化學檢驗方法驗證和確認的不同概念
2018-07-26
作者(zhe)：
瀏覽數：1482
方法驗證和確認的不同概念
化學檢測實驗室在檢測過程中如果要保證檢測結果的準確性, 關鍵控制要素之一就是對檢測方法的準確性和測試結果有效性實施掌控。在ISO/IEC17025:2017《檢測和校準實驗室能力通用要求》標準中在對檢測方法的控制要求中就提出了“方法驗證”和“方法確認”二個控制理念。國際上許多檢測機構及實驗室認可機構對“方法驗證”和“方法確認”都有明確的、不同的控制要求, 并規定了不同的技術控制指標。但在我國的許多化學檢測實驗室中, 檢測人員并不能完全正確地理解和執行“方法驗證”和“方法確認”, 有的實驗室人員在檢測過程中對待使用標準方法和非標準方法都采用同一理解方式和操作步驟, 拿到標準方法或非標方法就直接用于檢測, 以致在掌握檢測標準的技術能力方面、在把握非標方法的科學性、準確性和有效性控制方面存在很大的不確定度, 為檢測結果的準確性埋下隱患。筆者通過學習和分析, 認為化學檢測實驗室的技術人員應準確地理解“方法驗證”和“方法確認”這兩個概念, 采用不同的控制方法和技術手段, 以達到保證檢測結果準確、有效的目的, 并充分滿足客戶的檢測需求。
1) 方(fang)(fang)法(fa)驗(yan)(yan)證的(de)(de)(de)對象(xiang):在(zai)(zai)(zai)ISO/IEC 17025:2017《檢測和校(xiao)(xiao)準(zhun)實(shi)驗(yan)(yan)室(shi)能(neng)(neng)(neng)力通(tong)用(yong)(yong)要(yao)求》條款(kuan)中(zhong)規(gui)定“在(zai)(zai)(zai)引(yin)入檢測或(huo)校(xiao)(xiao)準(zhun)之前(qian), 實(shi)驗(yan)(yan)室(shi)應(ying)證實(shi)能(neng)(neng)(neng)夠正確地運用(yong)(yong)這(zhe)些(xie)標準(zhun)方(fang)(fang)法(fa)”, 在(zai)(zai)(zai)英文標準(zhun)的(de)(de)(de)這(zhe)一條款(kuan)中(zhong)采(cai)用(yong)(yong)了(le)(le)“verification”一詞, 英文可譯為“證實(shi)”或(huo)“驗(yan)(yan)證”。標準(zhun)方(fang)(fang)法(fa)是指由公認機構經過評價確認后向社會(hui)公開發(fa)布(bu)的(de)(de)(de)技(ji)術(shu)規(gui)范文件(jian)。ISO/IEC 17025:2017這(zhe)一條款(kuan)的(de)(de)(de)規(gui)定就意味著實(shi)驗(yan)(yan)室(shi)在(zai)(zai)(zai)使(shi)用(yong)(yong)標準(zhun)方(fang)(fang)法(fa)之前(qian), 應(ying)經過方(fang)(fang)法(fa)驗(yan)(yan)證, 或(huo)稱之為方(fang)(fang)法(fa)證實(shi), 即實(shi)驗(yan)(yan)室(shi)在(zai)(zai)(zai)使(shi)用(yong)(yong)標準(zhun)方(fang)(fang)法(fa)進行檢測前(qian)需要(yao)證實(shi)實(shi)驗(yan)(yan)室(shi)使(shi)用(yong)(yong)標準(zhun)方(fang)(fang)法(fa)的(de)(de)(de)技(ji)術(shu)能(neng)(neng)(neng)力是否達到了(le)(le)標準(zhun)的(de)(de)(de)規(gui)定要(yao)求。
2) 方(fang)法(fa)(fa)(fa)(fa)確(que)(que)(que)認(ren)(ren)的(de)(de)(de)(de)對(dui)象:在(zai)(zai)ISO/IEC 17025:2017《檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)和(he)(he)校準(zhun)(zhun)(zhun)實(shi)(shi)驗(yan)(yan)(yan)室(shi)(shi)(shi)(shi)(shi)(shi)(shi)能(neng)力通用(yong)(yong)(yong)(yong)要(yao)求(qiu)》條款中(zhong)(zhong)(zhong)(zhong)規定(ding)“實(shi)(shi)驗(yan)(yan)(yan)室(shi)(shi)(shi)(shi)(shi)(shi)(shi)應對(dui)非標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun)方(fang)法(fa)(fa)(fa)(fa)、實(shi)(shi)驗(yan)(yan)(yan)室(shi)(shi)(shi)(shi)(shi)(shi)(shi)設(she)(she)計(ji) (制定(ding)) 的(de)(de)(de)(de)方(fang)法(fa)(fa)(fa)(fa)、超(chao)(chao)(chao)出(chu)(chu)其(qi)(qi)預定(ding)范(fan)(fan)圍使(shi)(shi)(shi)(shi)用(yong)(yong)(yong)(yong)的(de)(de)(de)(de)標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun)方(fang)法(fa)(fa)(fa)(fa)、擴(kuo)充(chong)和(he)(he)修改(gai)過(guo)(guo)(guo)(guo)的(de)(de)(de)(de)標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun)方(fang)法(fa)(fa)(fa)(fa)進行確(que)(que)(que)認(ren)(ren), 以證實(shi)(shi)該(gai)(gai)方(fang)法(fa)(fa)(fa)(fa)適用(yong)(yong)(yong)(yong)于(yu)(yu)預期的(de)(de)(de)(de)用(yong)(yong)(yong)(yong)途”, 上述這(zhe)四種(zhong)方(fang)法(fa)(fa)(fa)(fa)均屬(shu)于(yu)(yu)非標(biao)(biao)(biao)(biao)(biao)(biao)方(fang)法(fa)(fa)(fa)(fa), 因(yin)(yin)為這(zhe)四類方(fang)法(fa)(fa)(fa)(fa)都(dou)是(shi)(shi)未(wei)通過(guo)(guo)(guo)(guo)公(gong)認(ren)(ren)機構的(de)(de)(de)(de)評價(jia)確(que)(que)(que)認(ren)(ren)并(bing)向社會公(gong)開發(fa)表、僅只由實(shi)(shi)驗(yan)(yan)(yan)室(shi)(shi)(shi)(shi)(shi)(shi)(shi)人員做了(le)(le)評價(jia)而使(shi)(shi)(shi)(shi)用(yong)(yong)(yong)(yong)的(de)(de)(de)(de)方(fang)法(fa)(fa)(fa)(fa)。ISO/IEC 17025標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun)英(ying)文中(zhong)(zhong)(zhong)(zhong)對(dui)確(que)(que)(que)認(ren)(ren)采(cai)用(yong)(yong)(yong)(yong)了(le)(le)“veridition”一(yi)詞(ci), 該(gai)(gai)條款的(de)(de)(de)(de)規定(ding)意味著實(shi)(shi)驗(yan)(yan)(yan)室(shi)(shi)(shi)(shi)(shi)(shi)(shi)在(zai)(zai)使(shi)(shi)(shi)(shi)用(yong)(yong)(yong)(yong)非標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun)方(fang)法(fa)(fa)(fa)(fa)、實(shi)(shi)驗(yan)(yan)(yan)室(shi)(shi)(shi)(shi)(shi)(shi)(shi)設(she)(she)計(ji) (制定(ding)) 的(de)(de)(de)(de)方(fang)法(fa)(fa)(fa)(fa)、超(chao)(chao)(chao)出(chu)(chu)其(qi)(qi)預定(ding)范(fan)(fan)圍使(shi)(shi)(shi)(shi)用(yong)(yong)(yong)(yong)的(de)(de)(de)(de)標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun)方(fang)法(fa)(fa)(fa)(fa)、擴(kuo)充(chong)和(he)(he)修改(gai)過(guo)(guo)(guo)(guo)的(de)(de)(de)(de)標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun)方(fang)法(fa)(fa)(fa)(fa)之前, 應經過(guo)(guo)(guo)(guo)方(fang)法(fa)(fa)(fa)(fa)確(que)(que)(que)認(ren)(ren), 即實(shi)(shi)驗(yan)(yan)(yan)室(shi)(shi)(shi)(shi)(shi)(shi)(shi)需要(yao)確(que)(que)(que)認(ren)(ren)實(shi)(shi)驗(yan)(yan)(yan)室(shi)(shi)(shi)(shi)(shi)(shi)(shi)所(suo)(suo)(suo)使(shi)(shi)(shi)(shi)用(yong)(yong)(yong)(yong)的(de)(de)(de)(de)非標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun)方(fang)法(fa)(fa)(fa)(fa)、實(shi)(shi)驗(yan)(yan)(yan)室(shi)(shi)(shi)(shi)(shi)(shi)(shi)設(she)(she)計(ji) (制定(ding)) 的(de)(de)(de)(de)方(fang)法(fa)(fa)(fa)(fa)、超(chao)(chao)(chao)出(chu)(chu)其(qi)(qi)預定(ding)范(fan)(fan)圍使(shi)(shi)(shi)(shi)用(yong)(yong)(yong)(yong)的(de)(de)(de)(de)標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun)方(fang)法(fa)(fa)(fa)(fa)、擴(kuo)充(chong)和(he)(he)修改(gai)過(guo)(guo)(guo)(guo)的(de)(de)(de)(de)標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun)方(fang)法(fa)(fa)(fa)(fa)所(suo)(suo)(suo)獲得(de)的(de)(de)(de)(de)檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)結(jie)果(guo)(guo)(guo)具有(you)科學性、準(zhun)(zhun)(zhun)確(que)(que)(que)性和(he)(he)有(you)效性。例如, 當需要(yao)檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)全(quan)毛織(zhi)物中(zhong)(zhong)(zhong)(zhong)某(mou)項成分(fen)(fen)(fen)(fen)指標(biao)(biao)(biao)(biao)(biao)(biao)時缺(que)少檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun), 實(shi)(shi)驗(yan)(yan)(yan)室(shi)(shi)(shi)(shi)(shi)(shi)(shi)因(yin)(yin)而采(cai)用(yong)(yong)(yong)(yong)了(le)(le)化(hua)纖(xian)織(zhi)物中(zhong)(zhong)(zhong)(zhong)該(gai)(gai)項成分(fen)(fen)(fen)(fen)指標(biao)(biao)(biao)(biao)(biao)(biao)檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun), 這(zhe)樣(yang)就是(shi)(shi)使(shi)(shi)(shi)(shi)用(yong)(yong)(yong)(yong)了(le)(le)超(chao)(chao)(chao)出(chu)(chu)其(qi)(qi)預定(ding)范(fan)(fan)圍使(shi)(shi)(shi)(shi)用(yong)(yong)(yong)(yong)的(de)(de)(de)(de)標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun)方(fang)法(fa)(fa)(fa)(fa)來(lai)檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce), 實(shi)(shi)驗(yan)(yan)(yan)室(shi)(shi)(shi)(shi)(shi)(shi)(shi)就應通過(guo)(guo)(guo)(guo)試(shi)驗(yan)(yan)(yan)證明采(cai)用(yong)(yong)(yong)(yong)化(hua)纖(xian)織(zhi)物中(zhong)(zhong)(zhong)(zhong)該(gai)(gai)成分(fen)(fen)(fen)(fen)指標(biao)(biao)(biao)(biao)(biao)(biao)檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun)可以用(yong)(yong)(yong)(yong)于(yu)(yu)全(quan)毛織(zhi)物的(de)(de)(de)(de)檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce), 所(suo)(suo)(suo)獲得(de)的(de)(de)(de)(de)檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)結(jie)果(guo)(guo)(guo)仍(reng)然是(shi)(shi)準(zhun)(zhun)(zhun)確(que)(que)(que)和(he)(he)有(you)效的(de)(de)(de)(de)。又(you)如, 元素檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun)方(fang)法(fa)(fa)(fa)(fa)規定(ding)的(de)(de)(de)(de)檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)設(she)(she)備(bei)是(shi)(shi)原(yuan)子(zi)吸(xi)收分(fen)(fen)(fen)(fen)光(guang)(guang)光(guang)(guang)度計(ji), 測(ce)(ce)(ce)定(ding)過(guo)(guo)(guo)(guo)程中(zhong)(zhong)(zhong)(zhong)分(fen)(fen)(fen)(fen)析(xi)每項元素需要(yao)使(shi)(shi)(shi)(shi)用(yong)(yong)(yong)(yong)不同(tong)(tong)的(de)(de)(de)(de)空心陰極燈, 但實(shi)(shi)驗(yan)(yan)(yan)室(shi)(shi)(shi)(shi)(shi)(shi)(shi)在(zai)(zai)檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)某(mou)一(yi)樣(yang)本時需要(yao)同(tong)(tong)時測(ce)(ce)(ce)定(ding)多種(zhong)元素, 因(yin)(yin)此(ci)希望使(shi)(shi)(shi)(shi)用(yong)(yong)(yong)(yong)等離(li)子(zi)耦合(he)發(fa)射光(guang)(guang)譜(pu)儀替(ti)代(dai)原(yuan)子(zi)吸(xi)收分(fen)(fen)(fen)(fen)光(guang)(guang)光(guang)(guang)度計(ji), 以達到一(yi)次性檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)多元素, 提(ti)高檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)速度的(de)(de)(de)(de)目(mu)的(de)(de)(de)(de), 因(yin)(yin)為出(chu)(chu)現了(le)(le)對(dui)原(yuan)標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun)方(fang)法(fa)(fa)(fa)(fa)中(zhong)(zhong)(zhong)(zhong)的(de)(de)(de)(de)設(she)(she)備(bei)替(ti)換, 則實(shi)(shi)驗(yan)(yan)(yan)室(shi)(shi)(shi)(shi)(shi)(shi)(shi)應確(que)(que)(que)認(ren)(ren)這(zhe)樣(yang)的(de)(de)(de)(de)設(she)(she)備(bei)替(ti)代(dai)所(suo)(suo)(suo)獲得(de)到的(de)(de)(de)(de)檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)結(jie)果(guo)(guo)(guo)是(shi)(shi)準(zhun)(zhun)(zhun)確(que)(que)(que)的(de)(de)(de)(de), 因(yin)(yin)此(ci)實(shi)(shi)驗(yan)(yan)(yan)室(shi)(shi)(shi)(shi)(shi)(shi)(shi)通過(guo)(guo)(guo)(guo)兩種(zhong)不同(tong)(tong)設(she)(she)備(bei)對(dui)同(tong)(tong)一(yi)樣(yang)本進行測(ce)(ce)(ce)試(shi), 并(bing)對(dui)所(suo)(suo)(suo)獲得(de)的(de)(de)(de)(de)檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)結(jie)果(guo)(guo)(guo)數(shu)列進行t檢(jian)(jian)(jian)(jian)驗(yan)(yan)(yan)評估, 證明二種(zhong)方(fang)法(fa)(fa)(fa)(fa)獲得(de)的(de)(de)(de)(de)檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)數(shu)據不存在(zai)(zai)顯著性差異, 進而確(que)(que)(que)認(ren)(ren)設(she)(she)備(bei)替(ti)換的(de)(de)(de)(de)結(jie)果(guo)(guo)(guo)是(shi)(shi)準(zhun)(zhun)(zhun)確(que)(que)(que)有(you)效的(de)(de)(de)(de)。從以上的(de)(de)(de)(de)實(shi)(shi)例看(kan), 都(dou)需要(yao)實(shi)(shi)驗(yan)(yan)(yan)室(shi)(shi)(shi)(shi)(shi)(shi)(shi)通過(guo)(guo)(guo)(guo)技術(shu)手段來(lai)確(que)(que)(que)認(ren)(ren)對(dui)原(yuan)標(biao)(biao)(biao)(biao)(biao)(biao)準(zhun)(zhun)(zhun)的(de)(de)(de)(de)擴(kuo)充(chong)或修改(gai)的(de)(de)(de)(de)技術(shu)路(lu)線是(shi)(shi)科學的(de)(de)(de)(de), 所(suo)(suo)(suo)獲得(de)的(de)(de)(de)(de)檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)結(jie)果(guo)(guo)(guo)是(shi)(shi)準(zhun)(zhun)(zhun)確(que)(que)(que)的(de)(de)(de)(de)和(he)(he)有(you)效的(de)(de)(de)(de), 并(bing)能(neng)滿足客戶的(de)(de)(de)(de)檢(jian)(jian)(jian)(jian)測(ce)(ce)(ce)需求(qiu)。
