云维保山有机化工有限公司

化验分析系统安全技术操作规程

（试行）

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日期：二零壹零年三月十日

目 录

第一部分 电石全分析操作法 ................................................ 1

1发气量测定 .......................................................................................................................................... 1

2酸不溶物、游离碳含量测定 .............................................................................................................. 1

2.1测定原理 .................................................................................................................................. 1 2.2试剂和溶液 .............................................................................................................................. 1 2.3测定方法 .................................................................................................................................. 1 3铁铝氧化物（R2O3）含量的测定 ...................................................................................................... 1

3.1测定原理 .................................................................................................................................. 1 3.2试剂和溶液 .............................................................................................................................. 2 3.3测定方法 .................................................................................................................................. 2 4全氧化钙含量的测定 .......................................................................................................................... 2

4.1测定原理 .................................................................................................................................. 2 4.2试剂和溶液 .............................................................................................................................. 2 4.3测定方法 .................................................................................................................................. 2 5硫化钙含量测定 .................................................................................................................................. 3

5.1测定原理 .................................................................................................................................. 3 5.2实际和溶液 .............................................................................................................................. 3 5.3测定方法 .................................................................................................................................. 3 6磷化钙含量测定 .................................................................................................................................. 4

6.1测定原理 .................................................................................................................................. 4 6.2试剂和溶液 .............................................................................................................................. 4 6.3测定方法 .................................................................................................................................. 4 7碳化钙含量计算 .................................................................................................................................. 5 8游离氧化钙含量计算 .......................................................................................................................... 5 9铁含量测定 .......................................................................................................................................... 6

9.1测定原理 .................................................................................................................................. 6 9.2试剂和溶液 .............................................................................................................................. 6 9.3测定方法 .................................................................................................................................. 6 10氧化铝含量计算 ................................................................................................................................ 6 11氧化铁含量测定 ................................................................................................................................ 7

11.1测定原理 ................................................................................................................................ 7 11.2试剂和溶液 ............................................................................................................................ 7 11.3测定方法 ................................................................................................................................ 7 12硅铁含量测定 .................................................................................................................................... 7

第二部分 石灰、焦炭分析规程 .............................................. 9

1分析样品的取样方法 .......................................................................................................................... 9

1.1取样要求 .................................................................................................................................. 9 1.2分析样品的取样方法 .............................................................................................................. 9 2检验项目及测定方法 ........................................................................................................................ 10

2.1石灰石检验项目及测定方法 ................................................................................................ 10 2.2工业用焦检验项目及测定方法 ............................................................................................ 11 3检验项目判定标准 ............................................................................................................................ 14

第三部分 工业锅炉水质分析 ............................................. 15

1水样的采集 ........................................................................................................................................ 15

1.1取样装臵 ................................................................................................................................ 15 1.2 水样的采集方法 ................................................................................................................. 15

1.3 水样的存放于运送 ............................................................................................................. 15 2悬浮固形物的测定 ............................................................................................................................ 16

2.1概要 ........................................................................................................................................ 16 2.2 仪器 ............................................................................................................................... 16 2.3 试剂 ............................................................................................................................... 16 2.4 测定方法 ............................................................................................................................... 16 3溶解固形物的测定（重量法） ........................................................................................................ 18

3.1 概要 ................................................................................................................................... 18 3.2 仪器 ................................................................................................................................... 18 3.3 测定方法 ........................................................................................................................... 18 4电导率的测定 .................................................................................................................................... 18

4.1 方法概要 ......................................................................................................................... 18 4.2 仪器 ..................................................................................................................................... 19 4.3 试剂 ................................................................................................................................... 19 4.4 操作步骤 ............................................................................................................................. 20 4.5 电导率与含盐量的关系 ..................................................................................................... 21 5 PH 的测定（电极法） ..................................................................................................................... 21

5.1 概要 ................................................................................................................................... 21 5.2 仪器 ................................................................................................................................... 22 5.3 试剂及配制 ..................................................................................................................... 23 5.４ pHs-3F型酸度计的使用方法 .......................................................................................... 23 6氯化物的测定（硝酸银容量法） .................................................................................................... 24

6.１ 概要 ................................................................................................................................... 24 6.２ 试剂及配制 ....................................................................................................................... 24 6.3 测定方法 ............................................................................................................................... 25 6.4 测定水样时注意事项 ......................................................................................................... 26 7碱度的测定（容量法） .................................................................................................................... 26

7.1 概要 ................................................................................................................................... 26 7.2 试剂及配制 ..................................................................................................................... 26 7.3 测定方法 ........................................................................................................................... 27 8硬度的测定（EDTA滴定法） ........................................................................................................... 28

8.1 概要 ....................................................................................................................................... 28 8.2 试剂及配制 ........................................................................................................................... 28 8.3 测定方法 ............................................................................................................................. 28 8.4 测定水样时注意事项 ......................................................................................................... 29 9磷酸盐的测定（磷矾钼黄分光光度法） ........................................................................................ 30

9.1 概要 ....................................................................................................................................... 30 9.2仪器 ........................................................................................................................................ 31 9.3 试剂及配制 ......................................................................................................................... 31 9.4 测定方法 ......................................................................................................................... 31 9.5 测定水样时注意事项 ........................................................................................................... 32 10磷酸盐的测定（磷钼蓝比色法） .................................................................................................. 32

10.1 概要 ................................................................................................................................. 32 10.2 仪器 ..................................................................................................................................... 32 10.3 试剂及配制 ......................................................................................................................... 32 10.4 测定方法 ........................................................................................................................... 32 10.5 测定水样时注于事项 ..................................................................................................... 33 11溶解氧的测定（两瓶法） .............................................................................................................. 33

11.1 概要 ................................................................................................................................... 33 11.2 仪器 ................................................................................................................................... 33 11.3 试剂及其配制 ................................................................................................................... 33

11.4 测定方法 ......................................................................................................................... 34 12溶解氧的测定（靛蓝二磺酸钠比色法） ...................................................................................... 35

12.1 概要 ................................................................................................................................... 35 12.2 仪器 ................................................................................................................................... 35 12.3 试剂及其配制 ................................................................................................................. 35 12.4 测定方法 ......................................................................................................................... 36 12.5 测定水样时注意事项 ....................................................................................................... 39 13亚硫酸盐的测定（碘量法） .......................................................................................................... 39

13.1 概要 ................................................................................................................................... 39 13.2 试剂及配制 ....................................................................................................................... 39 13.3 测定方法 ........................................................................................................................... 39 13.4 测定水样时注意事项 ..................................................................................................... 40 14油的测定（重量法） ...................................................................................................................... 40

14.1 概要 ................................................................................................................................. 40 14.2 仪器 ................................................................................................................................... 40 14.3 试剂及其配制 ................................................................................................................... 40 14.4 测定方法 ......................................................................................................................... 40 14.5 测定水样时注意事项 ....................................................................................................... 41 15铁的测定（磺基水杨酸分光光度法） .......................................................................................... 42

15.1 概要 ................................................................................................................................... 42 15.2 仪器 ................................................................................................................................... 42 15.3 试剂 ................................................................................................................................. 42 15.4 测定方法 ........................................................................................................................... 42 15.5 本方法注释 ....................................................................................................................... 43 16氯离子（有效氯）的分析 .............................................................................................................. 43

16.1原理：碘量法 ...................................................................................................................... 43 16.2操作步骤： .......................................................................................................................... 43 17废水分析操作规程 .......................................................................................................................... 44

17.1总排废水取样 ...................................................................................................................... 44 17.2 悬浮物(103~105℃烘干的总不可滤残渣)的测定 ........................................................... 45 17.3 硫化物含量的测定 ........................................................................................................... 45 18氨氮测定操作规程 .......................................................................................................................... 46

18.1概述 ...................................................................................................................................... 46 18.2水样的预处理 ...................................................................................................................... 46 18.3所需仪器 .............................................................................................................................. 47 18.4操作步骤 .............................................................................................................................. 47 18.5测定步骤 .............................................................................................................................. 47 18.6方法原理 .............................................................................................................................. 47 18.7干扰及消除 .......................................................................................................................... 47 18.8方法的适用范围 .................................................................................................................. 47 18.9所需仪器 .............................................................................................................................. 48 18.10所需试剂(配制试剂用水均应为无氨水) ........................................................................ 48 18.11校准曲线的绘制 ................................................................................................................ 48 18.12分析步骤 ............................................................................................................................ 48 18.13结果计算 ............................................................................................................................ 49 19化学需氧量的测定操作规程（重铬酸钾法） .............................................................................. 49

19.1概述 ...................................................................................................................................... 49 19.2测定原理（干扰及其消除） .............................................................................................. 49 19.3方法的适用范围 .................................................................................................................. 49 19.4所需仪器 .............................................................................................................................. 50 19.5所需试剂 .............................................................................................................................. 50