OIWTrainingManual水中油测油仪说明书

1、OIW TEST TRAINING MANUAL水中油测定培训手册MADE BY CHINA CORELAB INC.February 2004PART I 相关原理、法规、标准21.1 红外光度计测水中油工作原理21.2 法规2PART II ABOUT SOLVENT关于溶剂42.1 适合水中油分析的溶剂基本要求42.2 MSDS Comparison (MSDS比较)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四氯乙烯萃取法相对正己烷萃取的优缺点7PART III CVH TPH ANALYZER CALIBRATION仪器校正73.1 Standard preparation73.2 Set PRESENTATIOIN MODE 设置显示模式83.3 Zero TPH Analyzer 仪器调零83. 4 Calibrate TPH Analyzer仪器校正93. 5 Quality Control of Calibration校正检查和备档9PART IV WATER ANALYSIS 水样分析125.1 Analyzer Conditi

3、oning 仪器准备135.2 Take the Sample 样品准备145.3 Zero the Analyzer 仪器调零145.4 Transfer the Solvent Phase to the Cuvette 萃取液转移145.5 Read the Result读数15PART I 相关原理、法规、标准1.1 红外光度计测水中油工作原理碳氢化合物中的C-H键在一定的波长下有较强的吸收。主要是：芳环及环烃上的C-H在3030 cm-1特征吸收，甲烷基的CH2-H键在2960 cm-1有特征吸收，以及亚甲基CH-H在2930 cm-1波长的特征吸收。光源检测器样品池2930cm-1波

4、长过滤器用溶剂萃取水样中的有机碳化合物组分，它们在3.4m红外波段有强烈的吸收，利用其吸收强度与已知浓度的参照油相比较的方法来确定水中含油量。1.2 法规1.2.1南海区海洋油(气)田含油污水监测暂行规定(一九九七年九月一日)为更好地贯彻执行中华人民共和国海洋石油勘探开发环境保护管理条例，建立海洋油（气）田含油污水排放监测制度，保护海洋环境，特制定本暂行规定。本暂行规定适用于在南海区从事海洋油（气）田开发的作业者。国家海洋局南海分局（以下简称主管部门）负责本规定的实施和管理。海上油（气）田必须采用红外法（见南海区海洋油（气）田含油污水测定方法）测定污水含油量。在本暂行规定公布之前投产的油（气）

5、田，其污水含油量分析方法达不到本规定要求的，作业者应在六个月内使该分析方法达到要求。作业者必须在油（气）田含油污水排放口建立监测制度，每天监测四次，每隔6小时监测一次，当测定结果超过75ppm时，应增加监测次数；当连续超标排放24小时时，应报告主管部门，经同意后方可继续排放。作业者应使用主管部门提供的“海洋油气田含油污水分析结果登记表”（见附件一），并按季度上交主管部门。作业者应在每双月5日前，以油（气）田含油污水排放口为单位送水样（250毫升）到主管部门认定的实验室测定，其分析结果应按季度上报主管部门，若分析结果超过国家规定排放标准的，作业者应在当月内报告主管部门。检验单位采用的测定方法应符

6、合海洋石油开发工业含油污水分析方法（征求意见稿）的规定，并应在接到样品五天内提交提交检验报告。为进行实验室之间的相互校对工作，作业者必须在每年12月份以油（气）田采出水排放口为单位提供两水样（每份水样250毫升），其中一份送到主管部门当年所指定的实验室测定含油量。作业者送往陆地实验室的采出水样，必须在采样时加入1:1盐酸2mL固定保存。凡违反本暂行规定的，主管部门将根据中华人民共和国海洋石油勘探开发环境保护管理条例及条例实施办法的有关规定给予警告或罚款。本暂行规定自发布之日起执行。国家海洋局南海分局南海区海洋油（气）田含油污水测定方法方法概述：用溶剂萃取水样中的有机碳化合物组分，它们在3.4m

7、红外波段有强烈的吸收，利用其吸收强度与已知浓度的参照油相比较的方法来确定水中油含量。取样与保存：在污水排放口采集的的水样（不得少于200mL）现场应立即测定。如果不是当天测定，需加入1:1盐酸2mL固定保存。仪器：红外油份（碳氢化合物，有机碳化合物）浓度分析仪，或红外光光度计，测定波长必须在3.4m（即2930cm-1），量程不得低于0200ppm范围。试剂：四氯化碳（CCl4）分析纯氟里昂（1,1,2-三氟，1,2,2-三氯乙烷）分析纯参照标准：大部分红外油份浓度计都随机配备标准参照油，如果没有，由南海监测中心实验室负责提供。萃取：将采集的的样品摇匀，用刻度吸管吸取一定量体积于分液漏斗，以1

8、:1的体积比加入萃取剂，充分混合1分钟，取下层萃取液测定。如果仪器操作说明书另有要求而更改体积比的，应在含油污水分析结果登记表的备注中加以说明。测定结果：红外油份浓度计上所显示的结果即是水中油含量，以ppm或mg/L表示均可。注意：标准参照浓度，每隔两月应油专门负责人重新配制。每次测定前，都应校准量程，使仪器保持良好的工作状态。1.2.2分析标准比较IP426/98 ，GB/T 16488-1996，GB/T 17923-1999这两个标准是最复杂也是比较科学完全的水中油的分析方法。它先用硅镁吸附剂对萃取液进行处理，然后用红外光谱仪对萃取液在2600CM-13300CM-1进行扫描，得到光谱图

9、。然后分别读取出3030cm-1、2960 cm-1及2930 cm-1下的吸光度，经过一系列计算过程，从而得到芳烃、环烷烃，脂肪烃含量（把它们加起来就是石油烃含量）和动植物油的含量。其中IP426/98要求使用的溶剂是四氯乙烯，GB/T 16488-1996要求使用的溶剂是四氯化碳。GB/T 16488-1996中也提出了简化的只在2930 cm-1波长下的测定方法。实际上这一部分就是GB/T 17923-1999海洋石油开发工业含油污水分析方法。几种标准的比较IP426/98GB/T 16488-1996GB/T 17923-1999海洋局南海标准溶剂四氯乙烯四氯化碳四氯化碳四氯化碳或氟里

10、昂标准物质甲苯，十六烷、姥鲛烷甲苯，十六烷、姥鲛烷或现场原油或正十六烷、异辛烷和苯按65：25：10混和物经处理过的现场原油仪器厂家或南海监测中心实验室提供？测定波长2600-3300 cm-12400-3400 cm-1或2930cm-12930 cm-12930 cm-1硅镁吸附必须必须必须勿须1.3 NEW METHOD APPLIED BY PHILLIPS PHILLIPS选取的新测定方法仪器： CVH TPH ANALYZER溶剂： C2Cl4固定水样溶剂比：100mL水+40mL溶剂，即2.5倍浓缩PART II ABOUT SOLVENT关于溶剂2.1 适合水中油分析的溶剂基本

11、要求可采用的溶剂必须达到的要求：1. 在2930 cm-1下无吸收2. 与油混溶3. 不溶于水、不与水乳化4. 跟水有较大的比重差，易与水分离符合以上要求的的溶剂主要有CCl4, C2Cl4和Freon113. 正己烷是Phillips水中油仪器特定的分析方法采用的溶剂.2.2 MSDS COMPARISON (MSDS比较)四氯化碳（CCl4）四氯乙烯(C2Cl4)Freon113n-Hexane(C6H14)物理性质Appearance and odor外观和气味无色易挥发不易燃液体，具氯仿微甜气味无色易挥发不易燃液体，具微甜气味无色透明易挥发液体，微具乙醚气味无色透明液体,具烃类气味比重

12、 (water=1)1.581.621.570.663沸点 (°C)76.81214869分子量153.84168.52187.3786.2凝点 (°C)-23-19N/AN/A蒸汽压(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类及有机溶剂不溶于水溶于油类及有机溶剂不溶于水溶于油类及有机溶剂不溶于水溶于油类及有机溶剂火灾可燃性不可燃不可燃不可燃可燃闪点(°C)N/AN/AN/A-22LELN/AN/AN/A1.7%UELN/AN/AN/A7.7%自燃点(°C)N/AN/AN/A

13、223化学性质热分解产物CO2,HCl COCl2(光气) Cl2CO2,HCl COCl2(光气) Cl2HCl,HF,卤代羰基化合物CO化学稳定性稳定稳定避免与NaOH接触稳定稳定毒性总评价有毒有毒无毒有毒目标器官肝，肾损害肝无神经系统致癌性致癌物可能致癌无无环保性N/AN/A破坏臭氧层被禁止使用N/A工作场所最高允许浓度 (ppm)525无50个人防护日常使用PPE橡胶手套、护目镜、工作服通风要求必须在通风柜内使用废液处理残液以密封钢桶收集送岸上相关机构处理，不得排入下水道综合CCl4、C2Cl4及Freon113, C2Cl4会作为水中油分析不得不采用的溶剂。2.3 MSDS of C

14、2Cl4四氯乙烯; 全氯乙烯; Tetrachloroethylene; Perchloroethylene; CAS: 127-18-4理化性质无色液体,气味似乙醚。化学式C2Cl4。分子量165.83。相对密度1.6311(15/4)。熔点-22.4。沸点121。蒸气密度5.83。蒸气压2.11kPa(15.8mmHg22)。溶于约10000份体积水; 与乙醇、乙醚、氯仿、苯混溶。遇水可缓慢分解成三氯乙酸和盐酸。有水存在对铁、铝、锌有腐蚀(但可加稳定剂加以抑制)。非可燃性液体。高温引起分解,分解条件不同分解产物不一样,主要为盐酸、光气、一氧化碳。如有活性炭存在,加热至700分解生成六氯化苯

15、和六氯乙烷。被强氧化剂氧化。与钡粉、铍粉、锂屑、四氧化二氮、氢氧化钠发生剧烈化学反应。接触机会工业上主要用作溶剂、有机合成、金属去污剂和干洗剂、脱硫剂、热传递介质。医疗上用作驱虫药。一般居民通过大气、食品及饮水可能接触低水平的四氯乙烯。侵入途径本品可经呼吸道、消化道和皮肤吸收。毒理学简介人吸入TCL0: 96 ppm/7H。人（儿童）经口TDL0: 545 mg/kg。人（男性）吸入TCL0: 600 ppm/10M。大鼠经口LD50: 2629 mg/kg; 吸入LC50: 34200 mg/m3/8H。小鼠经口LD50: 8100 mg/kg; 吸入LC50: 5200 ppm/4H。兔经

16、皮LD  :3228mg/kg四氯乙烯进入人体后,在体内蓄积有限,约有98经肺排出,仅有2发生变化。主要转化为三氯乙酸和三氯乙醇,随尿排出。本品排出体外十分缓慢,吸入浓度为2.7mg/L的蒸气3.5小时后,经过两星期尚可测出,肺中平均滞留本品62; 浓度为1.3mg/L时,3小时后可达到平衡。本品毒性较三氯乙烯为低,麻醉作用较弱,主要抑制中枢神经系统,肝、肾毒害较轻。对眼、鼻、喉、咽有刺激。动物实验证实四氯乙烯对动物有致癌性,但针对洗衣及干洗工人所作的流行病学研究却发现四氯乙烯对人类致癌性的有无仍不确定。临床表现急性吸入主要表现为眼、鼻、喉、咽刺激症状,有眼灼痛、流涎、流涕、口干、口

17、内金属甜味、头痛和头部压迫感、眩晕、运动失调、甚至意识不清。一般于脱离接触后可恢复,并无后遗症。临床报道对肝有损害。急性口服中毒者,有头昏、头痛、倦睡、恶心、呕吐、腹痛、视物模糊、四肢麻木,可出现兴奋不安、抽搐乃至昏迷。也曾有因过量口服本品引起中毒死亡的报告。反复接触可引起皮炎。处理接触者,应立即离开现场。有刺激症状者需安静休息,进行必要的检查及处理,并观察24小时。急性中毒者应卧床休息,急救措施和对症治疗原则与内科相同。有昏迷、心跳及呼吸停止者,迅速进行脑、心、肺复苏; 对症处理。重度中毒患者可适当使用糖皮质激素。注意保护肝、肾功能。忌用肾上腺素。标准车间空气卫生标准：中国MAC 200 m

18、g/m3 (1996)美国ACGIH TLV-STEL 685 mg/m3 (100 ppm)美国ACGIH TLV-TWA 170 mg/m3 (25 ppm)美国MSHA STANDARD-air: TWA 100 ppm (670 mg/m3)美国OSHA PEL(所有行业): 8H TWA 100 ppm; CL 200; Pk 300/5M/3H埃及: TWA 5 ppm (35 mg/m3), 皮肤澳大利亚: TWA 50 ppm (335 mg/m3), STEL 150 ppm, 致癌物比利时: TWA 50 ppm (339 mg/m3), STEL 200 ppm (136

19、8 mg/m3)丹麦: TWA 30 ppm (200 mg/m3), 皮肤芬兰: TWA 50 ppm (335 mg/m3), STEL 75 ppm (520 mg/m3), 皮肤法国: TWA 50 ppm (335 mg/m3)德国: TWA 50 ppm (345 mg/m3), 致癌物匈牙利: STEL 50 mg/m3, 皮肤，致癌物日本: TWA 50 ppm (340 mg/m3)荷兰: TWA 35 ppm (240 mg/m3), 皮肤菲律宾: TWA 100 ppm (670 mg/m3)波兰: TWA 60 mg/m3俄罗斯: 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, 皮肤泰国: TWA 100 ppm, STEL 200 ppm英国: TWA 50 ppm (335 mg/m3), STEL 150 ppm保加利亚,哥伦比亚,约旦,韩国 参照美国 ACGIH TLV; 新西兰,新加坡,越南 参照美国 ACGIH TLV2.4 QUALITY REQUIREMENT OF C2Cl4 FOR OIW ANALYSISl Hydrocarbon conten

21、t should be less than 20ppm碳氢化合物杂质含量应少于20ppm.l Background absorption should not change after being washed with water背景吸收值在水洗之后应该没有变化, 即溶剂不含水溶性有机杂质.2.5 PROS AND CONS OF C2Cl4 EXTRACTION V.S. n-HEXANE EXTRACTION四氯乙烯萃取法相对正己烷萃取的优缺点Pros优点l Good accuracy and repeatability好的准确性和重复性l C2Cl4 is incombustible四

22、氯乙烯为不可燃物l Method is recognized by environmental regulation and standard test methods 测量方法来自环保法规和国家国际标准Cons缺点l More consumption of solvent溶剂用量较大l The extractant is more easily contaminated by water and suspended solids 萃取液更容被水和悬浮固体沾污l More personnel training is needed操作人员需较严格培训PART III CVH TPH ANALYZ

23、ER CALIBRATION仪器校正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 .用油田现场生产的原油作为标准油. 在使用之前将盛油容器放入50ºC水浴一小时,并摇晃容器以使油样混合均匀.2. Prepare 8 oil

24、-free 100mL volumetric flask. Label them with 10ppm, 20ppm, 40ppm, 60ppm, 80ppm, 100ppm, 200ppm, 300ppm, 400ppm. 准备8只洗净并烘干的100mL容量瓶，分别贴上10ppm, 20ppm, 40ppm, 60ppm, 80ppm, 100ppm, 200ppm, 300ppm, 400ppm标签。 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. 准确称取0.0025, 0.0050, 0.0100, 0.0200, 0.0250, 0.0500, 0.0750, 0.1000g标准油至贴好标签的容量瓶里。注入C2Cl4至刻度线。盖上瓶盖。摇晃5分钟，得到标称浓度为10ppm, 20ppm, 40ppm, 80ppm, 100ppm, 200ppm, 30

26、0ppm, 400ppm的标准溶液。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. 在进行以下校正工作之前确保仪器已经预热一小时以上. 设置显示模式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同进按下并按住CAL和ZERO键两秒以上, 就可以在不同的显示模式之间进行切换. 观察显示窗口, 切换显示模式到AbS.3.3 Zero TPH Analyzer 仪器调零1. 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.以浓盐酸浸泡除去黄色沉积物。四氯乙烯浸泡可除去沥青质深沉。水珠可用棉球吸除。洗净的样品池应无色，光学表面方向应清亮透明。检查样品池是否清洁干燥。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. 在样品池的一个毛面上做好标记。将它放入读数槽时总是让这面朝向面板方向，并按压样口池至槽底压不动为止。将比色池充满干净C2Cl4, 把它按正确方法放入样品槽内.3. Press and hold ZERO button until bAL= appears.按下并按住ZERO键直到bAL=显示出来,稍候片刻直到仪器正确调零. 3. 4 Calibrate TPH Analyzer仪器校正1. Press and hold CAL button until CAL appears on the display. Press

31、the RECALL button to switch the calibration mode to uSEr.压下并按住CAL键直到CAL显示出来. 按RECALL键, 将校正模式切换到uSEr.2. Momentarily press and release the CAL button. The display will read SA01.按CAL键, 显示器将显示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.将样品池以C2Cl4涮洗3次. 将它装满10ppm标样. 将样品池插入样品槽. 按RUN键并等

33、候直到一个数字显示出来. 按UP(RUN)或DOWN(RECALL)键, 将这一数字更改到与标样浓度相同.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. 倒空样品池. 重复步骤2和3, 从第二低标样按从低到高的顺序直到最高标样. 当最高标样设定好之后, 按CAL键, 并按ZERO键结束校正过程.3. 5 Quality Control of Calibration校正检查和备档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.作为质量控制的要求, 校正应该检查和备档. 可以用一个EXCEL工作表用来以表格加图形的方式记录仪器在不同浓度下的吸收值。 这个工作表可以打印并保存起来。3.5.1 Retrieve Calibration Table from OIW Analyzer调出校正表操作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键直到CAL显示. 按RECALL键将校正模式切换到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键, 显示器将显示n=, 接着是标准的数量. 再次按CA

37、L, A01=将显示, 接着显示的是吸光度值. 按CAL, 显示器将显示C01=, 接着是标样的浓度值.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.重复按CAL键, 显示器会依次显示吸光度及标样的浓度. 记录下各浓度下相应的吸光度值, 填入工作表中。The followin

38、g is a typical calibration table retrieve from the OIW analyzer.下图是一典型的从OIW分析仪里调出来的校正表。3.5.2 Check the Linearity of Range from 080ppm检查080ppm范围的校正线性度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. 因为080ppm区间是最常用也

40、最重要的范围，而且仪器在这区间浓度与吸收值呈线性关系（经实测并经生产厂家技术人员证实）。可以通过检查这区间里标样浓度与仪器吸收的线性度来检验校正的可靠性。The following plot is a calibration with acceptable linearity.下图是一张线性度可以接受的校正图。The following plot is a calibration with unacceptable linearity. Obviously, the 30ppm standard is dispersed.下图是一张线性度不可接受的校正图。显然，30ppm标样离群了。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. 如果只有一个离群点存在，放弃此校正点的标样。在电脑上调整该点的Abs值直到那个点正好落在直线上。按3.5.1描述的步骤将该点的Abs更改为修正值。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.如果离群点达两个以上，用该标样重新校正并检查一次。如果问题继续存在，重新配制标样并校正仪器。 3.5.3 Back-chec

43、k and documentation 标样读数和校正备档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.以标样注满样品池并读数. 在80ppm以下的量程里，如果任一标样的读数与其浓度差别超过2ppm；或者在80ppm以上的量程里，任一标样的读数与其浓度差别超过4ppm, 说明校正失败, 并且要从头开始重新校正.PART IV WATER ANALYSIS 水样分析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 仪器准备Turn on the Analyzer 1 hour before water analysis. 在分析工作前一小时打开分析仪。5.2 Take the Sample 样品准备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.先开启取样点阀门冲洗取样口30秒，小

51、心地用100mL量筒接取水样至100mL刻度处。5.2.2 Cool the water sample to room temperature in tap water bath.以凉水浴将水样冷至室温。5.2.3 Pour the water sample to a clean separatory funnel.将全部水样倒入洗净的分液漏斗中。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