高温消解-分光光度法测定稠油采出水中5种硅形态的含量  

Determination of 5 Morphologies of Silicon in Produced Water of Heavy Oil by Spectrophotometry after High Temperature Digestion

作　　者：白昱[1] 周律[1] 马可可 曹智 金志娜 孙森 BAI Yu;ZHOU Lu;MA Keke;CAO Zhi;JIN Zhina;SUN Sen(School of Environment,Tsinghua University,Beijing 100084,China;Jingrun Envirotech Co.,Ltd.y Beijing 101300,China;Fengcheng Field Operation Districts Petro China Xinjiang Oilfield Company,Karamay 834000,China)

机构地区：[1]清华大学环境学院,北京100084 [2]北京京润环保科技股份有限公司,北京101300 [3]中国石油新疆油田分公司风城油田作业区,克拉玛依834000

出　　处：《理化检验（化学分册）》2022年第2期173-180,共8页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：电化学与大直径陶瓷膜组合处理稠油采出水技术研究(20190505020300)。

摘　　要：基于硅钼黄法,以高温消解-分光光度法测定稠油采出水中活性硅、胶体硅、吸附硅、溶解性有机硅、颗粒硅等5种硅形态的含量(均以二氧化硅计)。取水样10.00 mL,分别按照以下步骤试验:①水样过聚四氟乙烯(PTFE)滤头,加入盐酸溶液,并用400 g·L^(-1)四水合酒石酸钾钠溶液1 mL和250 g·L^(-1)一水合草酸钾溶液1 mL掩蔽Fe^(3+)和PO_(4)^(3-)的干扰(总铁和总磷质量分别小于3000,250μg时适用),在试验组中加入仲钼酸铵用于显色反应(色度补偿组加入氯化铵),以水为参比,在400 nm处测定显色体系吸光度,以试验组和色度补偿组吸光度差值计算目标吸光度,并以此计算活性硅的质量浓度(ρ_(1));②水样过PTFE滤头,加入氢氟酸(将水中胶体硅分解为活性硅),在水热釜中于100℃消解20 min,加入氯化铝,用于消除多余F^(-),洗涤后定容,后续检测步骤同(1),所得结果(ρ_(2))与ρ_(1)的差值即为胶体硅的质量浓度;③水样不过滤,直接按照(2)提供的方法进行前处理和检测,所得结果(ρ_(3))与ρ_(2)的差值即为吸附硅的质量浓度;④在水样中加入氢氟酸和过硫酸钠(将水样中溶解性有机硅消解为活性硅),在水热釜中于120℃消解30 min,加入氯化铝,洗涤后定容,后续检测步骤同①,所得结果(ρ_(4))与ρ_(3)的差值即为溶解性有机硅的质量浓度;⑤在水样中加入氢氧化钠(用于消解水样中颗粒硅和胶体硅)和过硫酸钠,在水热釜中于200℃消解120 min,加入硫酸,洗涤后定容,后续检测步骤同①,所得结果(ρ_(5))与ρ_(4)的差值即为颗粒硅的质量浓度。二氧化硅基准物质配制的标准溶液系列经干扰掩蔽、消解、显色处理后检测,所得硅(以二氧化硅计)的质量均在500~5000μg内与其对应的吸光度呈线性关系,硅(以二氧化硅计)的检出限为4.0~7.1 mg·L^(-1)。分别在实验室内和实验室间对硅标准溶液进行精密度和准确度试验,实验室内和实验室间�Based on Si-Mo yellow method,the method for determination of 5 morphologies of silicon(calculated as SiO;),including active silicon,colloidal silicon,adsorbed silicon,dissolved organic silicon and granular silicon in the produced water of heavy oil was proposed by spectrophotometry after high temperature digestion.The water sample(10.00 mL)was taken and tested by the following steps,respectively.①Water sample was passed through PTFE filter,and mixed with hydrochloric acid.In the above solution,400 g·L^(-1) sodium potassium tartrate tetrahydrate solution of 1 mL and 250 g·L^(-1) potassium oxalate monohydrate solution of 1 mL were added to mask the interference of Fe^(3+) and PO_(4)^(3-)(suitable when the mass of total Fe^(3+) and P were less than 3000,250μg,respectively).In the experimental group,ammonium paramolybdate was used for color reaction(ammonium chloride was added in the chroma compensation group).With water as reference,the absorbance of the color system was measured at 400 nm.The target absorbance was calculated by the absorbance difference between the experimental group and the chroma compensation group,and the mass concentration of active silicon(ρ_(1))was calculated based on the target absorbance.②Water sample was passed through PTFE filter,hydrofluoric acid was added to decompose colloidal silicon in water into active silicon,and the above solution was digested in a hydrothermal kettle at 100℃ for 20 min.After aluminum chloride was added to eliminate excess F^(-),the mixed solution was washed,diluted,and done as follow-up steps with①.The mass concentration of colloidal silicon was obtained by difference between the result(ρ_(2))and ρ_(1).③Water sample was not filtered,and directly pretreated and detected in accordance with the method provided by②.The mass concentration of adsorbed silicon was obtained by the difference between the result(ρ_(3))and ρ_(2).④Hydrofluoric acid and sodium persulfate for digesting dissovled organic silicon to active silicon were added to the water sa

关 键 词：高温消解 分光光度法 硅形态 稠油采出水 

分 类 号：O657.32[理学—分析化学]