玻璃儀器計(jì)量

1、2016,玻璃量器檢定規(guī)程,請?jiān)诖溯斎肽母睒?biāo)題,GMP,法規(guī)要求,1,玻璃量器檢定規(guī)程,2,實(shí)例,3,Contents,目,錄,GMP,法規(guī)要求,1,玻璃量器檢定規(guī)程,2,實(shí)例,3,Contents,目,錄,1. GMP,法規(guī)要求,應(yīng)當(dāng)按照操作規(guī)程和校準(zhǔn)計(jì)劃定期對生產(chǎn)和檢驗(yàn)用衡器,量具、儀表、記錄和控制設(shè)備以及儀器進(jìn)行校準(zhǔn)和檢查,并保存相關(guān)記錄。校準(zhǔn)的量程范圍應(yīng)當(dāng)涵蓋實(shí)際生產(chǎn)和,檢驗(yàn)的使用范圍,第九十條,應(yīng)當(dāng)確保生產(chǎn)和檢驗(yàn)使用的關(guān)鍵衡器、量具、儀表、記,錄和控制設(shè)備以及儀器經(jīng)過校準(zhǔn)，所得出的數(shù)據(jù)準(zhǔn)確,可靠,第九十一條,1. GMP,法規(guī)要求,應(yīng)當(dāng)使用計(jì)量標(biāo)準(zhǔn)器具進(jìn)行校準(zhǔn)，且所用計(jì)量標(biāo)準(zhǔn)器具應(yīng)

2、,當(dāng)符合國家有關(guān)規(guī)定。校準(zhǔn)記錄應(yīng)當(dāng)標(biāo)明所用計(jì)量標(biāo)準(zhǔn)器,具的名稱、編號、校準(zhǔn)有效期和計(jì)量合格證明編號，確保,記錄的可追溯性,第九十二條,不得使用未經(jīng)校準(zhǔn)、超過校準(zhǔn)有效期、失準(zhǔn)的衡器、量具,儀表以及用于記錄和控制的設(shè)備、儀器,第九十一四條,第九十三條,衡器、量具、儀表、用于記錄和控制的設(shè)備以及儀器應(yīng)當(dāng)有,明顯的標(biāo)識，標(biāo)明其校準(zhǔn)有效期,GMP,法規(guī)要求,1,玻璃量器檢定規(guī)程,2,實(shí)例,3,Contents,目,錄,常用玻璃量器,滴定管、吸量管、容量,瓶、量筒、量杯等常用,玻璃量器,01,海水溶解氧滴定管,微量吸管、奧式吸管,比色管、離心管、刻,度試管、血糖管、消,化管,03,用于傳遞容量量值的,工作

3、標(biāo)準(zhǔn),02,專用玻璃量器,標(biāo)準(zhǔn)玻璃容器,玻璃量器的分類,PART 2.1,常用玻璃量器檢定規(guī)程,Verification regulation of working glass container,JJG 196-2006,常用玻璃量器檢定規(guī)程,2.1.1,常用玻璃量器的檢定范圍,1,種類,常用玻璃量具包括滴定,管、分度吸量管、單標(biāo),線吸量管、單標(biāo)線容量,瓶、量筒和量杯,分類,玻璃量器按其型式分為量,入式、量出式；按其準(zhǔn)確,度不同分為,A,級和,B,級，其,中量筒和量杯不分級,2.1.2,常用玻璃器具的檢驗(yàn)條件,檢定設(shè)備,儀器名稱,測量范圍,技術(shù)要求,備注,天平,200g,分度值,0.1mg,

4、天平,1000g,分度值,2mg,天平,5000g,分度值,10mg,砝碼組,1500,g,F2,級,電子天平除外,砝碼組,1500,mg,F2,級,電子天平除外,標(biāo)準(zhǔn)玻璃量器組,0.52000,ml,一、二等,應(yīng)符合,JJG-2001,精密溫度計(jì),1030,分度值,0.1,偏光應(yīng)力儀,定量測定,秒表,分辨力,0.1s,附件,檢定架、測溫筒、放大鏡、有蓋的稱量杯等,2.1.3,常用玻璃器具的檢驗(yàn)項(xiàng)目,應(yīng)力,密合性,流出時(shí)間,容量示值,外觀,只在首次檢定,2.1.3.1,外觀,玻璃器具標(biāo)記,05,trademark,廠名或商標(biāo),01,type,量入式用“In”，量出,式用“Ex”，吹出式用,吹”

5、或“Blow out,03,capacity and volume,總?cè)萘亢蛦挝?xxml,02,temperature,標(biāo)準(zhǔn)溫度,20,04,time,等待時(shí)間,xxs,06,accuracy,準(zhǔn)確度,A,或,B,有準(zhǔn),確度等級，但未標(biāo)明,按,B,處理,調(diào)零,調(diào)整應(yīng)力儀零,點(diǎn)，置全波段,將被檢量器平,直或者垂直放,入起偏鏡與檢,偏鏡之間的視,場中，轉(zhuǎn)向轉(zhuǎn),動量器，找到,最大應(yīng)力點(diǎn),轉(zhuǎn)動角,引入,1/4,波片,此時(shí)有應(yīng)力處出,現(xiàn)亮區(qū)，旋轉(zhuǎn)檢,偏鏡，使亮區(qū)逐,漸消失，消失程,度的判斷，應(yīng)以,藍(lán)灰色剛好被褐,色取代為止。讀,出轉(zhuǎn)角度,厚度,測量被測點(diǎn)厚,度,應(yīng)力值,f,d,單位長度光,程差,f,儀

6、器轉(zhuǎn)化系數(shù),3.14nm,檢偏鏡旋轉(zhuǎn),角,d,被測部位厚,度,cm,2.1.3.2,應(yīng)力,檢測方法,2.1.3.2,應(yīng)力,合格標(biāo)準(zhǔn),名稱,殘余內(nèi)應(yīng)力,量器（滴定管除外,單位厚度光程差,100nm/cm,滴定管、活塞芯和量瓶、量筒的塞蓋,單位厚度光程差,120nm/cm,玻璃活塞,滴定管,當(dāng)水注最高標(biāo)線,時(shí)，活塞在關(guān)閉,狀況下停留,20min,后，滲漏,量應(yīng)不大于最小,分度值,塑料活塞,滴定管,當(dāng)水注最高標(biāo)線,時(shí)，活塞在關(guān)閉,狀況下停留,50min,后，滲漏,量應(yīng)不大于最小,分度值,具塞量筒,量瓶,當(dāng)水注最高標(biāo)線,時(shí)，塞子緊蓋后,顛倒,10,次。每,次在倒置狀態(tài)下,至少停留,10s,不應(yīng)有水滲出

7、,2.1.3.3,密合性,2.1.3.4,流出時(shí)間,滴定管檢驗(yàn),1,3,2,將滴定管垂直加載檢定架上,活塞芯圖,上一層薄而均勻的,油脂，不應(yīng)有水滲出,充水于最高標(biāo)線，流液,口不應(yīng)接觸水器壁,活塞完全開啟時(shí)計(jì)時(shí),直到液面降到最低標(biāo),線為止，記錄時(shí)間,2.1.3.4,流出時(shí)間,滴定管合格標(biāo)準(zhǔn),標(biāo)稱容量,ml,1,2,5,10,25,50,100,分度值,ml,0.01,0.02,0.05,0.1,0.1,0.2,流出時(shí)間,s,A,2030,3045,4570,6090,70100,B,1535,2045,3570,5090,60100,等待時(shí)間,s,30,分度線寬度,mm,0.3,2.1.3.4,

8、流出時(shí)間,吸量管檢驗(yàn),1,3,2,注水至最高標(biāo)線以上,5cm,然后將液面調(diào)至最高標(biāo)線處,在保持不動的情況下,流出并計(jì)時(shí)，直至口,端不流為止,將吸量管垂直放置，并將流,液口輕靠水器壁（傾斜,30,2.1.3.4,流出時(shí)間,吸量管合格標(biāo)準(zhǔn),標(biāo)稱容量,ml,1,2,3,5,10,15,20,25,50,100,流出時(shí),間,s,A,712,1525,2030,2535,3040,3545,B,512,1025,1530,2035,2540,3045,標(biāo)稱容量,ml,0.1,0.2,0.25,0.5,1,2,5,10,25,50,流,出,時(shí),間,s,流,出,式,A,B,37,48,410,412,614

9、,717,1121,1525,吹,出,式,A,B,25,36,510,單標(biāo)線吸量管,分度吸量管,2.1.3.5,容量示值,檢定點(diǎn),類型,容量示值,ml,檢定點(diǎn),滴,定,管,1ml10ml,半容量,總?cè)萘?25ml,0ml5ml,0ml10ml,0ml15ml,0ml20ml,025ml,50ml,0ml10ml,0ml20ml,0ml30ml,0ml40ml,0ml50ml,100ml,0ml20ml,0ml40ml,0ml60ml,0ml80ml,0ml100,ml,分,度,吸,量,管,0.5ml,半容量,總?cè)萘?0.5ml,1/10 ,2/10,半容量,總?cè)萘?量杯、量筒,1/10 ,2/

10、10,半容量,總?cè)萘?量筒和量杯采用容量比較法，其余可采用衡量法或容量比較法,2.1.3.5,容量示值,衡量法前準(zhǔn)備,容器檢定前須對量器進(jìn)行清洗，清洗的方法,為：用重鉻酸鉀飽和溶液和濃硫酸的混合液,1:1,或,20,發(fā)煙硫酸進(jìn)行清洗。然后用,水沖凈，器壁上不應(yīng)有掛水等沾污現(xiàn)象，使,液面與器壁接觸處形成正常彎月面。清洗干,凈的被檢量器須在檢定前,4h,放入實(shí)驗(yàn)室內(nèi),室溫,水溫,介質(zhì),2.1.3.5,容量示值,衡量法檢定環(huán)境,室溫,20,5,，且室,溫變化不得大于1/h,水溫與室溫之差不得,大于2,檢定介質(zhì)為純水（蒸餾,水或去離子水,檢定環(huán)境,01,02,03,04,取一只容量大于被檢玻璃量器的,

11、潔凈有蓋稱量杯，稱得空杯質(zhì)量,調(diào)整被檢玻璃量器液面，記,錄水溫,t,讀數(shù)應(yīng)準(zhǔn)確到,0.1,將被檢玻璃量器內(nèi)的純水放入,稱量杯，稱得純水質(zhì)量,m,按照公式計(jì)算該玻璃量器,在標(biāo)準(zhǔn),20,時(shí)的實(shí)際容量,2.1.3.5,容量示值,衡量法檢測方法,V,20,m*K(t,2.1.3.5,容量示值,合格標(biāo)準(zhǔn),標(biāo)稱容量,ml,1,2,5,10,25,50,100,容量允,差,ml,A,0.010,0.010,0.025,0.04,0.05,0.10,B,0.020,0.020,0.050,0.08,0.10,0.20,標(biāo)稱容量,ml,1,2,3,5,10,15,20,25,50,100,流出,時(shí)間,s,A,0

12、.007,0.010,0.015,0.020,0.025,0.030,0.05,0.08,B,0.015,0.020,0.030,0.040,0.050,0.060,0.10,0.16,滴,定,管,單,標(biāo),線,吸,量,管,標(biāo)稱容量,ml,1,2,5,10,25,50,容量允差,ml,流出式,A,0.008,0.012,0.025,0.05,0.10,0.10,B,0.015,0.025,0.050,0.10,0.20,0.20,分,度,吸,量,管,堿性滴定管,玻璃器具,01,02,2.1.4,檢定周期,檢定周期為一年,檢定周期為三年,PART 2.2,專用玻璃量器,Specical glassware,JJG 10-2005,專用玻璃量器檢定規(guī)程,2.2.1,專用玻璃量器檢定項(xiàng)目,檢定項(xiàng)目,首次檢定,后續(xù)檢定,使用中檢驗(yàn),玻璃化學(xué)穩(wěn)定性,外觀及分度線,應(yīng)力,密合性,流出時(shí)間,容量,耐急熱、急冷,注：“+”表示應(yīng)檢項(xiàng)目,表示可不檢項(xiàng)目,刻度試管和比色管采用容量比較法,專用玻璃量