白酒中釩鉻錳鐵銅鎳砷鎘銻鉛的測定

白酒中釩、鉻、錳、鐵、銅、鎳、碑、鎘、銻、鉛的測定

電感耦合等離子體質(zhì)譜法（征求意見稿）編制說明一、 標(biāo)準(zhǔn)起草的基本情況（包括簡要的任務(wù)來源介紹、主要起草單位、起草人等）本項(xiàng)目由貴州省衛(wèi)生和計(jì)劃生育委員會(huì)組織食品安全地方標(biāo)準(zhǔn)評(píng)審委員會(huì)專家組進(jìn)行評(píng)審并通過立項(xiàng)，2015年5月11日以“衛(wèi)計(jì)辦函[2015]94號(hào)”下發(fā)任務(wù)。由貴州茅臺(tái)酒股份有限公司負(fù)責(zé)。本標(biāo)準(zhǔn)主要起草單位為：貴州茅臺(tái)酒股份有限公司本標(biāo)準(zhǔn)主要起草人為：王莉、汪地強(qiáng)、趙振宇、曾穩(wěn)穩(wěn)、榮茂、龍薇運(yùn)、江鋒、聶葉、袁河、劉松、李清亮、胡容、饒書愷、申鷹。二、 編制過程（包括編制原則、各階段工作過程等）1、 本標(biāo)準(zhǔn)的編制原則1.1必要性：白酒中無機(jī)元素的來源與釀造環(huán)境（土壤、糧食、水源）、釀造工藝、蒸餾工藝、蒸餾設(shè)備、陳釀工藝、勾兌、包裝等環(huán)節(jié)密切相關(guān)，其含量的高低對(duì)產(chǎn)品品質(zhì)具有重要影響。該方法一次能快速測定各釀造環(huán)節(jié)易遷移的風(fēng)險(xiǎn)元素含量，對(duì)白酒行業(yè)具有重要意義。1.2先進(jìn)性：該方法不需要傳統(tǒng)的消解步驟，處理步驟簡單并可實(shí)現(xiàn)一次性進(jìn)樣檢測10種元素，大大提高檢測效率，且將該技術(shù)應(yīng)用到白酒檢測并未有相關(guān)的國家標(biāo)準(zhǔn)。2、 工作過程2.1立項(xiàng)批準(zhǔn)2014年6月3日，貴州省衛(wèi)生和計(jì)劃生育委員會(huì)下發(fā)《關(guān)于征集2014年貴州省食品安全地方標(biāo)準(zhǔn)制（修）訂立項(xiàng)建議的函》（黔衛(wèi)計(jì)函【2014】29號(hào)）。我公司于2014年7月向衛(wèi)計(jì)委提交立項(xiàng)申請(qǐng)，并于2014年8月向食品安全地方標(biāo)準(zhǔn)審評(píng)委員會(huì)相關(guān)專家進(jìn)行項(xiàng)目申請(qǐng)說明。2015年5月11日貴州省衛(wèi)生和計(jì)劃生育委員會(huì)辦公室下發(fā)《省衛(wèi)生計(jì)生委辦公室關(guān)于同意＜貴州苕粉＞等25項(xiàng)貴州省食品安全地方標(biāo)準(zhǔn)立項(xiàng)的通知》（黔衛(wèi)計(jì)辦函【2015】94號(hào)）。2.2任務(wù)落實(shí)貴州茅臺(tái)酒股份有限公司技術(shù)中心負(fù)責(zé)試驗(yàn)、起草標(biāo)準(zhǔn)文本；貴州省分析測試研究院負(fù)責(zé)第一驗(yàn)證；貴州省產(chǎn)品質(zhì)量監(jiān)督檢測院負(fù)責(zé)第二驗(yàn)證；貴州省質(zhì)檢院仁懷分院（國家酒檢中心）負(fù)責(zé)第三驗(yàn)證。起草工作計(jì)劃于2016年5月前完成。2.3、各階段工作過程1） 2015年5月，在接到標(biāo)準(zhǔn)制定任務(wù)后，我們成立了《電感耦合等離子體質(zhì)譜法檢測白酒中無機(jī)元素》地方標(biāo)準(zhǔn)起草小組，明確起草人和工作任務(wù)。2） 2015年6月?2016年2月，根據(jù)前期大量的數(shù)據(jù)收集工作，以及對(duì)貴州省白酒釀造工藝的調(diào)查了解，分析各工藝環(huán)節(jié)易遷移進(jìn)入白酒的10種風(fēng)險(xiǎn)無機(jī)元素，并從方法的線性、檢出限、定量限、穩(wěn)定性、準(zhǔn)確度等方面進(jìn)行條件試驗(yàn)，在此基礎(chǔ)上編寫了標(biāo)準(zhǔn)文本初稿。3） 2016年2月24日，在貴州省分析測試研究院召開標(biāo)準(zhǔn)起草討論會(huì)，對(duì)標(biāo)準(zhǔn)文本初稿及樣品的制備方面進(jìn)行了探討，確定方法驗(yàn)證實(shí)施方案。4） 2016年2月25日-3月7日，完成標(biāo)準(zhǔn)文本初稿修改完善和驗(yàn)證樣品制備，在空白酒樣的基礎(chǔ)上約添加5ppb、50ppb、100ppb、500ppb的標(biāo)液，F(xiàn)e額外增加一個(gè)1000ppb的濃度梯度，各元素含量共設(shè)5個(gè)梯度，共計(jì)5份樣品。5） 2016年3月8號(hào)?4月10號(hào)，三家方法驗(yàn)證單位（貴州省分析測試研究院、貴州省產(chǎn)品質(zhì)量監(jiān)督檢測院、貴州省質(zhì)檢院仁懷分院（國家酒檢中心））拿到統(tǒng)一制備的樣品，分別按照標(biāo)準(zhǔn)文本初稿中的方法進(jìn)行了驗(yàn)證，包括回收率、精密度、穩(wěn)定性驗(yàn)證。6） 2016年4月，匯總分析驗(yàn)證數(shù)據(jù)，寫標(biāo)準(zhǔn)編制說明，起草組根據(jù)驗(yàn)證情況召開討論會(huì)，研究下一步工作。7） 2016年5月，組織公司技術(shù)委員會(huì)對(duì)標(biāo)準(zhǔn)文本進(jìn)行審核，并對(duì)文本進(jìn)行修改。3、主要實(shí)驗(yàn)（或驗(yàn)證）的分析報(bào)告現(xiàn)有的食品中無機(jī)元素的國標(biāo)測定方法，其測定元素相對(duì)單一，工作量大，已經(jīng)不滿足現(xiàn)代企業(yè)對(duì)食品安全監(jiān)控快速靈敏的要求，通過查閱大量國內(nèi)外無機(jī)元素分析方法并進(jìn)行比對(duì)分析，本方法采用ICP-MS對(duì)白酒中10種無機(jī)元素進(jìn)行分析，這10種無機(jī)元素是前期大量的測量數(shù)據(jù)并結(jié)合行業(yè)實(shí)際情況而確定。通過探討樣品中酒精等有機(jī)質(zhì)對(duì)各無機(jī)元素響應(yīng)值的干擾情況，最終省去了傳統(tǒng)的消解步驟，直接將樣品烘干除酒精，再用稀硝酸稀釋，定容，上機(jī)進(jìn)樣分析，大大提高工作效率，并以回收率、精密度、穩(wěn)定性對(duì)方法進(jìn)行了驗(yàn)證，建立了白酒中釩、鉻、錳、鐵、銅、鎳、砷、鎘、銻、鉛的測定方法。將5個(gè)白酒試樣分別稱取11份，按上述分析方法測定10種無機(jī)元素含量，分析結(jié)果如

■ZU主元素VCrMnFeNiCuAsCdSbPb0.01540.01040.03280.5340.01370.09400.01310.005850.005420.01010.01440.01070.03150.5070.01400.08970.01450.006000.005910.009700.01520.01050.03240.5100.01350.09360.01230.005850.005400.01010.01650.01050.03350.5230.01480.09340.01320.005810.004800.0103測0.01540.01060.03240.5150.01290.09660.01360.005210.005430.0106定0.01540.01130.03250.5390.01160.09410.01390.005900.005610.0114樣值0.01450.01050.03150.5440.01320.09240.01440.005860.005480.0105品0.01530.01040.03270.5030.01420.09090.01420.006000.006000.010110.01440.01030.03270.5330.01500.09250.01500.006010.005640.01130.01530.01050.03380.5420.01450.09360.01410.005860.005900.01060.01640.01140.03260.5200.01330.09770.01380.005300.005200.00980均值0.01530.01060.03260.5250.01370.09350.01380.005790.005530.0104RSD%4.583.402.142.777.112.425.564.726.295.340.05880.05520.07870.6280.05910.1390.06140.05650.05030.06300.05580.05710.08110.6800.06040.1490.05800.05310.04830.06780.05910.05530.07950.6010.05690.1410.05990.05500.04500.06390.05890.05520.07620.6020.05900.1340.05060.05410.04860.0551測0.06270.05470.07850.6370.06330.1510.05910.05160.04910.0632樣定0.05880.05620.07930.6790.05990.1390.05780.05500.05320.0638值0.05600.05990.08350.6230.05890.1390.06020.05340.05040.0668品0.05900.05680.07930.6570.06610.1520.05830.05860.04960.062220.06410.05800.08150.6600.06030.1400.05590.05480.04680.05690.05710.05640.07420.6750.05530.1320.06370.06220.04930.06370.05890.05110.07960.6430.05960.1380.06110.05680.05140.0693均值0.05900.05600.07920.6440.05990.1410.05870.05560.04930.0632RSD%4.233.933.154.484.804.645.815.274.466.680.1080.1100.1230.5870.1130.1920.1230.1160.1090.1000.1160.1150.1400.6660.1200.2040.1160.1230.1130.109樣測0.1120.1090.1220.5980.1080.2000.1300.1170.1010.110品定0.1100.1090.1430.6310.1150.1980.1280.1220.1120.1010.1140.1150.1220.6180.1270.2040.1190.1190.1080.1073值0.1100.1090.1360.5650.1140.2000.1290.1150.1100.1140.1090.1130.1260.5980.1060.2030.1230.1150.1010.1030.1100.1130.1290.6410.1190.1930.1280.1250.1070.111表1釩、鉻、錳、鐵、銅、鎳、砷、鎘、銻、鉛含量分析結(jié)果單位：mg/L單位：mg/L0.1150.1090.1380.6450.1180.1950.1310.1160.1150.1070.1140.1170.1420.6760.1290.1980.1280.1180.1130.1150.1150.1150.1390.5990.1190.2100.1170.1240.1100.109均值0.1120.1120.1330.6200.1170.2000.1250.1190.1090.108RSD%2.462.866.295.565.962.734.313.264.264.490.5320.5300.5431.050.5330.6340.5600.5610.5360.4530.5410.5400.5581.100.5410.5880.5970.5740.5650.4290.5230.5530.5331.040.5130.6280.5840.5500.5430.4580.5400.5330.5511.060.5340.6310.5900.5740.5010.457測0.5360.5340.5481.080.5380.6290.5480.5670.5330.450樣定0.5630.5390.5491.100.5400.6300.5770.5630.5150.460值0.5310.5730.5451.050.5290.6630.6100.6130.5560.457品0.5330.5380.5581.090.5490.6350.5600.5610.5330.42740.5460.5100.5631.090.5400.6290.5870.5680.5380.4540.5400.5340.5581.150.5330.6540.5690.5770.5500.4550.5380.5290.5451.030.5610.6430.5400.5930.5630.460均值0.5380.5370.5501.080.5370.6330.5750.5730.5390.451RSD%1.922.901.563.122.232.953.743.023.582.590.01990.01670.03671.660.01870.09920.01930.01180.01120.01610.02000.01580.04051.570.01940.09200.02050.01210.01150.01610.02090.01650.03721.640.01990.09750.02150.01200.01200.01500.01950.01650.03681.660.01790.08970.01930.01080.01120.0161測0.01970.01680.04011.570.01850.09750.02010.01140.01140.0153樣定0.02010.01670.03771.650.01930.1030.01780.01220.01060.0162值0.02070.01770.03491.660.02040.09930.01910.01230.01120.0176品0.01980.01680.03661.580.01890.09840.02040.01170.01150.016150.02060.01620.03941.660.01910.09720.02210.01080.01130.01500.01980.01750.04171.690.01890.09050.01940.01250.01080.01730.02080.01690.03581.610.01860.10020.01890.01280.01190.0162均值0.02020.01670.03791.630.01900.09670.01990.01190.01130.0161RSD%2.483.265.682.603.614.336.145.453.625.13由以上結(jié)果可以看出，對(duì)5個(gè)不同濃度的白酒樣品平行測定11次，相對(duì)標(biāo)準(zhǔn)偏差為1.56%?7.11%,符合分析要求。本方法穩(wěn)定，操作簡便，適用范圍廣，滿足白酒中釩、鉻、錳、鐵、銅、鎳、砷、鎘、銻、鉛的含量分析。4個(gè)實(shí)驗(yàn)室參與了本標(biāo)準(zhǔn)的比對(duì)驗(yàn)證，對(duì)5個(gè)不同濃度的樣品進(jìn)行了分析，結(jié)果見表2。

表2對(duì)比樣品分析結(jié)果 單位：mg/L主兒素VCrMnFeNiCuAsCdSbPb樣品1貴州省分析測試研究院0.01450.009600.03010.4920.01260.08710.01410.005500.005400.009500.01480.009800.02960.5180.01380.08810.01290.005400.005600.009600.01410.01080.03320.4940.01250.09750.01280.005800.005100.009900.01460.01020.03010.4990.01310.08890.01280.005400.005200.01010.01490.009900.02970.5210.01420.08760.01320.005600.005500.009700.01520.009600.03080.5010.01290.08890.01340.005700.005300.009600.01540.01030.03100.4970.01360.08840.01290.005800.005700.009800.01570.01030.02990.5210.01440.08960.01270.005800.005200.009900.01580.01060.03360.5170.01280.08750.01390.005500.005400.01010.01450.01020.03110.4960.01370.09020.01310.006100.005800.009600.01560.009700.02970.5100.01380.09910.01490.005600.005200.0107貴州省產(chǎn)品質(zhì)重監(jiān)督檢驗(yàn)院0.01450.01020.03100.5090.01380.09270.01300.005500.005600.009900.01420.009800.03120.4990.01270.08920.01270.005600.005400.01040.01460.009600.02960.4940.01240.1010.01290.005500.005200.01010.01520.009800.03220.5470.01320.09140.01430.005900.005200.009800.01460.01040.03150.5120.01370.08760.01350.006100.005700.01030.01430.01010.03260.5310.01310.09240.01310.006000.005400.009500.01470.009600.03390.5120.01360.09750.01330.005800.005200.009700.01450.009700.03080.4990.01410.09270.01280.005700.005100.01010.01430.01060.03240.5430.01400.08970.01310.005500.005600.01060.01440.01070.03370.5120.01340.09480.01290.005700.005100.009800.01570.01120.02990.5130.01320.09040.01440.006200.005300.00990貴州省產(chǎn)品質(zhì)量監(jiān)督檢驗(yàn)院仁懷分院0.01570.009800.03010.4980.01380.1020.01420.005900.005900.01090.01490.01120.03520.5510.01420.09840.01290.006200.006100.01120.01560.01130.03450.5390.01460.08760.01450.006400.005800.01130.01450.01100.03190.5490.01410.09960.01380.006300.005900.01070.01630.01070.03470.5510.01280.09450.01470.006000.005700.009900.01690.009900.03380.5450.01460.09870.01330.006100.006100.01120.01610.01150.02980.5400.01470.1020.01270.006400.006200.01080.01590.01140.03420.4970.01390.09810.01390.005800.005800.01120.01650.01080.03290.5170.01260.09720.01420.006100.005900.01110.01620.01010.03520.5380.01450.08880.01450.006300.005700.009800.01570.01120.03150.5560.01470.09630.01280.006200.006100.0108貴州茅臺(tái)酒股份有限公0.01540.01040.03280.5340.01370.09400.01310.005850.005420.01010.01440.01070.03150.5070.01400.08970.01450.006000.005910.009700.01520.01050.03240.5100.01350.09360.01230.005850.005400.01010.01650.01050.03350.5230.01480.09340.01320.005810.004800.01030.01540.01060.03240.5150.01290.09660.01360.005210.005430.0106

司0.01540.01130.03250.5390.01160.09410.01390.005900.005610.01140.01450.01050.03150.5440.01320.09240.01440.005860.005480.01050.01530.01040.03270.5030.01420.09090.01420.006000.006000.01010.01440.01030.03270.5330.01500.09250.01500.006010.005640.01130.01530.01050.03380.5420.01450.09360.01410.005860.005900.01060.01640.01140.03260.5200.01330.09770.01380.005300.005200.00980樣品2貴州省分析測試研究院0.05810.05510.07310.6170.05780.1380.05880.05860.04740.06210.05750.05460.07770.6320.05690.1310.05490.05450.04550.06040.05660.05180.07820.6080.06350.1340.05740.05390.04710.05820.05820.05240.08220.6530.05710.1360.06350.05770.05130.06130.05780.05460.07660.6170.05690.1470.05710.05420.04760.06750.05810.05820.07780.5980.05950.1350.06040.05380.05020.06310.05660.05390.08140.6260.05640.1450.05680.05470.04780.06080.05680.05530.07680.6890.05880.1370.06230.05150.04870.06650.05670.05390.07820.6340.05490.1460.05840.05360.04570.06070.05870.05510.07410.6780.06210.1370.06310.05740.05350.06150.05840.05480.07840.6320.05690.1330.05750.05290.04790.0683貴州省產(chǎn)品質(zhì)重監(jiān)督檢驗(yàn)院0.05910.05210.07310.6170.05880.1400.05810.05360.04770.06270.05850.05560.07870.6220.06290.1470.05530.05470.05120.06740.05760.05880.08220.6190.05640.1340.05920.05290.04780.06470.05720.05440.07720.6530.06110.1300.06260.05350.04870.05820.05880.05360.07660.6170.05670.1390.05710.05520.04540.06050.06110.05520.08480.6480.05740.1320.05870.05460.04760.06130.05760.05490.07760.6220.05650.1450.06340.05110.04610.06680.05780.05730.07690.6300.06340.1380.05860.05470.04810.06250.05570.05390.08120.6050.05810.1300.06110.05630.05230.06180.05670.05910.08230.6580.05710.1480.05930.05280.04790.06570.05640.05450.07870.6310.05570.1370.05580.05770.04670.0603貴州省產(chǎn)品質(zhì)量監(jiān)督檢驗(yàn)院仁懷分院0.06040.05900.07710.6490.06230.1460.06110.05410.05150.06560.05980.05580.08320.6160.05650.1370.05850.05660.04580.06640.05780.05850.08140.6620.06120.1440.06180.05780.05020.06030.05930.06010.07610.6670.06080.1440.05540.05910.05260.06580.06020.05840.08090.6300.05830.1360.06080.05460.05140.05940.06010.05760.08040.6600.06240.1450.06340.05020.05070.06460.06150.05850.07570.6090.05940.1310.06070.05590.04980.06830.05660.06010.08220.6850.05660.1430.06130.05830.05050.06480.05890.05760.08660.6560.06070.1440.06240.05590.05120.05770.05960.05260.07940.6600.05490.1490.05380.05710.04760.06410.06040.05890.08270.6920.05980.1340.06200.05680.04990.0589貴州茅臺(tái)酒股份有0.05880.05520.07870.6280.05910.1390.06140.05650.05030.06300.05580.05710.08110.6800.06040.1490.05800.05310.04830.06780.05910.05530.07950.6010.05690.1410.05990.05500.04500.06390.05890.05520.07620.6020.05900.1340.05060.05410.04860.0551

限公司0.06270.05470.07850.6370.06330.1510.05910.05160.04910.06320.05880.05620.07930.6790.05990.1390.05780.05500.05320.06380.05600.05990.08350.6230.05890.1390.06020.05340.05040.06680.05900.05680.07930.6570.06610.1520.05830.05860.04960.06220.06410.05800.08150.6600.06030.1400.05590.05480.04680.05690.05710.05640.07420.6750.05530.1320.06370.06220.04930.06370.05890.05110.07960.6430.05960.1380.06110.05680.05140.0693樣品3貴州省分析測試研究院0.1100.1110.1270.6510.1120.1910.1260.1130.1080.1110.1090.1080.1280.5930.1210.2030.1320.1250.1050.1020.1100.1080.1370.5810.1130.1930.1240.1130.1050.09800.1110.1120.1270.5990.1120.1920.1190.1160.1060.1010.1110.1100.1390.6270.1220.2110.1260.1210.1060.1020.1120.1130.1280.5950.1140.1930.1230.1130.1070.1000.1100.1090.1260.6550.1130.1880.1310.1170.1160.1030.1090.1170.1390.6020.1240.1960.1260.1240.1100.1070.1100.1090.1270.6000.1130.2120.1250.1150.1090.1010.1110.1110.1270.5830.1190.1920.1330.1160.1020.1000.1130.1120.1230.6210.1200.1900.1210.1130.1070.104貴州省產(chǎn)品質(zhì)重監(jiān)督檢驗(yàn)院0.1110.1100.1220.6110.1170.1890.1250.1130.1070.1020.1080.1090.1290.5930.1150.1920.1190.1220.1120.1080.1080.1100.1370.5830.1130.2030.1250.1130.1060.1040.1120.1170.1270.6320.1120.1920.1210.1160.1060.1010.1100.1110.1290.5960.1240.1950.1250.1200.1120.1010.1130.1120.1230.6160.1140.2140.1340.1130.1070.1090.1090.1090.1270.6030.1120.1950.1250.1160.1070.1020.1080.1090.1270.6320.1210.1850.1230.1240.1050.1080.1090.1100.1310.5800.1130.1970.1180.1150.1070.1010.1110.1190.1270.6010.1140.2090.1230.1160.1140.1100.1140.1150.1230.6440.1210.1930.1240.1180.1070.104貴州省產(chǎn)品質(zhì)量監(jiān)督檢驗(yàn)院仁懷分院0.1150.1170.1370.6450.1200.1970.1300.1210.1100.1090.1160.1060.1270.6130.1120.2050.1330.1130.1120.1090.1150.1160.1350.6370.1210.2010.1200.1250.1110.0980.1160.1170.1360.6260.1240.2080.1290.1230.1130.1060.1070.1150.1290.6470.1190.2080.1300.1210.1150.1020.1170.1090.1360.6160.1180.1880.1320.1200.1100.1060.1170.1150.1270.5890.1200.2060.1190.1190.1040.1100.1100.1160.1350.6380.1220.2070.1290.1240.1130.1040.1160.1080.1280.6500.1130.1920.1300.1230.1150.1060.1120.1160.1350.5920.1210.2060.1320.1130.1060.1020.1160.1160.1350.6420.1120.2120.1340.1210.1150.106貴州茅臺(tái)酒股0.1080.1100.1230.5870.1130.1920.1230.1160.1090.1000.1160.1150.1400.6660.1200.2040.1160.1230.1130.1090.1120.1090.1220.5980.1080.2000.1300.1170.1010.110

份有限公司0.1100.1090.1430.6310.1150.1980.1280.1220.1120.1010.1140.1150.1220.6180.1270.2040.1190.1190.1080.1070.1100.1090.1360.5650.1140.2000.1290.1150.1100.1140.1090.1130.1260.5980.1060.2030.1230.1150.1010.1030.1100.1130.1290.6410.1190.1930.1280.1250.1070.1110.1150.1090.1380.6450.1180.1950.1310.1160.1150.1070.1140.1170.1420.6760.1290.1980.1280.1180.1130.1150.1150.1150.1390.5990.1190.2100.1170.1240.1100.109樣品4貴州省分析測試研究院0.5290.5200.5401.020.5130.6090.5500.5360.5230.4360.5500.5300.5371.050.5200.6030.5470.5470.5270.4390.5260.5530.5241.120.5290.5950.5640.5560.5190.4350.5280.5170.5321.030.5040.6350.6190.6020.5800.4120.5710.5150.5351.030.5140.6010.5650.5460.5230.4110.5160.5080.5191.020.5110.6470.5560.5520.5200.4400.5190.5160.5711.040.5130.6150.6110.6100.5300.4380.5500.5200.5451.120.5560.6020.5650.5600.5270.4220.5240.5250.5821.050.5150.6060.5520.5370.5290.4200.5160.5370.5371.040.5460.6680.6100.5490.5310.4140.5350.5220.5181.090.5230.6030.5580.5610.5310.420貴州省產(chǎn)品質(zhì)重監(jiān)督檢驗(yàn)院0.5400.5280.5401.030.5160.6150.5600.5520.5200.4220.5200.5410.5261.040.5560.5980.5560.5580.5310.4520.5250.5260.5331.100.5150.6170.6130.5400.5570.4300.5270.5190.5761.060.5290.6060.5560.5460.5290.4750.5220.5200.5301.030.5140.6080.6100.6090.5210.4290.5080.5240.5651.090.5140.6330.5550.5610.5270.4350.5160.5390.5411.050.5630.6090.5710.6060.5140.4260.5200.5200.5361.020.5130.6030.5460.5560.5310.4720.5230.5060.5441.040.5200.6520.5740.5470.5740.4240.5170.5150.5271.120.5110.6150.5970.5480.5290.4370.5150.5160.5191.050.5030.6720.5690.5470.5310.437貴州省產(chǎn)品質(zhì)量監(jiān)督檢驗(yàn)院仁懷分院0.5560.5500.5861.100.5160.6570.5860.5400.5700.4770.5620.5260.5301.120.5460.6500.6200.5910.5720.4630.5490.5630.5791.110.5620.5960.5790.5940.5560.4770.5500.5580.5841.120.5710.6490.6180.6060.5610.4300.5260.5630.5711.120.5400.6040.5910.5880.5670.4630.5630.5330.5551.110.5490.6520.5450.5390.5190.4770.5630.5580.5701.120.5540.6440.6080.5800.5690.4450.5580.5580.5851.030.5170.6150.5850.5740.5580.4870.5280.5240.5431.120.5480.6580.5430.5950.5060.4260.5630.5630.5791.060.5040.6090.6190.5400.5690.4740.5580.5610.5691.190.5550.6550.6090.5890.5370.454貴州茅臺(tái)0.5320.5300.5431.050.5330.6340.5600.5610.5360.4530.5410.5400.5581.100.5410.5880.5970.5740.5650.429

酒股份有限公司0.5230.5530.5331.040.5130.6280.5840.5500.5430.4580.5400.5330.5511.060.5340.6310.5900.5740.5010.4570.5360.5340.5481.080.5380.6290.5480.5670.5330.4500.5630.5390.5491.100.5400.6300.5770.5630.5150.4600.5310.5730.5451.050.5290.6630.6100.6130.5560.4570.5330.5380.5581.090.5490.6350.5600.5610.5330.4270.5460.5100.5631.090.5400.6290.5870.5680.5380.4540.5400.5340.5581.150.5330.6540.5690.5770.5500.4550.5380.5290.5451.030.5610.6430.5400.5930.5630.460樣品5貴州省分析測試研究院0.01950.01620.03741.620.01860.09630.01970.01130.01150.01560.01860.01730.03681.590.02040.09470.01820.01250.01060.01540.01920.01650.03491.600.01820.08960.01940.01120.01130.01530.01920.01590.03761.720.02020.09450.01980.01080.01070.01550.01940.01600.04111.600.01850.09560.02010.01160.01140.01470.02130.01640.03661.640.01830.09410.02030.01180.01160.01610.01950.01620.04211.590.01870.09380.01890.01230.01150.01520.01980.01570.03751.610.01930.1020.01960.01170.01230.01650.01920.01630.03421.710.01810.09550.01950.01290.01140.01510.01870.01620.03911.630.01800.09580.01840.01160.01130.01520.01960.01710.03671.740.01840.1030.01930.01070.01160.0166貴州省產(chǎn)品質(zhì)重監(jiān)督檢驗(yàn)院0.02010.01590.03741.620.01850.09560.01940.01080.01140.01520.01950.01600.03521.730.01990.09410.01820.01130.01060.01450.02180.01740.03651.600.01870.1020.02010.01170.01150.01510.01920.01620.04181.590.01860.09550.01950.01230.01130.01610.01940.01670.03671.700.01940.09580.02140.01150.01150.01520.02020.01630.04011.640.02000.1020.01930.01120.01160.01460.01970.01540.03671.730.01840.1040.01970.01290.01230.01560.01960.01610.03731.610.01820.09630.02120.01160.01160.01540.01950.01630.03481.590.01820.09470.02030.01170.01130.01730.02060.01750.03691.630.01930.09160.01990.01080.01170.01550.01920.01620.03771.590.01810.09950.01860.01160.01240.0157貴州省產(chǎn)品質(zhì)量監(jiān)督檢驗(yàn)院仁懷分院0.01890.01690.03961.740.01970.09960.02040.01210.01190.01650.02020.01750.03481.610.01880.1000.01830.01190.01250.01490.01970.01810.04111.710.01890.1010.02110.01240.01140.01640.02080.01700.03861.600.02010.1070.02090.01220.01230.01610.02020.01730.03591.730.01930.1010.02040.01150.01250.01650.02140.01760.03941.740.01950.09150.01970.01230.01210.01630.02010.01590.03571.600.01880.1020.01990.01220.01140.01750.02020.01680.03951.720.02050.1050.02030.01240.01220.01690.01930.01690.04031.610.01940.1010.02060.01210.01090.01620.02080.01710.04121.730.01830.1020.02110.01080.01210.01710.02100.01730.03881.640.01990.1080.02080.01190.01240.0161貴州0.01990.01670.03671.660.01870.09920.01930.01180.01120.0161

茅臺(tái)酒股份有限公司0.02000.01580.04051.570.01940.09200.02050.01210.01150.01610.02090.01650.03721.640.01990.09750.02150.01200.01200.01500.01950.01650.03681.660.01790.08970.01930.01080.01120.01610.01970.01680.04011.570.01850.09750.02010.01140.01140.01530.02010.01670.03771.650.01930.1030.01780.01220.01060.01620.02070.01770.03491.660.02040.09930.01910.01230.01120.01760.01980.01680.03661.580.01890.09840.02040.01170.01150.01610.02060.01620.03941.660.01910.09720.02210.01080.01130.01500.01980.01750.04171.690.01890.09050.01940.01250.01080.01730.02080.01690.03581.610.01860.10020.01890.01280.01190.0162經(jīng)過統(tǒng)計(jì)分析，獲得本方法的重復(fù)性和再現(xiàn)性如下。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，在以下給定的平均值范圍內(nèi)，這兩個(gè)測試結(jié)果的絕對(duì)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)插法獲得：表3重復(fù)性限二土兒素VCrMnFeNiCuAsCdSbPb各兒素含量mg/L0.01520.01040.03200.5200.01360.09330.01360.005840.005550.0103r0.001700.001360.004030.04640.002080.01080.001950.0006570.0006970.0