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水質(zhì) 二氧化氯和亞氯酸鹽的測定連續(xù)滴定碘量法2

來源:本站發(fā)布時間：2018-10-16 18:31:36 瀏覽次數(shù):4575次

1 適用范圍

本標(biāo)準(zhǔn)規(guī)定了測定紡織染整工業(yè)廢水中二氧化氯和亞氯酸鹽的連續(xù)滴定碘量法。本標(biāo)準(zhǔn)適用于使用亞漂工藝的紡織染整工業(yè)排放廢水中二氧化氯和亞氯酸鹽的測定。當(dāng)取樣量為 150 ml時，二氧化氯的方法檢出限為 0.09 mg/L，測定下限為 0.36 mg/L；亞氯酸鹽（以亞氯酸根計）的方法檢出限為 0.08 mg/L，測定下限為 0.32 mg/L。

2.方法原理

二氧化氯和亞氯酸根在不同 pH值條件下，能氧化碘離子而析出碘。同一個樣品，在中性條件下，用硫代硫酸鈉溶液滴定二氧化氯與碘離子反應(yīng)轉(zhuǎn)化為亞氯酸鹽時析出的碘，再調(diào)節(jié)樣品 pH值為1～3，用硫代硫酸鈉溶液滴定亞氯酸鹽與碘離子反應(yīng)時析出的碘，通過連續(xù)滴定來測定二氧化氯和亞氯酸根含量。見反應(yīng)式（1）和反應(yīng)式（2）。

ClO2+I?→ClO2-+1/2I2 （1）

HClO2+4HI→2I2+HCl+2H2O （2）

3 干擾和消除

3.1 存在其它含氧氯化物，以及能與 I2 和I-發(fā)生氧化、還原反應(yīng)的物質(zhì)時，會產(chǎn)生干擾。

3.2 色度對滴定終點會產(chǎn)生干擾。水樣有色度時，應(yīng)取相同水樣做為滴定終點判斷的參比樣品。

4 試劑和材料

除非另有說明，分析時均使用符合國家標(biāo)準(zhǔn)的分析純化學(xué)試劑，實驗用水為蒸餾水或去離子水。

4.1 碘化鉀（KI）：晶體。

4.2 硫酸：ρ（H2SO4 ）=1.84 g/ml。

4.3 碘酸鉀（KIO3 ）：優(yōu)級純。使用前，應(yīng)于 105℃～110℃烘 2 h，置于干燥器內(nèi)冷卻至室溫，備用。

4.4 氫氧化鈉（NaOH）。

4.5 磷酸二氫鉀（KH2PO4 ·2H2O）。

4.6 磷酸氫二鈉（Na2HPO4 ·2H2O）。

4.7 硫代硫酸鈉（Na2S2O3·5H2O）。

4.8 無水碳酸鈉（Na2CO3 ）。

4.9 可溶性淀粉 [(C6H10O5 ) n ] 。

4.10 水楊酸（C7H6O3 ）。

4.11 氯化鋅（ZnCl 2 ）。

4.12 硫酸溶液：1+1（v/v），用硫酸（4.2）配制。

4.13 氫氧化鈉溶液：c（NaOH）=0.1 mol/L。

稱取 4 g氫氧化鈉（4.4）溶于少量水中，稀釋至 1000 ml。

4.14 緩沖溶液：pH=7。

稱取 34.0 g磷酸二氫鉀（4.5）和 35.5 g磷酸氫二鈉（4.6）于燒杯中，加水溶解后，稀釋至 1000 ml。

4.15 碘酸鉀標(biāo)準(zhǔn)溶液：c（1/6KIO3 ）=0.0500 mol/L。

稱取 1.7835 g（精確至 0.0001 g）碘酸鉀（4.3），用水溶解并定容至 1000 ml容量瓶，搖勻。貯存于棕色玻璃試劑瓶中，避光保存。

4.16 硫代硫酸鈉標(biāo)準(zhǔn)溶液：c（Na2S2O3 ）≈0.05 mol/L。

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[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.000243s SQL = SELECT `catid` FROM `fangfa_category` WHERE `catdir`='hangyebiaozhun' LIMIT 1
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[ 2024-08-19T05:23:05+08:00 ] NOTIC: [2048] Declaration of ContentModel::add() should be compatible with Model::add($data = '', $options = Array) ContentModel.class.php 第 587 行.
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[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.005669s SQL = SHOW COLUMNS FROM fangfa_content
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[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.000335s SQL = SELECT `cid` FROM `fangfa_content` WHERE ( `url` = '201810/6.html' ) AND ( `status` = 9 ) LIMIT 1
[ 2024-08-19T05:23:05+08:00 ] NOTIC: [8192] mysql_escape_string(): This function is deprecated; use mysql_real_escape_string() instead. DbMysql.class.php 第 400 行.
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.000334s SQL = SELECT * FROM `fangfa_content` WHERE ( `url` = '201810/6.html' ) LIMIT 1
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.005241s SQL = SHOW COLUMNS FROM fangfa_content_article
[ 2024-08-19T05:23:05+08:00 ] NOTIC: [8192] mysql_escape_string(): This function is deprecated; use mysql_real_escape_string() instead. DbMysql.class.php 第 400 行.
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.000260s SQL = SELECT * FROM `fangfa_content_article` WHERE ( `cid` = '6' ) LIMIT 1
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.005181s SQL = SHOW COLUMNS FROM fangfa_model_field
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.000364s SQL = SELECT `fieldid` FROM `fangfa_model_field` WHERE `status`='1' AND `modelid`='1'
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.003287s SQL = SHOW COLUMNS FROM fangfa_content_tag
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[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.000174s SQL = SELECT fangfa_tag.name FROM `fangfa_content_tag` LEFT JOIN fangfa_tag ON (fangfa_tag.tagid=fangfa_content_tag.tagid) WHERE ( fangfa_content_tag.keyid = 'c-6' ) ORDER BY fangfa_tag.tagid DESC
[ 2024-08-19T05:23:05+08:00 ] NOTIC: [2] Invalid argument supplied for foreach() ContentModel.class.php 第 448 行.
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[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.004827s SQL = SHOW COLUMNS FROM fangfa_comment
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.000170s SQL = SELECT COUNT(*) AS tp_count FROM `fangfa_comment` WHERE newsid =6 and status=1 LIMIT 1
[ 2024-08-19T05:23:05+08:00 ] NOTIC: [8] Undefined index: content FcontentAction.class.php 第 149 行.
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.000135s SQL = SELECT * FROM `fangfa_comment` WHERE newsid =6 and status=1 ORDER BY id DESC
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.004709s SQL = SHOW COLUMNS FROM fangfa_content
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.000402s SQL = SELECT * FROM `fangfa_content` WHERE ((`cid` > 6 and `sort`=1 ) or `sort`<1) and `status` = 9 and `catid`=22 ORDER BY sort desc,cid asc LIMIT 1
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.000333s SQL = SELECT * FROM `fangfa_content` WHERE ((`cid` < 6 and `sort`=1 )or `sort`>1) and `status` = 9 and `catid`=22 ORDER BY sort asc,cid DESC LIMIT 1
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.004944s SQL = SHOW COLUMNS FROM fangfa_content_count
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.000178s SQL = SELECT * FROM `fangfa_content_count` WHERE `cid` = 6 LIMIT 1
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.000199s SQL = UPDATE `fangfa_content_count` SET `hits`=4576 WHERE cid='6'
[ 2024-08-19T05:23:05+08:00 ] NOTIC: [2048] Declaration of RelationModel::_after_insert() should be compatible with Model::_after_insert($data, $options) RelationModel.class.php 第 415 行.
[ 2024-08-19T05:23:05+08:00 ] NOTIC: [2048] Declaration of CategoryModel::_after_insert() should be compatible with Model::_after_insert($data, $options) CategoryModel.class.php 第 15 行.
[ 2024-08-19T05:23:05+08:00 ] NOTIC: [2048] Declaration of CategoryModel::add() should be compatible with Model::add($data = '', $options = Array) CategoryModel.class.php 第 15 行.
[ 2024-08-19T05:23:05+08:00 ] NOTIC: [2048] Declaration of CategoryModel::save() should be compatible with Model::save($data = '', $options = Array) CategoryModel.class.php 第 15 行.
[ 2024-08-19T05:23:05+08:00 ] NOTIC: [2048] Declaration of CategoryModel::delete() should be compatible with Model::delete($options = Array) CategoryModel.class.php 第 15 行.
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.004303s SQL = SHOW COLUMNS FROM fangfa_category
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.000318s SQL = SELECT `catid` FROM `fangfa_category` WHERE ( `catid` IN (1,2,3,4,5,6,40) ) AND ( `isshow` = 1 ) ORDER BY `sort` ASC
[ 2024-08-19T05:23:05+08:00 ] NOTIC: [8] Undefined index: child %%62^622^622796EB%%article_view.html.php 第 46 行.
[ 2024-08-19T05:23:05+08:00 ] NOTIC: [8] Undefined index: child %%62^622^622796EB%%article_view.html.php 第 46 行.
[ 2024-08-19T05:23:05+08:00 ] NOTIC: [8] Undefined index: child %%62^622^622796EB%%article_view.html.php 第 46 行.
[ 2024-08-19T05:23:05+08:00 ] NOTIC: [2] Missing argument 1 for Ad::__construct(), called in D:\wamp\chyc\include\library\ThinkPHP\Common\functions.php on line 259 and defined Ad.class.php 第 40 行.
[ 2024-08-19T05:23:05+08:00 ] NOTIC: [2] Missing argument 2 for Ad::__construct(), called in D:\wamp\chyc\include\library\ThinkPHP\Common\functions.php on line 259 and defined Ad.class.php 第 40 行.
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[ 2024-08-19T05:23:05+08:00 ] NOTIC: [2] Invalid argument supplied for foreach() function.ffcategory.php 第 84 行.
[ 2024-08-19T05:23:05+08:00 ] NOTIC: [8] Undefined variable: pagesize function.fflink.php 第 26 行.
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.005132s SQL = SHOW COLUMNS FROM fangfa_friendlink
[ 2024-08-19T05:23:05+08:00 ] SQL: RunTime:0.000231s SQL = SELECT * FROM `fangfa_friendlink` WHERE ( `status` = 1 ) ORDER BY created DESC
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[70] => D:\wamp\chyc\include\tag\function.ffgetpage.php
[71] => D:\wamp\chyc\include\tag\function.ffad.php
[72] => D:\wamp\chyc\include\tag\function.ffset.php
[73] => D:\wamp\chyc\include\Smarty\internals\core.get_include_path.php
[74] => D:\wamp\chyc\data\front\runtime\templates_c\%%0C^0C5^0C52E3C7%%header.html.php
[75] => D:\wamp\chyc\admin\Lib\Model\CategoryModel.class.php
[76] => D:\wamp\chyc\include\library\ThinkPHP\Lib\Think\Core\Model\RelationModel.class.php
[77] => D:\wamp\chyc\data\cache\category_1.php
[78] => D:\wamp\chyc\data\cache\category_2.php
[79] => D:\wamp\chyc\data\cache\category_3.php
[80] => D:\wamp\chyc\data\cache\category_4.php
[81] => D:\wamp\chyc\data\cache\category_5.php
[82] => D:\wamp\chyc\data\cache\category_6.php
[83] => D:\wamp\chyc\data\cache\category_40.php
[84] => D:\wamp\chyc\data\cache\category_20.php
[85] => D:\wamp\chyc\data\cache\category_26.php
[86] => D:\wamp\chyc\data\ads\ad_1.php
[87] => D:\wamp\chyc\include\Ad.class.php
[88] => D:\wamp\chyc\data\front\runtime\templates_c\%%FD^FD7^FD7FB2B1%%footer.html.php
[89] => D:\wamp\chyc\include\tag\function.fflink.php

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