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1、白酒中機、銘、鎰、鐵、銅、銀、礎(chǔ)、鎘、鑲、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、標準起草的基本情況(包括簡要的任務(wù)來源介紹、主要起草單位、起草人等)本項目由貴州省衛(wèi)生和計劃生育委員會組織食品安全地方標準評審委員會專家組進行評審并通過立項,2015年5月11日以“衛(wèi)計辦函201594號”下發(fā)任務(wù)。由貴州茅臺酒股份有 限公司負責。本標準主要起草單位為:貴州茅臺酒股份有限公司本標準主要起草人為:王莉、汪地強、趙振宇、曾穩(wěn)穩(wěn) 、榮茂、龍薇運、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、本標準的編制原則必要性:白酒中無機元素的來
2、源與釀造環(huán)境(土壤、糧食、水源)、釀造工藝、蒸儲工藝、 蒸儲設(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)易遷移的風險元素含量,對白酒行業(yè)具有重要意義。先進性:該方法不需要傳統(tǒng)的消解步驟,處理步驟簡單并可實現(xiàn)一次性進樣檢測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)的國家標準。2、工作過程立項批準2014年6月3日,貴州省衛(wèi)生和計劃生育委員會下發(fā)關(guān)于征集2014年貴州省食品安全地方標準制(修)訂立項建議的函(黔衛(wèi)計函【2014】29號)。我公司于2014年7月向衛(wèi)計委提交立項申請,并于 2014年8月向食品安全地
3、方標準審評委員會相關(guān)專家進行項目申請說明。2015年5月11日貴州省衛(wèi)生和計劃生育委員會辦公室下發(fā)省衛(wèi)生計生委辦公室關(guān)于同意 貴州苕粉 等25項貴州省食品安全地方標準立項的通知(黔衛(wèi)計辦函 【2015】94號)。任務(wù)落實貴州茅臺酒股份有限公司技術(shù)中心負責試驗、起草標準文本;貴州省分析測試研究院負責第一驗證;貴州省產(chǎn)品質(zhì)量監(jiān)督檢測院負責第二驗證;貴州省質(zhì)檢院仁懷分院(國家酒檢中心)負責第三驗證。起草工作計劃于2016年5月前完成。、各階段工作過程2015年5月,在接到標準制定任務(wù)后,我們成立了電感耦合等離子體質(zhì)譜法檢測白 酒中無機元素地方標準起草小組,明確起草人和工作任務(wù)。2015年6月2016
4、年2月,根據(jù)前期大量的數(shù)據(jù)收集工作,以及對貴州省白酒釀造工藝的調(diào)查了解,分析各工藝環(huán)節(jié)易遷移進入白酒的10種風險無機元素,并從方法的線性、檢出限、定量限、穩(wěn)定性、準確度等方面進行條件試驗,在此基礎(chǔ)上編寫了標準文本初稿。2016年2月24日,在貴州省分析測試研究院召開標準起草討論會,對標準文本初稿 及樣品的制備方面進行了探討,確定方法驗證實施方案。2016年2月25日-3月7日,完成標準文本初稿修改完善和驗證樣品制備,在空白酒樣的基礎(chǔ)上約添加 5ppb、50ppb、100ppb、500ppb的標液,F(xiàn)e額外增加一個 1000ppb的濃度 梯度,各元素含量共設(shè) 5個梯度,共計5份樣品。2016年3
5、月8號4月10號,三家方法驗證單位(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 照標準文本初稿中的方法進行了驗證,包括回收率、精密度、穩(wěn)定性驗證。2016年4月,匯總分析驗證數(shù)據(jù), 寫標準編制說明,起草組根據(jù)驗證情況召開討論會, 研究下一步工作。2016年5月,組織公司技術(shù)委員會對標準文本進行審核,并對文本進行修改。3、主要實驗(或驗證)的分析報告現(xiàn)有的食品中無機元素的國標測定方法,其測定元素相對單一, 工作量大,已經(jīng)不滿足現(xiàn)代企業(yè)對食品安全監(jiān)控快速靈敏的要求,通過查閱大量國內(nèi)外無機元素分析方法并進行比對分析,本方法采用IC
6、P-MS對白7W中10種無機元素進行分析,這 10種無機元素是前期大量的測 量數(shù)據(jù)并結(jié)合行業(yè)實際情況而確定。通過探討樣品中酒精等有機質(zhì)對各無機元素響應(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,上機進 樣分析,大大提高工作效率,并以回收率、精密度、穩(wěn)定性對方法進行了驗證,建立了白酒中 鈕、銘、鎰、鐵、銅、饃、神、鎘、睇、鉛的測定方法。將5個白酒試樣分別稱取 11份,按上述分析方法測定10種無機元素含量,分析結(jié)果如下表1 :元素VCrMnFeNiCuAsCdSbPb樣 品1測士值0.01540.01040.03280.5340.01370.09400.0
7、1310.005850.005420.01010.01440.01070.03150.5070.01400.08970.01450.006000.005910.009700.01520.01050.03240.5100.01350.09360.01230.005850.005400.01010.01650.01050.03350.5230.01480.09340.01320.005810.004800.01030.01540.01060.03240.5150.01290.09660.01360.005210.005430.01060.01540.01130.03250.5390.01160.0
8、9410.01390.005900.005610.01140.01450.01050.03150.5440.01320.09240.01440.005860.005480.01050.01530.01040.03270.5030.01420.09090.01420.006000.006000.01010.01440.01030.03270.5330.01500.09250.01500.006010.005640.01130.01530.01050.03380.5420.01450.09360.01410.005860.005900.01060.01640.01140.03260.5200.01
9、330.09770.01380.005300.005200.00980均 值0.01530.01060.03260.5250.01370.09350.01380.005790.005530.0104RSD%4.583.402.142.777.112.425.564.726.295.34樣品2測士值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
10、.05990.05500.04500.06390.05890.05520.07620.6020.05900.1340.05060.05410.04860.05510.06270.05470.07850.6370.06330.1510.05910.05160.04910.06320.05880.05620.07930.6790.05990.1390.05780.05500.05320.06380.05600.05990.08350.6230.05890.1390.06020.05340.05040.06680.05900.05680.07930.6570.06610.1520.05830.058
11、60.04960.06220.06410.05800.08150.6600.06030.1400.05590.05480.04680.05690.05710.05640.07420.6750.05530.1320.06370.06220.04930.06370.05890.05110.07960.6430.05960.1380.06110.05680.05140.0693均 值0.05900.05600.07920.6440.05990.1410.05870.05560.04930.0632RSD%4.233.933.154.484.804.645.815.274.466.68樣品3測士值0.
12、1080.1100.1230.5870.1130.1920.1230.1160.1090.1000.1160.1150.1400.6660.1200.2040.1160.1230.1130.1090.1120.1090.1220.5980.1080.2000.1300.1170.1010.1100.1100.1090.1430.6310.1150.1980.1280.1220.1120.1010.1140.1150.1220.6180.1270.2040.1190.1190.1080.1070.1100.1090.1360.5650.1140.2000.1290.1150.1100.1140.
13、1090.1130.1260.5980.1060.2030.1230.1150.1010.1030.1100.1130.1290.6410.1190.1930.1280.1250.1070.111表1鈕、銘、鎰、鐵、銅、饃、神、鎘、睇、鉛含量分析結(jié)果單位: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0.1120.1120.133
14、0.6200.1170.2000.1250.1190.1090.108RSD%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0.5360.5340.5481.080.538
15、0.6290.5480.5670.5330.450樣士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
16、.6430.5400.5930.5630.460均 值0.5380.5370.5501.080.5370.6330.5750.5730.5390.451RSD%1.922.901.563.122.232.953.743.023.582.590.01990.01670.03671.660.01870.09920.01930.01180.01120.01610.02000.01580.04051.570.01940.09200.02050.01210.01150.01610.02090.01650.03721.640.01990.09750.02150.01200.01200.01500.0195
17、0.01650.03681.660.01790.08970.01930.01080.01120.0161測0.01970.01680.04011.570.01850.09750.02010.01140.01140.0153樣士0.02010.01670.03771.650.01930.1030.01780.01220.01060.0162值0.02070.01770.03491.660.02040.09930.01910.01230.01120.0176品0.01980.01680.03661.580.01890.09840.02040.01170.01150.016150.02060.016
18、20.03941.660.01910.09720.02210.01080.01130.01500.01980.01750.04171.690.01890.09050.01940.01250.01080.01730.02080.01690.03581.610.01860.10020.01890.01280.01190.0162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5個不同濃度的白酒中品平行測定11次,相對
19、標準偏差為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,滿足白酒中鈕、 銘、鎰、 鐵、銅、銀、碑、鎘、睇、鉛的含量分析。2。4個實驗室參與了本標準的比對驗證,對5個不同濃度的樣品進行了分析,結(jié)果見表70ftVCrMnFeNiCuAsCdSbPb樣 品1貴州 省分 析測 試研 究院0.01450.009600.03010.4920.01260.08710.01410.005500.005400.009500.01480.009800.02960.5180.01380.08810.01290.005400.005600.009600.01410.01080.03320.49
20、40.01250.09750.01280.005800.005100.009900.01460.01020.03010.4990.01310.08890.01280.005400.005200.01010.01490.009900.02970.5210.01420.08760.01320.005600.005500.009700.01520.009600.03080.5010.01290.08890.01340.005700.005300.009600.01540.01030.03100.4970.01360.08840.01290.005800.005700.009800.01570.010
21、30.02990.5210.01440.08960.01270.005800.005200.009900.01580.01060.03360.5170.01280.08750.01390.005500.005400.01010.01450.01020.03110.4960.01370.09020.01310.006100.005800.009600.01560.009700.02970.5100.01380.09910.01490.005600.005200.0107貴州 省廣 品質(zhì) 里監(jiān) 督檢 驗院0.01450.01020.03100.5090.01380.09270.01300.0055
22、00.005600.009900.01420.009800.03120.4990.01270.08920.01270.005600.005400.01040.01460.009600.02960.4940.01240.1010.01290.005500.005200.01010.01520.009800.03220.5470.01320.09140.01430.005900.005200.009800.01460.01040.03150.5120.01370.08760.01350.006100.005700.01030.01430.01010.03260.5310.01310.09240.0
23、1310.006000.005400.009500.01470.009600.03390.5120.01360.09750.01330.005800.005200.009700.01450.009700.03080.4990.01410.09270.01280.005700.005100.01010.01430.01060.03240.5430.01400.08970.01310.005500.005600.01060.01440.01070.03370.5120.01340.09480.01290.005700.005100.009800.01570.01120.02990.5130.013
24、20.09040.01440.006200.005300.00990貴州 省廣 品質(zhì) 里監(jiān) 督檢 驗院 仁懷 分院0.01570.009800.03010.4980.01380.1020.01420.005900.005900.01090.01490.01120.03520.5510.01420.09840.01290.006200.006100.01120.01560.01130.03450.5390.01460.08760.01450.006400.005800.01130.01450.01100.03190.5490.01410.09960.01380.006300.005900.010
25、70.01630.01070.03470.5510.01280.09450.01470.006000.005700.009900.01690.009900.03380.5450.01460.09870.01330.006100.006100.01120.01610.01150.02980.5400.01470.1020.01270.006400.006200.01080.01590.01140.03420.4970.01390.09810.01390.005800.005800.01120.01650.01080.03290.5170.01260.09720.01420.006100.0059
26、00.01110.01620.01010.03520.5380.01450.08880.01450.006300.005700.009800.01570.01120.03150.5560.01470.09630.01280.006200.006100.0108貴州 茅臺 酒股 份有 限公0.01540.01040.03280.5340.01370.09400.01310.005850.005420.01010.01440.01070.03150.5070.01400.08970.01450.006000.005910.009700.01520.01050.03240.5100.01350.09
27、360.01230.005850.005400.01010.01650.01050.03350.5230.01480.09340.01320.005810.004800.01030.01540.01060.03240.5150.01290.09660.01360.005210.005430.0106表2對比樣品分析結(jié)果單位:mg/L司0.01540.01130.03250.5390.01160.09410.01390.005900.005610.01140.01450.01050.03150.5440.01320.09240.01440.005860.005480.01050.01530.01
28、040.03270.5030.01420.09090.01420.006000.006000.01010.01440.01030.03270.5330.01500.09250.01500.006010.005640.01130.01530.01050.03380.5420.01450.09360.01410.005860.005900.01060.01640.01140.03260.5200.01330.09770.01380.005300.005200.00980樣 品2貴州 省分 析測 試研 究院0.05810.05510.07310.6170.05780.1380.05880.05860
29、.04740.06210.05750.05460.07770.6320.05690.1310.05490.05450.04550.06040.05660.05180.07820.6080.06350.1340.05740.05390.04710.05820.05820.05240.08220.6530.05710.1360.06350.05770.05130.06130.05780.05460.07660.6170.05690.1470.05710.05420.04760.06750.05810.05820.07780.5980.05950.1350.06040.05380.05020.063
30、10.05660.05390.08140.6260.05640.1450.05680.05470.04780.06080.05680.05530.07680.6890.05880.1370.06230.05150.04870.06650.05670.05390.07820.6340.05490.1460.05840.05360.04570.06070.05870.05510.07410.6780.06210.1370.06310.05740.05350.06150.05840.05480.07840.6320.05690.1330.05750.05290.04790.0683貴州 省廣 品質(zhì)
31、量監(jiān) 督檢 驗院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.
32、06110.05520.08480.6480.05740.1320.05870.05460.04760.06130.05760.05490.07760.6220.05650.1450.06340.05110.04610.06680.05780.05730.07690.6300.06340.1380.05860.05470.04810.06250.05570.05390.08120.6050.05810.1300.06110.05630.05230.06180.05670.05910.08230.6580.05710.1480.05930.05280.04790.06570.05640.0545
33、0.07870.6310.05570.1370.05580.05770.04670.0603貴州 省廣 品質(zhì)督檢 驗院 仁懷 分院0.06040.05900.07710.6490.06230.1460.06110.05410.05150.06560.05980.05580.08320.6160.05650.1370.05850.05660.04580.06640.05780.05850.08140.6620.06120.1440.06180.05780.05020.06030.05930.06010.07610.6670.06080.1440.05540.05910.05260.06580.0
34、6020.05840.08090.6300.05830.1360.06080.05460.05140.05940.06010.05760.08040.6600.06240.1450.06340.05020.05070.06460.06150.05850.07570.6090.05940.1310.06070.05590.04980.06830.05660.06010.08220.6850.05660.1430.06130.05830.05050.06480.05890.05760.08660.6560.06070.1440.06240.05590.05120.05770.05960.05260
35、.07940.6600.05490.1490.05380.05710.04760.06410.06040.05890.08270.6920.05980.1340.06200.05680.04990.0589貴州 茅臺 酒股 份有0.05880.05520.07870.6280.05910.1390.06140.05650.05030.06300.05580.05710.08110.6800.06040.1490.05800.05310.04830.06780.05910.05530.07950.6010.05690.1410.05990.05500.04500.06390.05890.0552
36、0.07620.6020.05900.1340.05060.05410.04860.0551限公 司0.06270.05470.07850.6370.06330.1510.05910.05160.04910.06320.05880.05620.07930.6790.05990.1390.05780.05500.05320.06380.05600.05990.08350.6230.05890.1390.06020.05340.05040.06680.05900.05680.07930.6570.06610.1520.05830.05860.04960.06220.06410.05800.0815
37、0.6600.06030.1400.05590.05480.04680.05690.05710.05640.07420.6750.05530.1320.06370.06220.04930.06370.05890.05110.07960.6430.05960.1380.06110.05680.05140.0693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
38、.1930.1240.1130.1050.09800.1110.1120.1270.5990.1120.1920.1190.1160.1060.1010.1110.1100.1390.6270.1220.2110.1260.1210.1060.1020.1120.1130.1280.5950.1140.1930.1230.1130.1070.1000.1100.1090.1260.6550.1130.1880.1310.1170.1160.1030.1090.1170.1390.6020.1240.1960.1260.1240.1100.1070.1100.1090.1270.6000.113
39、0.2120.1250.1150.1090.1010.1110.1110.1270.5830.1190.1920.1330.1160.1020.1000.1130.1120.1230.6210.1200.1900.1210.1130.1070.104貴州 省廣 品質(zhì) 里監(jiān) 督檢 驗院0.1110.1100.1220.6110.1170.1890.1250.1130.1070.1020.1080.1090.1290.5930.1150.1920.1190.1220.1120.1080.1080.1100.1370.5830.1130.2030.1250.1130.1060.1040.1120.1
40、170.1270.6320.1120.1920.1210.1160.1060.1010.1100.1110.1290.5960.1240.1950.1250.1200.1120.1010.1130.1120.1230.6160.1140.2140.1340.1130.1070.1090.1090.1090.1270.6030.1120.1950.1250.1160.1070.1020.1080.1090.1270.6320.1210.1850.1230.1240.1050.1080.1090.1100.1310.5800.1130.1970.1180.1150.1070.1010.1110.1
41、190.1270.6010.1140.2090.1230.1160.1140.1100.1140.1150.1230.6440.1210.1930.1240.1180.1070.104貴州 省廣 品質(zhì) 里監(jiān) 督檢 驗院 仁懷 分院0.1150.1170.1370.6450.1200.1970.1300.1210.1100.1090.1160.1060.1270.6130.1120.2050.1330.1130.1120.1090.1150.1160.1350.6370.1210.2010.1200.1250.1110.0980.1160.1170.1360.6260.1240.2080.129
42、0.1230.1130.1060.1070.1150.1290.6470.1190.2080.1300.1210.1150.1020.1170.1090.1360.6160.1180.1880.1320.1200.1100.1060.1170.1150.1270.5890.1200.2060.1190.1190.1040.1100.1100.1160.1350.6380.1220.2070.1290.1240.1130.1040.1160.1080.1280.6500.1130.1920.1300.1230.1150.1060.1120.1160.1350.5920.1210.2060.132
43、0.1130.1060.1020.1160.1160.1350.6420.1120.2120.1340.1210.1150.106貴州 茅臺 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0.1100.1090.1430.6310.1150.1980.1280.1220.1120.1010.1140.1150.1220.618
44、0.1270.2040.1190.1190.1080.1070.1100.1090.1360.5650.1140.2000.1290.1150.1100.1140.1090.1130.1260.5980.1060.2030.1230.1150.1010.1030.1100.1130.1290.6410.1190.1930.1280.1250.1070.1110.1150.1090.1380.6450.1180.1950.1310.1160.1150.1070.1140.1170.1420.6760.1290.1980.1280.1180.1130.1150.1150.1150.1390.599
45、0.1190.2100.1170.1240.1100.109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.
46、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 省廣 品質(zhì) 里監(jiān) 督
47、檢 驗院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.
48、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 省廣 品質(zhì) 里監(jiān) 督檢 驗院 仁懷 分院0.5560.5500.5861.100.5160.6570.586
49、0.5400.5700.4770.5620.5260.5301.120.5460.6500.6200.5910.5720.4630.5490.5630.5791.110.5620.5960.5790.5940.5560.4770.5500.5580.5841.120.5710.6490.6180.6060.5610.4300.5260.5630.5711.120.5400.6040.5910.5880.5670.4630.5630.5330.5551.110.5490.6520.5450.5390.5190.4770.5630.5580.5701.120.5540.6440.6080.5800
50、.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0.5320.5300.5431.050.5330.6340.5600.5610.5360.4530.5410.5400.5581.100.5410.5880.5970.5740.
51、5650.429酒股 份有 限公 司0.5230.5530.5331.040.5130.6280.5840.5500.5430.4580.5400.5330.5511.060.5340.6310.5900.5740.5010.4570.5360.5340.5481.080.5380.6290.5480.5670.5330.4500.5630.5390.5491.100.5400.6300.5770.5630.5150.4600.5310.5730.5451.050.5290.6630.6100.6130.5560.4570.5330.5380.5581.090.5490.6350.5600.5
52、610.5330.4270.5460.5100.5631.090.5400.6290.5870.5680.5380.4540.5400.5340.5581.150.5330.6540.5690.5770.5500.4550.5380.5290.5451.030.5610.6430.5400.5930.5630.460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
53、.01650.03491.600.01820.08960.01940.01120.01130.01530.01920.01590.03761.720.02020.09450.01980.01080.01070.01550.01940.01600.04111.600.01850.09560.02010.01160.01140.01470.02130.01640.03661.640.01830.09410.02030.01180.01160.01610.01950.01620.04211.590.01870.09380.01890.01230.01150.01520.01980.01570.037
54、51.610.01930.1020.01960.01170.01230.01650.01920.01630.03421.710.01810.09550.01950.01290.01140.01510.01870.01620.03911.630.01800.09580.01840.01160.01130.01520.01960.01710.03671.740.01840.1030.01930.01070.01160.0166貴州 省廣 品質(zhì) 量監(jiān) 督檢 驗院0.02010.01590.03741.620.01850.09560.01940.01080.01140.01520.01950.0160
55、0.03521.730.01990.09410.01820.01130.01060.01450.02180.01740.03651.600.01870.1020.02010.01170.01150.01510.01920.01620.04181.590.01860.09550.01950.01230.01130.01610.01940.01670.03671.700.01940.09580.02140.01150.01150.01520.02020.01630.04011.640.02000.1020.01930.01120.01160.01460.01970.01540.03671.730.
56、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 省廣 品質(zhì) 里監(jiān) 督檢 驗院 仁懷 分院0.01890.0169
57、0.03961.740.01970.09960.02040.01210.01190.01650.02020.01750.03481.610.01880.1000.01830.01190.01250.01490.01970.01810.04111.710.01890.1010.02110.01240.01140.01640.02080.01700.03861.600.02010.1070.02090.01220.01230.01610.02020.01730.03591.730.01930.1010.02040.01150.01250.01650.02140.01760.03941.740.01
58、950.09150.01970.01230.01210.01630.02010.01590.03571.600.01880.1020.01990.01220.01140.01750.02020.01680.03951.720.02050.1050.02030.01240.01220.01690.01930.01690.04031.610.01940.1010.02060.01210.01090.01620.02080.01710.04121.730.01830.1020.02110.01080.01210.01710.02100.01730.03881.640.01990.1080.02080
59、.01190.01240.0161貴州0.01990.01670.03671.660.01870.09920.01930.01180.01120.0161茅臺 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.
60、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
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