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硅鐵多元素含量的測定電感耦合等離子體原子發射光譜法國家標準化管理委員會國家市場監督管理總局發布國家標準化管理委員會I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則》的規定起草。本文件代替GB/T24194—2009《硅鐵鋁、鈣、錳、鉻、鈦、銅、磷和鎳含量的測定電感耦合等離子體原子發射光譜法》,與GB/T24194—2009相比,除結構調整和編輯性改動外,主要技術變化如下:b)增加了甘露醇試劑(見5.7);c)更改了試料量(見8.2,2009年版的7.2);d)更改了試樣溶液的制備(見8.4.1,2009年版的7.4.1);e)更改了校準曲線溶液的制備(見8.4.2,2009年版的7.4.2);f)增加了結果的表示(見9.2);g)用重復性限和再現性限替代了允許差(見第10章,2009年版的第9章)。請注意本文件某些內容可能涉及專利。本文件的發布機構不承擔識別專利的責任。本文件由中國鋼鐵工業協會提出。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:鄂爾多斯市西金礦冶有限責任公司、武漢鋼鐵有限公司、青島遠誠創智科技有限公司、內蒙古鄂爾多斯電力冶金集團股份有限公司、烏蘭察布市產品質量計量檢驗檢測中心、內蒙古工業大學、廣東中色研達新材料科技股份有限公司、寧夏科通新材料科技有限公司、青海百通高純材料開發有限公司、天津精一儀器儀表有限公司、青海華晟鐵合金冶煉有限責任公司、冶金工業信息標準研究院。本文件于2009年首次發布,本次為第一次修訂。1GB/T24194—2024硅鐵多元素含量的測定電感耦合等離子體原子發射光譜法警告——使用本文件的人員應有正規實驗室工作的實踐經驗。本文件并未指出所有可能的安全問的測定。各元素測定范圍見表1。分析元素測定范圍(質量分數)/%Fe0.50~3.00Al0.005~3.000.005~3.00Mn0.005~0.500.005~0.500.005~0.50P0.005~0.060.002~0.10Ni0.002~0.10Mg0.002~0.20V0.001~0.20Nb0.0005~0.02Pb0.0005~0.010.0005~0.010.005~0.05B0.0010~0.032規范性引用文件下列文件中的內容通過文中的規范性引用而構成本文件必不可少的條款。其中,注日期的引用文本文件。2GB/T24194—2024GB/T4010鐵合金化學分析用試樣的采取和制備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性的基本方法GB/T6682分析實驗室用水規格和試驗方法GB/T8170數字修約規則與極限數值的表示和判定GB/T12806實驗室玻璃儀器單標線容量瓶GB/T12807實驗室玻璃儀器分度吸量管GB/T12808實驗室玻璃儀器單標線吸量管GB/T36244電感耦合等離子體原子發射光譜儀JJG768發射光譜儀3術語和定義本文件沒有需要界定的術語和定義。4原理準溶液制作的校準曲線計算出分析元素質量分數。5試劑分析中除另有說明外,僅使用認可的分析純試劑和符合GB/T6682規定的二級及以上蒸餾水或與其純度相當的水。5.6鹽酸,1+3。5.8標準溶液稱取1.0000g金屬鐵(質量分數大于99.95%)于250mL燒杯中,加入40mL鹽酸(1+1),低溫加丙烯或聚乙烯的專用試劑瓶中。此溶液1mL含1000.0μg鐵。分取10.00mL鐵標準貯備溶液(5.8.1.1)于200mL容量瓶中,加入10mL鹽酸(1+1),用水稀釋3GB/T24194—2024a)稱取1.0000g金屬鋁(質量分數大于99.95%)于250mL聚四氟乙烯燒杯中,加入30mL鹽b)稱取1.0000g金屬鋁(質量分數大于99.95%)于250mL聚四氟乙烯燒杯中,加入30mL氫此溶液1mL含1000.0pg鋁。稱取2.4973g先于105℃±5℃干燥并于干燥器中冷卻至室溫的碳酸鈣(質量分數大于99.99%)分取10.00mL鈣標準貯備溶液(5.8.3.1)于200mL容量瓶中,加入10mL鹽酸(1+1),用水稀釋此溶液1mL含50.0μg鈣。稱取1.0000g電解錳[質量分數大于99.95%,預先用硝酸(1+3)洗凈表面氧化膜,再放入無水乙此溶液1mL含1000.0μg錳。分取10.00mL錳標準貯備溶液(5.8.4.1)于100mL容量瓶中,用水稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。4GB/T24194—20245.8.5鉻標準溶液5.8.5.1鉻標準貯備溶液,稱取1.0000g金屬鉻(質量分數大于99.95%)于250mL燒杯中,加入50mL鹽酸(1+1),滴加過分取10.00mL鉻標準貯備溶液(5.8.5.1)于100mL容量瓶中,加入10mL鹽酸(1+1)用水稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。此溶液1mL含100.0μg鉻。5.8.5.3鉻標準溶液,50.0pg/mL分取5.00mL鉻標準貯備溶液(5.8.5.1)于100mL容量瓶中,加入10mL鹽酸(1+1)用水稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。5.8.6鈦標準溶液稱取0.5000g金屬鈦(或海綿鈦,質量分數大于99.9%)于100mL鉑皿或聚四氟乙烯燒杯中,加入10mL氫氟酸和20mL硫酸(1+1)溶解,加熱蒸發至冒硫酸煙,用水沖洗鉑皿或聚四氟乙烯燒杯,繼續加熱至冒硫酸煙使氟驅盡。冷卻至室溫,加約50mL水溶解鹽類,移入1000mL容量瓶中,用硫酸(1+9)洗凈鉑皿或聚四氟乙烯燒杯,洗液合并于容量瓶中,并用硫酸(1+9)稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。此溶液1mL含500.0μg鈦。5.8.6.2鈦標準溶液,100.0μg/mL分取20.00mL鈦標準貯備溶液(5.8.6.1)于100mL容量瓶中,用硫酸(5+95)稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。分取10.00mL鈦標準貯備溶液(5.8.6.1)于100mL容量瓶中,用硫酸(5+95)稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。5.8.7磷標準溶液稱取2.1968g預先經105℃±5℃干燥至恒量并冷卻至室溫的基準磷酸二氫鉀(KH?PO?),置于300mL燒杯中,用適量水溶解,煮沸,冷卻,移入1000mL容量瓶中,用水稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。分取20.00mL磷標準貯備溶液(5.8.7.1)于100mL容量瓶中,用水稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。5GB/T24194—2024分取20.00mL磷標準溶液(5.8.7.2)于100mL容量瓶中,用水稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。此溶液1mL含20.0μg磷。5.8.8銅標準溶液稱取0.5000g金屬銅(質量分數大于99.95%)于250mL燒杯中,加20mL硝酸(1+1),低溫加熱溶解,加熱煮沸,除去氮氧化物,冷卻至室溫。移入1000mL容量瓶中,用水稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。分取10.00mL銅標準貯備溶液(5.8.8.1)于100mL容量瓶中,加10mL硝酸(1+1),用水稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。5.8.9鎳標準溶液稱取0.5000g金屬鎳(質量分數大于99.95%)于250mL燒杯中,加20mL硝酸(1+1),低溫加熱溶解,煮沸驅盡氯氧化物,冷卻至室溫,移入1000mL容量瓶中,用水稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。此溶液1mL含500.0μg鎳。分取10.00mL鎳標準貯備溶液(5.8.9.1)于100mL容量瓶中,加10mL硝酸(1+1),用水稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。此溶液1mL含50.0pg鎳。5.8.10鎂標準溶液稱取0.5000g金屬鎂(質量分數大于99.95%)于500mL燒杯中,加20mL鹽酸(1+1),加熱溶解,冷卻至室溫,移入1000mL容量瓶中,用水稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。此溶液1mL含500.0μg鎂。分取10.00mL鎂標準貯備溶液(5.8.10.1)于100mL容量瓶中,加10mL鹽酸(1+1),用水稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。5.8.11釩標準溶液稱取0.8926g預先在105℃±5℃烘干4h置于干燥器中的光譜純五氧化二釩于250mL燒杯中,加20mL鹽酸(1+1),滴加過氧化氫(p,1.10g/mL)加熱溶解,煮沸,冷卻至室溫,移入1000mL容量瓶中,用水稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。6分取10.00mL釩標準貯備溶液(5.8.11.1)于100mL容量瓶中,加10mL鹽酸(1+1),用水稀釋至5.8.12鈮標準溶液稱取0.1431g經研缽研細并在105℃±5℃烘干2h的光譜純五氧化二鈮(Nb?O?)于150mL石英坩堝中,加入3g焦硫酸鉀,攪拌均勻后再覆蓋1g焦硫酸鉀,于600℃加熱熔融,冷卻,加入20mL聚乙烯的專用試劑瓶中。分取10.00mL鈮標準貯備溶液(5.8.12.1)于1005.8.13鉛標準溶液稱取0.1600g硝酸鉛于250mL燒杯中,加20mL水,5mL硝酸(1+1)溶解,移入1000mL容量分取10.00mL鉛標準貯備溶液(5.8.13.1)于100mL容量瓶中,用水稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。此溶液1mL含10.0μg鉛。5.8.14銻標準溶液稱取0.2740g酒石酸銻鉀(C?H?KO?Sb·1/2H?O)于250mL燒杯中,加20mL鹽酸(1+4)溶解,移入1000mL容量瓶中,用鹽酸(1+9)稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。分取10.00mL銻標準貯備溶液(5.8.14.1)于100mL容量瓶中,用鹽酸(1+9)稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。5.8.15鋯標準溶液稱取0.353g氧氯化鋯(ZrOCl?·8H?O)于250mL燒杯中,加40mL鹽酸(1+4)溶解,移入1000mL容量瓶中,用鹽酸(1+9)稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。分取20.00mL鋯標準貯備溶液(5.8.15.1)于100mL容量瓶中,用鹽酸(1+9)稀釋至刻度,混勻,貯于聚丙烯或聚乙烯的專用試劑瓶中。7稱取2.8611g預先經105℃±5℃干燥至恒量并冷卻至室溫的基準試劑硼酸于250mL燒杯稱取1.2699g三氧化二釔(質量分數大于99.9%,預先經1000℃灼燒1h),置于500mL燒杯中,加入50mL鹽酸(1+1),加熱溶解,冷卻至室溫,移入1000mL容量瓶中,用水稀釋至刻度,混此溶液1mL含1000.0μg釔。此溶液1mL含100.0μg釔。鹽酸(1+1),用水稀釋至刻5.10純鐵(質量分數大于99.98%或分析元素含量已知)。6.2電感耦合等離子體(ICP-AES)原子發射光譜儀。可以使用任何型號的電感耦合等離子體原子發射光譜儀,儀器應符合GB/T36244和JJG768的要求。電感耦合等離子體原子發射光譜儀的性能試元素可能干擾元素元素波長/nm可能干擾元素V—PBY7取樣和制樣8.2試樣量試樣量/g檢測范圍I組,適用于高硅硅鐵、普通硅鐵和低鋁硅鐵的常規元素Ⅱ、Ⅲ組,適用于高純硅鐵、硼元素的測定89GB/T24194—2024稱取相當于試樣量中鐵含量的純鐵(5.10),精準至0.001g,純鐵的稱樣量見表4,隨同試樣做空白試驗。表4試樣量及純鐵量試樣量/g稱取純鐵的量/g0.20000.0450.50000.110注1:檢測高硅硅鐵中雜質時不加純鐵。注2:對于PGFeSi65、PGFeSi40牌號的硅鐵,根據待測樣品中相當的鐵含量計算稱量純鐵的量。慢滴加約5mL氫氟酸(5.2),至激烈反應停止,加入5mL鹽酸(5.6),輕輕小幅度搖動,低溫加熱至試約2mL~3mL溶液,取下,稍冷,加入20mL鹽酸(5.6),加熱溶解鹽類,冷卻至室溫。將試液移入100mL聚四氟乙烯或石英容量瓶中,用水稀釋至刻度,混勻。如果用內標法測量,在稀釋之前,加入將試樣(見表3)置于200mL聚四氟乙烯燒杯中,用聚乙烯吸量管或刻度聚乙烯滴管準確加入5mL氫氟酸(5.2),加入5mL甘露醇(5.7),緩慢滴加10mL硝酸(5.1),反應比較劇烈,每次滴加硝酸反應緩慢后再小幅度轉動聚四氟乙烯燒杯,直至試樣完全溶解至溶液清亮,室溫放置30min。將溶液移入100mL聚四氟乙烯容量瓶中,用水稀釋至刻度,混勻。如用內標法測量,在稀釋之前,加入用相當于試樣中鐵含量(見表4)的純鐵7份(5.10)代替試樣,分別置于200mL聚四氟乙烯燒杯中,按8.4.1步驟將其溶解,冷卻至室溫,將溶液轉移至100mL聚四氟乙烯容量瓶中,按表5、表6和GB/T24194—2024表7加入被測元素的校準溶液。校準溶液的濃度范圍要覆蓋所分析元素的濃度范圍,某一校準溶液中各分析元素不應都是最高或最低,每一校準曲線需要由5點(含5點)以上校準溶液組成,并成合適梯次靈敏線或者適當稀釋試樣溶液和校準溶液。如果用內標法,用移液管加5.00mL釔標準溶液表5制作校準曲線的標準溶液I組元素標準溶液V——100mL容量瓶中加入標準溶液的體積/mLc——標準溶液稀釋后的濃度/(μg/mL)序號濃度/(pg/mL)體積或濃度012345鐵V0C0鋁V0C0鈣V0C0錳V0C0鉻V0C0鈦V0C0磷V0C0注1:鐵元素僅適用于高硅硅鐵中鐵含量的檢測。注2:本表中校準曲線對應的濃度范圍是待測試樣量為0.2000g的待測元素的含量范圍。元素標準溶液V——100mL容量瓶中加入標準溶液的體積/mLc——標準溶液稀釋后的濃度/(μg/mL)序號濃度/(μg/mL)體積或濃度012345鋁V0C0GB/T24194—2024表6制作校準曲線的標準溶液Ⅱ組(續)元素標準溶液V———100mL容量瓶中加入標準溶液的體積/mLc——標準溶液稀釋后的濃度/(μg/mL)序號濃度/(ug/mL)體積或濃度012345鈣5.8.3.2V00.502.0025.00C00.252.50錳5.8.4.3V00.502.0020.00C00.252.50鉻5.8.5.3V00.502.00C00.250.502.50鈦5.8.6.3V00.502.00C00.250.502.50磷5.8.7.2V00.502.004.00C00.252.002.505.8.8.2V00.200.502.00C00.100.252.50鎳5.8.9.2V00.200.502.00C00.100.252.50鎂5.8.10.2V00.2020.00C00.100.502.50釩5.8.11.2V00.1020.00C00.050.502.50鈮5.8.12.2V00.5020.00C00.050.100.502.00鉛5.8.13.2V00.502.00C00.050.100.200.300.50銻5.8.14.2V00.502.00C00.050.100.200.300.50鋯5.8.15.220.0V02.00C00.200.402.00注:本表中校準曲線對應的濃度范圍是待測試樣量為0.5000g的待測元素的含量范圍。GB/T24194—2024表7制作校準曲線的標準溶液Ⅲ組元素標準溶液V———100mL容量瓶中加入標準溶液的體積/mLc——標準溶液稀釋后的濃度/(μg/mL)序號濃度/(pg/mL)體積或濃度012345硼V0C0注:本表中校準曲線對應的濃度范圍是待測試樣量為0.5000g的待測元素的含量范圍。如果使用內標,準備用Y(371.03nm)作內標并計算每個元素與釔的強度比的軟件,內標強度應與分析物強度同時測量。開啟點火鍵,點火后確認儀器運行參數在確認范圍內,霧化系統及等離子火焰工作正常,穩定數分鐘。開始用最低濃度校準溶液(零號相當于空白試驗),再按順序吸入校準溶液,在每次吸入去離子水或稀硝酸溶液。至少重復測量2次,取兩個讀數的平均值。以被測元素濃度為橫坐標,光譜在與8.4.4.1相同條件下測量空白試液和試樣溶液的光譜強度,每次測量之間吸入去離子水沖洗,至少重復測量2次。取兩個讀數的平均值,計算機采集所測定的試樣溶液中待測元素的凈強度,由校準曲線計算出各元素的含量結果。9結果的計算及表示 (1)GB/T24194—2024m?——試樣質量,單位為克(g)。9.2結果的表示同一試樣兩次獨立測定的分析結果差值的絕對值不大于重復性限r,則取算數平均值作為分析結果。如果兩次獨立測定的分析結果差值的絕對值大于重復性限r,則按照附錄B的規定追加測定次數并確定分析結果。數值修約按GB/T8170的規定進行。元素測定范圍(質量分數)/%PVB注:式中m是分析元素的含量(質量分數),%。在重復性條件下,獲得的兩次獨立測試結果的絕對差值不大于重復性限(r),大于重復性限(r)的情況不超過5%。GB/T24194—2024在再現性條件下,獲得的兩次獨立測試結果的絕對差值不大于再現性限(R),大于再現性限(R)的情況不超過5%。試驗報告應包括以下內容:a)實驗室名稱和地址;b)試驗報告的簽發日期;c)本文件編號;d)識別試樣的細節;e)分析結果;g)在測定過程中注意到的任何特性和本文件中沒有規定的可能對試樣和認證標準物質的結果產(規范性)電感耦合等離子體光譜儀的性能試驗本附錄中給出的性能試驗目的在于使用不同類型的儀器對等離子體光譜儀的性能進行適當的測定,允許不同的儀器使用不同的操作條件,但等離子體光譜儀最終能產生一致的結果。制定利用電感耦合等離子體原子發射光譜(ICP-AES)分析標準方法。A.2校準溶液制備3份溶液,含待測物濃度水平分別為0濃度水平(0×DL)、10倍檢測限(10×DL)、1000倍檢測限(1000×DL)的校準溶液,這些溶液中要含有與待測樣品相似溶度的酸、溶劑和基體元素(鐵元素)。制備校準的檢出限(DL)值可以參考實驗室值或表3中的值。A.3程序和操作按儀器說明書和實驗室的定量分析的實踐經驗對等離子體原子發射光譜儀進行最初的調節。吸入1000倍檢測限的校準溶液,在溶液進入等離子體后等待10s,以保證穩定霧化。對待測元素設定操作和儀器條件,將選擇的波長定位在最高峰處,選擇適當的光電倍增管(對于非自動選擇的設備),保證測到的光強度為4位有效數字,設定積分時間為3s。吸入空白試液約10s,以預設積分時間測定10次。吸入10倍檢測限試液約10s,以預設積分時間測定10次。吸入1000倍檢測限試液約10s,以預設積分時間測定10次。A.4背景等效濃度(BEC)和檢測限的確定由空白試液和10倍檢測限溶液的平均強度、10倍檢測限溶液的濃度和10次空白強度的標準偏差,按式(A.1)計算分析曲線的斜率,按式(A.2)計算背景等效濃度(BEC),按式(A.3)計算檢測限(DL)。M=c?/(I?—Ih)……(A.1)式中:M——分析曲線的斜率;C2——10倍檢測限溶液的濃度;I?——10倍檢測限溶液10次原始強度的平均值;Ib——空白溶液10次原始強度的平均值。BEC=M×IDL=3S,M式中:DL——檢測限,單位為微克每毫升(μg/mL);Sb——10次空白強度讀數的標準偏差。GB/T24194—2024A.5短期精度(RSD)由1000倍檢測限溶液10次原始平均強度(I?)與空白溶液10次原始平均強度(I?)按式(A.4)計算1000倍檢測限溶液的凈平均強度(IN?)。IN?=I?Ib…………(A.4)式中:IN?——1000倍檢測限溶液(1000×DL)的凈平均強度;I?——1000倍檢測限溶液10次原始強度的平均值。RSD是元素濃度為1000倍檢測限溶液的估計值。按式(A.5)計算1000倍檢測限溶液(1000×DL)的凈強度相對標準偏差。………………(A.5)式中:S?——1000倍檢測限溶液10次強度讀數的標準偏差。否再次測定否再次測定X4是Xra-xnl≤1.3u=X+X?+X+X否圖B.1試樣分析結果接受程序流程圖水平j實驗室i12345678912.8812.7002.6892.6982.6962.8052.7312.7302.7242.9572.7302.7042.7152.6962.8722.7352.6802.6982.8162.7112.7012.7062.6962.8382.7212.7602.715232.1872.1502.0902.1352.0642.2092.1452.1302.1422.1852.1702.1252.1322.0642.2922.1462.1002.1342.1792.1552.1352.1432.0642.1632.1312.1602.14040.9550.9600.9540.9670.9420.9510.9490.9670.9670.9590.9610.9530.9600.9460.9450.9460.9660.9680.9470.9600.9590.9610.9510.9420.9550.9640.96850.6620.6610.6590.65806560.6670.6580.6660.6580.6710.6610.6610.6590.6680.6660.6590.6630.6620.6700.6580.6630.6560.6630.6690.6640.6620.662水平j實驗室i123456789123表C.2Al精密度試驗原始數據(續)水平j實驗室i12345678940.6180.6210.6000.6150.6110.6010.6110.6200.5990.6170.6260.6100.6220.6110.5980.6140.5800.6110.6140.6230.6000.6180.6110.5900.6120.6000.6105672.1582.1912.1132.1322.1002.0792.1822.1702.1212.1712.2022.1282.1422.1002.0962.1602.1802.1232.1772.1802.1392.1362.1002.0992.1762.2402.12582.4822.5112.4082.4432.4202.4132.4692.5002.4232.4272.5092.4282.4522.4202.4012.4982.3802.4252.4602.5002.4252.4362.4202.4002.4682.5002.42992.7772.8162.7182.7392.7402.6902.7592.7602.7152.8012.8072.7292.7422.7402.6912.7802.7202.7162.7992.8302.7342.7312.7402.6482.7612.6702.7210.00990.01000.01010.00950.00950.01090.00890.00970.00980.00980.01000.00990.00940.00940.01060.00940.00950.00920.00950.01000.01060.00930.00940.00980.00930.01000.00960.02320.02300.02480.02230.02600.02290.02170.02300.02430.02380.02400.02390.02310.02600.02360.02190.02370.02250.02270.02300.02330.02360.02600.02210.02180.02390.02290.05350.05600.05440.05260.05800.05070.05130.05200.05300.05320.05500.05400.05210.05800.05200.050.50.05250.05150.05260.05200.05350.05120.05800.04980.05090.05300.05230.07310.07700.07440.07240.07400.07200.06930.07200.07230.07180.080.00.07480.07200.07400.07120.06920.07300.07220.07250.08100.07550.07160.07400.06930.06930.07250.07150.04540.04700.04610.04480.04600.04430.04210.04510.04500.04510.04900.04500.04560.04600.04440.04230.04600.04430.04440.04500.04550.04420.04600.04550.04190.04580.0447GB/T24194—2024表C.2Al精密度試驗原始數據(續)水平j實驗室i1234567890.01100.01000.01290.01080.01210.01130.01070.01220.01070.01080.01000.01240.01140.01150.01030.00960.01100.01090.01100.01100.01230.01020.01l]0.01040.010.50.01180.01l1表C.3Ca精密度試驗原始數據水平j實驗室i12345678912345678GB/T24194—2024表C.3Ca精密度試驗原始數據(續)水平j實驗室i1234567899表C.4Mn精密度試驗原始數據水平j實驗室i12345678912表C.4Mn精密度試驗原始數據(續)水平j實驗室i12345678930.02140.02260.020.50.02220.02260.02210.02080.02180.02180.02200.02310.02180.02240.02250.02160.02020.02350.02150.02250.02310.02090.02210.02250.02550.02060.02170.021640.04520.05080.05000.04650.04660.04780.04770.04770.04680.04450.05100.05000.04720.04680.04800.04770.04450.04690.04400.05090.05000.04760.04670.04300.04780.04550.047450.20760.22070.22580.21400.19700.21300.21100.20600.21500.20730.22120.22140.21800.19500.20700.21200.20000.21600.20750.22020.20150.21200.19800.18800.21100.19000.205060.29600.32860.30000.30200.30200.29900.30500.29800.30100.29720.32880.30000.30400.30100.29900.30600.28000.30500.29760.32870.30000.30100.30200.27200.30600.28000.304070.21640.24850.20000.23800.20100.22200.22400.23000.22400.21940.23730.20000.23600.20300.22000.22200.23000.21900.21880.24230.22000.23200.20200.20900.22300.23000.225080.29310.32540.30000.30900.29900.29700.29600.29000.29700.29030.32820.29000.30700.30000.29700.29600.28000.30500.28980.32550.30000.30200.29900.29400.29800.29400.301090.13110.14080.13000.13400.13000.13100.13100.13000.13500.13200.14130.13000.14200.13100.13200.13600.13000.13600.13050.14120.12800.13800.13100.12700.13200.12000.13100.08710.08720.08500.08360.08100.08340.08280.08400.08430.08580.08740.08610.08290.08100.08210.08300.08600.08410.08770.08770.08590.08390.08100.09020.08290.08400.08400.05670.05940.04890.05380.05350.05330.05280.05500.05560.05640.05820.04990.05290.05340.05330.05370.05800.05570.05740.05850.05120.05340.05380.05100.05340.05700.05580.05520.05610.04910.05390.05200.05140.05060.05200.05210.05500.05710.05240.05440.05210.05190.05060.05360.05240.05480.05660.05540.05480.05210.04980.05070.05350.05230.04890.04820.04200.04520.04560.04490.04440.04700.04620.04660.04780.04800.04560.04570.04430.04450.04500.04590.04750.04810.04800.04480.04560.04310.04440.04640.0458表C.4Mn精密度試驗原始數據(續)水平j實驗室i1234567890.0761表C.5Cr精密度試驗原始數據水平j實驗室i1234567891234567表C.5Cr精密度試驗原始數據(續)水平j實驗室i12345678989表C.6Ti精密度試驗原始數據水平j實驗室i1234567891表C.6Ti精密度試驗原始數據(續)水平j實驗室i12345678920.09140.08650.08240.08740.08510.08780.08530.08330.085.60.09010.09000.08380.08820.08510.08540.08580.08800.08430.09150.08880.08400.08690.08510.08060.08550.08520.086330.11870.11520.12090.11700.11400.11400.11000.11000.11400.11940.11600.12160.11400.11400.11300.11100.11800.11500.11720.11550.12040.11200.11400.10100.11100.11200.113040.03950.03890.03870.03920.04090.03800.03900.03910.03970.03870.03920.03800.040.60.04090.03860.03920.03650.03940.03980.03910.03560.03980.04090.03530.03910.03720.039550.13480.12660.13010.13200.13300.12500.13400.12700.13000.13390.12740.12980.13400.13300.12600.13300.12000.13500.13360.12740.13240.13100.13300.11300.13400.12000.133060.11210.10940.11320.10200.11200.10300.10900.10800.10900.11130.11030.11280.10400.1l100.10300.10900.10000.10800.11160.11120.11270.10300.11100.09030.11000.11000.110070.12020.12330.11790.11400.11800.11600.12100.12000.11900.12110.120.70.11850.11600.11900.11500.12100.12000.11700.12250.12200.11840.11500.11900.10700.12000.12000.118080.08110.20140.18650.18800.19600.19400.20000.19500.20100.08090.20320.18770.18700.19700.18900.19700.19000.19700.07930.20370.18710.18900.19500.17700.19800.19600.201090.25420.25220.24890.24200.24900.24300.24200.25000.25600.25950.25230.24920.23900.24800.24300.24800.24000.25700.25840.25190.24950.24400.24800.21600.24600.24000.24900.00770.00830.00790.00760.00760.00730.00730.00810.00780.00770.00780.00850.00740.00760.00740.00740.00850.00790.00760.00810.00800.00750.00760.00580.00740.00890.00760.01900.01890.01920.01870.02010.01770.01810.01900.01870.01920.01840.01980.01910.02010.01810.01810.01800.01890.01930.01870.01910.01810.02010.01540.01810.02100.01860.02410.02310.02540.02360.02390.02230.02260.02400.02270.02380.02380.02490.02410.02390.02210.02250.02500.02290.02390.02330.02430.02330.02390.01980.02270.02400.0227GB/T24194—2024表C.6Ti精密度試驗原始數據(續)水平j實驗室i1234567890.050.5表C.7P精密度試驗原始數據水平j實驗室i123456789123456表C.7P精密度試驗原始數據(續)水平j實驗室i123456789789GB/T24194—2024水平j實驗室i12345678910.00630.00800.00790.00790.00810.00700.00700.00780.00800.00630.00740.00780.00810.00810.00730.00710.00830.00810.00610.00780.007.50.00780.00810.00690.00740.00800.008020.00200.00250.00320.00280.00230.00240.00240.00280.00300.00200.00250.00350.00290.00230.00240.00230.00320.00310.00190.00250.00310.00280.00230.00200.00250.00300.003230.00190.00230.00280.00250.00220.00220.00220.00240.00240.00140.00240.00290.00260.00220.00210.00210.00270.00230.00170.00240.00280.00240.00220.00190.00220.00240.002340.02300.02770.02810.02950.02990.02630.02720.02590.02810.02320.03120.02850.02910.02990.02700.02740.02700.02840.02350.02890.02780.03020.02990.02500.02730.02640.028250.02410.02920.02950.03210.03110.02800.02830.02730.03010.02390.02880.02990.03180.03110.02820.02830.02740.03050.02450.02910.03010.03140.03110.02700.02830.02810.030660.06890.07830.07190.06220.08200.07490.07350.07140.07200.06870.07970.07250.06180.08200.07330.07290.07370.07210.06860.07920.07280.06200.08210.07350.07340.07290.072570.01860.01900.01810.01840.01830.01830.01840.01810.01990.01880.01990.01870.01850.01830.01830.01830.01660.02010.01880.01970.01890.01830.01810.01610.01840.01770.020580.07990.09230.08110.07180.09590.08790.08670.08430.08270.08020.09000.08160.07200.09600.08680.08720.08940.08310.08080.09110.08140.07230.09590.08170.08710.08620.083290.03540.04390.04100.03100.04430.04010.03980.03980.04000.03570.04200.04080.03100.04420.04040.03980.04010.04030.03500.04330.04090.03090.04420.03830.03990.04030.03990.00520.00470.00430.00430.00440.00410.00420.00440.00430.00510.00440.00420.00440.00430.00420.00400.00480.00420.00500.00450.00500.00420.00440.00330.00410.00500.00410.00650.00620.00490.00580.00560.00550.00550.00590.00550.00650.00580.00550.00590.00540.00550.00540.00650.00560.00640.00610.00530.00580.00550.00470.00540.00710.0057GB/T24194—2024表C.8Cu精密度試驗原始數據(續)水平j實驗室i123456789表C.9Ni精密度試驗原始數據水平j實驗室i12345678912345GB/T24194—2024表C.9Ni精密度試驗原始數據(續)水平j實驗室1234567896789GB/T24194—2024表C.10Mg精密度試驗原始數據水平j實驗室i12345678910.01300.01190.00990.01350.01400.01150.01260.01300.01270.01280.01310.01020.01240.01400.01280.01250.01180.01290.01320.01220.01240.01210.01400.01160.01220.01140.012520.00880.00780.00750.00810.00930.00690.00790.00860.00860.00880.00720.00790.00820.00930.00680.00810.00780.00850.00880.00770.00790.00840.00920.00740.00820.00780.008430.01200.01050.00980.01010.01130.00900.01090.01070.01130.01170.00960.00990.01050.01120.01110.01030.01000.01110.01140.01000.01020.01190.01130.01040.01100.00940.010940.00850.00840.00790.00690.00700.00880.00830.00830.00740.00820.00930.00740.00710.00700.00900.00780.00790.00730.00790.00890.00750.00700.00700.00720.00810.00800.007350.05930.06100.05890.05570.05030.06050.05720.06000.05720.05940.06160.05970.05590.05020.05850.05860.05850.05700.05900.06110.05940.05630.05040.05810.05810.05370.057160.03720.04020.03520.03540.02980.03490.03530.03780.03480.03740.04040.03590.03510.02980.03590.03580.03600.03520.03750.04040.03620.03520.02980.03060.03560.03830.035070.01480.01790.01520.01920.01360.01450.01460.01370.01480.01490.02000.01490.01980.01370.01500.01450.01480.01440.01500.01880.01480.02020.01370.01260.01460.01440.014680.09650.10530.09950.08920.07610.09810.09590.10000.09470.09640.10610.09910.08900.07600.09960.09610.09700.09500.09640.10550.09930.08970.07610.09070.09610.10000.094690.00960.00920.00950.01060.01020.00740.00850.00960.00860.00940.01170.00910.01040.01020.00750.00920.00950.00890.00970.01100.00960.01010.01020.00850.00890.00980.00870.00260.00330.00340.00320.00360.00500.00210.00330.00300.00240.00360.00380.00330.00360.00590.00200.00400.00310.00240.00330.00350.00320.00360.00460.00220.00410.00330.00250.00270.00480.00370.00400.00350.00240.00370.00350.00260.00270.00410.00370.00400.00400.00190.00390.00330.00260.00270.00420.00380.00400.00370.00220.00400.0031水平j實驗室i123456789水平j實驗室i12345678912345GB/T24194—2024表C.11V精密度試驗原始數據(續)水平j實驗室il234567896789GB/T24194—2024表C.12Nb精密度試驗原始數據水平j實驗室i12345678910.00650.00050.00620.00060.00710.00860.00640.00740.00630.00640.00040.00610.000.50.00740.00860.00640.00440.00640.00600.00050.00660.00060.00770.00870.00640.00780.006420.00500.00300.00590.00050.00690.00650.00420.00600.00530.00490.00300.00610.00040.00700.00640.00440.00510.00530.00490.00300.00610.00050.00710.00640.00430.00560.005430.00830.00400.00690.00090.00750.00850.00640.00810.00700.00830.00400.00750.00100.00730.00850.00630.00710.00710.00840.00400.00720.00090.00740.00860.00640.00690.007140.00310.00200.00200.00160.00350.00410.00180.00410.00250.00310.00200.00200.00150.00340.00410.00180.00290.00250.00380.00200.00200.00150.00350.00420.00180.00260.002450.01050.00900.01140.00960.00800.00760.00700.00380.00110.01080.00900.01070.00970.00800.00760.00710.00230.00180.01120.00900.01090.00990.00810.00770.00700.00310.002160.00950.00700.00870.00090.00820.00810.00500.01020.01110.00950.00800.00890.00080.00830.00820.00600.00920.0100.00920.00800.00890.00090.00840.00820.00600.00860.009170.01080.00700.00950.00080.00770.01510.00850.00460.00910.01060.00500.00910.00090.00790.01520.00860.00480.00910.01040.00600.00930.00090.00790.01500.00860.00460.009980.01870.00600.01770.00180.01800.01920.00180.0210.01840.01780.00600.01740.00140.01820.01930.00180.02170.01830.01810.00600.01770.00160.01810.01900.00180.02130.017490.02290.01100.02190.01200.02060.00860.01000.02260.01400.02230.01000.02190.01200.020.60.00860.00900.02290.01400.02210.01000.02170.01200.02070.00870.01000.02210.01400.00050.00010.00080.00060.00100.00060.00020.00070.00060.00080.00010.00100.00070.00110.00060.00010.00100.000.60.00070.00010.00120.00060.00110.00060.00020.00120.00070.00160.00040.00230.00160.00230.00110.00040.00170.00160.00170.00040.00200.00150.00230.00110.00030.00200.00160.00180.00040.00280.00140.00210.00110.00040.00250.0016GB/T24194—2024表C.12Nb精密度試驗原始數據(續)水平j實驗室il23456789表C.13Pb精密度試驗原始數據水平j實驗室i12345678910.00010.000.50.00000.00070.00030.00020.00000.00110.00070.00000.00050.00000.00060.00020.00020.00000.00070.00060.00000.00050.00000.00080.00020.00020.00000.00050.000720.00060.00050.00000.00060.00030.00010.00000.00020.00060.00060.00050.00000.00070.00030.00010.00000.00100.00060.00000.00050.00000.00060.00030.00030.00000.00080.000730.00040.000.50.00000.00050.000.20.00030.00000.00090.00050.00010.00050.00000.00060.00020.00020.00000.00080.00050.00030.00050.00000.00040.00020.00030.00000.00070.000640.00060.00050.00000.00050.00050.00160.00000.00070.00040.00070.00050.00000.00050.00050.00150.00000.00130.00040.00030.000.50.00000.000.50.000.50.00140.00000.000.50.000.550.00090.00050.00000.00030.00020.00130.00000.00090.00090.00100.00050.00000.00020.00020.00150.00000.00120.00090.00080.000.50.00000.00020.00020.00120.00000.00070.0009表C.13Pb精密度試驗原始數據(續)水平j實驗室i1234567896789GB/T24194—2024表C.14Sb精密度試驗原始數據水平j實驗室i12345678910.00020.00050.00020.00060.00090.00020.00100.00110.00020.00020.000.50.00020.00070.00090.00020.00110.00220.00020.000.50.00050.00020.00050.00090.00050.00110.00110.000220.00070.00050.00150.00100.00040.00050.00130.00130.00020.00180.00050.00160.00110.00040.00050.00150.00130.00020.00100.00050.00130.00100.00040.00050.00130.00190.000230.00080.00050.00390.00370.00040.00050.00130.00710.00020.00070.00050.00400.00390.00040.00020.00120.00630.00020.00050.00050.00410.00380.00040.00050.00130.00020.000240.00200.00050.00020.00070.00020.00020.00050.00000.00050.00210.000.50.00020.00070.00020.00020.00050.00000.00050.00120.00050.00020.00060.00020.00020.00050.00000.000550.00030.00050.00020.00100.00030.00110.00020.00020.00050.00030.00050.00020.00110.00030.00100.00020.00020.00050.00020.00050.00020.00090.00030.00070.00020.00020.000560.00680.0050.0020.00510.00510.00570.00320.00200.00500.00710.0050.0020.00550.00510.00520.00320.00200.00400.00830.0050.0020.00540.00510.00490.00320.00200.004070.00150.00050.00020.00130.00070.00070.00020.00020.00040.00100.00050.00020.00120.00070.00050.00020.00020.00030.00230.0050.00020.00130.00070.00020.00020.00020.00038

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