OIW Training Manual水中油測(cè)油儀說明書

1、OIW TEST TRAINING MANUAL水中油測(cè)定培訓(xùn)手冊(cè)MADE BY CHINA CORELAB INC.February 2004PART I 相關(guān)原理、法規(guī)、標(biāo)準(zhǔn)21.1 紅外光度計(jì)測(cè)水中油工作原理21.2 法規(guī)2PART II ABOUT SOLVENT關(guān)于溶劑42.1 適合水中油分析的溶劑基本要求42.2 MSDS Comparison (MSDS比較)42.3 Detailed MSDS of C2Cl452.4 Quality Requirements of C2Cl4 for OIW Analysis72.5 Pros and Cons of C2Cl4 Extrac

2、tion v.s. n-Hexane Extraction四氯乙烯萃取法相對(duì)正己烷萃取的優(yōu)缺點(diǎn)7PART III CVH TPH ANALYZER CALIBRATION儀器校正73.1 Standard preparation73.2 Set PRESENTATIOIN MODE 設(shè)置顯示模式83.3 Zero TPH Analyzer 儀器調(diào)零83. 4 Calibrate TPH Analyzer儀器校正93. 5 Quality Control of Calibration校正檢查和備檔9PART IV WATER ANALYSIS 水樣分析125.1 Analyzer Conditi

3、oning 儀器準(zhǔn)備135.2 Take the Sample 樣品準(zhǔn)備145.3 Zero the Analyzer 儀器調(diào)零145.4 Transfer the Solvent Phase to the Cuvette 萃取液轉(zhuǎn)移145.5 Read the Result讀數(shù)15PART I 相關(guān)原理、法規(guī)、標(biāo)準(zhǔn)1.1 紅外光度計(jì)測(cè)水中油工作原理碳?xì)浠衔镏械腃-H鍵在一定的波長(zhǎng)下有較強(qiáng)的吸收。主要是：芳環(huán)及環(huán)烴上的C-H在3030 cm-1特征吸收，甲烷基的CH2-H鍵在2960 cm-1有特征吸收，以及亞甲基CH-H在2930 cm-1波長(zhǎng)的特征吸收。光源檢測(cè)器樣品池2930cm-1波

4、長(zhǎng)過濾器用溶劑萃取水樣中的有機(jī)碳化合物組分，它們?cè)?.4m紅外波段有強(qiáng)烈的吸收，利用其吸收強(qiáng)度與已知濃度的參照油相比較的方法來確定水中含油量。1.2 法規(guī)1.2.1南海區(qū)海洋油(氣)田含油污水監(jiān)測(cè)暫行規(guī)定(一九九七年九月一日)為更好地貫徹執(zhí)行中華人民共和國海洋石油勘探開發(fā)環(huán)境保護(hù)管理?xiàng)l例，建立海洋油（氣）田含油污水排放監(jiān)測(cè)制度，保護(hù)海洋環(huán)境，特制定本暫行規(guī)定。本暫行規(guī)定適用于在南海區(qū)從事海洋油（氣）田開發(fā)的作業(yè)者。國家海洋局南海分局（以下簡(jiǎn)稱主管部門）負(fù)責(zé)本規(guī)定的實(shí)施和管理。海上油（氣）田必須采用紅外法（見南海區(qū)海洋油（氣）田含油污水測(cè)定方法）測(cè)定污水含油量。在本暫行規(guī)定公布之前投產(chǎn)的油（氣）

5、田，其污水含油量分析方法達(dá)不到本規(guī)定要求的，作業(yè)者應(yīng)在六個(gè)月內(nèi)使該分析方法達(dá)到要求。作業(yè)者必須在油（氣）田含油污水排放口建立監(jiān)測(cè)制度，每天監(jiān)測(cè)四次，每隔6小時(shí)監(jiān)測(cè)一次，當(dāng)測(cè)定結(jié)果超過75ppm時(shí)，應(yīng)增加監(jiān)測(cè)次數(shù)；當(dāng)連續(xù)超標(biāo)排放24小時(shí)時(shí)，應(yīng)報(bào)告主管部門，經(jīng)同意后方可繼續(xù)排放。作業(yè)者應(yīng)使用主管部門提供的“海洋油氣田含油污水分析結(jié)果登記表”（見附件一），并按季度上交主管部門。作業(yè)者應(yīng)在每雙月5日前，以油（氣）田含油污水排放口為單位送水樣（250毫升）到主管部門認(rèn)定的實(shí)驗(yàn)室測(cè)定，其分析結(jié)果應(yīng)按季度上報(bào)主管部門，若分析結(jié)果超過國家規(guī)定排放標(biāo)準(zhǔn)的，作業(yè)者應(yīng)在當(dāng)月內(nèi)報(bào)告主管部門。檢驗(yàn)單位采用的測(cè)定方法應(yīng)符

6、合海洋石油開發(fā)工業(yè)含油污水分析方法（征求意見稿）的規(guī)定，并應(yīng)在接到樣品五天內(nèi)提交提交檢驗(yàn)報(bào)告。為進(jìn)行實(shí)驗(yàn)室之間的相互校對(duì)工作，作業(yè)者必須在每年12月份以油（氣）田采出水排放口為單位提供兩水樣（每份水樣250毫升），其中一份送到主管部門當(dāng)年所指定的實(shí)驗(yàn)室測(cè)定含油量。作業(yè)者送往陸地實(shí)驗(yàn)室的采出水樣，必須在采樣時(shí)加入1:1鹽酸2mL固定保存。凡違反本暫行規(guī)定的，主管部門將根據(jù)中華人民共和國海洋石油勘探開發(fā)環(huán)境保護(hù)管理?xiàng)l例及條例實(shí)施辦法的有關(guān)規(guī)定給予警告或罰款。本暫行規(guī)定自發(fā)布之日起執(zhí)行。國家海洋局南海分局南海區(qū)海洋油（氣）田含油污水測(cè)定方法方法概述：用溶劑萃取水樣中的有機(jī)碳化合物組分，它們?cè)?.4m

7、紅外波段有強(qiáng)烈的吸收，利用其吸收強(qiáng)度與已知濃度的參照油相比較的方法來確定水中油含量。取樣與保存：在污水排放口采集的的水樣（不得少于200mL）現(xiàn)場(chǎng)應(yīng)立即測(cè)定。如果不是當(dāng)天測(cè)定，需加入1:1鹽酸2mL固定保存。儀器：紅外油份（碳?xì)浠衔铮袡C(jī)碳化合物）濃度分析儀，或紅外光光度計(jì)，測(cè)定波長(zhǎng)必須在3.4m（即2930cm-1），量程不得低于0200ppm范圍。試劑：四氯化碳（CCl4）分析純氟里昂（1,1,2-三氟，1,2,2-三氯乙烷）分析純參照標(biāo)準(zhǔn)：大部分紅外油份濃度計(jì)都隨機(jī)配備標(biāo)準(zhǔn)參照油，如果沒有，由南海監(jiān)測(cè)中心實(shí)驗(yàn)室負(fù)責(zé)提供。萃?。簩⒉杉牡臉悠窊u勻，用刻度吸管吸取一定量體積于分液漏斗，以1

8、:1的體積比加入萃取劑，充分混合1分鐘，取下層萃取液測(cè)定。如果儀器操作說明書另有要求而更改體積比的，應(yīng)在含油污水分析結(jié)果登記表的備注中加以說明。測(cè)定結(jié)果：紅外油份濃度計(jì)上所顯示的結(jié)果即是水中油含量，以ppm或mg/L表示均可。注意：標(biāo)準(zhǔn)參照濃度，每隔兩月應(yīng)油專門負(fù)責(zé)人重新配制。每次測(cè)定前，都應(yīng)校準(zhǔn)量程，使儀器保持良好的工作狀態(tài)。1.2.2分析標(biāo)準(zhǔn)比較IP426/98 ，GB/T 16488-1996，GB/T 17923-1999這兩個(gè)標(biāo)準(zhǔn)是最復(fù)雜也是比較科學(xué)完全的水中油的分析方法。它先用硅鎂吸附劑對(duì)萃取液進(jìn)行處理，然后用紅外光譜儀對(duì)萃取液在2600CM-13300CM-1進(jìn)行掃描，得到光譜圖

9、。然后分別讀取出3030cm-1、2960 cm-1及2930 cm-1下的吸光度，經(jīng)過一系列計(jì)算過程，從而得到芳烴、環(huán)烷烴，脂肪烴含量（把它們加起來就是石油烴含量）和動(dòng)植物油的含量。其中IP426/98要求使用的溶劑是四氯乙烯，GB/T 16488-1996要求使用的溶劑是四氯化碳。GB/T 16488-1996中也提出了簡(jiǎn)化的只在2930 cm-1波長(zhǎng)下的測(cè)定方法。實(shí)際上這一部分就是GB/T 17923-1999海洋石油開發(fā)工業(yè)含油污水分析方法。幾種標(biāo)準(zhǔn)的比較IP426/98GB/T 16488-1996GB/T 17923-1999海洋局南海標(biāo)準(zhǔn)溶劑四氯乙烯四氯化碳四氯化碳四氯化碳或氟里

10、昂標(biāo)準(zhǔn)物質(zhì)甲苯，十六烷、姥鮫烷甲苯，十六烷、姥鮫烷或現(xiàn)場(chǎng)原油或正十六烷、異辛烷和苯按65：25：10混和物經(jīng)處理過的現(xiàn)場(chǎng)原油儀器廠家或南海監(jiān)測(cè)中心實(shí)驗(yàn)室提供？測(cè)定波長(zhǎng)2600-3300 cm-12400-3400 cm-1或2930cm-12930 cm-12930 cm-1硅鎂吸附必須必須必須勿須1.3 NEW METHOD APPLIED BY PHILLIPS PHILLIPS選取的新測(cè)定方法儀器： CVH TPH ANALYZER溶劑： C2Cl4固定水樣溶劑比：100mL水+40mL溶劑，即2.5倍濃縮PART II ABOUT SOLVENT關(guān)于溶劑2.1 適合水中油分析的溶劑基本

11、要求可采用的溶劑必須達(dá)到的要求：1. 在2930 cm-1下無吸收2. 與油混溶3. 不溶于水、不與水乳化4. 跟水有較大的比重差，易與水分離符合以上要求的的溶劑主要有CCl4, C2Cl4和Freon113. 正己烷是Phillips水中油儀器特定的分析方法采用的溶劑.2.2 MSDS COMPARISON (MSDS比較)四氯化碳（CCl4）四氯乙烯(C2Cl4)Freon113n-Hexane(C6H14)物理性質(zhì)Appearance and odor外觀和氣味無色易揮發(fā)不易燃液體，具氯仿微甜氣味無色易揮發(fā)不易燃液體，具微甜氣味無色透明易揮發(fā)液體，微具乙醚氣味無色透明液體,具烴類氣味比重

12、 (water=1)1.581.621.570.663沸點(diǎn) (°C)76.81214869分子量153.84168.52187.3786.2凝點(diǎn) (°C)-23-19N/AN/A蒸汽壓(psia20°C)1.770.256.460.1蒸汽比重(air=1)45.82.93.0溶解性不溶于水溶于油類及有機(jī)溶劑不溶于水溶于油類及有機(jī)溶劑不溶于水溶于油類及有機(jī)溶劑不溶于水溶于油類及有機(jī)溶劑火災(zāi)可燃性不可燃不可燃不可燃可燃閃點(diǎn)(°C)N/AN/AN/A-22LELN/AN/AN/A1.7%UELN/AN/AN/A7.7%自燃點(diǎn)(°C)N/AN/AN/A

13、223化學(xué)性質(zhì)熱分解產(chǎn)物CO2,HCl COCl2(光氣) Cl2CO2,HCl COCl2(光氣) Cl2HCl,HF,鹵代羰基化合物CO化學(xué)穩(wěn)定性穩(wěn)定穩(wěn)定避免與NaOH接觸穩(wěn)定穩(wěn)定毒性總評(píng)價(jià)有毒有毒無毒有毒目標(biāo)器官肝，腎損害肝無神經(jīng)系統(tǒng)致癌性致癌物可能致癌無無環(huán)保性N/AN/A破壞臭氧層被禁止使用N/A工作場(chǎng)所最高允許濃度 (ppm)525無50個(gè)人防護(hù)日常使用PPE橡膠手套、護(hù)目鏡、工作服通風(fēng)要求必須在通風(fēng)柜內(nèi)使用廢液處理殘液以密封鋼桶收集送岸上相關(guān)機(jī)構(gòu)處理，不得排入下水道綜合CCl4、C2Cl4及Freon113, C2Cl4會(huì)作為水中油分析不得不采用的溶劑。2.3 MSDS of C

14、2Cl4四氯乙烯; 全氯乙烯; Tetrachloroethylene; Perchloroethylene; CAS: 127-18-4理化性質(zhì)無色液體,氣味似乙醚。化學(xué)式C2Cl4。分子量165.83。相對(duì)密度1.6311(15/4)。熔點(diǎn)-22.4。沸點(diǎn)121。蒸氣密度5.83。蒸氣壓2.11kPa(15.8mmHg22)。溶于約10000份體積水; 與乙醇、乙醚、氯仿、苯混溶。遇水可緩慢分解成三氯乙酸和鹽酸。有水存在對(duì)鐵、鋁、鋅有腐蝕(但可加穩(wěn)定劑加以抑制)。非可燃性液體。高溫引起分解,分解條件不同分解產(chǎn)物不一樣,主要為鹽酸、光氣、一氧化碳。如有活性炭存在,加熱至700分解生成六氯化苯

15、和六氯乙烷。被強(qiáng)氧化劑氧化。與鋇粉、鈹粉、鋰屑、四氧化二氮、氫氧化鈉發(fā)生劇烈化學(xué)反應(yīng)。接觸機(jī)會(huì)工業(yè)上主要用作溶劑、有機(jī)合成、金屬去污劑和干洗劑、脫硫劑、熱傳遞介質(zhì)。醫(yī)療上用作驅(qū)蟲藥。一般居民通過大氣、食品及飲水可能接觸低水平的四氯乙烯。侵入途徑本品可經(jīng)呼吸道、消化道和皮膚吸收。毒理學(xué)簡(jiǎn)介人吸入TCL0: 96 ppm/7H。人（兒童）經(jīng)口TDL0: 545 mg/kg。人（男性）吸入TCL0: 600 ppm/10M。大鼠經(jīng)口LD50: 2629 mg/kg; 吸入LC50: 34200 mg/m3/8H。小鼠經(jīng)口LD50: 8100 mg/kg; 吸入LC50: 5200 ppm/4H。兔經(jīng)

16、皮LD  :3228mg/kg四氯乙烯進(jìn)入人體后,在體內(nèi)蓄積有限,約有98經(jīng)肺排出,僅有2發(fā)生變化。主要轉(zhuǎn)化為三氯乙酸和三氯乙醇,隨尿排出。本品排出體外十分緩慢,吸入濃度為2.7mg/L的蒸氣3.5小時(shí)后,經(jīng)過兩星期尚可測(cè)出,肺中平均滯留本品62; 濃度為1.3mg/L時(shí),3小時(shí)后可達(dá)到平衡。本品毒性較三氯乙烯為低,麻醉作用較弱,主要抑制中樞神經(jīng)系統(tǒng),肝、腎毒害較輕。對(duì)眼、鼻、喉、咽有刺激。動(dòng)物實(shí)驗(yàn)證實(shí)四氯乙烯對(duì)動(dòng)物有致癌性,但針對(duì)洗衣及干洗工人所作的流行病學(xué)研究卻發(fā)現(xiàn)四氯乙烯對(duì)人類致癌性的有無仍不確定。臨床表現(xiàn)急性吸入主要表現(xiàn)為眼、鼻、喉、咽刺激癥狀,有眼灼痛、流涎、流涕、口干、口

17、內(nèi)金屬甜味、頭痛和頭部壓迫感、眩暈、運(yùn)動(dòng)失調(diào)、甚至意識(shí)不清。一般于脫離接觸后可恢復(fù),并無后遺癥。臨床報(bào)道對(duì)肝有損害。急性口服中毒者,有頭昏、頭痛、倦睡、惡心、嘔吐、腹痛、視物模糊、四肢麻木,可出現(xiàn)興奮不安、抽搐乃至昏迷。也曾有因過量口服本品引起中毒死亡的報(bào)告。反復(fù)接觸可引起皮炎。處理接觸者,應(yīng)立即離開現(xiàn)場(chǎng)。有刺激癥狀者需安靜休息,進(jìn)行必要的檢查及處理,并觀察24小時(shí)。急性中毒者應(yīng)臥床休息,急救措施和對(duì)癥治療原則與內(nèi)科相同。有昏迷、心跳及呼吸停止者,迅速進(jìn)行腦、心、肺復(fù)蘇; 對(duì)癥處理。重度中毒患者可適當(dāng)使用糖皮質(zhì)激素。注意保護(hù)肝、腎功能。忌用腎上腺素。標(biāo)準(zhǔn)車間空氣衛(wèi)生標(biāo)準(zhǔn)：中國MAC 200 m

18、g/m3 (1996)美國ACGIH TLV-STEL 685 mg/m3 (100 ppm)美國ACGIH TLV-TWA 170 mg/m3 (25 ppm)美國MSHA STANDARD-air: TWA 100 ppm (670 mg/m3)美國OSHA PEL(所有行業(yè)): 8H TWA 100 ppm; CL 200; Pk 300/5M/3H埃及: TWA 5 ppm (35 mg/m3), 皮膚澳大利亞: TWA 50 ppm (335 mg/m3), STEL 150 ppm, 致癌物比利時(shí): TWA 50 ppm (339 mg/m3), STEL 200 ppm (136

19、8 mg/m3)丹麥: TWA 30 ppm (200 mg/m3), 皮膚芬蘭: TWA 50 ppm (335 mg/m3), STEL 75 ppm (520 mg/m3), 皮膚法國: TWA 50 ppm (335 mg/m3)德國: TWA 50 ppm (345 mg/m3), 致癌物匈牙利: STEL 50 mg/m3, 皮膚，致癌物日本: TWA 50 ppm (340 mg/m3)荷蘭: TWA 35 ppm (240 mg/m3), 皮膚菲律賓: TWA 100 ppm (670 mg/m3)波蘭: TWA 60 mg/m3俄羅斯: TWA 50 ppm, STEL 10

20、 mg/m3瑞典: TWA 10 ppm (70 mg/m3), STEL 25 ppm (170 mg/m3)瑞士: TWA 50 ppm (345 mg/m3), STEL 100 ppm, 皮膚泰國: TWA 100 ppm, STEL 200 ppm英國: TWA 50 ppm (335 mg/m3), STEL 150 ppm保加利亞,哥倫比亞,約旦,韓國 參照美國 ACGIH TLV; 新西蘭,新加坡,越南 參照美國 ACGIH TLV2.4 QUALITY REQUIREMENT OF C2Cl4 FOR OIW ANALYSISl Hydrocarbon conten

21、t should be less than 20ppm碳?xì)浠衔镫s質(zhì)含量應(yīng)少于20ppm.l Background absorption should not change after being washed with water背景吸收值在水洗之后應(yīng)該沒有變化, 即溶劑不含水溶性有機(jī)雜質(zhì).2.5 PROS AND CONS OF C2Cl4 EXTRACTION V.S. n-HEXANE EXTRACTION四氯乙烯萃取法相對(duì)正己烷萃取的優(yōu)缺點(diǎn)Pros優(yōu)點(diǎn)l Good accuracy and repeatability好的準(zhǔn)確性和重復(fù)性l C2Cl4 is incombustible四

22、氯乙烯為不可燃物l Method is recognized by environmental regulation and standard test methods 測(cè)量方法來自環(huán)保法規(guī)和國家國際標(biāo)準(zhǔn)Cons缺點(diǎn)l More consumption of solvent溶劑用量較大l The extractant is more easily contaminated by water and suspended solids 萃取液更容被水和懸浮固體沾污l More personnel training is needed操作人員需較嚴(yán)格培訓(xùn)PART III CVH TPH ANALYZ

23、ER CALIBRATION儀器校正3.1 Standard preparation1. Use the processed oil in the oil field as standard oil. Put the oil container in a 50ºC water bath for 1 hour. Shake the oil container to mix the content before being weighed .用油田現(xiàn)場(chǎng)生產(chǎn)的原油作為標(biāo)準(zhǔn)油. 在使用之前將盛油容器放入50ºC水浴一小時(shí),并搖晃容器以使油樣混合均勻.2. Prepare 8 oil

24、-free 100mL volumetric flask. Label them with 10ppm, 20ppm, 40ppm, 60ppm, 80ppm, 100ppm, 200ppm, 300ppm, 400ppm. 準(zhǔn)備8只洗凈并烘干的100mL容量瓶，分別貼上10ppm, 20ppm, 40ppm, 60ppm, 80ppm, 100ppm, 200ppm, 300ppm, 400ppm標(biāo)簽。 Accurately weigh 0.0025, 0.0050, 0.0100, 0.0200, 0.0250, 0.0500, 0.0750 and 0.1000 gram of stan

25、dard oil to the labeled volumetric flask. Fill the flasks with C2Cl4 to the volume marks. Stopper the flasks and and shake them for 5 minutes. 準(zhǔn)確稱取0.0025, 0.0050, 0.0100, 0.0200, 0.0250, 0.0500, 0.0750, 0.1000g標(biāo)準(zhǔn)油至貼好標(biāo)簽的容量瓶里。注入C2Cl4至刻度線。蓋上瓶蓋。搖晃5分鐘，得到標(biāo)稱濃度為10ppm, 20ppm, 40ppm, 80ppm, 100ppm, 200ppm, 30

26、0ppm, 400ppm的標(biāo)準(zhǔn)溶液。Standard series to be appliedNo.Nominal ConcentrationReal Concentration110ppm25ppm220ppm50ppm340ppm100ppm480ppm200ppm5100ppm250ppm6200ppm500ppm7300ppm750ppm8400ppm1000ppm3.2 Set PRESENTATIOIN MODE1Make sure the Analyzer has been turned on for at least 1 hour before the following st

27、eps. 在進(jìn)行以下校正工作之前確保儀器已經(jīng)預(yù)熱一小時(shí)以上. 設(shè)置顯示模式Press and hold both the CAL and ZERO buttons for two seconds to check and switch the display modes. Set the presentation mode in AbS Mode同進(jìn)按下并按住CAL和ZERO鍵兩秒以上, 就可以在不同的顯示模式之間進(jìn)行切換. 觀察顯示窗口, 切換顯示模式到AbS.3.3 Zero TPH Analyzer 儀器調(diào)零1. Check whether the cuvette is clean an

28、d dry. To be soaked in the concentrated HCl will remove the scale, and to be soaked or rinsed in C2Cl4 will remove brown heavy oil deposition. The water droplets shoud be removed with absorption cotton held by a tweezers. A clean cuvette should be colorless, and look transparent and clear in the dir

29、ection of optical sides.以濃鹽酸浸泡除去黃色沉積物。四氯乙烯浸泡可除去瀝青質(zhì)深沉。水珠可用棉球吸除。洗凈的樣品池應(yīng)無色，光學(xué)表面方向應(yīng)清亮透明。檢查樣品池是否清潔干燥。2. Fill cuvette with C2Cl4 in the reservoir, and place it in the holder in the right way. Mark one of the frosted sides. Place the cuvette into the sample holder all the way down to the stop always with t

30、he marked frosted side facing front. 在樣品池的一個(gè)毛面上做好標(biāo)記。將它放入讀數(shù)槽時(shí)總是讓這面朝向面板方向，并按壓樣口池至槽底壓不動(dòng)為止。將比色池充滿干凈C2Cl4, 把它按正確方法放入樣品槽內(nèi).3. Press and hold ZERO button until bAL= appears.按下并按住ZERO鍵直到bAL=顯示出來,稍候片刻直到儀器正確調(diào)零. 3. 4 Calibrate TPH Analyzer儀器校正1. Press and hold CAL button until CAL appears on the display. Press

31、the RECALL button to switch the calibration mode to uSEr.壓下并按住CAL鍵直到CAL顯示出來. 按RECALL鍵, 將校正模式切換到uSEr.2. Momentarily press and release the CAL button. The display will read SA01.按CAL鍵, 顯示器將顯示SA01.3. Rinse the cuvette with C2Cl4 for 3 times, then rinse and fill it with the lowest standard. Insert the c

32、uvette into the sample holder in the right way described in Zero TPH Analyzer Section. Press the RUN button and wait until a number appears. Increase or decrease the number by pressing UP(RUN) or DOWN(RECALL) button to the referenced standard OIW level.將樣品池以C2Cl4涮洗3次. 將它裝滿10ppm標(biāo)樣. 將樣品池插入樣品槽. 按RUN鍵并等

33、候直到一個(gè)數(shù)字顯示出來. 按UP(RUN)或DOWN(RECALL)鍵, 將這一數(shù)字更改到與標(biāo)樣濃度相同.4. Dump the cuvette, and repeat step 2 and 3, to advance from the second lowest standard(SA02) to the highest standard(SA08) in the increasing concentration order. After the 8th standard has been run, press CAL button to show SA09, and press ZERO

34、button to end the calibration. 倒空樣品池. 重復(fù)步驟2和3, 從第二低標(biāo)樣按從低到高的順序直到最高標(biāo)樣. 當(dāng)最高標(biāo)樣設(shè)定好之后, 按CAL鍵, 并按ZERO鍵結(jié)束校正過程.3. 5 Quality Control of Calibration校正檢查和備檔As the quality control procedure, the calibration can be reviewed.An MS EXCEL spreadsheet can be used to log and plot the absorption to concentration of the

35、 calibration. This sheet would documented.作為質(zhì)量控制的要求, 校正應(yīng)該檢查和備檔. 可以用一個(gè)EXCEL工作表用來以表格加圖形的方式記錄儀器在不同濃度下的吸收值。 這個(gè)工作表可以打印并保存起來。3.5.1 Retrieve Calibration Table from OIW Analyzer調(diào)出校正表操作1. Press and hold CAL button until CAL appears on the display. Press the RECALL button to switch the calibration mode to Edi

36、t.按下并按住CAL鍵直到CAL顯示. 按RECALL鍵將校正模式切換到Edit.2. Press CAL button. The display will read n=, then 06. Press CAL button again, A01= will be displayed followed by the current absorption value, press CAL again the display will show C01= followed by the desired concentration. 按CAL鍵, 顯示器將顯示n=, 接著是標(biāo)準(zhǔn)的數(shù)量. 再次按CA

37、L, A01=將顯示, 接著顯示的是吸光度值. 按CAL, 顯示器將顯示C01=, 接著是標(biāo)樣的濃度值.3. Press CAL again, the display will show the rest of standards absorption values(response values) and desired concentrations. Log these data and put them into the a prepared worksheet.重復(fù)按CAL鍵, 顯示器會(huì)依次顯示吸光度及標(biāo)樣的濃度. 記錄下各濃度下相應(yīng)的吸光度值, 填入工作表中。The followin

38、g is a typical calibration table retrieve from the OIW analyzer.下圖是一典型的從OIW分析儀里調(diào)出來的校正表。3.5.2 Check the Linearity of Range from 080ppm檢查080ppm范圍的校正線性度Because the 080ppm range is most commonly used, and at the same time, the OIW analyzer works linearly in this range（which is confirmed by manufacturer

39、and also by standards checking in CoreLab）, the linearity can be checked to evaluate the reliability of calibration. The R2(square of related coefficient) is automatically calculated by Excel. The higher the R2 is, the better the linearity is. The acceptable limit is more than 0.999. 因?yàn)?80ppm區(qū)間是最常用也

40、最重要的范圍，而且儀器在這區(qū)間濃度與吸收值呈線性關(guān)系（經(jīng)實(shí)測(cè)并經(jīng)生產(chǎn)廠家技術(shù)人員證實(shí)）?？梢酝ㄟ^檢查這區(qū)間里標(biāo)樣濃度與儀器吸收的線性度來檢驗(yàn)校正的可靠性。The following plot is a calibration with acceptable linearity.下圖是一張線性度可以接受的校正圖。The following plot is a calibration with unacceptable linearity. Obviously, the 30ppm standard is dispersed.下圖是一張線性度不可接受的校正圖。顯然，30ppm標(biāo)樣離群了。Dispe

41、rsed Point If there is only one dispersed point, discard the standard. Modify the abs of that point until it is right on the line. Follow Step 3.5.1 to edit the calibration table with the modified abs. 如果只有一個(gè)離群點(diǎn)存在，放棄此校正點(diǎn)的標(biāo)樣。在電腦上調(diào)整該點(diǎn)的Abs值直到那個(gè)點(diǎn)正好落在直線上。按3.5.1描述的步驟將該點(diǎn)的Abs更改為修正值。If the number of disperse

42、d point is more than two, the calibration fails. With the same calibration standards, calibrate the analyzer again. If the problem cant be solved, new series of standards has to be made and the OIW analyzer needs to be calibrated with it.如果離群點(diǎn)達(dá)兩個(gè)以上，用該標(biāo)樣重新校正并檢查一次。如果問題繼續(xù)存在，重新配制標(biāo)樣并校正儀器。 3.5.3 Back-chec

43、k and documentation 標(biāo)樣讀數(shù)和校正備檔Fill the cuvette with standard and read the OIW. In the range from 10ppm to 80ppm, if any of the differences between the standards and readings is more than 1; or in the range from 80ppm to 400ppm, any of the differences between the standards and the readings is more tha

44、n 3, the calibration fails and has to be executed again.以標(biāo)樣注滿樣品池并讀數(shù). 在80ppm以下的量程里，如果任一標(biāo)樣的讀數(shù)與其濃度差別超過2ppm；或者在80ppm以上的量程里，任一標(biāo)樣的讀數(shù)與其濃度差別超過4ppm, 說明校正失敗, 并且要從頭開始重新校正.PART IV WATER ANALYSIS 水樣分析QUICK REFERENCE OF OIW ANALYSIS Tips:a) Test and Calibration must be resumed in the vent hood, and the operation

45、personal must wear chemical resistance gloves. b) Hold the frosted sides and never touch optical surfaces when handling the cuvette.c) Mark one of the frosted sides, always let the marked side face front when calibrating and running samples on the analyzer.d) Make sure the cuvette is pushed down all

46、 the way to the stop.e) All the glassware must be cleaned and rinsed with clean C2Cl4 before use.f) The solution to be read on the analyzer must be free of water.Take 100mL water sampleMeasure 40mL C2Cl4C2Cl4 Reservoir and DispenserPipelineStopper sample cyliner. Cool sample to room temperature in w

47、ater bathTransfer water sample to the separatory funnelAdd about half of C2Cl4 into sample cylinderTurn on Anlayzer for 1 hour before testing water sample I D L EFill a cuvette with C2Cl4. Stopper the Cuvette and Insert it into sample holderPress ZERO Button and wait Z E R OAny Water Drop?YesAdd abo

48、ut 1 gram of Na2SO4 NoStopper the test tube. Carefully shake the test tube, then wait for the salt to depositPress the RUN button and waitTake the reading as OIW R U NWith the extractant, rinse the cuvette fill it.Stopper the cuvetteStopper the separatory funnel and shake it vigorously for 2 minutes

49、Stand for 10 minutesVisual InspectionNoSuspended Solids?YesVisually Inpsect the solvent layerFilter about 3/5 of the solvent phase to a test tubeDrain about 3/5 of the solvent phase to a test tubeStopper sample cyliner Shake it vigorously.Transfer extrctant to the separatory funnelAdd all the rest o

50、f C2Cl4 to the sample bottle.5.1 Analyzer Conditioning 儀器準(zhǔn)備Turn on the Analyzer 1 hour before water analysis. 在分析工作前一小時(shí)打開分析儀。5.2 Take the Sample 樣品準(zhǔn)備5.2.1 Open the sample tap to let the water run for 30 seconds. Carefully fill the graduated cylinder with water sample to 100mL mark.先開啟取樣點(diǎn)閥門沖洗取樣口30秒，小

51、心地用100mL量筒接取水樣至100mL刻度處。5.2.2 Cool the water sample to room temperature in tap water bath.以涼水浴將水樣冷至室溫。5.2.3 Pour the water sample to a clean separatory funnel.將全部水樣倒入洗凈的分液漏斗中。5.2.4Take 40mL clean C2Cl4. Inject about half of the solvent into the sample bottle. Cap the bottle, shake it vigorously to dissolve oil on the wall. Transfer C2Cl4 to the separatory funnel. Inject the rest of measured C2Cl4 into the sample bottle. Cap the sample bottle, shake it. Then transfer the C2Cl4