混合校準空白溶液和校準溶液(續(xù))鎳鐵牌號(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加入多元素混合標準溶液B(5.17)mL校準系列溶液中元素濃度ng/mL校準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測定根據(jù)待測鎳鐵樣品的含鎳量,選擇合適鎳和鐵比例的校準系列溶液(見表3)。待電感耦合等離子體質譜儀運行穩(wěn)定后,于待測元素和內標元素質量數(shù)處(見表2),依次測定標準系列溶液(按8.5配制)、空白試液(按8.3制備)、分析試液(按8.4制備)中待測元素和內標元素的離子流信號強度。以標準溶液中待測元素的質量濃度為橫坐標,待測元素與內標元素的離子流信號強度比值為縱坐標,繪制校準曲線。各元素校準曲線相關系數(shù)應在0.9990以上,否則需重新進行校準或重新配制標準溶液進行標準化。測量試液中的待測元素的信號強度,減去空白試驗溶液的強度即為凈強度,由工作曲線查得待測元素的濃度,以ng/mL計。9分析結果計算及表示9.1分析結果的計算按式(3)計算待測元素含量(ωM),以質量分數(shù)(%)表示。ωM=×100…………(3)式中:ρ—由校準曲線得到的元素質量濃度,單位為納克每毫升(ng/mL);V—試液體積,單位為毫升(mL);m—試料質量,單位為克(g)。7GB/T43901—20249.2分析結果的確定與表示同一試樣兩次獨立分析結果差值的絕對值不大于重復性限,則取算術平均值作為分析結果。如果兩次獨立分析結果差值的絕對值大于重復性限,則按照附錄A的規(guī)定追加測量次數(shù)并確定分析結果。分析結果按GB/T8170修約,保留兩位有效數(shù)字。10精密度精密度試驗是2022年由10個實驗室對11個鎳鐵樣品中的砷、錫、銻、鉛和鉍5個元素進行測定。樣品信息參見附錄B中的表B.1。精密度試驗原始數(shù)據(jù)見附錄B的表B.2~表B.6。各實驗室對每個樣品測試3次。在GB/T6379.1定義的可重復性條件下進行兩次測定,第3次測定是使用同一臺儀器在不同時間,在新的校準之后進行的。按照GB/T6379.2的規(guī)則對共同精密度試驗得到的結果數(shù)據(jù)進行統(tǒng)計處理。各元素含量與試驗結果的重復性限、室內再現(xiàn)性和再現(xiàn)性限的函數(shù)關系式見表4。表4精密度函數(shù)關系式元素水平范圍/%重復性/%室內再現(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)關系式計算得出的各元素均勻分布含量的重復性限、再現(xiàn)性限值見表5。表5均勻分布含量的重復性限(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在重復性限(r)條件下,獲得的兩次獨立測試結果的絕對差值不大于重復性限(r),以大于重復性限(r)的情況不超過5%為前提。在室內再現(xiàn)性限(Rw)條件下,獲得的兩次獨立測試結果的絕對差值不大于室內再現(xiàn)性(Rw),以大于室內再現(xiàn)性(Rw)的情況不超過5%為前提。在再現(xiàn)性限(R)條件下,獲得的兩次獨立測試結果的絕對差值不大于再現(xiàn)性限(R),以大于再現(xiàn)性限(R)的情況不超過5%為前提。11試驗報告試驗報告應包括下列內容:a)實驗室的名稱和地址;b)試驗報告的簽發(fā)日期;c)本文件編號;d)識別試樣必要的細節(jié);9GB/T43901—2024e)分析結果;f)結果的編號;g)在測定過程中觀察到的異?，F(xiàn)象和本文件中沒有規(guī)定的可能對試樣和認證標準物質的結果產生影響的任何操作。10GB/T43901—2024附錄A(規(guī)范性)試驗結果接受程序流程圖試驗結果接受程序流程圖如圖A.1所示。標引符號說明:r—重復性限;X—分析值。圖A.1試驗結果接受程序流程圖2424附錄B(資料性)精密度試驗原始數(shù)據(jù)共同精密度樣品信息如表B.1所示。精密度試驗原始數(shù)據(jù)見表B.2~表B.6。表B.1共同精密度試驗樣品信息%(質量分數(shù))試樣編號牌號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)元素精密度試驗原始數(shù)據(jù)12%(質量分數(shù))水平j測定次數(shù)n實驗室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)元素精密度試驗原始數(shù)據(jù)(續(xù))%(質量分數(shù))水平j測定次數(shù)n實驗室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)元素精密度試驗原始數(shù)據(jù)14%(質量分數(shù))水平j測定次數(shù)n實驗室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)元素精密度試驗原始數(shù)據(jù)(續(xù))%(質量分數(shù))水平j測定次數(shù)n實驗室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)元素精密度試驗原始數(shù)據(jù)16%(質量分數(shù))水平j測定次數(shù)n實驗室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)元素精密度試驗原始數(shù)據(jù)(續(xù))%(質量分數(shù))水平j測定次數(shù)n實驗室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)元素精密度試驗原始數(shù)據(jù)18%(質量分數(shù))水平j測定次數(shù)n實驗室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)元素精密度試驗原始數(shù)據(jù)(續(xù))%(質量分數(shù))水平j測定次數(shù)n實驗室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)元素精密度試驗原始數(shù)據(jù)20%(質量分數(shù))水平j測定次數(shù)n實驗室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