鑄造碳化鎢中雜質(zhì)元素測定-送審稿

1YS/T×××—202×鑄造碳化鎢粉雜質(zhì)元素含量的測定電感耦合等離子體原子發(fā)射光譜法本文件規(guī)定了采用電感耦合等離子體原子發(fā)射光譜法測定鑄造碳化鎢粉、碳化鎢粉和鎢粉中鐵、鋁、錳、鎂、鎳、鈦、釩、鈷、銅、鉻、鈣、鉬、鉭、鈮含量的測定方法。本文件適用于鑄造碳化鎢粉、碳化鎢粉和鎢粉中鐵、鋁、錳、鎂、鎳、鈦、釩、鈷、銅、鉻、鈣、鉬、鉭、鈮含量的測定。鋁、錳、鎂、鎳、鈦、釩、鈷、銅、鉻、鈣、鉬、鈮、鉭測定范圍：0.0020%~0.2500%；鐵測定范圍：0.0020%～0.5000%。2規(guī)范性引用文件下列文件中的內(nèi)容通過文中的規(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/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3術(shù)語和定義本文件沒有需要界定的術(shù)語和定義。4原理試料用氫氟酸-硝酸溶解，高純鎢基體匹配配制標(biāo)準(zhǔn)工作曲線，于電感耦合等離子體原子發(fā)射光譜儀上測定試液中各雜質(zhì)元素的發(fā)射強(qiáng)度，由工作曲線法計(jì)算出各元素的質(zhì)量分?jǐn)?shù)。5試劑或材料除非另有說明，在分析中僅使用確認(rèn)為優(yōu)級純的試劑。5.1水，GB/T6682，二級。5.2高純鎢粉（wW≥99.99%）。5.3硝酸(ρ=1.42g/mL）。5.4氫氟酸(ρ=1.14g/mL）。5.5標(biāo)準(zhǔn)貯存溶液：采用有證的標(biāo)準(zhǔn)物質(zhì)，鐵、鋁、錳、鎂、鎳、鈦、釩、鈷、銅、鉻、鈣、鉬、鉭、鈮質(zhì)量濃度均為1000μg/mL。5.6混合標(biāo)準(zhǔn)溶液:分別移取鐵、鋁、錳、鎂、鎳、鈦、釩、鈷、銅、鉻、鈣、鉬、鉭、鈮標(biāo)準(zhǔn)貯存溶液（5.5）5.00mL于一個100mL聚丙烯容量瓶（5.9）中，用水稀釋至刻度，混勻。各元素質(zhì)量濃度均為50μg/mL。2YS/T×××—202×5.7高純氬氣(φAr≥99.99%）。5.8聚四氟乙烯消解管（50mL或100mL）或聚四氟乙烯燒杯（100mL）。5.9聚丙烯容量瓶（100mL）。6儀器6.1電感耦合等離子體原子發(fā)射光譜儀，配耐氫氟酸腐蝕材質(zhì)進(jìn)樣系統(tǒng)。6.2電熱消解儀、微波消解儀或電熱板。7樣品樣品為粉末狀。8試驗(yàn)步驟8.1試料碳化鎢粉樣品稱取0.2000g，鎢粉樣品稱取0.1900g，精確至0.0001g。8.2平行試驗(yàn)平行做兩份試驗(yàn)，取其平均值。8.3空白試驗(yàn)稱取0.1900g高純鎢粉（5.2精確至0.0001g，隨同試料做空白試驗(yàn)。8.4測定8.4.1將試料(8.1)置于聚四氟乙烯消解管或聚四氟乙烯燒杯(5.8)中，用少量水沖洗管壁，加入2mL氫氟酸(5.4)，5mL硝酸(5.3)，于溫度設(shè)置為180℃的電熱消解儀（6.2）中消解25min±5min或微波消解儀（6.2）、電熱板（6.2）上溶解。試料溶解完全后，將試液移入100mL聚丙烯容量瓶（5.9）中，用水稀釋至刻度，混勻。8.4.2在電感耦合等離子體原子發(fā)射光譜儀上，于選定的測試條件下測定試液及試料空白的發(fā)射強(qiáng)度，從相應(yīng)的標(biāo)準(zhǔn)工作曲線計(jì)算經(jīng)空白校正的各元素的質(zhì)量濃度。8.5工作曲線的繪制8.5.1平行稱取高純鎢粉（5.2）七份，按分析步驟8.4.1進(jìn)行操作，將溶解完全的鎢基體分別轉(zhuǎn)入七個容量瓶中，再分別加入0mL、0.10mL、1.00mL、2.00mL、5.00mL、10.00mL混合標(biāo)準(zhǔn)溶液（5.6第七個容量瓶加入1.00mL鐵標(biāo)準(zhǔn)貯存溶液（5.5用水稀釋至刻度，搖勻。8.5.2儀器優(yōu)化后，按推薦的分析波長（表1濃度由低到高測量標(biāo)準(zhǔn)系列溶液中被測元素的發(fā)射光強(qiáng)度。以質(zhì)量濃度為橫坐標(biāo)，分析線發(fā)射光強(qiáng)度為縱坐標(biāo)，繪制工作曲線。3YS/T×××—202×表1分析波長鐵鋁錳鎂鎳鈦釩鈷銅鉻鈣鉬鉭鈮注：由于儀器型號不同，個別微量元素發(fā)射光譜推薦譜9試驗(yàn)數(shù)據(jù)處理各元素含量以質(zhì)量分?jǐn)?shù)wi計(jì)，數(shù)值以%計(jì)，按公式（1）計(jì)算：100……（1）式中：ρ——試液中元素的質(zhì)量濃度，單位為微克每毫升(μg/mLρ0——空白溶液中元素的質(zhì)量濃度，單位為微克每毫升(μg/mLV——試液總體積，單位為毫升（mLm——試料的質(zhì)量，單位為克（g）。計(jì)算結(jié)果表示至小數(shù)點(diǎn)后四位。數(shù)字修約按GB/T8170規(guī)定執(zhí)行。10精密度10.1重復(fù)性在重復(fù)性條件下獲得的兩次獨(dú)立測試結(jié)果的測定值，在以下給出的平均值范圍內(nèi)，兩個測試結(jié)果的絕對差值不超過重復(fù)性限（r超過重復(fù)性限（r）的情況不超過5%。重復(fù)性限（r）按表3數(shù)據(jù)采用線性內(nèi)插法或外延法求得。精密度試驗(yàn)原始數(shù)據(jù)參見附錄A。4YS/T×××—202×表2重復(fù)性限10.2再現(xiàn)性在再現(xiàn)性條件下獲得的兩次獨(dú)立測試結(jié)果的絕對差值不大于再現(xiàn)性限（R超過再現(xiàn)性限（R）的情況不超過5%。再現(xiàn)性限（R）按表4數(shù)據(jù)采用線性內(nèi)插法或外延法求得。精密度試驗(yàn)原始數(shù)據(jù)參見附錄A。表3再現(xiàn)性限11試驗(yàn)報告試驗(yàn)報告至少應(yīng)給出以下幾個方面的內(nèi)容：——樣品；——本文件編號；——分析結(jié)果及其表示；——與基本分析步驟的差異；——測定中觀察到的異?，F(xiàn)象；——試驗(yàn)日期。5YS/T×××—202×附錄A（資料性）精密度試驗(yàn)原始數(shù)據(jù)精密度數(shù)據(jù)是在2022年由8家實(shí)驗(yàn)室對高溫碳化鎢、鑄造碳化鎢中雜質(zhì)含量的4個不同水平樣品進(jìn)行共同試驗(yàn)確定的。每個實(shí)驗(yàn)室對每個水平的雜質(zhì)含量在重復(fù)性條件下獨(dú)立測定7次。測定的原始數(shù)據(jù)見表A.1-A.14。表A.1鐵精密度試驗(yàn)原始數(shù)據(jù)水平數(shù)wFe/%n=7）123456711234567821234567831234567841236YS/T×××—202×445678表A.2鋁精密度試驗(yàn)原始數(shù)據(jù)水平數(shù)實(shí)驗(yàn)室wAl/%n=7）平均值/%S/%123456711?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.00200.0024?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020021?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.0020?0.0020?0.00200.00240.00290.0038?0.0020?0.0020031234567841234567YS/T×××—202×478表A.3錳精密度試驗(yàn)原始數(shù)據(jù)水平數(shù)實(shí)驗(yàn)室wMn/%n=7）平均值/%S/%123456711?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020021?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003123456784123456788YS/T×××—202×表A.4鎂精密度試驗(yàn)原始數(shù)據(jù)水平數(shù)實(shí)驗(yàn)室wMg/%n=7）平均值/%S/%123456711?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020021?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003123456784123456789YS/T×××—202×表A.5鎳精密度試驗(yàn)原始數(shù)據(jù)水平數(shù)實(shí)驗(yàn)室wNi/%n=7）平均值/%S/%123456711?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.00200212345678312345678412345678YS/T×××—202×表A.6鈦精密度試驗(yàn)原始數(shù)據(jù)水平數(shù)實(shí)驗(yàn)室wTi/%n=7）平均值/%S/%123456711?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.00200212345678312345678412345678YS/T×××—202×表A.7釩精密度試驗(yàn)原始數(shù)據(jù)水平數(shù)實(shí)驗(yàn)室wV/%n=7）平均值/%S/%123456711?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020021?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.00200312345678412345678YS/T×××—202×表A.8鈷精密度試驗(yàn)原始數(shù)據(jù)水平數(shù)實(shí)驗(yàn)室wCo/%n=7）平均值/%S/%123456711?0.0020?0.00200234?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020067?0.0020?0.00208212345678312345678412345678YS/T×××—202×表A.9銅精密度試驗(yàn)原始數(shù)據(jù)水平數(shù)實(shí)驗(yàn)室wCu/%n=7）平均值/%S/%123456711?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020021?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.00200312345678412345678YS/T×××—202×表A.10鉻精密度試驗(yàn)原始數(shù)據(jù)水平數(shù)實(shí)驗(yàn)室wCr/%n=7）平均值/%S/%123456711?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.00200212345678312345678412345678YS/T×××—202×表A.11鈣精密度試驗(yàn)原始數(shù)據(jù)水平數(shù)實(shí)驗(yàn)室wCa/%n=7）平均值/%S/%123456711?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020021?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.00200312345678412345678YS/T×××—202×表A.12鉬精密度試驗(yàn)原始數(shù)據(jù)水平數(shù)實(shí)驗(yàn)室wMo/%n=7）平均值/%S/%123456711?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020021?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002004?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002005?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002006?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002007?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002008?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.00200312345678412345678YS/T×××—202×表A.13鉭精密度試驗(yàn)原始數(shù)據(jù)水平數(shù)實(shí)驗(yàn)室wTa/%n=7）平均值/%S/%123456711?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002002?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.002003?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0020?0.0