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１目录第一章测定总则及一般规定····························································１§1—1总则·············································································２§1—2一般规定······································································２第二章水样的采集········································································６§2—1取样装置······································································７§2—2水样的采集方式·····························································７§2—3水样的存放与运送··························································７§2—4水质全分析的工作步骤····················································８第三章水质全分析项目测定方法及其结果的校核·································８§3—1电导率的测定································································９§3—2pH的测定（pH电极法）··············································１２§3—3钠的测定（pNa的测定）···············································１４§3—4浊度的测定································································１６§3—5碱度的测定（容量法）·················································１８§3—6游离二氧化碳的测定（直接法）·····································１９§3—7亚硝酸盐的测定（格里斯分光光度法）····························２０§3—8—1化学耗氧量的测定（高锰酸钾法）······························２１§3—8—2化学耗氧量的测定（重铬酸钾快速法）························２３§3—9全固体的测定·····························································２４§3—10溶解固体的测定·························································２６§3—11悬浮固体的测定·························································２７§3—12全硅及活硅的测定（氢氟酸转化分光光度法）·················２８§3—13钙的测定（EDTA滴定法）··········································３１§3—14氯化物的测定（硝酸银容量法）····································３２§3—15铝的测定（分光光度法）·············································３４§3—16硬度的测定（EDTA滴定法）·······································３６§3—17硫酸盐的测定（分光光度法）·······································３９§3—18—1铁的测定（磺基水杨酸分光光度法）·························４０§13—18—2铁的测定（邻菲罗啉分光光度法）···························４１§3—19硝酸盐的测定（苯酚磺酸比色法）·································４３§3—20钾的测定（原子吸收分析法）·······································４５§3—21活性硅的测定（钼蓝比色法）·······································４６§3—22铁铝氧化物的测定（重量法）·······································４８§3—23酸度的测定（容量法）················································４９§3—24磷酸盐的测定（磷钒钼黄分光光度法）···························５０§3—25铜的测定（双环已酮草酰二腙分光光度法）·····················５１§3—26溶解氧的测定（两瓶法）·············································５３§3—27亚硫酸盐的测定（碘量法）··········································５５§3—28残余氯的测定（比色法）·············································５５２§3—29硫化氢的测定（比色法）·············································５７§3—30腐植酸盐的测定（容量法）··········································５９§3—31微量油的测定（紫外分光光度法）·································６０§3—32油的测定（重量法）···················································６１§3—33亚铁的测定（邻菲啰啉分光光度法）······························６２§3—34水质全分析结果的校核················································６４§3—35磷酸盐的测定（磷钼蓝比色法）……………………………………62第一章测定总则及一般规定§1—1总则1．实验室应具有化学分析的一般仪器和设备，如分析天平，分光光度计，电导仪、pH、pNa、pX计等和常用的玻璃仪器以及电炉、高温炉、烘箱、水浴锅、计算器等设备。此外，还应有良好的通风设备和所需等级的化学药品。2．为保证分析数据的质量，分析操作者应掌握各分析方法的基本原理和基本操作技能，并对所测试的结果能进行计算和初步审核。3．对使用的贵重精密仪器或进行低含量分析时，为了保证仪器的灵敏度和分析数据的可靠性，必须采取防尘，防震、防止酸、碱气体腐蚀的有效措施。4．使用对人体有害的药品（例如汞，氢氟酸及有毒害的有机试剂等）时，应采取必要的防护和保健措施。§1—2一般规定1．仪器校正：为了保证分析结果的准确性，对分析天平砝码，应定期（1~2）年进行校正；对分光光度计等分析仪器应根据说明书进行校正，对容量仪器，如：滴定管、移液管、容量瓶等，可根据实验的要求进行校正。2．空白试验：2．1在一般测定中，为提高分析结果的准确度，以空白水代替水样，用测定水样的方法和步骤进行测定，其测定值称为空白值。然后对水样测定结果进行空白值校正。2．2在微量成分比色分析中，为校正空白水中待测成分含量，需要进行单倍试剂的空白试验。单倍试剂空白试验，与一般空白试验相同。双倍试剂空白试验是指试剂加入量为测定水样所用试剂量的两倍，测定方法和步骤均与测定水样相同。根据单、双倍试剂空白试验结果可求出空白水中待测成分的含量，对水样测定结果进行空白值校正。3．空白水质量；测定方法中的“空白水”是指用来配制试剂和作空白试验用的水，如蒸馏水、除盐水、高纯水等。对空白水的质量要求规定如下：空白水名称质量要求蒸馏水电导率3µS/㎝(25℃)高锰酸钾试验合格除盐水电导率1µS/㎝（25℃）高锰酸钾试验合格高纯水电导率（混床出口，25℃）0.2µS/㎝;Cu,Fe,Na3µg/L;SiO23µg/L３4．干燥器；干燥器内一般用氯化钙或变色硅胶作干燥剂。当氯化钙干燥剂表面有潮湿现象或变色硅胶颜色变红时，表明干燥剂失效，应进行更换。5．蒸发浓缩：当溶液的浓度较低时，可取一定量溶液先在低温电炉上进行蒸发，浓缩至体积较小后，再移至水浴锅里进行蒸发。在蒸发过程中，应注意防尘和爆沸溅出。6．灰化：在重量分析中，沉淀物进行灼烧前，必须在电炉上将滤纸彻底灰化后，方可移入高温炉燃烧。在灰化过程中应注意不得有着火现象发生，必须盖上坩埚盖，但为了有足够的氧气进行坩埚，坩埚盖不应盖严。7．恒重：测定中规定的恒重是指在灼烧（烘干）和冷却条件相同的情况下，最后两次称量之差不大于0.4mg。如在测定中另有规定者，不在此限。8．试剂纯度：在测定中若无特殊指明者均用分析纯（A.R）或化学纯(C.P)试剂。标定溶液浓度时，基准物质应是保证试剂或一级试剂（优级纯）。当试剂不合要求时，可将试剂提纯使用或采用更高级别的试剂。9．试剂配制：测定中所用试剂的配制除有明确规定者外，均为水溶液。10．试剂加入量：测定中，如以滴数表示，均应按每20滴相当于1mL来计算。11．标准溶液标定：标准溶液的标定一般应取两份或两份以上试样进行平行试验，当平行试验的相对偏差在±0.2~0.4%以内时，才能取平均值计算其浓度。12．工作曲线的制作和校核：用分光光度法测定水样时，应测定五个以上标准溶液的吸光度值才能制作工作曲线。有条件时应使用计算器对数据进行回归处理，以便提高工作曲线的可靠性。工作曲线视测定要求，应定期校核。一般可配制1~3个标准液，对工作曲线再进行水样测定。制作工作曲线时，要用移液管准确吸取标准溶液，标准溶液的体积数一般应保持三位有效数字。13．溶液浓度的表示法溶液的浓度是表示一定量的溶液所含液质的量。实际应用上，都是根据需要来配制各种浓度的溶液。根据我国法定计量单位规定，可用（物质的）质量分数、（物质的）体积分数和（物质的）浓度（即物质的量浓度）等来表示。13.1质量分数以前称为重量百分浓度.它表示物质B(溶质B)的质量与溶液的质量比,用符号(WB)表示。即WB=混合物的质量的质量物质B=溶液的质量的质量溶质B习惯上为方便起见也可用百分数（%）表示。13.2体积分数（质量浓度）表示物质B（溶质B）的质量除以混合物（WB）的体积用符号ρB表示，即ρB=溶液的体积的质量溶质B单位可用百分数表示，也可用克每升（g/L），或毫克每升（mg/L），或微克每升（µg/L）。若溶液用百分数表示，以指示剂称呼者，其浓度则不标注（体积分数）。13.3体积比浓度体积比浓度是指液体试剂与溶剂按x+y的体积关系配制溶液，符号（x+y）。如硫酸溶液（1+3）是指1体积的浓硫酸与3体积的水混合而成的硫酸溶液。13.4滴定度４滴定度是指1mL溶液中所含相当于待测成分的质量，用符号T表示。单位为毫克每毫升（mg/mL）,或微克每毫升（µg/mL）。13.5浓度（即物质的量浓度）物质的量浓度简称浓度，以前称为（体积）摩尔浓度和当量浓度。它是用物质B（溶质B）的物质的量除以混合物（溶液）的体积，用符号CB表示，在化学也表示成[B]。即[B]=VB溶液的体积的物质的量溶质单位为摩尔每升（mol/L