水质全分析标准

目 录

第一章 测定总则及一般规定················································································ １

§1—1 总则······································································································ １ §1—2 一般规定······························································································ １ 第二章 水样的采集································································································ ５

§2—1 取样装置······························································································ ５ §2—2 水样的采集方式·················································································· ５ §2—3 水样的存放与运送·············································································· ６ §2—4 水质全分析的工作步骤······································································ ６ 第三章 水质全分析项目测定方法及其结果的校核············································ ７

§3—1 电导率的测定······················································································ ７ §3—2 pH的测定（pH电极法） ······························································ １０ §3—3 钠的测定（pNa的测定） ······························································ １２ §3—4 浊度的测定······················································································ １４ § 3—5 碱度的测定（容量法）································································· １６ §3—6 游离二氧化碳的测定（直接法）·················································· １７ §3—7 亚硝酸盐的测定（格里斯分光光度法）······································ １８ §3—8—1 化学耗氧量的测定（高锰酸钾法）········································ １９ §3—8—2 化学耗氧量的测定（重铬酸钾快速法）································ ２１ §3—9 全固体的测定·················································································· ２２ §3—10 溶解固体的测定············································································ ２４ §3—11 悬浮固体的测定 ············································································ ２５ §3—12 全硅及活硅的测定（氢氟酸转化分光光度法）························ ２６ §3—13 钙的测定（EDTA滴定法） ························································ ２９ §3—14 氯化物的测定（硝酸银容量法）················································ ３０ §3—15 铝的测定（分光光度法）···························································· ３２ §3—16 硬度的测定（EDTA滴定法） ···················································· ３４ §3—17 硫酸盐的测定（分光光度法）···················································· ３６ §3—18—1 铁的测定（磺基水杨酸分光光度法）·································· ３８ §13—18—2 铁的测定（邻菲罗啉分光光度法）···································· ３９ §3—19 硝酸盐的测定（苯酚磺酸比色法）············································ ４１ §3—20 钾的测定（原子吸收分析法）···················································· ４３ §3—21 活性硅的测定（钼蓝比色法）···················································· ４４ §3—22 铁铝氧化物的测定（重量法）···················································· ４６ §3—23 酸度的测定（容量法）································································ ４７ §3—24 磷酸盐的测定（磷钒钼黄分光光度法）···································· ４７ §3—25 铜的测定（双环已酮草酰二腙分光光度法）···························· ４８ §3—26 溶解氧的测定（两瓶法）···························································· ５０ §3—27 亚硫酸盐的测定（碘量法）························································ ５２ §3—28 残余氯的测定（比色法）···························································· ５３

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§3—29 硫化氢的测定（比色法）···························································· ５５ §3—30 腐植酸盐的测定（容量法）························································ ５６ §3—31 微量油的测定（紫外分光光度法）············································ ５７ §3—32 油的测定（重量法）···································································· ５９ §3—33 亚铁的测定（邻菲啰啉分光光度法）········································ ６０ §3—34 水质全分析结果的校核································································ ６１

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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,Na<3μg/L;SiO2<3μg/L

4．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

１

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=

物质B的质量溶质B的质量=

混合物的质量溶液的质量 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=

溶质B的质量

溶液的体积 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

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]=

溶质B的物质的量

溶液的体积V２