EN71-3 重金屬測(cè)試方法確認(rèn).docx

洋紫荊油墨（中山）有限公司檢測(cè)實(shí)驗(yàn)室EN71-3 重金屬測(cè)試方法驗(yàn)證報(bào)告1目的確定實(shí)驗(yàn)室具有實(shí)施該標(biāo)準(zhǔn)的檢驗(yàn)?zāi)芰?，?yàn)證該標(biāo)準(zhǔn)在實(shí)驗(yàn)室運(yùn)行的穩(wěn)定性、準(zhǔn)確性。2. 測(cè)試方法： EN71-3：20113. 方法描述: 樣品加入一定量的0.07mol/L的鹽酸溶液，模擬材料在吞咽后與胃酸持續(xù)接觸一段時(shí)間的條件下，從玩具材料中提取出的溶出物用ICP-OES測(cè)定可溶性元素的含量。4. 試劑：-鹽酸溶液I:c( HCl)=(0.07士0.005) mol/L;-鹽酸溶液2:c(HCD=(0.14士0.010)mol/L;-鹽酸溶液3:c(HCI)約等于1 mol/L;-鹽酸溶液4:c(HC1)約等于2 mol/L;-鹽酸溶液5:c(HCI)約等于6 mol/L;-正庚烷;-水（三級(jí)或以上）5. 儀器： 電子天平、離心機(jī)、孔徑為0.5mm的金屬篩、ICP-OES6. 測(cè)試過(guò)程： 稱(chēng)取過(guò)篩后的樣品0.2g于50mL錐形瓶中，加入10mL 37的0.07mol/L的鹽酸溶液，搖動(dòng)1min，調(diào)PH值為1-1.5，避光、在37恒溫條件下震動(dòng)1h再靜置1h，接著立即過(guò)濾，濾液用ICP-OES測(cè)試。7. 工作曲線(xiàn):根據(jù)標(biāo)準(zhǔn)要求，同時(shí)結(jié)合實(shí)驗(yàn)室樣品的需求選擇工作曲線(xiàn)的線(xiàn)性工作范圍，在此范圍內(nèi)具有良好的線(xiàn)性，相關(guān)結(jié)果見(jiàn)下表：表1測(cè)試項(xiàng)目線(xiàn)性范圍（mg/L）擬合公式相關(guān)系數(shù)（R）鋁（Al）0-5y=261400x+4082.80.99998銻（Sb）0-5y=12710x-1143.70.99996砷（As）0-5y=10560x+159.10.99996鋇（Ba）0-5y=449300x+7078.50.99996硼（B）0-5y=186800x+1184.40.99999鎘（Cd）0-1y=332500x+543.60.99998鉻（Cr）0-5y=413600x+3868.30.99997鈷（Co）0-5y=273500x+4385.40.99997銅（Cu）0-5y=542000x+3006.50.99998鉛（Pb）0-5y=61880x+72.30.99999錳（Mn）0-5y=2732000x-23617.80.99999汞（Hg）0-1y=26770x+67.60.99998鎳（Ni）0-5y=232000x+3434.00.99997硒（Se）0-5y=11920x+331.50.99989鍶（Sr）0-0.2y=35230000x-3114.11.00000錫（Sn）0-5y=30280x-868.10.99995鋅（Zn）0-5y=352400x+7742.40.999938. 方法檢出限 分析低濃度標(biāo)液10次，計(jì)算標(biāo)準(zhǔn)偏差（SD），檢出限即為3SD。相關(guān)檢測(cè)數(shù)據(jù)及計(jì)算結(jié)果如下：表2 低濃度標(biāo)液10次檢測(cè)數(shù)據(jù)測(cè)試項(xiàng)目12345678910鋁（Al）0.0430.0450.0450.0470.0450.0450.0470.0480.0460.046銻（Sb）0.0440.0450.0450.0460.0460.0450.0460.0460.0440.044砷（As）0.0450.0460.0450.0460.0460.0450.0460.0460.0440.044鋇（Ba）0.0460.0480.0490.0500.0490.0490.0500.0490.0490.049硼（B）0.0560.0560.0510.0490.0460.0510.0510.0500.0490.048鎘（Cd）0.00080.00090.00090.00080.00090.00090.00100.00100.00100.0010鉻（Cr）0.0460.0440.0450.0450.0450.0460.0460.0470.0470.045鈷（Co）0.01030.01000.00910.01040.01080.01040.01030.01040.01020.0104銅（Cu）0.0490.0510.0510.0550.0520.0520.0530.0530.0530.051鉛（Pb）0.01020.00950.00960.01070.01010.00970.01100.01070.00970.0089錳（Mn）0.0010.0010.0010.0010.0010.0010.0010.0010.0010.001汞（Hg）0.0120.0110.0100.0100.0090.0090.0090.0090.0080.009鎳（Ni）0.0500.0510.0520.0520.0520.0520.0520.0520.0520.051硒（Se）0.0460.0490.0490.0470.0480.0510.0490.0480.0480.048鍶（Sr）0.0100.0100.0110.0100.0110.0110.0100.0110.0110.011錫（Sn）0.0520.0530.0540.0540.0540.0550.0550.0550.0560.055鋅（Zn）0.0480.0500.0510.0520.0510.0510.0510.0520.0510.050根據(jù)標(biāo)準(zhǔn)偏差計(jì)算公式=i=1n(xi-x)2n-1 計(jì)算各化合物的標(biāo)準(zhǔn)偏及方法檢出限表3測(cè)試項(xiàng)目標(biāo)準(zhǔn)偏差(mg/L)方法檢出限（樣液）(mg/L)方法檢出限（試樣）(mg/kg)鋁（Al）0.0010.0030.15銻（Sb）0.0010.0030.15砷（As）0.0010.0030.15鋇（Ba）0.0010.0030.15硼（B）0.0030.0090.45鎘（Cd）0.0000.0000鉻（Cr）0.0010.0030.15鈷（Co）0.0010.0030.15銅（Cu）0.0020.0050.25鉛（Pb）0.0010.0030.15錳（Mn）0.0000.0000汞（Hg）0.0010.0030.15鎳（Ni）0.0010.0030.15硒（Se）0.0010.0030.15鍶（Sr）0.0010.0030.15錫（Sn）0.0010.0030.15鋅（Zn）0.0010.0030.15由于以上檢出限由統(tǒng)計(jì)而來(lái)，所以需要對(duì)其進(jìn)行驗(yàn)證，重復(fù)測(cè)試10次期望的檢出限濃度，計(jì)算平均值與標(biāo)稱(chēng)值的偏差，以下為驗(yàn)證結(jié)果：表4測(cè)試項(xiàng)目12345678910鋁（Al）0.0430.0450.0450.0470.0450.0450.0470.0480.0460.046銻（Sb）0.0440.0450.0450.0460.0460.0450.0460.0460.0440.044砷（As）0.0450.0460.0450.0460.0460.0450.0460.0460.0440.044鋇（Ba）0.0460.0480.0490.0500.0490.0490.0500.0490.0490.049硼（B）0.0560.0560.0510.0490.0460.0510.0510.0500.0490.048鎘（Cd）0.00080.00090.00090.00080.00090.00090.00100.00100.00100.0010鉻（Cr）0.0460.0440.0450.0450.0450.0460.0460.0470.0470.045鈷（Co）0.01030.010.00910.01040.01080.01040.01030.01040.01020.0104銅（Cu）0.0490.0510.0510.0550.0520.0520.0530.0530.0530.051鉛（Pb）0.01020.00950.00960.01070.01010.00970.01100.01070.00970.0089錳（Mn）0.0010.0010.0010.0010.0010.0010.0010.0010.0010.001汞（Hg）0.0120.0110.0100.0100.0090.0090.0090.0090.0080.009鎳（Ni）0.0500.0510.0520.0520.0520.0520.0520.0520.0520.051硒（Se）0.0460.0490.0490.0470.0480.0510.0490.0480.0480.048鍶（Sr）0.0100.0100.0110.0100.0110.0110.0100.0110.0110.011錫（Sn）0.0520.0530.0540.0540.0540.0550.0550.0550.0560.055鋅（Zn）0.0480.0500.0510.0520.0510.0510.0510.0520.0510.050經(jīng)驗(yàn)證的方法檢出限及報(bào)告限如下表：表5 測(cè)試項(xiàng)目10次測(cè)試平均值標(biāo)稱(chēng)值偏差偏差要求方法檢出限（樣液）(mg/L)方法檢出限（試樣）(mg/kg)報(bào)告限(mg/kg)鋁（Al）0.04570.050-8.6100.0502.55銻（Sb）0.04510.050-9.8100.0502.55砷（As）0.04530.050-9.4100.0502.52.5鋇（Ba）0.04880.050-2.4100.0502.55硼（B）0.05070.0501.4100.0502.55鎘（Cd）0.000920.001-8.0100.0010.050.1鉻（Cr）0.04560.050-8.8100.0502.55鈷（Co）0.01020.0102.0100.0100.52銅（Cu）0.0520.0504.0100.0502.55鉛（Pb）0.01000.0100100.0100.52錳（Mn）0.00100.0010100.0010.055汞（Hg）0.00960.010-4.0100.0100.51鎳（Ni）0.05160.0503.2100.0502.55硒（Se）0.04830.050-3.4100.0502.55鍶（Sr）0.01060.0106.0100.0100.51錫（Sn）0.05430.0508.6100.0502.55鋅（Zn）0.05070.0501.4100.0502.559. 方法的準(zhǔn)確性和重復(fù)性方法的準(zhǔn)確性通過(guò)回收率試驗(yàn)進(jìn)行測(cè)試，加標(biāo)回收率的計(jì)算公式為：回收率=加標(biāo)樣品濃度-樣品濃度加標(biāo)濃度100% ，相關(guān)結(jié)果見(jiàn)下表表6測(cè)試項(xiàng)目樣品濃度(mg/kg)加標(biāo)樣品濃度(mg/kg)加標(biāo)濃度(mg/kg)回收率(%)鋁（Al）52525100銻（Sb）5202580砷（As）2202580鋇（Ba）5232592硼（B）52825112鎘（Cd）1202580鉻（Cr）30522588鈷（Co）2212584銅（Cu）5222588鉛（Pb）5212584錳（Mn）5212584汞（Hg）12.62.5104鎳（Ni）5222588硒（Se）5202580鍶（Sr）12.22.588錫（Sn）5232592鋅（Zn）5222588方法的重復(fù)性通過(guò)重復(fù)對(duì)樣品進(jìn)行確定，對(duì)樣品進(jìn)行8次重復(fù)測(cè)量，相關(guān)如下：表7測(cè)試項(xiàng)目測(cè)試結(jié)果 （mg/kg）RSD(%)12345678鋁（Al）999888886.2銻（Sb）55555555砷（As）2.52.52.52.52.52.52.52.5鋇（Ba）91929290919289911.2硼（B）55555555鎘（Cd）0.10.10.10.10.10.10.10.1鉻（Cr）55555555鈷（Co）22222