硅钼黄分光光度法测定光伏行业含氟废水中可溶性硅
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摘要
目前,我国光伏行业发展加快,但随之产生了大量含氟废水。为了准确测定光伏行业含氟废水中可溶性硅含量,本文主要采用硅钼黄分光光度法进行试验研究。通过建立硅钼黄法测定除氟处理前后含氟废水中可溶性硅含量的检测分析方法,并对水样中存在的Al3+、F-、P元素等干扰离子进行了干扰试验。试验结果表明:水样中低浓度的Al3+、F-等离子的存在对可溶性的硅含量的测定基本无干扰,P元素的干扰较为严重,而草酸可以掩蔽磷的干扰,1 mg磷酸对应0.6 mL 10 g/L草酸溶液时干扰效果最佳;c(Si)在0～2.0 mg·L-1时线性良好,R2>0.999;通过精密度试验结果表明样品的加标回收率为100%±3.00%,在c (Si)为34.475 mg·L-1和3.332 mg·L-1时,相对标准偏差均<3%。因此,测定光伏行业含氟废水中的可溶性硅可以选择硅钼黄分光光度法来进行。
At present, the development of China's photovoltaic industry has accelerated, but a large amount of fluorine-containing wastewater has been produced. In order to accurately determine the soluble silicon content in fluorine-containing wastewater of photovoltaic industry, this paper mainly uses silicon molybdenum yellow spectrophotometry to conduct experimental research. The method of detection and analysis of soluble silicon content in fluorine-containing wastewater before and after defluorination treatment was established by establishing silico-molybdenum yellow method, and interference tests were carried out on interfering ions such as Al3+, F-and P in water samples. The test results show that the presence of low concentration of Al3+and F-plasma in the water sample has no interference on the determination of soluble silicon content, and the interference of P element is more serious, while oxalic acid can mask the interference of phosphorus, and 1 mg of phosphoric acid corresponds to 0.6 mL 10 g/L oxalic acid solution has the best interference effect; c(Si) has good linearity at 0～2.0 mg·L-1, R2>0.999; the precision test results show that the spiked recovery of the sample is 100%±3.00%, When c(Si) was 34.475 mg·L-1 and 3.332 mg·L-1, the relative standard deviations were <3%. Therefore, the determination of soluble silicon in the fluorine-containing wastewater of the photovoltaic industry can be carried out by using the molybdenum-lime yellow spectrophotometry.
At present, the development of China's photovoltaic industry has accelerated, but a large amount of fluorine-containing wastewater has been produced. In order to accurately determine the soluble silicon content in fluorine-containing wastewater of photovoltaic industry, this paper mainly uses silicon molybdenum yellow spectrophotometry to conduct experimental research. The method of detection and analysis of soluble silicon content in fluorine-containing wastewater before and after defluorination treatment was established by establishing silico-molybdenum yellow method, and interference tests were carried out on interfering ions such as Al3+, F-and P in water samples. The test results show that the presence of low concentration of Al3+and F-plasma in the water sample has no interference on the determination of soluble silicon content, and the interference of P element is more serious, while oxalic acid can mask the interference of phosphorus, and 1 mg of phosphoric acid corresponds to 0.6 mL 10 g/L oxalic acid solution has the best interference effect; c(Si) has good linearity at 0～2.0 mg·L-1, R2>0.999; the precision test results show that the spiked recovery of the sample is 100%±3.00%, When c(Si) was 34.475 mg·L-1 and 3.332 mg·L-1, the relative standard deviations were <3%. Therefore, the determination of soluble silicon in the fluorine-containing wastewater of the photovoltaic industry can be carried out by using the molybdenum-lime yellow spectrophotometry.
引文
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[23]徐金兰,王宝泉,王志盈,等.石灰沉淀-混凝沉淀处理含氟废水的试验[J].水处理技术,2003,29(5):282-285.
[24]Xu J L,Wang B Q,Wang Z Y,et al.Treatment of wastewater-containing fluoride by lime-sedimentation and coagulation precipitation[J].Technology of Water Treatment,2003,29(5):282-285.
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[27]隋欣,王宝辉,邵丽英,等.硅钼黄光度法测定油田产出水中低聚硅[J].南京师大学报(自然科学版),2009,32(2):78-81.
[28]Sui X,Wang B H,Shao L Y,et al.Si-Mo spectrometry of silicon oil gomer in produced water by oilfield[J].Journal of Nanjing Normal University(Engineering and Technology Edition),2009,32(2):78-81.
[2]Lei S M,Guo Z H.Hazards of fluoride pollution and technical research progress of treating fluoride containing wastewater[J].Metal Mine,2012,41(4):152-155.
[3]刘烽,王慧,徐海斌,等.火法冶炼镍基体料中硅含量的测定:分光光度法与ICP-AES的比较[J].光谱实验室,2013,30(4):001773-1776.
[4]Liu F,Wang H,Xu H B,et al.Determination of silicon in nickel base material:Comparison of two methods-by spectrophotometry and ICP-AES[J].Chinese Journal of Spectroscopy Laboratory,2013,30(4):1773-1776.
[5]刘丽娟,张娜,刘瑜,等.硅钼黄分光光度法测定硅微粉中二氧化硅[J].冶金分析,2009,29(10):63-65.
[6]Liu L J,Zhang N,Liu Y,et al.Determination of silicon oxide in silica fume by molybdosilicate yellow spectrophotometry[J].Metallurgical Analysi,2009,29(10):63-65.
[7]梁琼英,欧阳钢锋.硅含量测定方法的新进展[J].广州化工,2000,28(1):48-49.
[8]Liang Q Y,Ouyang G F.The advances in the determination of silion content[J].Guangzhou Chemical Industry,2000,28(1):48-49.
[9]刘海波,左文武,林文周,等.化学-混凝沉淀法处理低浓度含氟废水研究[J].中国给水排水,2008,24(11):76-79.
[10]Liu H B,Zuo W W,Lin W Z,et al.Treatment of lowconcentration fluorides wastewater by chemical/coagulation and sedimentation process[J].Chin Water Wastewater,2008,24(11):76-79.
[11]韩建勋,贺爱国.含氟废水处理方法[J].有机氟工业,2004,(3):27-36.
[12]Han J X,He A G.Methods of treatment of wastewater containing fluorine[J].Organo-Fluorine Industry,2004,(3):27-36.
[13]翟庆洲,金永哲,邵长路,等.硅钼蓝光度法测定沸石分子筛中的硅[J].光谱实验室,1998,(3):82-84.
[14]Zhai Q Z,Kim Y C,Zhang Z T,et al.Determination of silicon in zeolite molecular sieves by molybdosilicate blue photometry[J].Chinese Journal of Spectroscopy Laboratory,1998,(3):82-84.
[15]张建珍,王锦荣,刘家齐.聚合硅酸解聚-硅钼蓝分光光度法测定矿石中二氧化硅[J].冶金分析,2010,30(9):65-69.
[16]Zhang J Z,Wang J R,Liu J Q.Determination of silicon dioxide in ore by polymerized silicic acid depolymerization-molybdosilicate blue spectrophotometry[J].Metallurgical Analysi,2010,30(9):65-69.
[17]郑瑞芝,陈岚,王键,等.硅钼黄法测定海水中硅消除P干扰的研究[J].海洋环境科学,2010,29(6):917-919.
[18]Zheng R Z,Chen L,Wang J,et al.Eliminating P interference in determination of Si in seawater with silicomolybdic yellow method[J].Marine Environmental Science,2010,29(6):917-919.
[19]张希祥,王煤,段德智.氧化钙粉末处理高浓度含氟废水的实验研究[J].四川大学学报(工程科学版),2001,33(6):111-113.
[20]Zhang X X,Wang M,Duan D Z.Treatment of wastewater containing high concentration fluorine with lime powder[J].Journal of Sichuan University(Engineering Science edition),2001,33(6):111-113.
[21]闫秀芝,王淑芬.CaCl2+磷酸盐法处理含氟废水的探讨[J].环境保护科学,1998,(2):12-14.
[22]Yan X Z,Wang S F.Discussion on treating of fluoric wastewater by CaCl2and phosphate[J].Environ Protec Sci,1998,(2):12-14.
[23]徐金兰,王宝泉,王志盈,等.石灰沉淀-混凝沉淀处理含氟废水的试验[J].水处理技术,2003,29(5):282-285.
[24]Xu J L,Wang B Q,Wang Z Y,et al.Treatment of wastewater-containing fluoride by lime-sedimentation and coagulation precipitation[J].Technology of Water Treatment,2003,29(5):282-285.
[25]Strickland J D H.The preparation and properties of silicomolybdic acid.II.The preparation and properties ofβ-silicomolybdic acid[J].Journal of the American Chemical Society,1952,74(4):862-867.
[26]Charlot G.Colorimetric determination of elements[M].Elsevier Pub Co,1964:372.
[27]隋欣,王宝辉,邵丽英,等.硅钼黄光度法测定油田产出水中低聚硅[J].南京师大学报(自然科学版),2009,32(2):78-81.
[28]Sui X,Wang B H,Shao L Y,et al.Si-Mo spectrometry of silicon oil gomer in produced water by oilfield[J].Journal of Nanjing Normal University(Engineering and Technology Edition),2009,32(2):78-81.