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1GB/T8152.6—202×鉛精礦化學分析方法第6部分:鉍含量的測定氫化物發(fā)生-原子熒光光譜法、火焰原子吸收光譜法和Na2EDTA滴定法警示—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⒈WC符合國家有關法規(guī)規(guī)定的條件。本文件規(guī)定了鉛精礦中鉍含量的測定方法。本文件適用于鉛精礦中鉍含量的測定。方法1(原子熒光光譜法)測定范圍:0.010%~0.50%;10.00%。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/T6682分析實驗室用水規(guī)格和試驗方法3術語和定義本文件沒有需要界定的術語和定義。4方法1氫化物發(fā)生-原子熒光光譜法試樣經(jīng)鹽酸、硝酸、氟化氫銨和高氯酸分解,在鹽酸介質中,用硫脲-抗壞血酸進行預還原,在氫化物發(fā)生器中,鉍被硼氫化鉀還原成氫化物,用氬氣導入石英爐原子化器中,于原子熒光光譜儀上測量其熒光強度。4.2試劑與材料除非另有說明,在分析中僅使用確認為分析純的試劑和蒸餾水或去離子水或相當純度的水。4.2.1氟化氫銨4.2.2鹽酸(ρ=1.19g/mL)。4.2.3硝酸(ρ=1.42g/mL)。4.2.4氫溴酸(ρ=1.49g/mL)。4.2.5高氯酸(ρ=1.67g/mL)。2GB/T8152.6—202×4.2.6硝酸(1+1)。4.2.7硝酸(4+96)4.2.8鹽酸(1+9)。4.2.9氫氧化鈉溶液(5g/L)。4.2.10硫脲-抗壞血酸混合溶液(50g/L):稱取硫脲、抗壞血酸各5g,用水溶解后,稀釋至100mL,混勻,現(xiàn)用現(xiàn)配。4.2.11硼氫化鉀(20g/L):稱取20g硼氫化鉀溶于1000mL氫氧化鈉溶液(4.2.9)中,現(xiàn)用現(xiàn)配。4.2.12鉍標準貯存溶液:稱取0.1000g鉍(wBi≥99.99于250mL燒杯中,加入20mL硝酸(4.2.6),蓋上表面皿,加熱至完全溶解,微沸驅除氮的氧化物,冷卻,移入100mL容量瓶中,用水稀釋至刻度,混勻。此溶液1mL含1000μg鉍。4.2.13鉍標準溶液:移取1.00mL鉍標準貯存溶液(4.2.12)于1000mL容量瓶中,加入10mL鹽酸(4.2.2),用水稀釋至刻度,混勻。此溶液1mL含1μg鉍。4.3儀器原子熒光光譜儀,附鉍高強度空心陰極燈。在儀器最佳工作條件下,凡能達到下列指標者均可使用:——檢出限:Bi不大于0.1ng/mL;——精密度:用最高濃度的標準溶液測量10次熒光強度,其標準偏差應不超過平均熒光強度的3.0%;用最低濃度的標準溶液(不是“零”濃度標準溶液)測量10次熒光強度,其標準偏差不超過最高濃度標準溶液平均熒光強度的0.50%;——工作曲線線性:將工作曲線按濃度等分成5段,最高段的熒光強度差值與最低段的熒光強度差值之比,應不小于0.80。4.4樣品4.4.1樣品粒度應不大于100μm。4.4.2樣品應在105℃±5℃烘箱中烘干2h,并置于干燥器中冷卻至室溫備用。4.5試驗步驟4.5.1試料稱取0.20g試樣(4.4),精確至0.0001g。4.5.2平行試驗平行做兩份試驗。4.5.3空白試驗隨同試樣做空白試驗。4.5.4測定4.5.4.1將試料(4.5.1)置于250mL燒杯中,用少量水潤濕。加0.3g氟化氫銨(4.2.1)、10mL鹽酸(4.2.2),加蓋表皿低溫加熱溶解,蒸發(fā)至5mL,加入5mL硝酸(4.2.3),繼續(xù)加熱溶解,3GB/T8152.6—202×蒸發(fā)至5mL,加入3mL高氯酸(4.2.5),升高溫度蒸至冒濃煙至碳除完,蒸至近干,取下稍冷,加入5mL硝酸(4.2.3),用硝酸(4.2.7)吹洗表皿及杯壁,低溫加熱至可溶性鹽類溶解,取下至完全冷卻,移入100mL容量瓶中,以硝酸(4.2.7)稀釋至刻度,混勻。4.5.4.2按表1分取上述溶液(4.5.3.1)于100mL容量瓶中,補加鹽酸(4.2.2)保證溶液鹽酸濃度為10%、10mL硫脲-抗壞血酸混合溶液(4.2.9以水稀釋至刻度,混勻。室溫下放置30min。表1試樣量及分取試液體積0.01-0.252.0010mL>0.25-0.504.5.4.3采用原子熒光光譜儀,按照儀器工作條件以鹽酸(4.2.8)為載流、硼氫化鉀(4.2.11)為還原劑、氬氣為屏蔽氣和載氣,測量鉍的熒光強度,減去空白溶液的熒光強度,在工作曲線上查出鉍的質量濃度。4.5.5鉍標準曲線的繪制移取0mL、1.00mL、2.00mL、4.00mL、6.00mL、8.00mL、10.00mL鉍標準(4.2.13)于一組100mL容量瓶中、加入10mL鹽酸(4.2.2加入10mL硫脲-抗壞血酸混合溶液(4.2.10用水稀釋至刻度,混勻。在與待測試液(4.5.3.2)相同條件下,測量標準溶液的熒光強度,減去“零”濃度標準溶液的熒光強度,以鉍質量濃度為橫坐標,熒光強度為縱坐標,繪制標準曲線。4.5.6試驗數(shù)據(jù)處理鉍的含量以質量分數(shù)wBi計,數(shù)值以%表示,按式(1)計算:PV101式中:P1——自工作曲線上查得的鉍的質量濃度,單位為微克每升(μg/L);V0——試液總體積,單位為毫升(mL);V1——分取試液體積,單位為毫升(mL);V2——分取試液稀釋后的體積,單位為毫升(mLm1——試料的質量,單位為克(g)。計算結果表示至小數(shù)點后二位。若質量分數(shù)小于0.10%時,表示至小數(shù)點后三位。4.6精密度4.6.1重復性在重復性條件下獲得的兩次獨立測試結果的測定值,在表2給出的平均值范圍內(nèi),這兩個測4GB/T8152.6—202×試結果的絕對差值不超過重復性限(r),超過重復性限(r)的情況不超過5%,重復性限(r)按表2數(shù)據(jù)采用線性內(nèi)插法或外延法求得。測試的原始數(shù)據(jù)見附錄A。表2重復性限wBi/%0.0150.100.220.350.45r/%0.0020.010.020.030.034.6.2再現(xiàn)性在再現(xiàn)性條件下獲得的兩次獨立測試結果的測定值,在表3給出的平均值范圍內(nèi),這兩個測試結果的絕對差值不超過再現(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3數(shù)據(jù)采用線性內(nèi)插法或外延法求得。表3再現(xiàn)性限wBi/%0.0150.100.220.350.45R/%0.0040.020.030.050.065.方法2火焰原子吸收光譜法5.1方法提要處,使用空氣-乙炔火焰,測量鉍的吸光度,計算鉍量。5.2試劑與材料除非另有說明,在分析中僅使用確認為分析純的試劑和一級水。5.2.1氟化氫銨。5.2.2鹽酸(ρ=1.19g/mL)。5.2.3硝酸(ρ=1.42g/mL)。5.2.4氫溴酸(ρ=1.49g/mL)。5.2.5高氯酸(ρ=1.67g/mL)。5.2.6硝酸(1+1)。5.2.7鉍標準貯存溶液:稱取0.1000g鉍(wBi≥99.99%)于250mL燒杯中,加入20mL硝酸(5.2.6),蓋上表面皿,加熱至完全溶解,微沸驅除氮的氧化物,冷卻,移入100mL容量瓶中,用水稀釋至刻度,混勻。此溶液1mL含1000μg鉍。5.2.8鉍標準溶液:移取25.00mL鉍標準貯存溶液于250mL容量瓶中,加入25mL硝酸(5.2.3用水稀釋至刻度,混勻。此溶液1mL含100μg鉍。5.4儀器原子吸收光譜儀,附鉍空心陰極燈。5GB/T8152.6—202×在儀器最佳工作條件下,凡能達到下列指標者均可使用:——特征濃度:在與測量溶液基體相一致的溶液中,鉍的特征濃度應不大于0.35μg/mL;——精密度:用最高濃度的標準溶液測量10次吸光度,其標準偏差應不超過平均吸光度的1.0%,用最低濃度的標準溶液(不是“零”標準溶液)測量10次吸光度,其標準偏差應不超過最高濃度標準溶液平均吸光度的0.5%;——工作曲線的線性:將工作曲線按濃度等分成5段,最高段的吸光度差值與最低段的吸光度差值之比應不小于0.80。5.5樣品5.4.1樣品粒度應不大于100μm。5.4.2樣品應在105℃±5℃烘箱中烘干2h,并置于干燥器中冷卻至室溫備用。5.5試驗步驟稱取0.20g試樣,精確至0.0001g。5.5.2平行試驗平行做兩份試驗。5.5.3空白試驗隨同試料做空白試驗。5.5.4測定5.5.4.1將試料(5.5.1)置于250mL燒杯中,用少量水潤濕。加0.3g氟化氫銨(5.2.1)、10mL鹽酸(5.2.2),加蓋表皿低溫加熱溶解,蒸發(fā)至5mL,加入5mL硝酸(5.2.3),繼續(xù)加熱溶解,蒸發(fā)至5mL,加入3mL高氯酸(5.2.5),升高溫度蒸至冒濃煙至碳除完,蒸至近干,取下稍冷,加入5mL硝酸(5.2.3),用水吹洗表皿及杯壁,低溫加熱至可溶性鹽類溶解,取下至完全冷卻,移入50mL容量瓶中,以水稀釋至刻度,混勻。),5.5.4.2試液分取根據(jù)表4分取試液,置于100mL容量瓶中,補加相應硝酸(5.2.6)體積,用水稀釋至刻度,混勻。表4試液分取體積鉍含量,%分取試液體積,mL加入硝酸(5.2.6)體積,mL0.01~0.25//>0.25~1.0020>1.00~2.005.5.4.3使用空氣-乙炔火焰,于原子吸收光譜儀波長223.1nm處,以水調(diào)零,測量系列標準溶液的吸光度,減去系列標準溶液中“零”濃度溶液的吸光度,以鉍的濃度為橫坐標,吸光度為縱坐6GB/T8152.6—202×標繪制工作曲線。5.5.5工作曲線的繪制5.5.5.1移取0、0.50、1.00、2.00、4.00、6.00、8.00、10.00mL鉍標準溶液(5.2.8)于一組100mL容量瓶中,加入10mL硝酸(5.2.3),以水稀釋至刻度,混勻。5.5.5.2使用空氣-乙炔火焰,于原子吸收光譜儀223.1nm處,以水調(diào)零,測量系列標準溶液的吸光度,減去系列標準溶液中“零濃度”濃度溶液的吸光度,以鉍的濃度為橫坐標,吸光度為縱坐標,繪制工作曲線。5.5.6試驗數(shù)據(jù)處理鉍量以質量分數(shù)wBi計,數(shù)值以%表示,按式(2)計算:式中:P2——自工作曲線上查得的測定試液中鉍元素的質量濃度,單位為微克每毫升(μg/mL);P3——自工作曲線上查得的空白溶液中鉍元素的質量濃度,單位為微克每毫升(μg/mL);V3——試液總體積,單位為毫升(mL);V4——分取試液體積,單位為毫升(mL);V5——測定試液的體積,單位為毫升(mLm2——試料的質量,單位為克(g);計算結果表示到小數(shù)點后兩位,若質量分數(shù)小于0.10%時,表示到小數(shù)點后三位。5.6精密度在重復性條件下獲得的兩次獨立測試結果的測定值,在表5給出的平均值范圍內(nèi),這兩個測試結果的絕對差值不超過重復性限(r),超過重復性限(r)的情況不超過5%,重復性限(r)按表5數(shù)據(jù)采用線性內(nèi)插法或外延法求得。測試的原始數(shù)據(jù)見附錄A。表5重復性限wBi/%0.0150.360.56r/%0.0020.020.030.040.060.085.6.2再現(xiàn)性在再現(xiàn)性條件下獲得的兩次獨立測試結果的測定值,在表6給出的平均值范圍內(nèi),這兩個測試結果的絕對差值不超過再現(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6數(shù)據(jù)采用線性內(nèi)插法或外延法求得。表6再現(xiàn)性限7GB/T8152.6—202×wBi/%0.0150.360.56R/%0.0040.0500.0700.120.150.206.方法3Na2EDTA滴定法6.1方法提要試樣經(jīng)鹽酸、硝酸、氟化氫銨和高氯酸分解,以硫脲掩蔽銅,用抗壞血酸還原鐵(Ⅲ)和酒石酸絡合殘留的銻,在pH1.5~1.7的酸性溶液中,以Na2EDTA標準滴定溶液滴定,測其鉍量。6.2試劑和材料除非另有說明,本文件中所用試劑均為分析純及以上純度的試劑,所用水符合GB/T6682規(guī)定的三級及以上純度的水。6.2.1抗壞血酸。6.2.2氟化氫銨。6.2.3鹽酸(ρ=1.19g/mL)。6.2.4硝酸(ρ=1.42g/mL)。6.2.5氫溴酸(ρ=1.49g/mL)。6.2.6高氯酸(ρ=1.67g/mL)。6.2.7硝酸(1+1)。6.2.8硝酸(1+2)。6.2.9硝酸(4+96)。6.2.10乙酸鈉飽和溶液。6.2.11硫脲飽和溶液。6.2.12酒石酸溶液(100g/L)。6.2.13乙二胺四乙酸二鈉(Na2EDTA)標準滴定溶液(0.01mol/L)。6.2.13.1配制:稱取3.8gNa2EDTA置于300mL燒杯中,加水微熱溶解,冷卻至室溫,移入1000mL容量瓶中,用水稀釋至刻度,混勻。放置三天后標定。6.2.13.2標定:移取20.00mL鉍標準溶液(6.2.14)三份,分別置于250mL三角燒杯中,加入約100mL水,加入0.2g抗壞血酸(6.2.1)、5mL硫脲飽和溶液(6.2.11)、5mL酒石酸溶液(6.2.12搖勻,用Na2EDTA標準滴定溶液(6.2.13)滴定至黃色變淺,加2~3滴二甲酚橙指示劑(6.2.15用乙酸鈉飽和溶液(6.2.10)調(diào)節(jié)pH為1.5~1.7(用pH計測量),繼續(xù)用Na2EDTA標準滴定溶液(6.2.13)滴定至紅色變?yōu)榱咙S色為終點。按公式(3)計算Na2EDTA標準滴定溶液的濃度:8GB/T8152.6—202×式中:C——Na2EDTA標準滴定溶液的濃度,單位為摩爾每升(mol/L);p4——鉍標準溶液的濃度,單位為毫克每毫升(mg/mL);V7——移取鉍標準溶液的體積,單位為毫升(mL);208.98——鉍的摩爾質量,單位為克每摩爾(g/molV8——滴定標準溶液時所消耗的Na2EDTA標準滴定溶液的體積,單位為毫升(mLV6——滴定空白時所消耗的Na2EDTA標準滴定溶液的體積,單位為毫升(mL)。取三次標定結果的平均值作為標準滴定溶液的濃度,保留四位有效數(shù)字。三次標定結果的極差值應不大于5×10-5mol/L,否則重新標定。6.2.14鉍標準溶液(1.0000mg/mL):稱取0.5000g金屬鉍(wBi≥99.99%)置于250mL燒杯中,加入100mL硝酸(6.2.8),蓋上表皿,低溫加熱溶解至完全,取下冷卻至室溫,用硝酸(6.2.9)吹洗杯壁及表皿,移入500mL容量瓶中,并用硝酸(6.2.9)稀釋至刻度,搖勻。此溶液1mL含1.0000mg鉍。6.2.15二甲酚橙指示劑(5g/L)。6.3樣品6.3.1.粒度應不大于100μm。6.3.2樣品應在105℃±5℃烘箱中烘干2h,并置于干燥器中冷卻至室溫備用。6.4試驗步驟6.4.1試料稱取0.20g試樣,精確至0.0001g。6.4.2平行試驗平行做兩份試驗。6.4.3空白試驗隨同試料做空白試驗。6.4.4測定6.4.4.1將試料(6.4.1)置于250mL燒杯中,用少量水潤濕。加0.3g氟化氫銨(6.2.2)、10mL鹽酸(6.2.3),加蓋表皿低溫加熱溶解,蒸發(fā)至5mL,加5mL硝酸(6.2.4),繼續(xù)加熱溶解,蒸發(fā)至5mL,加3mL高氯酸(6.2.6),升高溫度蒸至冒濃煙至碳除完,取下稍冷,加5mL硝酸(6.2.4),用硝酸(6.2.9)吹洗表皿及杯壁,加熱煮沸使可溶性鹽類溶解,取下,冷卻至室溫。),6.4.4.2加入約100mL水,加入0.2g抗壞血酸(6.2.1)、5mL硫脲飽和溶液(6.2.11)、5mL酒石酸溶液(6.2.12),搖勻,用乙酸鈉飽和溶液(6.2.10)調(diào)節(jié)pH為1.5~1.7(用pH計測量),加2~3滴二甲酚橙指示劑(6.2.15),用Na2EDTA標準滴定溶液(6.2.13)滴定至紅色變?yōu)榱咙S9GB/T8152.6—202×色為終點。6.4.5試驗數(shù)據(jù)處理鉍含量以鉍的質量分數(shù)wBi計,按公式(4)計算:式中:c——Na2EDTA標準滴定溶液的濃度,單位為摩爾每升(mol/L);V9——滴定試樣溶液時所消耗的Na2EDTA標準滴定溶液的體積,單位為毫升(mL);V10——滴定空白溶液時所消耗的Na2EDTA標準滴定溶液的體積,單位為毫升(mL208.98——鉍的摩爾質量,單位為克每摩爾(g/mol);m3——試樣的質量,單位為克(g計算結果表示到小數(shù)點后2位。6.5精密度6.5.1重復性在重復性條件下獲得的兩次獨立測試結果的測定值,在表7給出的平均值范圍內(nèi),這兩個測試結果的絕對差值不超過重復性限(r),超過重復性限(r)的情況不超過5%,重復性限(r)按表5數(shù)據(jù)采用線性內(nèi)插法或外延法求得。測試的原始數(shù)據(jù)見附錄A。表5重復性限wBi/%2.193.065.709.53r/%0.090.100.176.5.2再現(xiàn)性在再現(xiàn)性條件下獲得的兩次獨立測試結果的測定值,在表6給出的平均值范圍內(nèi),這兩個測試結果的絕對差值不超過再現(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6數(shù)據(jù)采用線性內(nèi)插法或外延法求得。表6再現(xiàn)性限wBi/%2.183.065.709.53R/%0.210.230.280.357試驗報告試驗報告至少應給出以下幾個方面的內(nèi)容:──試驗對象;──本文件編號;──分析結果及其表示;GB/T8152.6—202×──與基本試驗步驟的差異;──觀察到的異常現(xiàn)象;──試驗日期。GB/T8152.6—202×(資料性)精密度試驗原始數(shù)據(jù)精密度數(shù)據(jù)是2024年由15~18家實驗室對鉍含量的3個~6個不同水平樣品進行共同試驗確定的。每個實驗室對每個水平的鉍含量在重復性條件下獨立測定11次。測試的原始數(shù)據(jù)見表A.1~表A.3。表A.1方法一精密度試驗原始數(shù)據(jù)實驗室i水平1水平2水平3水平4水平510.01380.09600.212*0.3360.4380.01390.09730.2160.3360.4390.01410.09730.2170.3410.4400.01420.09870.2170.3430.4410.01420.09890.2170.3440.4440.01440.09940.2180.3460.4460.01480.09980.2180.3510.4480.01490.1010.2190.3520.4510.01500.1020.2190.3580.4540.01520.1030.2200.3580.4540.01530.1040.2210.3590.45420.01290.09810.2100.3370.4350.01300.09850.2130.3390.4370.01330.09870.2140.3390.4400.01340.09890.2150.3450.4440.01340.09950.2160.3450.4470.01350.09960.2170.3460.4480.01360.09960.2180.3490.4490.01370.1010.2180.3520.4510.01380.1010.2180.3570.4520.01380.1020.2200.3580.4550.01390.1030.2210.3590.46030.01430.0955**0.2080.349*0.455**0.01440.0990**0.2090.352*0.459**0.01470.0998**0.2100.358*0.468**0.01480.101**0.2130.359*0.471**0.01490.2180.362*0.479**0.01500.2190.369*0.483**0.01520.2190.369*0.486**0.01530.2200.371*0.489**0.01550.2220.375*0.494**0.01560.2230.375*0.498**0.01600.2330.383*0.506**40.01330.09310.218*0.361*0.483**0.01340.09320.218*0.362*0.485**GB/T8152.6—202×0.01360.09760.220*0.362*0.487**0.01360.09920.230*0.378*0.487**0.01370.09920.231*0.381*0.501**0.01370.1000.233*0.381*0.502**0.01380.1000.234*0.383*0.506**0.01390.1010.237*0.384*0.512**0.01400.1030.237*0.384*0.512**0.01400.1040.239*0.387*0.513**0.01410.1060.240*0.387*0.515**50.01410.09950.2150.3530.4490.01420.1000.2170.3560.4520.01430.1010.2190.3600.4530.01440.1020.2190.3640.4530.01450.1030.2200.3640.4560.01460.1030.2210.3660.4560.01460.1030.2210.3670.4560.01480.1040.2230.3690.4570.01510.1040.2240.3700.4590.01510.1050.2250.3700.4610.01540.1070.231**0.3720.46160.01470.1010.2150.3410.4450.01470.1020.2160.3420.4490.01480.1020.2170.3450.4490.01490.1020.2190.3480.4500.01490.1030.2200.3490.4510.01490.1030.2210.3520.4510.01490.1040.2210.3520.4540.01510.1050.2230.3520.4570.01510.1060.2240.3540.4600.01530.1070.2260.3560.4610.01530.1080.2270.3630.46470.01300.0940.2260.3620.484**0.01340.0950.2270.3650.489**0.01350.0950.2270.3660.490**0.01350.0950.2270.3660.492**0.01350.0950.2270.3660.492**0.01360.0960.2270.3680.492**0.01360.0970.2280.3680.492**0.01370.0980.2290.3700.493**0.01430.0990.2290.3710.493**0.01440.1000.2290.3760.495**0.01450.1010.2290.3770.495**80.01400.09500.200**0.3300.440GB/T8152.6—202×0.01400.09600.210**0.3400.4400.01400.09700.210**0.3500.4400.01400.09900.210**0.3500.4400.01400.09900.210**0.3500.4500.01500.1000.210**0.3600.4500.01500.1010.210**0.3600.4500.01500.1020.220**0.3600.4600.01500.1040.220**0.3600.4600.01500.1050.230**0.3600.4600.01600.1060.240**0.3600.46090.0132**0.0952*0.2160.3390.4330.0138**0.0959*0.2190.3430.4410.0139**0.0965*0.2190.3470.4430.0142**0.0986*0.2190.3480.4460.0147**0.101*0.2230.3490.4470.0149**0.2250.3550.4470.0152**0.2250.3560.4490.0155**0.2270.3580.4540.0158**0.2280.3580.4540.0159**0.2280.3590.4560.0162**0.2320.3620.4620.01450.0970*0.2190.3530.4400.01490.0990*0.2190.3560.4420.01510.2210.3580.4450.01520.2210.3590.4460.01520.2230.3610.4460.01520.2240.3620.4470.01540.2240.3650.4470.01550.2250.3650.4480.01550.2250.3660.4500.01560.2270.3670.4530.01590.235*0.3690.4540.01360.09600.2080.3290.4320.01380.09680.2140.3360.4370.01400.09760.2150.3360.4400.01410.09820.2160.3380.4410.01420.1000.2170.3410.4430.01420.1010.2190.3440.4460.01440.1020.2230.3450.4520.01470.1030.2240.3470.4560.01490.1040.2250.3480.4580.01500.1050.2260.3510.4590.01530.1060.2270.3590.461GB/T8152.6—202×0.0130**0.09830.2060.3410.4510.0137**0.09870.2070.3460.4520.0143**0.09900.2090.3470.4560.0155**0.09950.2090.3490.4570.0156**0.09970.2100.3500.4570.0158**0.09970.2100.3500.4580.0159**0.1000.2130.3510.4590.0159**0.1000.2140.3520.4590.0159**0.1000.2150.3550.4620.0160**0.1000.2160.3560.4620.0161**0.1010.2190.3580.4630.01280.1020.2080.3480.4380.01280.1040.2100.3480.4390.01320.1050.2110.3500.4440.01340.1050.2130.3510.4480.01340.1050.2170.3510.4490.01350.1070.2170.3510.4510.01350.1080.2180.3530.4520.01350.1100.2180.3540.4520.01350.1100.2180.3540.4520.01380.1100.2230.3550.4560.01400.2240.3560.4580.01410.09720.2100.3430.4390.01410.09830.2100.3460.4410.01430.09840.2100.3460.4410.01460.09870.2120.3490.4410.01460.09890.2150.3490.4430.01460.09980.2160.3490.4470.01480.1000.2160.3530.4490.01480.1000.2170.3550.4490.01490.1010.2180.3550.4500.01510.1020.2200.3570.4510.01590.1040.2200.3580.4540.01580.09840.2140.3280.4340.01590.09850.2150.3330.4440.01600.09930.2160.3380.4440.01620.09980.2160.3460.4450.01630.1000.2170.3490.4460.01640.1010.2170.3490.4460.01650.1010.2180.3500.4470.01660.1020.2200.3510.4480.01670.1020.2220.3540.4480.01670.1020.2220.3550.452GB/T8152.6—202×0.01720.1020.2250.3600.4580.01320.09350.3280.4320.01330.09360.3300.4340.01340.09390.3300.4360.01350.09410.200*0.3310.4380.01350.09420.203*0.3370.4400.01400.09550.204*0.3380.4420.01420.09720.205*0.3420.4420.01420.09870.208*0.3440.4450.01430.09890.210*0.3490.4480.01440.09890.218*0.3520.4500.01450.1040.219*0.3550.465*0.01550.09900.2180.3430.4380.01570.1000.2190.3440.4410.01580.1020.2210.3480.4460.01590.1030.2220.3500.4490.01600.1030.2230.3510.4510.01630.1050.2250.3520.4520.01630.1060.2270.3530.4530.01640.1060.2280.3550.4550.01660.1070.2290.3560.4560.01700.1090.2300.3590.4590.01720.2330.3620.4600.01370.09720.2070.3300.4340.01370.09730.2080.3360.4380.01380.09790.2100.3390.4410.01380.09890.2100.3390.4410.01390.09910.2110.3390.4450.01400.09950.2130.3410.4460.01410.09950.2150.3420.4520.01450.1000.2150.3450.4530.01490.1000.2170.3470.4560.01490.1030.2180.3520.4610.01490.1040.2190.3560.468實驗室i水平1水平2水平3水平4水平5水平610.01420.3480.5440.9640.01470.3510.5530.9730.01480.3530.5560.9890.01490.3540.5570.9910.01510.3560.5610.9920.01530.3570.5660.993GB/T8152.6—202×0.01560.3610.5680.01570.3630.5710.01610.3650.5712.0010.01620.3660.5732.0040.01660.3680.5752.02020.01510.3470.5340.9640.01520.3470.5430.9730.01550.3530.5520.9830.01550.3540.5530.9860.01600.3550.5570.9940.01600.3580.5580.01610.3590.5590.01650.3600.5590.01650.3680.5630.01710.3710.5660.01720.3710.5702.01330.01400.3290.561**0.9871.280**1.850**0.01420.3380.569**0.9951.290**1.860**0.01430.3390.570**0.9961.30**1.870**0.01440.3410.575**0.9981.320**1.90**0.01450.3470.581**1.340**1.920**0.01460.3490.583**1.350**1.930**0.01470.3520.585**1.360**1.940**0.01480.3560.587**1.370**1.950**0.01490.3590.588**1.380**1.980**0.01510.3600.590**1.380**1.990**0.01520.3670.591**1.40**2.00**40.01460.3490.5440.9810.01470.3530.5530.9850.01500.3550.5580.9860.01530.3580.5610.9950.01530.3590.5610.9960.01550.3610.5620.01580.3620.5620.01600.3620.5640.01620.3630.5692.0120.01660.3640.5722.0140.01680.3660.5752.03450.0151*0.3470.5440.9880.0154*0.3550.5590.9890.0157*0.3560.5620.9900.0161*0.3560.5630.9940.0162*0.3590.5630.996GB/T8152.6—202×0.0164*0.3600.5640.9980.0170*0.3610.5670.9980.0172*0.3630.5680.0172*0.3650.5710.0175*0.3670.5732.0030.0177*0.3680.5742.00560.01480.3530.5460.9730.01490.3530.5550.9860.01490.3540.5580.9870.01510.3550.5580.9880.01520.3550.5640.9970.01530.3580.5660.9990.01550.3620.5680.01550.3620.5720.01620.3660.5762.0050.01620.3690.5762.0130.01670.3710.5772.01570.01420.3560.535**0.9510.01440.3590.5580.9590.01470.3620.5580.9800.01510.3620.5590.9820.01520.3630.5620.9830.01520.3630.5650.9850.01530.3630.5650.9860.01580.3630.5660.9890.01590.3640.5660.01600.3670.5670.01690.3680.56780.01500.3500.5400.9800.01500.3500.5400.9800.01500.3500.5400.9900.01500.3500.5400.9900.01500.3600.5500.9900.01500.3600.5500.01500.3600.5500.01600.3600.5500.01600.3600.5700.01600.3600.5700.01600.3600.57090.0144*0.3460.5530.9870.01520.3470.5570.9890.01580.3480.5570.9980.01580.3530.557GB/T8152.6—202×0.01590.3540.5610.01600.3550.5620.01620.3560.5630.01630.3580.5660.01640.3590.5682.0010.01650.3600.5682.0040.01670.3650.5712.0080.0137*0.3660.562*0.0138*0.3660.568*0.0139*0.3660.570*0.0139*0.3670.572*0.0140*0.3670.573*0.0140*0.3670.574*2.0010.0140*0.3670.575*2.0090.0141*0.3680.575*2.0120.0141*0.3680.576*2.0140.0141*0.3690.577*2.0240.0142*0.3690.583**2.0390.01380.3360.5400.9731.263*0.01390.3410.5460.9801.287*0.01410.3420.5490.9881.289*0.01420.3440.5510.9921.304*0.01420.3460.5520.9961.315*0.01440.3480.5530.9981.326*0.01450.3510.5571.327*0.01480.3520.5621.338*0.01510.3580.5661.341*0.01520.3590.5711.347*0.01530.3600.5751.385*0.0147**0.3610.5681.014**1.268**1.848**0.0152**0.3620.5701.026**1.279**1.849**0.0153**0.3630.5711.040**1.287**1.862**0.0155**0.3640.5721.040**1.289**1.869**0.0156**0.3710.5741.043**1.290**1.877**0.0156**0.3730.5751.044**1.292**1.880**0.0162**0.3730.5771.048**1.294**1.881**0.0165**0.3740.5781.058**1.295**1.885**0.0171**0.3800.5781.060**1.308**1.905**0.0174**0.3820.5791.060**1.315**1.911**0.0178**0.3860.5801.062**1.320**1.920**0.0134*0.3500.5480.9980.0135*0.3510.5520.9980.0136*0.3510.557GB/T8152.6—202×0.0136*0.3540.5580.0136*0.3540.5650.0138*0.3580.5660.0138*0.3580.5670.0140*0.3600.5680.0143*0.3600.5680.0148*0.3610.5700.015*0.3650.5710.01510.3510.522**0.9691.3041.9310.01530.3530.523**0.9701.3331.9410.01540.3590.532**0.9721.3411.9440.01550.3590.534**0.9781.3431.9630.01570.3590.542**0.9821.3451.9730.01570.3590.543**0.9991.3631.9790.01590.3600.556**1.0011.3711.9830.01610.3630.560**1.0011.3731.9890.01620.3660.562**1.0031.3781.9910.01620.3670.567**1.0051.3822.0010.01620.3690.572**1.0101.3852.0040.01460.3490.526**0.9730.01480.3490.536**0.9790.01490.3530.548**0.9860.01520.3570.550**0.9960.01530.3570.558**0.9960.01540.3580.562**0.9990.01550.3580.563**0.01580.3600.568**0.01590.3610.573**0.01620.3610.574**2.0060.01630.3680.574**2.0120.01450.3440.5360.9751.3111.9120.01480.3480.5410.9791.3251.9550.01490.3490.5470.9801.3411.9840.01500.3550.5490.9851.3321.9670.01500.3570.5520.9871.3311.9450.01560.3600.5540.9891.3391.9330.01580.3610.5560.9891.3411.9550.01600.3650.5560.9901.3421.9450.01640.3650.5620.9921.3451.9770.01650.3680.5640.9951.3351.9650.01660.3690.5660.9991.3441.9590.01440.3620.5410.9610.01490.3620.5490.968GB/T8152.6—202×0.01500.3670.5580.9760.01510.3680.5590.9810.01560.3690.5590.9870.01560.3700.5620.9920.01570.3710.5620.9950.01600.3720.5630.9980.01600.3740.5640.01610.3810.5660.01650.3840.5720.01420.338**0.5410.9671.287*1.934*0.01430.338**0.5410.9681.321*1.945*0.01470.34**0.5420.9791.325*1.947*0.01470.347**0.5490.9801.341*1.947*0.01480.350**0.5490.9821.356*1.952*0.01480.351**0.5520.9891.364*1.972*0.01510.352**0.5530.9901.364*1.980*0.01530.356**0.5630.9921.368*2.012*0.01530.361**0.5671.394*2.028*0.01550.367**0.5691.398*2.036*0.01550.368**0.5711.402*2.037*實驗室i水平1水平2水平3水平412.1843.0005.6389.4512.2113.0205.6459.4602.2523.0385.6579.4662.1653.0515.6969.4672.1763.0545.7009.4772.1983.0755.7129.4942.2193.0775.7229.5042.1803.0865.7239.5232.2013.1155.7239.5452.1623.1155.7359.5652.2113.1195.8019.59522.1483.0325.6379.4482.1483.0325.6409.4602.1583.0865.6439.4652.1663.0895.6839.4682.1683.0925.6869.4782.1833.1015.7189.5112.1853.1095.7449.5202.2133.1105.7939.5262.2173.1125.7939.534GB/T8152.6—202×2.2483.1125.7959.5402.2493.1225.7989.60232.0803.0505.6309.4802.1003.0505.6909.4902.1103.0605.6909.5002.1203.0605.7009.5002.1203.0705.7209.5202.1403.0805.7309.5302.1503.0805.7409.5502.1603.0905.7509.5602.1703.1105.7709.6002.1803.1205.7909.6102.1903.1505.8009.65042.119*3.0125.6499.4532.1633.0335.6859.4792.1763.0455.6879.4862.1853.0645.6989.4952.1883.0725.6999.5012.1953.0765.7019.5032.1983.0835.7129.5052.1983.0895.7369.5132.2033.0965.7539.5172.2053.1035.7769.5262.2153.1055.8069.53452.098**3.000**5.5659.3982.108**3.002**5.6509.4462.144**3.013**5.6709.4562.156**3.023**5.6749.4862.198**3.039**5.6989.4922.203**3.056**5.7009.5132.221**3.098**5.7039.5232.221**3.132**5.7179.5632.236**3.134**5.7359.5652.237**3.146**5.7439.5702.256**3.170**5.8029.651*62.1383.0455.6349.4782.1593.0505.6749.4862.1593.0525.6889.4882.1633.0545.7009.4972.1663.0665.7069.4982.1683.0685.7319.5122.1683.0685.7319.5362.1803.0905.7489.555GB/T8152.6—202×2.1833.1125.7529.5572.1833.1145.7569.5822.1863.1185.7609.60872.1783.0015.7159.5052.1873.0085.7669.5312.2163.0095.7679.5492.2173.0125.7849.5772.2273.0535.7879.5782.2343.0565.7979.5782.2343.0605.7989.5852.2443.0695.8219.6352.2573.0795.8629.6382.2633.0845.8709.6392.2643.1125.8879.64282.1602.9805.5709.4702.1702.9905.5709.4802.1803.0005.6109.4902.1903.0305.6309.5302.1903.0405.6509.5502.2003.0605.6509.5602.2103.0705.6609.5902.2103.0755.6809.6102.2303.0805.6809.6302.2303.0905.7009.6602.2503.0905.7309.66092.1113.0175.6379.3522.1493.0335.6569.4012.1553.0595.6849.4392.1693.0695.6919.4622.1753.0725.7219.4892.1843.0935.7239.5112.1913.0935.7249.5172.1973.1005.7399.5232.2213.1015.7449.5612.2233.1045.

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