第5部分：鉛、銅、鎘、鈷含量的測定編制說明（預(yù)審稿）主編單位：葫蘆島鋅業(yè)股份有限公司2025年9月(XXXXXXXXXXXXX)第頁1.1任務(wù)由葫蘆島鋅業(yè)股份有限公司起草，深圳市中金嶺南有色股份有限公司韶關(guān)冶煉廠、昆明冶金研究院有限公司、水口山有色金屬有限責任公司湖南水口山有色金屬有限責任公司、紫金礦業(yè)集團股份有限公司、山西北方銅業(yè)有限公司、河南豫光金鉛股份有限公司、大冶有色設(shè)計研究院有限公司、云南華聯(lián)鋅銦股份有限公司、株洲冶煉集團股份有限公司、中國檢驗認證集團廣西有限公司、湖南有色金屬研究院有限責任公司、北礦檢測技術(shù)股份有限公司、銅陵有色金屬集團有限公司、國標(北京)檢驗認證有限公司、云南馳宏鋅鍺股份有限公司、中國有色桂林礦產(chǎn)地質(zhì)研究院有限公司、長沙礦冶院檢測技術(shù)有限責任公司、中國檢驗認證集團廣東黃埔有限公司、江西銅業(yè)鉛鋅金屬有限公司。本標準主要起草人及工作職責見表1。表1本標準主要起草人及工作職責序號單位名稱人員起草或驗證情況1葫蘆島鋅業(yè)股份有限公司XXXX起草單位2深圳市中金嶺南有色金屬股份有限公司韶關(guān)冶煉廠何劍文黃曉玲一驗單位3昆明冶金研究院有限公司阮淑呈一驗單位4湖南水口山有色金屬有限責任公司羅永鋒蹇金英一驗單位5紫金礦業(yè)集團股份有限公司一驗單位6山西北方銅業(yè)有限公司一驗單位7河南豫光金鉛股份有限公司尹玉環(huán)王九菊一驗單位8大冶有色設(shè)計研究院有限公司馮加豪王永彬一驗單位9云南華聯(lián)鋅銦股份有限公司一驗單位10株洲冶煉集團股份有限公司路蹀方子儀二驗單位11中國檢驗認證集團廣西有限公司張璐二驗單位12湖南有色金屬研究院有限責任公司李艷唐飛燕二驗單位13北礦檢測技術(shù)股份有限公司宋凱悅二驗單位14銅陵有色金屬集團控股有限公司二驗單位15國標(北京)檢驗認證有限公司朱澤坤于磊二驗單位16云南馳宏鋅鍺股份有限公司二驗單位17中國有色桂林礦產(chǎn)地質(zhì)研究院有限公司王蔣亮廖云安二驗單位18長沙礦冶院檢測技術(shù)有限責任公司龔健易嘉二驗單位19中國檢驗認證集團廣東黃埔有限公司二驗單位20江西銅業(yè)鉛鋅金屬有限公司二驗單位1.3主要工作過程(1)根據(jù)工業(yè)和信息化部標準計劃項目()的安排要求，》起草任務(wù)，(2)2023年11月，確定標準制訂方案和研制計劃進度計劃。(3)2024年1月，，(4)年2月～2024年6月，開展方法試驗工作，先后完成了樣品溶解方法試驗、條件選擇試驗、共存元素干擾試驗、加標回收試驗和精密度試驗等研究，(5)年8月，陸續(xù)收到各驗證單位的試驗報告及反饋意見，根據(jù)驗證單位的反饋進行數(shù)理統(tǒng)計分析確定測定方法及測定范圍。采用操作簡便、精密度高、準確度好、在行業(yè)內(nèi)應(yīng)用普及的分析方法，能很好的滿足行業(yè)對鋅精礦中鉛、銅、鎘、鈷含量的測定要求，提高了本標準的可操作性和適用性。為此，對試料量、試液體積、分取體積、測定體積及補加鹽酸量作了相應(yīng)調(diào)整。表SEQ表\*ARABIC2元素種類和測量范圍表質(zhì)量分數(shù)%試樣質(zhì)量g試樣總體積mL分取體積mL測定試液體積mL分取后補加硝酸（3.4）體積mLCo>0.0020～0.0101.0025Co>0.010～0.0500.4050Pb、Cu、Cd>0.10～0.50Co>0.050～0.200.20100Pb、Cu>0.50～2.50Cd>0.50～2.000.201002010010Pb>2.50～6.00Cu>2.50～5.000.20100510010在GB/T8151-2012鋅精礦化學分析方法中第5、6、8、16部分，試料用鹽酸、硝酸分解，未考慮樣品中硅、碳含量高時對試樣的測定的影響。實際調(diào)研發(fā)現(xiàn)，鋅精礦中硅含量最高可達10%，也有特殊樣品含碳量較高，還有難溶樣品，如果不進行處理，樣品混濁影響測試結(jié)果。因此，試驗選擇加入1～5mL氟化氫銨飽和溶液（3.5），加入15mL鹽酸(3.1),加5mL硝酸(3.2)溶解試樣（試樣含碳量較高或有難溶雜質(zhì)，分次加入2mL高氯酸重復(fù)處理）。選取代表樣品含碳樣品2#、8#，難溶樣品10#、15#,進行溶樣方法試驗，試驗結(jié)果見表3。表3含碳樣品、難溶樣品的溶解方式樣品編號鹽酸+硝酸鹽酸+硝酸+高氯酸2#、8#樣品溶解不完全，有較多黑色殘渣懸浮溶液表面樣品溶解徹底，沒有黑色殘渣10#、15#樣品溶解不完全，底部有些許黑色殘樣品溶解徹底，沒有黑色殘渣試驗表明：采用鹽酸-硝酸溶解樣品，溶液有較多黒碳漂浮物及少量殘渣；采用鹽酸-硝酸-高氯酸溶解樣品，溶樣清亮，樣品溶解完全，因此含碳樣品及難溶樣品需要加高氯酸，否則溶解不完全。正常樣品（不含碳且易溶解）加高氯酸和不加高氯酸測試銅含量的數(shù)據(jù)對照。選取代表樣品4#、5#、7#、9#，試驗結(jié)果見表4。表4加高氯酸和不加高氯酸銅含量測試數(shù)據(jù)對照樣品編號鹽酸+硝酸鹽酸+硝酸+高氯酸4#1.291.275#0.110.117#0.500.499#4.984.85試驗表明：加入高氯酸后銅的結(jié)果沒有變化，同時加入高氯酸后延長溶解樣品時間，所以不含碳及易溶解樣品不需要加入高氯酸。SiO2選取代表2#（含SiO25%）、5#（含SiO27%）、11#（含SiO210%），鉛、鎘、銅試驗結(jié)果見表5。表5含硅樣品的溶解方式測試鉛、鎘、銅（%）樣品編號含SiO2量稱樣量體積鹽酸+硝酸鹽酸+硝酸+氟化氫銨PbCuCdPbCuCd2#5%0.2000g100mL1.061.150.281.131.120.295#7%0.2000g100mL1.950.120.162.040.120.1611#10%0.2000g100mL0.130.100.280.120.110.27溶液現(xiàn)象稍有渾濁清澈試驗表明：鋅精礦樣品測試鉛鎘銅，雖然SiO2含量不同，由于稱樣量為0.2000g，溶液均為稍有渾濁，加入氟化氫銨飽和溶液后，溶液清澈，便于測試，不易造成儀器堵塞。由試驗數(shù)據(jù)可見加入氟化氫銨對鉛、鎘、銅的數(shù)值沒有影響，因鋅精礦大部分含SiO2，因此溶解樣品時加入適量氟化氫銨可使樣品溶解效果更好。選取代表樣品2#（含SiO25%）、5#（含SiO27%）、11#（含SiO210%）、15#（含SiO20.6%），鈷含量試驗結(jié)果見表6。表6含SiO2樣品的溶解方式測試鈷（%）樣品編號含硅量稱樣量體積鹽酸+硝酸鹽酸+硝酸+氟化氫銨15#0.6%1.00g25mL0.00510.006215#0.6%1.00g25mL0.00560.00682#5%1.00g25mL0.00320.00362#5%1.00g25mL0.00340.00385#7%1.00g25mL0.00550.00585#7%1.00g25mL0.00520.0056溶液現(xiàn)象樣品溶解不徹底，溶液呈渾濁狀態(tài)。樣品溶解徹底，底部有少許不溶物。11#10%0.400g50mL0.0170.01811#10%0.400g50mL0.0180.017溶液現(xiàn)象樣品溶解不徹底，溶液少許渾濁。樣品溶解徹底。試驗表明：11#樣品稱樣量為0.40g,含硅量為10%時，加入氟化氫銨對測試結(jié)果沒有影響，當樣品稱樣量為1.00g時，不論含硅量高低，加入氟化氫銨后結(jié)果偏高。由此可知：當稱樣量越高，瓶體積越小，溶液越渾濁，加入氟化氫銨后可使試樣溶解更徹底，否則結(jié)果偏低。選取代表樣品2#、5#、15#測試鉛、鎘、銅、鈷，分別加入0～5mL飽和氟化氫銨溶液，試驗結(jié)果見表7和表8。表7飽和氟化氫銨加入量測試鉛、鎘、銅的結(jié)果（%）樣品編號含SiO2量稱樣量體積飽和氟化氫銨加入量0mL1mL2mLPbCuCdPbCuCdPbCuCd2#5%0.20g100mL1.061.150.281.151.120.281.131.100.285#7%0.20g100mL1.970.120.161.920.110.162.000.110.1711#10%0.20g100mL0.130.100.280.130.110.290.140.100.28溶液現(xiàn)象稍有渾濁清澈清澈樣品編號含SiO2量稱樣量體積飽和氟化氫銨加入量3mL4mL5mLPbCuCdPbCuCdPbCuCd2#5%0.20g100mL1.081.120.281.121.090.291.121.100.275#7%0.20g100mL1.960.120.161.950.110.162.000.120.1611#10%0.20g100mL0.130.110.270.130.100.280.130.100.28溶液現(xiàn)象清澈清澈清澈試驗表明：鋅精礦樣品測試鉛鎘銅，加入不同量的飽和氟化氫銨加對鉛鎘銅測試的結(jié)果沒有影響，不加飽和氟化氫銨溶液均為稍有渾濁，加入氟化氫銨飽和溶液后，溶液清澈，便于測試，不易造成儀器堵塞。表8飽和氟化氫銨加入量鈷的試驗結(jié)果%樣品編號含硅量稱樣量體積0mL1mL2mL3mL4mL5mL8#2.5%0.20g100mL0.0820.0830.0850.0900.0800.079實驗現(xiàn)象稍有渾濁清澈清澈清澈清澈清澈2#5%1.00g25mL0.00320.00410.00380.00380.00370.0037實驗現(xiàn)象渾濁渾濁渾濁稍有渾濁稍有渾濁較清澈清澈5#7%1.00g25mL0.00550.00590.00620.00580.00590.0059實驗現(xiàn)象渾濁渾濁渾濁稍有渾濁稍有渾濁較清澈清澈11#10%0.40g50mL0.170.170.190.180.180.17實驗現(xiàn)象稍有渾濁稍有渾濁較清澈清澈較清澈清澈清澈清澈試驗表明：當樣品稱樣量為1.00g時，只要加入飽和氟化氫銨溶液，鈷的測試結(jié)果偏高，隨著飽和氟化氫銨溶液加入量的增加溶液逐漸清澈。當樣品稱樣量為0.40和0.20g時，飽和氟化氫銨溶液對測試結(jié)果沒有影響，隨著飽和氟化氫銨溶液加入量的增加溶液逐漸清澈。鈷的測定范圍0.0020%～0.20%，將Co含量為0.0020%～0.010%的稱樣量改為0.5g進25mL容量瓶，鈷的標準第一點標準應(yīng)改為0.4μg/mL，測試結(jié)果見表22表9鈷的測試結(jié)果（%）樣品結(jié)果0.4μg/mL0.420.4μg/mL0.400.4μg/mL0.480.4μg/mL0.350.4μg/mL0.330.4μg/mL0.420.4μg/mL0.380.4μg/mL0.400.4μg/mL0.380.4μg/mL0.39試驗表明：將Co0.0020～0.010的稱樣量改為0.5g進25ml容量瓶，樣品濃度變低接近測定下限，測試結(jié)果不穩(wěn)定。3.3.1本試驗采用硝酸介質(zhì)測定，試驗考察了介質(zhì)硝酸濃度對測定結(jié)果的影響。選取5#樣品和4.00μg/mL鉛、銅、鎘標準溶液，1.60μg/mL鈷標準溶液，在硝酸不同的體積分數(shù)下進行測定，結(jié)果見表9。表10酸度的影響樣品或標準溶液5%硝酸10%硝酸15%硝酸20%硝酸5#Pb(%)2.002.051.98-5#Cu(%)0.120.110.12-5#Cd(%)0.160.160.17-5#Co(%)0.00580.00590.00600.00614.00(μg/mL)Pb4.023.983.99-4.00(μg/mL)Cu4.003.969.98-4.00(μg/mL)Cd3.983.984.02-1.60(μg/mL)Co1.621.611.581.60試驗表明，硝酸的體積分數(shù)為5%、10%、15%對鉛、銅、鎘、鈷的測定無明顯影響。硝酸的體積分數(shù)為20%對鈷的測定無明顯影響，本試驗選擇硝酸的體積分數(shù)5%的溶液作為鉛、銅、鎘的測定介質(zhì)，選擇硝酸的體積分數(shù)5%或20%的溶液作為鈷的測定介質(zhì)。分別向鉛標準溶液（2.00）、銅標準溶液（2.00）、鎘標準溶液（2.00）、鈷標準溶液（0.80）中，按表20加入共存元素，加入10mL硝酸（3.4），用水稀釋至刻度，混勻?？疾旄鞴泊嬖貙︺U、銅、鎘、鈷的測定的影響。試驗結(jié)果見表11。表11共存元素對Pb、Cu、Cd、Co的影響干擾元素Pb2.00μg/mLPb6.00μg/mLCu2.00μg/mLCu6.00μg/mLCd2.00μg/mLCd6.00μg/mLCo0.80μg/mLCo2.40μg/mLZn120mg1.976.042.015.982.006.020.822.42Fe40mg1.985.961.946.011.985.960.792.38As4mg2.015.991.985.982.025.950.802.39F1mg1.996.012.025.952.035.940.812.41Sn1mg1.995.981.966.031.976.000.822.44Sb0.4mg2.006.021.996.061.996.020.782.38Ag0.2mg2.016.002.045.962.015.980.812.43Ni0.1mg2.005.982.015.982.005.960.822.39Hg0.4mg1.986.031.996.001.986.020.832.39Pb12mg————————2.006.011.956.020.792.38Cu10mg2.036.00————————2.025.990.782.40Cd4mg1.986.051.996.02————————0.802.42Co0.4mg2.025.962.016.042.006.06————————以上混合元素1.986.002.015.982.006.040.822.41試驗表明，上述雜質(zhì)在標準要求的范圍內(nèi)對鉛鎘銅鈷沒有影響。方法對照試驗按照本試驗步驟測得鉛、鎘、銅結(jié)果，與GB/T8151.20-2012《鋅精礦分析方法》第20部分電感耦合等離子體原子發(fā)射光譜法測得鉛、鎘、銅進行比對，結(jié)果見表12。表12本試驗方法與ICP-AES法結(jié)果對比（%）樣品編號測試元素本試驗結(jié)果平均值ICP-AES法結(jié)果平均值4#Pb5.175.336#Pb4.134.1512#Pb0.130.144#Cu1.291.2812#Cu0.110.1110#Cu3.453.505#Cd0.160.161#Cd1.051.073#Cd2.282.35試驗表明：本試驗方法與ICP-AES法結(jié)果對比，數(shù)據(jù)基本一致。按分析步驟，對樣品試樣進行了精密度試驗，結(jié)果見表13、14、15、16。（其他參與起草單位的精密度數(shù)據(jù)見“十三、附件-試驗數(shù)據(jù)處理及精密度計算”）。表13Pb精密度試驗數(shù)據(jù)（%）樣品編號12#10#1#6#4#7#8#5#11#2#10.120.481.284.185.185.963.682.040.121.0520.140.481.224.025.056.043.461.920.131.1030.130.481.314.205.115.893.701.990.131.1040.130.491.254.125.116.203.652.000.131.1250.120.501.284.105.135.933.682.040.131.0660.140.481.304.165.165.923.481.960.131.0770.130.471.314.085.185.813.662.000.131.1080.130.501.264.185.226.003.601.950.131.1090.130.491.254.225.286.063.532.060.141.13100.130.491.294.065.296.003.571.970.141.05110.130.481.254.165.225.853.682.080.131.10平均值0.1300.4851.2734.1355.1755.9693.6082.0010.1311.089SD0.006320.009340.02900.06330.07390.1090.08620.04970.005390.0274RSD4.871.922.281.531.431.822.392.484.122.51表14Cu精密度試驗數(shù)據(jù)（%）樣品編號12#7#4#10#9#8#5#11#2#10.110.481.283.364.930.150.110.101.1020.110.501.253.45.140.150.110.101.1530.110.481.263.384.930.140.110.101.1240.100.521.263.424.940.160.100.101.0650.110.511.283.464.840.150.120.101.1060.110.511.293.495.040.150.120.111.0570.110.501.313.464.850.140.110.101.1280.120.521.313.465.160.150.110.101.0890.110.511.313.494.940.160.110.111.07100.110.501.333.55.040.150.110.111.10110.100.501.323.524.960.140.110.101.09平均值0.1090.5031.2913.4494.9790.1490.1110.1031.095SD0.005390.01350.02700.05220.1050.007010.005390.004670.0291RSD4.942.682.091.512.114.704.864.552.66表15Cd精密度試驗數(shù)據(jù)（%）樣品編號10#11#13#1#3#8#5#2#10.140.280.501.092.260.150.160.2820.140.290.491.002.180.160.160.2730.130.280.491.052.260.170.160.2840.130.280.471.022.330.160.170.2850.140.300.481.062.360.150.160.2960.140.280.501.052.230.160.160.2870.130.280.481.042.330.160.160.2880.140.290.471.072.340.170.150.2990.130.270.491.022.280.160.160.28100.140.290.481.052.240.160.170.28110.150.280.481.062.260.160.160.28平均值0.1370.2840.4851.0462.2790.1600.1610.281SD0.006470.008090.01040.02540.05500.006320.005390.00539RSD4.712.852.142.432.413.953.351.92表16Co精密度試驗數(shù)據(jù)（%）樣品編號2#5#11#4#14#8#15#10.00360.00580.0180.120.160.0790.006520.00360.00600.0160.120.180.0850.006930.00340.00580.0170.110.180.0820.006640.00360.00620.0180.120.190.0830.007050.00410.00590.0170.130.170.0870.006460.00370.00550.0190.130.170.0780.006770.00350.00650.0170.120.170.0900.007180.00370.00580.0180.120.170.0810.006390.00380.00590.0170.120.170.0860.0073100.00370.00590.0170.130.170.0800.0068110.00370.00580.0170.120.180.0840.0065平均值0.003670.005920.01740.1220.1740.08320.00674SD0.0001790.0002560.0008090.006030.008090.003660.000314RSD4.884.334.664.954.664.394.66選取試樣，加入一定量的鉛、銅、鎘、鈷標準溶液，按照本法進行加標回收試驗，分析結(jié)果見表17、18、19、20。表17Pb的回收率試驗數(shù)據(jù)試樣編號稱樣量/g元素含量/%試樣含鉛量/μg加入鉛量/μg測得鉛量/μg回收率/%1#0.20001.2725401500401198.061#0.20001.2725402500496196.8410#0.20000.4998010001981100.110#0.20000.4998015002548104.7表18Cu的回收率試驗數(shù)據(jù)試樣編號稱樣量/g元素含量/%試樣含鉛量/μg加入鉛量/μg測得鉛量/μg回收率/%4#0.20001.2925801500400795.134#0.20001.29258025005112101.37#0.20000.50100010002025102.57#0.20000.50100015002528101.9表19Cd的回收率試驗數(shù)據(jù)試樣編號稱樣量/g元素含量/%試樣含鉛量/μg加入鉛量/μg測得鉛量/μg回收率/%1#0.20001.05210015003655103.71#0.20001.0521002500456698.6413#0.20000.4896010002025102.513#0.20000.4896015002528101.9表20Co的回收率試驗數(shù)據(jù)試樣編號稱樣量/g元素含量/%試樣含鉛量/μg加入鉛量/μg測得鉛量/μg回收率/%4#0.20000.12240250502104.84#0.20000.1224050072597.0013#1.00000.00676750119104.013#1.00000.00676710016295.00經(jīng)整合修訂，通過條件試驗，建立原子吸收光譜法測定鋅精礦中鉛、銅、鎘、鈷的量，測定范圍為：鉛含量0.10%～6.00%；銅含量0.10%～5.00%；鎘含量0.10%～2.00%；鈷含量0.0020%～0.20%，方法精密度相對標準偏差在1.77%～5.00%之間，加標回收率在95%～105%之間，該方法快速、方便，精密度好，準確度高，建議將本方法采納為新的國家標準分析方法。根據(jù)《GB/T6379.2-2004確定標準測量方法重復(fù)性和再現(xiàn)性的基本方法》規(guī)定，對20家起草單位提供的精密度試驗數(shù)據(jù)進行了數(shù)理統(tǒng)計分析，詳情見本文件“十三、附件-試驗數(shù)據(jù)處理及精密度計算”。在重復(fù)性條件下獲得的兩次獨立測試結(jié)果的測試值，在表21給出的平均值范圍內(nèi)，這兩個測試結(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21數(shù)據(jù)采用線性內(nèi)插法或外延法求得。表21重復(fù)性限（r）ωPb/%0.120.501.264.095.186.01r/%0.020.040.070.190.240.32ωCu/%0.110.521.283.524.96/r/%0.020.050.090.130.17/ωCd/%0.120.280.481.042.25/r/%0.020.030.040.070.09/ωCo/%0.00370.00650.0180.1170.179/r/%0.00050.00080.0020.0170.023/在再現(xiàn)性條件下獲得的兩次獨立測試結(jié)果的測試值，在表22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22數(shù)據(jù)采用線性內(nèi)插法或外延法求得。表22方法1再現(xiàn)性限（R）ωPb/%0.120.501.264.095.186.01R/%0.020.060.110.300.370.41ωCu/%0.110.521.283.524.96/R/%0.020.080.130.200.30/ωCd/%0.120.280.481.042.25/R/%0.030.050.060.130.18/ωCo/%0.00370.00650.0180.1170.179/R/%0.00130.00160.0030.0220.024/本標準不涉及專利問題。鋅精礦是生產(chǎn)金屬鋅、鋅化合物等的主要原料。金屬鋅主要用于鋼鐵、冶金、機械、電氣、化工、輕工、軍事和醫(yī)藥等領(lǐng)域。中國鉛鋅礦資源比較豐富，鋅儲量9384萬噸，居世界第4位。隨著鋅量需求不斷地增加，鋅精礦產(chǎn)量也在不斷增加，鋅產(chǎn)業(yè)的發(fā)展前景十分開闊。本文件《鋅精礦化學分析方法第5部分：鉛、銅、鎘、鈷含量的測定火焰原子吸收光譜法》是將原GB/T8151.5-2012《鋅精礦化學分析方法第5部分：鉛量的測定火焰原子吸收光譜法》和GB/T8151.6-2012《鋅精礦化學分析方法第6部分：銅量的測定火焰原子吸收光譜法》、GB/T8151.8-2012《鋅精礦化學分析方法第8部分：鎘量的測定火焰原子吸收光譜法》、GB/T8151.16-2005《鋅精礦化學分析方法第16部分：鈷量的測定火焰原子吸收光譜法》的整合修訂，修訂后的文件鉛元素的測定范圍為0.10%?6.00%，調(diào)整銅元素的測定范圍為0.10%?5.00%，調(diào)整后能滿足實際貿(mào)易中需求，為企業(yè)生產(chǎn)及市場交易結(jié)算提供有力的指導(dǎo)，具有重要的現(xiàn)實性和必要性。原子吸收光譜法具有靈敏度高、分析精度高、分析速度快、應(yīng)用范圍廣，操作簡單，容易掌握等優(yōu)點?；鹧嬖游展庾V法普遍應(yīng)用于低含量元素的測定，檢測方法公認度高，原子吸收光譜儀是實驗室普遍使用的檢測設(shè)備。原文件采用火焰原子吸收光譜法進行測量，該標準的編寫符合GB/T1.1-2020《標準化工作導(dǎo)則》的編制要求。本文件充分考慮了目前國內(nèi)鋅精礦中鉛、銅、鎘、鈷含量檢測的實際技術(shù)水平。本標準方法成熟，分析數(shù)據(jù)準確可靠、可行，能夠準滿足現(xiàn)有的產(chǎn)品標準要求。本標準技術(shù)先進、結(jié)構(gòu)合理、文字簡練、條理清晰、可操作性強，達到了國內(nèi)先進水平。無七、與現(xiàn)行法律、、強制性國家標準及相關(guān)標準協(xié)調(diào)配套情況本標準與有關(guān)的現(xiàn)行法律、法規(guī)和強制性國家標準沒有沖突。本標準與現(xiàn)行標準及制定中的標準無重復(fù)交叉情況。八、重大分歧意見的處理經(jīng)過和依據(jù)無十一、廢止現(xiàn)行標準的建議建議本標準代替GB/T8151.5-2012《鋅精礦化學分析方法第5部分：鉛量的測定火焰原子吸收光譜法》和GB/T8151.6-2012《鋅精礦化學分析方法第6部分：銅量的測定火焰原子吸收光譜法》、GB/T8151.8-2012《鋅精礦化學分析方法第8部分：鎘量的測定火焰原子吸收光譜法》、GB/T8151.16-2005《鋅精礦化學分析方法第16部分：鈷量的測定火焰原子吸收光譜法》?！朵\精礦化學分析方法第5部分：鉛、銅、鎘、鈷含量的測定火焰原子吸收光譜法》試驗數(shù)據(jù)處理及精密度計算：年8月-2024年11月，湖南水口山有色金屬有限責任公司、紫金礦業(yè)集團股份有限公司、山西北方銅業(yè)有限公司、河南豫光金鉛股份有限公司、大冶有色設(shè)計研究院有限公司、云南華聯(lián)鋅銦股份有限公司、株洲冶煉集團股份有限公司、中國檢驗認證集團廣西有限公司、湖南有色金屬研究院有限責任公司、北礦檢測技術(shù)股份有限公司、銅陵有色金屬集團有限公司、國標(北京)檢驗認證有限公司、云南馳宏鋅鍺股份有限公司、中國有色桂林礦產(chǎn)地質(zhì)研究院有限公司、長沙礦冶院檢測技術(shù)有限責任公司、中國檢驗認證集團廣東黃埔有限公司、江西銅業(yè)鉛鋅金屬有限公司等20家單位共同參與了《鋅精礦化學分析方法1實驗室編號表SEQ表\*ARABIC1實驗室編號編號實驗室名稱編號實驗室名稱1葫蘆島鋅業(yè)股份有限公司11中國檢驗認證集團廣西有限公司2深圳市中金嶺南有色金屬股份有限公司韶關(guān)冶煉廠12湖南有色金屬研究院有限責任公司3昆明冶金研究院有限公司13北礦檢測技術(shù)股份有限公司4湖南水口山有色金屬有限責任公司14銅陵有色金屬集團控股有限公司5紫金礦業(yè)集團股份有限公司15國標(北京)檢驗認證有限公司6山西北方銅業(yè)有限公司16云南馳宏鋅鍺股份有限公司7河南豫光金鉛股份有限公司17中國有色桂林礦產(chǎn)地質(zhì)研究院有限公司8大冶有色設(shè)計研究院有限公司18長沙礦冶院檢測技術(shù)有限責任公司9云南華聯(lián)鋅銦股份有限公司19中國檢驗認證集團廣東黃埔有限公司10株洲冶煉集團股份有限公司20江西銅業(yè)鉛鋅金屬有限公司2精密度數(shù)據(jù)確認精密度數(shù)據(jù)是由20家試驗室對5至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銅、鉛、鎘、鈷含量在重復(fù)性條件下獨立測定5-11次。表1為各實驗室編號。各實驗室原始數(shù)據(jù)見表2-表80,表2Pb試驗數(shù)據(jù)實驗室i測定結(jié)果12#10#1#6#4#7#8#5#11#2#110.120.481.284.185.185.963.461.920.121.0520.140.481.224.025.056.043.481.950.131.0530.130.481.314.205.115.893.531.960.131.0640.130.491.254.125.116.203.571.970.131.0750.120.501.284.105.135.933.61.990.131.160.140.481.304.165.165.923.652.000.131.170.130.471.314.085.185.813.662.000.131.180.130.501.264.185.226.003.682.040.131.190.130.491.254.225.286.063.682.040.131.1100.130.491.294.065.296.003.682.060.141.12110.130.481.254.165.225.853.72.080.141.13平均值0.1300.4851.2734.1355.1755.9693.6082.0010.1311.089SD0.006320.009340.02900.06330.07390.1090.086230.049690.00540.0274RSD/%4.871.922.281.531.431.822.392.484.122.51測定次數(shù)n11111111111111111111Min0.120.471.224.025.055.813.461.920.121.05Max0.140.51.314.225.296.203.72.080.141.13Gmin1.5811.6541.8171.8091.6971.4631.7181.6282.0231.428Gmax1.5811.5571.2851.3501.5492.1231.0651.5921.6851.495G95(n)2.3552.3552.3552.3552.3552.3552.3552.3552.3552.355G99(n)2.5642.5642.5642.5642.5642.5642.5642.5642.5642.564檢查結(jié)果無異常無異常無異常無異常無異常無異常無異常無異常無異常無異常表3Pb試驗數(shù)據(jù)實驗室i測定結(jié)果12#10#1#6#4#7#8#5#11#2#210.14*0.56*1.264.185.136.073.371.880.120.9720.120.481.223.995.185.973.41.890.120.9830.120.491.233.865.035.923.411.950.120.9940.120.481.243.995.035.913.411.950.121.0250.130.511.233.975.095.983.421.950.131.0560.120.521.243.955.135.953.421.980.141.0670.120.481.223.985.186.013.451.980.141.0680.130.481.234.055.096.033.462.010.151.0790.120.511.243.965.085.943.462.020.151.11100.120.481.223.995.165.973.512.060.161.12110.120.491.234.115.176.033.552.090.181.15平均值0.1240.4981.2334.0035.1155.9803.4421.9780.1391.053SD0.006740.02520.01190.08500.05560.05020.051930.064620.01970.0590RSD/%5.455.060.972.121.090.841.513.2714.185.61測定次數(shù)n11111111111111111111Min0.120.481.223.865.035.913.371.880.120.97Max0.140.561.264.185.186.073.552.090.181.15Gmin0.5390.7211.0691.6801.5381.3941.3831.5190.9681.402Gmax2.4272.4512.2902.0861.1621.7932.0831.7302.0741.648G95(n)2.3552.3552.3552.3552.3552.3552.3552.3552.3552.355G99(n)2.5642.5642.5642.5642.5642.5642.5642.5642.5642.564檢查結(jié)果0.14為岐離值（保留）0.56為岐離值（保留）無異常無異常無異常無異常無異常無異常無異常無異常表4Pb試驗數(shù)據(jù)實驗室i測定結(jié)果12#10#1#6#4#7#8#5#11#2#310.120.551.224.205.206.153.511.950.11.0620.130.531.284.195.186.213.521.980.111.0730.120.511.254.265.216.183.531.980.111.0940.130.511.254.175.166.123.592.010.111.0950.110.501.264.255.186.153.592.030.121.160.120.501.294.185.196.223.62.030.121.1170.120.491.244.195.206.193.612.040.121.1180.120.511.234.125.216.233.622.050.121.1290.110.501.264.215.186.143.632.070.121.12100.110.481.204.195.236.133.652.090.131.12110.130.491.224.165.166.183.652.110.131.12平均值0.1200.5061.2454.1935.1916.1733.5912.0310.1171.101SD0.007750.01960.02700.03900.02170.03740.050090.04890.00900.0212RSD/%6.453.882.170.930.420.611.392.417.711.92測定次數(shù)n11111111111111111111Min0.110.481.24.125.166.123.511.950.11.06Max0.130.531.294.265.236.233.652.110.131.12Gmin1.2911.3431.6851.8641.4271.4081.6151.6551.9101.930Gmax1.2911.2041.6521.7241.8051.5301.1801.6181.4070.901G95(n)2.3552.3552.3552.3552.3552.3552.3552.3552.3552.355G99(n)2.5642.5642.5642.5642.5642.5642.5642.5642.5642.564檢查結(jié)果無異常無異常無異常無異常無異常無異常無異常無異常無異常無異常表5Pb試驗數(shù)據(jù)實驗室i測定結(jié)果12#10#1#6#4#7#8#5#11#2#410.1310.5021.404.025.215.983.422.010.1281.0520.1530.4921.424.115.375.923.482.010.1311.0630.1550.4811.423.955.105.833.512.060.1331.0840.1370.4801.323.985.005.983.522.060.1351.0950.1590.5041.414.155.286.013.522.070.1351.0960.1430.4831.374.034.985.923.562.080.1371.1170.1460.4971.364.074.995.953.572.080.1381.1680.1420.4951.444.035.135.963.612.110.1391.1690.1510.4981.434.055.085.893.612.150.14031.19100.1540.4871.363.995.225.983.652.170.1411.19110.1390.4961.384.025.066.033.672.190.1461.21平均值0.1460.4921.3924.0365.1295.9503.5912.0310.1171.101SD0.008760.008370.03680.05750.1270.05710.050090.04890.00900.0212RSD/%5.981.702.651.422.480.961.392.417.711.92測定次數(shù)n11111111111111111111Min0.1310.481.323.954.985.833.511.950.11.06Max0.1590.5041.444.155.376.033.652.110.131.12Gmin1.7551.4671.9501.5021.1722.1021.6151.6551.9101.930Gmax1.4431.4011.3081.9771.8931.4011.1801.6181.4070.901G95(n)2.3552.3552.3552.3552.3552.3552.3552.3552.3552.355G99(n)2.5642.5642.5642.5642.5642.5642.5642.5642.5642.564檢查結(jié)果無異常無異常無異常無異常無異常無異常無異常無異常無異常無異常表6Pb試驗數(shù)據(jù)實驗室i測定結(jié)果12#10#1#6#4#7#8#5#11#2#510.130.521.194.185.205.883.381.900.121.1320.120.531.254.005.265.853.362.010.121.1030.120.531.203.975.175.873.361.950.121.1540.120.511.264.105.356.033.472.010.131.0850.120.511.244.085.395.903.512.060.131.0760.130.511.234.205.315.963.402.030.131.0570.130.531.224.155.346.003.532.030.131.09平均值0.1240.5201.2274.0975.2895.9273.4301.9990.1261.096SD0.005350.01000.02560.08770.08150.06970.072110.05490.00530.0346RSD/%4.301.922.092.141.541.182.102.754.253.16測定次數(shù)n7777777777Min0.120.511.193.975.175.853.361.90.121.05Max0.130.531.264.25.396.033.532.060.131.15Gmin0.8021.0001.4491.4501.4541.1070.9711.7951.0691.322Gmax1.0691.0001.2821.1731.2441.4761.3871.1190.8021.570G95(n)2.0202.0202.0202.0202.0202.0202.0202.0202.0202.020G99(n)2.1392.1392.1392.1392.1392.1392.1392.1392.1392.139檢查結(jié)果無異常無異常無異常無異常無異常無異常無異常無異常無異常無異常表7Pb試驗數(shù)據(jù)實驗室i測定結(jié)果12#10#1#6#4#7#8#5#11#2#610.1310.5051.3154.2325.3456.0763.7722.0640.1221.13620.1360.4921.2984.1565.3246.0193.6931.9920.1161.08430.1390.4881.2924.2675.2896.2073.7051.9260.1181.15340.1320.4961.3114.3355.3546.1353.5392.0690.1201.14050.1290.491.3244.2945.2646.1293.6262.1020.1141.12460.130.5151.334.3565.3225.8623.6372.0830.1211.08970.1330.5061.3044.2165.1365.9383.5442.0220.1191.13080.1270.4821.3194.1745.0916.0463.7261.9860.1221.13290.1320.5011.3184.0955.1296.2273.5862.0190.1141.111100.1300.4991.2854.2225.3625.8263.5091.9640.1151.152110.1290.5191.3024.2415.2936.2213.6372.0090.1251.146平均值0.1320.4991.3094.2355.2646.0623.6342.0210.1191.127SD0.003410.01140.01400.07700.09860.14030.084360.05390.00370.0235RSD/%2.592.281.071.821.872.312.322.673.092.08測定次數(shù)n11111111111111111111Min0.1270.4821.2854.0955.0915.8263.5091.9260.1141.084Max0.1390.5191.334.3565.3626.2273.7722.1020.1251.153Gmin1.3581.5271.7141.8221.7591.6851.4821.7711.2911.833Gmax2.1571.7271.5121.5680.9891.1741.6361.4951.7121.108G95(n)2.3552.3552.3552.3552.3552.3552.3552.3552.3552.355G99(n)2.5642.5642.5642.5642.5642.5642.5642.5642.5642.564檢查結(jié)果無異常無異常無異常無異常無異常無異常無異常無異常無異常無異常表8Pb試驗數(shù)據(jù)實驗室i測定結(jié)果12#10#1#6#4#7#8#5#11#2#710.1250.4891.284.095.185.933.512.070.1251.0820.1310.4991.274.115.175.863.492.080.1291.0730.1270.4801.274.175.185.843.622.060.1281.0840.1320.4971.274.135.185.933.682.080.1271.1150.1290.4911.274.135.185.893.662.070.1271.1060.1260.4871.284.125.175.863.522.060.1261.0970.1330.4851.274.125.185.913.552.060.1251.0980.1290.4921.274.155.185.893.532.080.1281.0890.1250.4971.274.145.175.913.602.080.1291.08100.1310.4931.274.125.185.883.632.080.1271.08110.1280.4951.30**4.125.185.903.612.070.1291.09平均值0.1290.4911.2754.1275.1775.8913.5822.0720.1271.086SD0.002800.005770.009340.02100.004670.02910.064620.008740.001490.0112RSD/%2.171.170.730.510.090.491.800.421.171.03測定次數(shù)n11111111111111111111Min0.1250.481.274.095.175.843.492.060.1251.07Max0.1330.4991.304.175.185.933.682.080.1291.11Gmin1.3331.9710.4871.7731.5571.7471.4211.3521.5261.461Gmax1.5281.3242.7252.0330.5841.3421.5190.9361.1602.110G95(n)2.3552.3552.3552.3552.3552.3552.3552.3552.3552.355G99(n)2.5642.5642.5642.5642.5642.5642.5642.5642.5642.564檢查結(jié)果無異常無異常1.30為離群值（舍棄）無異常無異常無異常無異常無異常無異常無異常表9Pb試驗數(shù)據(jù)實驗室i測定結(jié)果12#10#1#6#4#7#8#5#11#2#810.130.501.144.005.005.953.422.010.101.0520.110.491.184.005.026.063.581.960.121.0330.120.511.264.045.025.963.612.040.120.9940.130.491.273.964.995.643.511.910.131.0550.100.501.204.024.905.723.301.900.091.0660.110.481.283.964.955.763.461.870.101.0370.110.521.203.934.895.693.441.890.110.9980.130.55*1.193.984.965.753.391.900.121.0590.120.481.213.984.885.763.251.930.121.06100.120.511.233.974.905.763.351.980.101.04110.140.491.243.944.985.783.391.970.121.05平均值0.1200.5021.2183.9804.9545.8033.4271.9420.1121.036SD0.01180.02040.04240.03320.05320.1290.110100.05420.01250.0250RSD/%9.864.073.480.831.072.233.212.7911.182.41測定次數(shù)n11111111111111111111Min0.10.481.143.934.885.643.251.870.090.99Max0.140.551.284.045.026.063.612.040.131.06Gmin1.6901.0691.8451.5081.3851.2581.6101.3251.7451.854Gmax1.6902.3611.4591.8091.2481.9881.6601.8121.4540.945G95(n)2.3552.3552.3552.3552.3552.3552.3552.3552.3552.355G99(n)2.5642.5642.5642.5642.5642.5642.5642.5642.5642.564檢查結(jié)果無異常0.55為岐離值（保留）無異常無異常無異常無異常無異常無異常無異常無異常表10Pb試驗數(shù)據(jù)實驗室i測定結(jié)果12#10#1#6#4#7#8#5#11#2#910.130.541.274.165.356.233.731.940.121.1120.130.541.264.165.316.253.771.940.121.1230.120.531.274.115.296.213.711.940.121.1240.120.541.274.185.286.293.781.940.121.1150.130.541.264.115.296.243.691.940.121.1260.130.541.274.105.246.193.721.930.131.1170.120.531.274.165.266.223.741.930.121.1280.130.531.264.185.306.233.711.940.131.1290.120.531.264.165.306.273.791.940.131.11100.130.541.16**4.155.336.223.721.940.131.12110.120.531.264.125.276.263.771.940.121.12平均值0.1250.5351.2554.1455.2936.2373.7391.9380.1241.116SD0.005220.005220.03210.02910.03100.02870.033300.004050.00500.0050RSD/%4.160.982.550.700.590.460.890.214.080.45測定次數(shù)n11111111111111111111Min0.120.531.16**4.15.246.193.691.930.121.11Max0.130.541.274.185.356.293.791.940.131.12Gmin1.0441.0442.9781.5301.7001.6491.4742.0230.7211.261Gmax0.8700.8700.4541.2181.8471.8391.5290.4491.2610.721G95(n)2.3552.3552.3552.3552.3552.3552.3552.3552.3552.355G99(n)2.5642.5642.5642.5642.5642.5642.5642.5642.5642.564檢查結(jié)果無異常無異常1.16為離群值（舍棄）無異常無異常無異常無異常無異常無異常無異常表11Pb試驗數(shù)據(jù)實驗室i測定結(jié)果12#10#1#6#4#7#8#5#11#2#1010.130.491.284.275.295.983.562.000.131.0920.120.461.294.275.295.983.562.000.121.1030.120.471.304.245.296.163.612.000.121.0840.130.501.324.275.286.203.582.000.121.0750.120.491.334.275.296.203.582.000.111.0960.120.501.324.255.256.203.582.030.111.0970.140.491.284.225.296.243.631.990.131.1080.150.501.274.215.346.143.632.010.121.1190.140.511.294.205.396.223.562.000.131.12100.150.501.324.195.306.203.582.010.131.13110.150.501.314.195.336.223.662.010.121.13平均值0.1340.4921.3014.2355.3046.1583.5942.0050.1221.101SD0.01290.01470.02020.03360.03720.09230.033840.01040.00750.0197RSD/%9.632.991.550.790.701.500.940.526.161.79測定次數(shù)n11111111111111111111Min0.120.461.274.195.255.983.561.990.111.07Max0.150.511.334.275.396.243.662.030.131.13Gmin1.0602.1631.5281.3271.4411.9310.9941.4041.5741.567Gmax1.2721.2361.4381.0562.3200.8871.9612.4581.0901.475G95(n)2.3552.3552.3552.3552.3552.3552.3552.3552.3552.355G99(n)2.5642.5642.5642.5642.5642.5642.5642.5642.5642.564檢查結(jié)果無異常無異常無異常無異常無異常無異常無異常無異常無異常無異常表12Pb試驗數(shù)據(jù)實驗室i測定結(jié)果12#10#1#6#4#7#8#5#11#2#1110.1270.5061.2814.1775.2186.1673.5992.0160.1271.14620.1260.4991.2654.1085.2016.1783.5951.9870.1231.11930.1260.4911.2794.1245.1486.2013.5932.0010.1211.10940.1250.5001.2554.0985.1566.1893.5802.0050.1121.08950.1340.5121.2774.1355.1806.1943.5902.0410.1141.09860.1250.5201.2604.1425.1616.1783.5892.0560.1181.12470.1390.5121.2904.1985.1496.1723.5962.0140.1181.11980.1180.5101.2814.2045.1796.1663.5622.0580.1211.12490.1290.4991.2684.1335.1646.2083.5672.0340.1181.121100.1300.5101.2704.1395.1706.1933.5682.0470.1231.129110.1310.4901.2754.0895.1886.1763.5782.0470.1311.115平均值0.1280.5041.2734.1415.1746.1843.5832.0280.1211.118SD0.005460.009430.01030.03810.02200.01400.013070.02430.00550.0152RSD/%4.261.870.810.920.420.230.361.204.531.36測定次數(shù)n11111111111111111111Min0.1180.491.2554.0895.1486.1663.5621.9870.1121.089Max0.1390.521.294.2045.2186.2083.5992.0580.1311.146Gmin1.8661.5331.7281.3541.1831.2721.6341.6821.5631.875Gmax1.9831.6491.6661.6612.0021.7261.1961.2441.9131.869G95(n)2.3552.3552.3552.3552.3552.3552.3552.3552.3552.355G99(n)2.5642.5642.5642.5642.5642.5642.5642.5642.5642.564檢查結(jié)果無異常無異常無異常無異常無異常無異常無異常無異常無異常無異常表13Pb試驗數(shù)據(jù)實驗室i測定結(jié)果12#10#1#6#4#7#8#5#11#2#1210.120.511.244.034.976.183.551.990.111.0720.120.511.284.035.076.123.612.000.111.0530.120.481.164.065.025.903.592.040.111.0140.120.501.203.904.805.643.301.910.111.0550.120.521.213.994.855.683.251.920.101.0660.120.491.283.924.955.703.261.870.121.0270.120.521.183.934.895.693.341.890.121.0380.120.59**1.193.904.965.753.291.880.111.0490.130.491.253.984.885.723.191.930.111.06100.110.511.273.974.895.733.351.910.111.04110.120.471.203.944.965.783.321.900.121.06平均值0.1200.5081.2243.9684.9315.8083.3681.9310.1121.045SD0.004470.03160.04230.05530.07780.18230.145730.05490.00600.0186RSD/%3.736.213.451.391.583.144.332.845.391.78測定次數(shù)n11111111111111111111Min0.110.471.163.94.85.643.191.870.11.01Max0.130.591.284.065.076.183.612.040.121.07Gmin2.2361.2101.5061.2331.6830.9231.2231.1101.9601.854Gmax2.2362.5921.3341.6611.7882.0401.6591.9891.3571.366G95(n)2.3552.3552.3552.3552.3552.3552.3552.3552.3552.355G99(n)2.5642.5642.5642.5642.5642.5642.5642.5642.5642.564檢查結(jié)果無異常0.59為離群值（舍棄）無異常無異常無異常無異常無異常無異常無異常無異常表14Pb試驗數(shù)據(jù)實驗室i測定結(jié)果12#10#1#6#4#7#8#5#11#2#1310.130.511.274.195.366.153.611.970.141.1020.130.501.284.125.376.033.641.980.131.1230.130.511.304.155.386.123.621.960.121.1140.140.501.274.175.366.103.641.970.131.1350.130.521.284.215.336.163.551.980.131.1060.140.491.284.195.316.093.422.000.131.1370.130.511.294.125.305.973.411.970.121.1280.130.491.274.055.316.113.611.960.121.1290.130.501.284.225.336.223.642.010.131.12100.140.511.304.215.366.253.621.950.131.09110.130.501.304.145.336.173.621.960.121.12平均值0.1330.5041.2844.1615.3406.1253.5801.9740.1271.115SD0.004670.009240.01210.05130.02720.07980.085320.018040.00650.0129RSD/%3.521.840.941.230.511.302.380.915.081.16測定次數(shù)n11111111111111111111Min0.130.491.274.055.35.973.411.950.121.09Max0.140.521.34.225.386.253.642.010.141.13Gmin0.5841.4751.1312.1631.4701.9371.9921.3101.1251.898Gmax1.5571.7701.3571.1521.4701.5720.7032.0161.9681.195G95(n)2.3552.3552.3552.3552.3552.3552.3552.3552.3552.355G99(n)2.5642.5642.5642.5642.5642.5642.5642.5642.5642.564檢查結(jié)果無異常無異常無異常無異常無異常無異常無異常無異常無異常無異常表15Pb試驗數(shù)據(jù)實驗室i測定結(jié)果12#10#1#6#4#7#8#5#11#2#1410.120.521.264.165.256.103.591.990.121.1320.120.521.274.185.316.093.622.000.121.1130.120.511.264.215.316.093.681.990.131.1240.120.511.284.295.326.113.551.990.121.1150.120.521.304.305.286.093.521.970.121.1160.130.521.294.255.306.073.611.980.121.1270.130.521.304.265.206.163.571.970.121.1280.120.501.294.165.316.163.602.000.131.1390.130.501.284.155.306.153.612.000.131.11100.130.501.294.155.236.153.572.000.131.12110.120.501.294.155.306.203.552.