水质的净化与检测的实验报告。 1.实验目的 2.实验原理 3.主要仪器和试剂 4、实验步骤和实验现
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1实验目的及要求
掌握铬法测定污水COD的方法及原理,同时了解其他水质指标,如SS、NH3-N、PO43-。
1.2实验原理
(1)重铬酸钾法测定污水COD
实验原理:化学需氧量是用化学氧化剂氧化水中有机物污染物时所消耗的氧化剂量,用氧量(mg/L)表示。化学需氧量愈高,也表示水中有机污染物愈多。常用的氧化剂主要是重铬酸钾和高锰酸钾。以高锰酸钾作氧化剂时,测得的值称CODMn。以重铬酸钾作氧化剂时,测得
的值称CODCr,或简称COD。
重铬酸钾法测COD的原理是在水样中加如一定量的重铬酸钾和催化剂硫酸银,在强酸性介质中加热回流一段时间,部分重铬酸钾被水样中可氧化物质还原,用硫酸亚铁铵滴定剩余的重铬酸钾,根据消耗重铬酸钾的量计算COD的值。
(2)污水中悬浮物(SS)的测定
测定方法:用0.45m滤膜过滤水样,留在滤料上并于103-105℃烘至恒重的固体,经103-105℃烘干后得到SS含量。
(3)污水氨氮的测定---纳氏试剂分光光度法
测定范围:本方法测定氨氮浓度范围以氨计为0.050mg/L-0.30mg/L。
测定原理:氨氮是指以游离态的氨或铵离子形式存在的氨。氨氮与纳氏试剂反应生成黄棕色的络合物,在400nm-500nm波长范围内与光吸收成正比,可用分光光度法进行测定。
3实验仪器、材料、试剂及注意事项
(一)重铬酸钾法测定污水COD实验条件:
(A)仪器
微波闭式COD消解仪、氟塑消解罐,25mL或50mL酸式滴定管、锥形瓶、移液管、容量瓶等。
(B)试剂
重铬酸钾标准溶液(c(l/6 K2Cr2O7=0.2500mol/L),试亚铁灵指示
液,硫酸亚铁铵标准溶液{c(NH4)2Fe(SO4)2·6H2O=0.1mol/L},H2SO4-Ag2SO4溶液
(C)测量范围
1/4
0.25mol/L重铬酸钾溶液测定大于50mg/LCOD,0.025mol/L测定5-50mol/L的COD值。
(二)污水中悬浮物(SS)的测定仪器及注意事项
烘箱,分析天平,干燥器,孔径为0.45um、直径45-60mm滤膜,玻璃漏斗,真空泵,内径为30-50mm称量瓶,无齿扁嘴镊子,蒸馏水或同等纯度的水。
注意事项:
(1)树叶、木棒、水草等杂质应从水样中除去。
(2)废水粘度高时,可加2-4倍蒸馏水稀释,摇均匀待沉淀物下降后再过滤。
(3)也可采用石棉坩埚进行过滤。
(三)污水氨氮测定的试剂、材料、仪器及注意事项
试剂和材料:
(1)无氨蒸馏水:在每升蒸馏水中加0.1mL浓硫酸进行重蒸馏。或用离子交换法,蒸馏水通过强酸性阳离子交换树脂(氢型)柱来制取。无氨水贮存在带有磨口玻璃塞的玻璃瓶内,每升中加10g强酸性阳离子交换树脂(氢型),以利保存。
(2)硫酸铝溶液:称取18g硫酸铝[Al2(SO4)3·18H2O]溶于100mL
水。
(3)50%(m+V)氢氧化钠溶液:称取25g氢氧化钠(NaOH)水中。
(4)酒石酸钾钠溶液:称取50g酒石酸钾钠(KNaC4H6O6·4H2O)溶于100mL水中,加热煮沸驱氨,待冷却后用水稀释至100mL。
(5)纳氏试剂:称取80g氢氧化钾KOH),溶于60mL水中。称取20g碘化钾(KI)溶于60mL水中。称取8.7g氯化汞,加热溶于125mL水中,然后趁热将该溶液缓慢地加到碘化钾溶液中,边加边搅拌,直到红色沉淀不再溶解为止。在搅拌下,将冷却的氢氧化钾溶液缓慢滴加到上述混合液中,并稀释至400mL,于暗处静置24h,倾出上清液,贮于棕色瓶内,用橡胶塞塞紧,存放在暗处,此试剂至少稳定一个月。
(6)磷酸盐缓冲溶液:称取7.15g无水磷酸二氢钾(KH2PO4)及45.08g
磷酸氢二钾(K2HPO4·3H2O)溶于500mL水中。
(7)2%(m+V)硼酸溶液:称取20g硼酸(H3BO3),溶于1000mL水中。
(8)氨氮标准溶液(10mg/L):吸取10.00mL氨氮贮备溶液于1000mL容量瓶中,稀释至标线,用时现配。
仪器:
500mL全玻璃蒸馏器,20mm比色皿,分光光度计
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