火力发电厂水汽分析方法

jicopen · 发表于 2007-10-19 14:02:03

5 氢氧化钠溶液（2mol/L）见联氨的测定（GB/T 6906—86）6 优级纯浓盐酸：比重1.19 7 铜标准溶液（0.1mg/ml）称取<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue=".1" unitname="g">0.1000g</chmetcnv>铜（铜含量99.9%以上），溶于20ml硝酸溶液（1+1）中，煮沸除去氮的氧化物，冷却后注入<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="1" unitname="l">1L</chmetcnv>容量瓶中，用无硅水稀释至刻度。8 铜工作溶液（1μg/mL）吸取10ml铜标准溶液注入<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="1" unitname="l">1L</chmetcnv>容量瓶中，加20ml硝酸溶液（1+1），用无硅水稀释至刻度。  <div align="center"><table class="MsoNormalTable" cellspacing="0" cellpadding="0" border="1" style="BORDER-RIGHT: medium none; BORDER-TOP: medium none; BORDER-LEFT: medium none; BORDER-BOTTOM: medium none; BORDER-COLLAPSE: collapse; mso-table-layout-alt: fixed; mso-padding-alt: 0cm 5.4pt 0cm 5.4pt; mso-border-alt: solid windowtext .5pt; mso-border-insideh: .5pt solid windowtext; mso-border-insidev: .5pt solid windowtext;"><tbody><tr style="HEIGHT: 28.55pt; mso-yfti-irow: 0; mso-yfti-firstrow: yes; mso-yfti-lastrow: yes;"><td width="144" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: windowtext 1pt solid; WIDTH: 108.35pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 28.55pt; BACKGROUND-COLOR: transparent; mso-border-alt: solid windowtext .5pt;">GB/T 6906-86</td><td width="283" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 212.3pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 28.55pt; BACKGROUND-COLOR: transparent; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">  联
氨
的
测
定（比色法）</td></tr></tbody></table></div> 1 硫酸溶液[C(1/2H2SO4)=2mol/L]吸取56ml浓硫酸（比重1.84）缓缓注入500～700ml蒸馏水中，冷却后稀释至1000ml。2 1%淀粉指示剂称取<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="1" unitname="g">1.0g</chmetcnv>可溶性淀粉置于玛瑙研钵中，加入少许试剂水研磨成糊状物，徐徐注入100ml煮沸的试剂水中，再继续煮沸5min，放置取上层清液使用。此溶液应使用前配制。 3 硫代硫酸钠标准溶液[ C(Na2S2O3)= 0.1mol/L]3.1 配制称取<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="26" unitname="g">26g</chmetcnv>硫代硫酸钠（Na2S2O3·5H2O）或<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="16" unitname="g">16g</chmetcnv>无水硫代硫酸钠（Na2S2O3），溶于<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="1" unitname="l">1L</chmetcnv>已煮沸并冷却的试剂水中。将溶液储存于具有磨口塞的棕色试剂瓶中，放置一周后过滤备用。3.2 标定<chsdate wst="on" isrocdate="False" islunardate="False" day="30" month="12" year="1899">3.2.1</chsdate>
以重铬酸钾作基准标定称取于<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="120" unitname="℃">120℃</chmetcnv>烘至恒重的基准重铬酸钾<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue=".15" unitname="g">0.15g</chmetcnv>（称准至<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue=".0002" unitname="g">0.0002g</chmetcnv>）。置于碘量瓶中，加入25ml试剂水溶液，加<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="2" unitname="g">2g</chmetcnv>碘化钾及2mol/L硫酸溶液20ml混匀。于暗处放置10min，加150ml试剂水，用0.1ml/L硫代硫酸钠溶液滴定，到溶液呈淡黄色时，加1%淀粉指示剂1mL，继续滴定至溶液由蓝色变成亮绿色。同时做空白试验。硫代硫酸钠标准溶液物质的量浓度C，按式（1）计算：<span style="

OSITION: relative; TOP: 15pt; mso-text-raise: -15.0pt;"><shapetype id="_x0000_t75" coordsize="21600,21600" path="m@4@5l@4@11@9@11@9@5xe" filled="f" stroked="f" opreferrelative="t" ospt="75"><stroke joinstyle="miter"></stroke><formulas><f eqn="if lineDrawn pixelLineWidth 0"></f><f eqn="sum @0 1 0"></f><f eqn="sum 0 0 @1"></f><f eqn="prod @2 1 2"></f><f eqn="prod @3 21600 pixelWidth"></f><f eqn="prod @3 21600 pixelHeight"></f><f eqn="sum @0 0 1"></f><f eqn="prod @6 1 2"></f><f eqn="prod @7 21600 pixelWidth"></f><f eqn="sum @8 21600 0"></f><f eqn="prod @7 21600 pixelHeight"></f><f eqn="sum @10 21600 0"></f></formulas><path gradientshapeok="t" oconnecttype="rect" oextrusionok="f"></path><lock aspectratio="t" vext="edit"></lock></shapetype><shape id="_x0000_i1025" type="#_x0000_t75" oole="" style="WIDTH: 117pt; HEIGHT: 33.75pt;"><imagedata src="file:///C:\DOCUME~1\电力科技\LOCALS~1\Temp\msohtml1\01\clip_image001.wmz" otitle=""></imagedata></shape>    （1）式中：G——重铬酸钾的重量，g；　　  V1——标定时消耗硫代硫酸钠溶液的体积，ml；　　  V2——空白实验消耗硫代硫酸钠溶液的体积，ml；0.04903——重铬酸钾（1/6K2Cr2O7）的摩尔质量，g/mmol。  <chsdate wst="on" isrocdate="False" islunardate="False" day="30" month="12" year="1899">3.2.2</chsdate>
用碘标准溶液标定取20.00mlC(1/2I2)=0.1mol/L碘标准溶液，注入碘量瓶中，加150ml蒸馏水，用0.1mol/L硫代硫酸钠溶液滴定，溶液呈淡黄色时，加1ml1%淀粉指示剂，继续滴定至溶液蓝色消失。同时作空白试验：取150ml蒸馏水，加0.05ml碘标准溶液，1ml1%淀粉指示剂，用0.1mol/L硫代硫酸钠溶液滴定至溶液蓝色消失。硫代硫酸钠溶液的物质的量浓度C按下式计算：<span style="

OSITION: relative; TOP: 14pt; mso-text-raise: -14.0pt;"><shape id="_x0000_i1026" type="#_x0000_t75" oole="" style="WIDTH: 84.75pt; HEIGHT: 33.75pt;"><imagedata src="file:///C:\DOCUME~1\电力科技\LOCALS~1\Temp\msohtml1\01\clip_image003.wmz" otitle=""></imagedata></shape>式中：V
——碘标准溶液的体积，ml；   0.05
——空白试验加入碘标准溶液的体积，ml；　　  c1——碘标准溶液的物质的量浓度，mol/L；　　  a
——滴定消耗硫代硫酸钠溶液的体积，ml；b
——空白试验消耗硫代硫酸钠溶液的体积，ml。 4 碘标准溶液[C(1/2I2)=0.1mol/L]4.1 配制称取<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="13" unitname="g">13g</chmetcnv>碘及<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="35" unitname="g">35g</chmetcnv>碘化钾，溶于少量试剂水中，待全部溶解后，用Ⅰ级试剂水稀释至1000ml混匀。贮存于具有磨口的棕色瓶中。4.2 标定（用0.1mol/L硫代硫酸钠标准溶液）标定方法按<chsdate wst="on" isrocdate="False" islunardate="False" day="30" month="12" year="1899">4.2.2</chsdate>用C(1/2I2)=0.1mol/L碘标准溶液标定硫代硫酸钠方法进行。5 盐酸溶液（1+99）6 氢氧化钠溶液[C(NaOH)=2mol/L]称取分析纯氢氧化钠<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="40" unitname="g">40g</chmetcnv>，以约400ml无硅水溶解，待冷却后用无硅水定容至500ml。7 1%酚酞指示剂（乙醇溶液）；见氯根的测定（GB/T 6905.1—86）8 对二甲氨基苯甲醛-硫酸溶液量取100ml浓硫酸，在不断搅拌下徐徐加入已有300ml试剂水的烧杯中冷却后，加入<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="15" unitname="克">15克</chmetcnv>对二甲氨基苯甲醛，待完全溶解后移入500ml容量瓶，用试剂水稀释至刻度，贮存于棕色瓶中放置在暗处。（※每换新试剂，必须重新绘制工作曲线） 9 联氨标准溶液（0.1mg/ml）

jicopen · 发表于 2007-10-19 14:04:00

9 联氨标准溶液（0.1mg/ml）9.1 配制称取<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue=".41" unitname="g">0.410g</chmetcnv>硫酸联氨（N2H4·H2SO4）或<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue=".328" unitname="g">0.328g</chmetcnv>盐酸联氨，溶于已加有74ml浓盐酸的500mlⅠ级试剂水中，转入<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="1" unitname="l">1L</chmetcnv>容量瓶中，用Ⅰ级试剂水稀释至刻度（此溶液为联氨储备液）。9.2 标定量取20.2ml储备液，用试剂水稀释至100ml，用2mol/L氢氧化钠溶液滴定至酚酞终点，记录消耗氢氧化钠溶液的体积A ml。再取20.0ml储备液，注入250ml具有磨口塞的锥型瓶中，用Ⅰ级试剂水稀释至100ml，加入（A+2）ml 2mol/L氢氧化钠溶液，用棕色滴定管精确加入10ml0.1mol/L碘标准溶液，充分混匀，置暗处3min。加入1mol/L硫酸溶液2.5ml用0.1mol/L硫代硫酸钠标准溶液滴定过剩的碘。接近终点时（滴定至溶液呈淡黄色），加入1ml1%淀粉指示剂，继续滴定至蓝色消失，记录硫代硫酸钠标准溶液消耗量，并同时进行空白实验。储备液的联氨浓度（N2H4,μg/L）按式（2）计算：<span style="

OSITION: relative; TOP: 12pt; mso-text-raise: -12.0pt;"><shapetype id="_x0000_t75" coordsize="21600,21600" path="m@4@5l@4@11@9@11@9@5xe" filled="f" stroked="f" opreferrelative="t" ospt="75"><stroke joinstyle="miter"></stroke><formulas><f eqn="if lineDrawn pixelLineWidth 0"></f><f eqn="sum @0 1 0"></f><f eqn="sum 0 0 @1"></f><f eqn="prod @2 1 2"></f><f eqn="prod @3 21600 pixelWidth"></f><f eqn="prod @3 21600 pixelHeight"></f><f eqn="sum @0 0 1"></f><f eqn="prod @6 1 2"></f><f eqn="prod @7 21600 pixelWidth"></f><f eqn="sum @8 21600 0"></f><f eqn="prod @7 21600 pixelHeight"></f><f eqn="sum @10 21600 0"></f></formulas><path gradientshapeok="t" oconnecttype="rect" oextrusionok="f"></path><lock aspectratio="t" vext="edit"></lock></shapetype><shape id="_x0000_i1025" type="#_x0000_t75" oole="" style="WIDTH: 104.25pt; HEIGHT: 30.75pt;"><imagedata src="file:///C:\DOCUME~1\电力科技\LOCALS~1\Temp\msohtml1\01\clip_image001.wmz" otitle=""></imagedata></shape>     （2）式中：b——空白实验消耗硫代硫酸钠标准溶液的体积，ml；      a——标定联氨溶液消耗硫代硫酸钠标准溶液的体积，ml；      c——硫代硫酸钠标准溶液的物质的量浓度，mol/L；      V——联氨标准溶液的体积，ml；      8——联氨的（1/4N2H4）的摩尔质量，g/mol。 10 联氨工作溶液（1μg/ml）根据贮备液的浓度，取适量溶液，用盐酸溶液（1+99）稀释100倍。11 联氨工作溶液（10μg/L）移取联氨标准溶液（0.1mg/ml）10ml于1000ml容量瓶中，定容。再从容量瓶中移取10ml溶液于另一1000ml容量瓶中，定容。12 联氨工作溶液（100μg/L）移取联氨标准溶液（0.1mg/ml）10ml于1000ml容量瓶中，定容。再从容量瓶中移取100ml溶液于另一1000ml容量瓶中，定容。   <div align="center"><table class="MsoNormalTable" cellspacing="0" cellpadding="0" border="1" style="BORDER-RIGHT: medium none; BORDER-TOP: medium none; BORDER-LEFT: medium none; BORDER-BOTTOM: medium none; BORDER-COLLAPSE: collapse; mso-table-layout-alt: fixed; mso-padding-alt: 0cm 5.4pt 0cm 5.4pt; mso-border-alt: solid windowtext .5pt; mso-border-insideh: .5pt solid windowtext; mso-border-insidev: .5pt solid windowtext;"><tbody><tr style="HEIGHT: 28.55pt; mso-yfti-irow: 0; mso-yfti-firstrow: yes; mso-yfti-lastrow: yes;"><td width="144" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: windowtext 1pt solid; WIDTH: 108.35pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 28.55pt; BACKGROUND-COLOR: transparent; mso-border-alt: solid windowtext .5pt;">GB/T 14424-93</td><td width="283" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 212.3pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 28.55pt; BACKGROUND-COLOR: transparent; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">余  氯  的  测  定
（邻联甲苯胺目视比色法）</td></tr></tbody></table></div> 1 邻联甲苯胺溶液将<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue=".14" unitname="g">0.14g</chmetcnv>邻联甲苯胺二酸盐（3,3-二氯酸二甲基联苯胺）溶于50ml除盐水中，边搅拌边加到50ml盐酸（3+7）中。装入褐色瓶中保存。时间不超过6个月。 1        磷酸盐缓冲贮备液（0.5mol/L）将无水磷酸氢二钠放在105～110℃烘箱内烘2h，取出置于干燥器内冷却至室温，称取<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="22.86" unitname="g">22.86g</chmetcnv>；另将磷酸二氢钾放在105～110℃烘箱内同样处理，并称取<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="46.14" unitname="g">46.14g</chmetcnv>，将上述两种试剂共同溶于除盐水中，稀释至<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="1" unitname="l">1L</chmetcnv>。2        磷酸盐缓冲工作液（0.1mol/L）取上述磷酸盐缓冲贮备液200ml加除盐水稀释至<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="1" unitname="l">1L</chmetcnv>。3        重铬酸钾-铬酸钾溶液称取<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="4.65" unitname="g">4.65g</chmetcnv>铬酸钾和<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="1.55" unitname="g">1.55g</chmetcnv>重铬酸钾溶于磷酸盐缓冲工作液中（

H6.5），移到<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="1" unitname="l">1L</chmetcnv>容量瓶中，加磷酸盐缓冲工作液稀释至刻度。4        亚砷酸钠溶液称取0.5亚砷酸钠溶于除盐水中，稀释至100ml。6 永久性剩余氯标准色溶液（1.0～10.0ml）按表25所示的比例分别准确移取重铬酸钾-铬酸钾溶液以及磷酸盐缓冲工作液于100ml具塞比色管中，混匀。表46<div align="center"><table class="MsoNormalTable" cellspacing="0" cellpadding="0" border="1" style="BORDER-RIGHT: medium none; BORDER-TOP: medium none; BORDER-LEFT: medium none; BORDER-BOTTOM: medium none; BORDER-COLLAPSE: collapse; mso-table-layout-alt: fixed; mso-yfti-tbllook: 480; mso-padding-alt: 0cm 5.4pt 0cm 5.4pt; mso-border-alt: solid windowtext .5pt; mso-border-insideh: .5pt solid windowtext; mso-border-insidev: .5pt solid windowtext;"><tbody><tr style="HEIGHT: 30.5pt; mso-yfti-irow: 0; mso-yfti-firstrow: yes; page-break-inside: avoid;"><td width="156" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1.5pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 116.9pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 30.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext 1.5pt; mso-border-bottom-alt: solid windowtext .5pt; mso-border-right-alt: solid windowtext .5pt;">余氯浓度/mg/L</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1.5pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 30.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">0.10</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1.5pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 30.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">0.20</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1.5pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 30.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">0.30</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1.5pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 30.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">0.40</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1.5pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 30.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">0.50</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1.5pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 30.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">0.60</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1.5pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 30.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">0.70</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1.5pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 30.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">0.80</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1.5pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 30.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">0.90</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1.5pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 30.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">1.00</td></tr><tr style="HEIGHT: 15.6pt; mso-yfti-irow: 1; page-break-inside: avoid;"><td width="156" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 116.9pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext .5pt; mso-border-right-alt: solid windowtext .5pt;">重铬酸钾-铬酸钾溶液/ml</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">1.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">2.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">3.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">4.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">5.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">6.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">7.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">8.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">9.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">10.0</td></tr><tr style="HEIGHT: 15.6pt; mso-yfti-irow: 2; mso-yfti-lastrow: yes; page-break-inside: avoid;"><td width="156" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 116.9pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1.5pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext 1.5pt; mso-border-right-alt: solid windowtext .5pt;">磷酸盐缓冲工作液（

H6.5）/ml</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1.5pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">99.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1.5pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">98.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1.5pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">97.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1.5pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">96.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1.5pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">95.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1.5pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">94.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1.5pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">93.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1.5pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">92.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1.5pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">91.0</td><td width="42" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 31.8pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1.5pt solid; HEIGHT: 15.6pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext 1.5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">90.0</td></tr></tbody></table></div>注：余氯标准比色溶液保存在暗处，当产生沉淀时就不能使用。  <div align="center"><table class="MsoNormalTable" cellspacing="0" cellpadding="0" border="1" style="BORDER-RIGHT: medium none; BORDER-TOP: medium none; BORDER-LEFT: medium none; BORDER-BOTTOM: medium none; BORDER-COLLAPSE: collapse; mso-table-layout-alt: fixed; mso-padding-alt: 0cm 5.4pt 0cm 5.4pt; mso-border-alt: solid windowtext .5pt; mso-border-insideh: .5pt solid windowtext; mso-border-insidev: .5pt solid windowtext;"><tbody><tr style="HEIGHT: 28.55pt; mso-yfti-irow: 0; mso-yfti-firstrow: yes; mso-yfti-lastrow: yes;"><td width="144" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: windowtext 1pt solid; WIDTH: 108.35pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 28.55pt; BACKGROUND-COLOR: transparent; mso-border-alt: solid windowtext .5pt;">SS-<chsdate wst="on" isrocdate="False" islunardate="False" day="18" month="1" year="1984">18-1-84</chsdate></td><td width="283" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 212.3pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 28.55pt; BACKGROUND-COLOR: transparent; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">化学耗氧量的测定（重铬酸钾法）</td></tr></tbody></table></div> 1 硫酸银-硫酸溶液称取<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="11" unitname="g">11g</chmetcnv>硫酸银溶于<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="1" unitname="l">1L</chmetcnv>浓硫酸中。2 邻菲罗啉—亚铁溶液（试亚铁灵指示剂）称取<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="1.48" unitname="g">1.48g</chmetcnv>邻菲罗啉与<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue=".7" unitname="g">0.70g</chmetcnv>硫酸亚铁（FeSO4·7H2O），溶于100ml二次蒸馏水中。 3 重铬酸钾标准溶液[ C(1/6K2Cr2O7)= 0.025mol/L]将重铬酸钾（K2Cr2O7）基准试剂在玛瑙研钵中研碎，于100～110℃的烘箱内干燥3～4h，取出放在干燥器中冷却至室温，称取<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="1.226" unitname="g">1.226g</chmetcnv>，用少量高纯水溶解后，移入<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="1" unitname="l">1L</chmetcnv>容量瓶中并稀释至刻度。 4 硫酸亚铁铵标准溶液  C[FeSO4·(NH4)2SO4·6H2O]= 0.025mol/L4.1 配制称取<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="10" unitname="g">10g</chmetcnv>硫酸亚铁铵[FeSO4·(NH4)2SO4·6H2O]溶于500ml煮沸后冷却的二次蒸馏水中，加20ml浓硫酸，冷却后，加二次蒸馏水稀释到<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="1" unitname="l">1L</chmetcnv>。4.2 标定取重铬酸钾标准溶液20ml注入250ml三角瓶中，加二次蒸馏水稀释至100ml，加30ml浓硫酸，冷却后，加邻菲罗啉-亚铁溶液2-3滴，用硫酸亚铁铵溶液滴定，溶液从蓝绿色变为红棕色即为终点。记录硫酸亚铁铵溶液消耗的体积（ml）。硫酸亚铁铵标准溶液的物质的量浓度mol/L按下式（1）计算：<span style="

OSITION: relative; TOP: 12pt; mso-text-raise: -12.0pt;"><shape id="_x0000_i1026" type="#_x0000_t75" oole="" style="WIDTH: 47.25pt; HEIGHT: 30.75pt;"><imagedata src="file:///C:\DOCUME~1\电力科技\LOCALS~1\Temp\msohtml1\01\clip_image003.wmz" otitle=""></imagedata></shape>       （1）式中： n——重铬酸钾标准溶液的体积，ml；　　　 a——重铬酸钾标准溶液物质的量浓度,mol/L；       b——标定时，消耗硫酸亚铁铵标准溶液的体积，ml；<div align="center"><table class="MsoNormalTable" cellspacing="0" cellpadding="0" border="1" style="BORDER-RIGHT: medium none; BORDER-TOP: medium none; BORDER-LEFT: medium none; BORDER-BOTTOM: medium none; BORDER-COLLAPSE: collapse; mso-table-layout-alt: fixed; mso-padding-alt: 0cm 5.4pt 0cm 5.4pt; mso-border-alt: solid windowtext .5pt; mso-border-insideh: .5pt solid windowtext; mso-border-insidev: .5pt solid windowtext;"><tbody><tr style="HEIGHT: 28.55pt; mso-yfti-irow: 0; mso-yfti-firstrow: yes; mso-yfti-lastrow: yes;"><td width="144" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: windowtext 1pt solid; WIDTH: 108.35pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 28.55pt; BACKGROUND-COLOR: transparent; mso-border-alt: solid windowtext .5pt;">SS-<chsdate wst="on" isrocdate="False" islunardate="False" day="18" month="2" year="1984">18-2-84</chsdate></td><td width="283" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 212.3pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 28.55pt; BACKGROUND-COLOR: transparent; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">化学耗氧量的测定（高锰酸钾法）</td></tr></tbody></table></div> 1 硫代硫酸钠标准溶液[C(Na2S2O5)=0.1mol/L]2 硫酸[c(1/2H2SO4)=4mol/L]3 1%淀粉指示剂见联氨的测定（GB/T 6906—86）

jicopen · 发表于 2007-10-19 14:04:56

4 高锰酸钾标准溶液[1/5KMnO4 = 0.1mol/L]4.1 配制称取<chmetcnv wst="on" unitname="g" sourcevalue="3.3" hasspace="False" negative="False" numbertype="1" tcsc="0"></chmetcnv>3.3g<chmetcnv></chmetcnv>高锰酸钾溶于1050ml蒸馏水中，缓慢煮沸15～20min，冷却后于暗处密闭保存两周，以“4号”玻璃过滤器过滤，滤液贮存于具有磨口塞的棕色瓶中。4.2 标定<chsdate year="1899" month="12" day="30" islunardate="False" isrocdate="False" wst="on"></chsdate>4.2.1<chsdate></chsdate>    以草酸钠作基准标定称取于105～110℃烘至恒重的基准草酸钠<chmetcnv wst="on" unitname="g" sourcevalue=".2" hasspace="False" negative="False" numbertype="1" tcsc="0"></chmetcnv>0.2g<chmetcnv></chmetcnv>（准确至0.2mg），溶于100ml蒸馏水中，加8ml浓硫酸，用50ml滴定管以高锰酸钾溶液滴定，近终点时，加热至<chmetcnv wst="on" unitname="℃" sourcevalue="65" hasspace="False" negative="False" numbertype="1" tcsc="0"></chmetcnv>65℃<chmetcnv></chmetcnv>，继续滴定至溶液所呈粉红色保持35s。同时做空白实验。　　高锰酸钾标准溶液物质的量浓度（c）按下式计算：<span style="

OSITION: relative; TOP: 14pt; mso-text-raise: -14.0pt;"><shapetype id="_x0000_t75" coordsize="21600,21600" ospt="75" opreferrelative="t" path="m@4@5l@4@11@9@11@9@5xe" filled="f" stroked="f"></shapetype><stroke joinstyle="miter"></stroke><stroke></stroke><formulas></formulas><f eqn="if lineDrawn pixelLineWidth 0"></f><f></f><f eqn="sum @0 1 0"></f><f></f><f eqn="sum 0 0 @1"></f><f></f><f eqn="prod @2 1 2"></f><f></f><f eqn="prod @3 21600 pixelWidth"></f><f></f><f eqn="prod @3 21600 pixelHeight"></f><f></f><f eqn="sum @0 0 1"></f><f></f><f eqn="prod @6 1 2"></f><f></f><f eqn="prod @7 21600 pixelWidth"></f><f></f><f eqn="sum @8 21600 0"></f><f></f><f eqn="prod @7 21600 pixelHeight"></f><f></f><f eqn="sum @10 21600 0"></f><f></f><formulas></formulas><path oextrusionok="f" gradientshapeok="t" oconnecttype="rect"></path><path></path><lock aspectratio="t" vext="edit"></lock><lock></lock><shapetype></shapetype><shape id="_x0000_i1025" type="#_x0000_t75" oole="" style="WIDTH: 105pt; HEIGHT: 33pt;"></shape><imagedata src="file:///C:\DOCUME~1\电力科技\LOCALS~1\Temp\msohtml1\01\clip_image001.wmz" otitle=""></imagedata><imagedata></imagedata><shape></shape>式中： G——草酸钠的质量，g；　　   a——标定时消耗高锰酸钾的体积，ml；　　   b——空白实验时消耗高锰酸钾溶液的体积,ml；　　   0.06700——草酸钠（Na<chmetcnv wst="on" unitname="C" sourcevalue="2" hasspace="False" negative="False" numbertype="1" tcsc="0"></chmetcnv>2C<chmetcnv></chmetcnv>2O4）的摩尔质量,g/mmol。  <chsdate year="1899" month="12" day="30" islunardate="False" isrocdate="False" wst="on"></chsdate>4.2.2<chsdate></chsdate>    用0.1mol/L硫代硫酸钠标准溶液标定取20.00ml待标定的高锰酸钾溶液，加<chmetcnv wst="on" unitname="g" sourcevalue="2" hasspace="False" negative="False" numbertype="1" tcsc="0"></chmetcnv>2g<chmetcnv></chmetcnv>碘化钾及20ml[c(1/2H2SO4)=4mol/L]硫酸，摇匀，于暗处放置5min。加150ml蒸馏水，用0.1mol/L硫代硫酸钠标准溶液滴定，滴到溶液呈淡黄色时，加1ml1.0%淀粉指示剂，继续滴定至溶液蓝色消失。高锰酸钾标准溶液的物质的量浓度（c）按下式计算：<span style="

OSITION: relative; TOP: 12pt; mso-text-raise: -12.0pt;"><shape id="_x0000_i1026" type="#_x0000_t75" oole="" style="WIDTH: 45.75pt; HEIGHT: 30.75pt;"></shape><imagedata src="file:///C:\DOCUME~1\电力科技\LOCALS~1\Temp\msohtml1\01\clip_image003.wmz" otitle=""></imagedata><imagedata></imagedata><shape></shape>式中： a——消耗硫代硫酸钠标准溶液的体积，ml：　　   b——硫代硫酸钠标准溶液的物质的量浓度，mol/L；　　   V——高锰酸钾溶液的体积，ml。  5 高锰酸钾标准溶液[1/5KMnO4 = 0.01mol/L]取0.1mol/L高锰酸钾标准溶液，用煮沸后冷却的二次蒸馏水稀释至10倍制得。其浓度不需标定，由计算得出。　　注：① 0.01mol/L高锰酸钾标准溶液的浓度容易改变，应在使用时配制。　　    ② 0.1mol/L高锰酸钾标准溶液的当量浓度，需定期进行标定。  <div align="center"><table class="MsoNormalTable" cellspacing="0" cellpadding="0" border="1" style="BORDER-RIGHT: medium none; BORDER-TOP: medium none; BORDER-LEFT: medium none; BORDER-BOTTOM: medium none; BORDER-COLLAPSE: collapse; mso-table-layout-alt: fixed; mso-padding-alt: 0cm 5.4pt 0cm 5.4pt; mso-border-alt: solid windowtext .5pt; mso-border-insideh: .5pt solid windowtext; mso-border-insidev: .5pt solid windowtext;"><tbody><tr style="HEIGHT: 28.55pt; mso-yfti-irow: 0; mso-yfti-firstrow: yes; mso-yfti-lastrow: yes;"><td width="144" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: windowtext 1pt solid; WIDTH: 108.35pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 28.55pt; BACKGROUND-COLOR: transparent; mso-border-alt: solid windowtext .5pt;">SS-<chsdate year="1984" month="12" day="2" islunardate="False" isrocdate="False" wst="on"></chsdate>12-2-84<chsdate></chsdate></td><td width="283" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 212.3pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 28.55pt; BACKGROUND-COLOR: transparent; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">溶解氧的测定（靛蓝二磺酸钠比色法）</td></tr></tbody></table></div>  1 靛蓝二磺酸钠贮备液    称取<chmetcnv wst="on" unitname="g" sourcevalue=".18" hasspace="False" negative="False" numbertype="1" tcsc="0"></chmetcnv>0.18g<chmetcnv></chmetcnv>靛蓝二磺酸钠（按含量100%计算），加数滴水润湿后加0.5ml浓硫酸，在沸水浴上加热30min，冷却后用水溶解并稀释至50ml。2 葡萄糖贮备液称取<chmetcnv wst="on" unitname="g" sourcevalue="1" hasspace="False" negative="False" numbertype="1" tcsc="0"></chmetcnv>1.0g<chmetcnv></chmetcnv>葡萄糖溶于少量水中，并稀释至50ml。此溶液应保持在低于<chmetcnv wst="on" unitname="℃" sourcevalue="10" hasspace="False" negative="False" numbertype="1" tcsc="0"></chmetcnv>10℃<chmetcnv></chmetcnv>的冰箱中，或者使用时配制。3 氢氧化钾溶液称取<chmetcnv wst="on" unitname="g" sourcevalue="64.6" hasspace="False" negative="False" numbertype="1" tcsc="0"></chmetcnv>64.6g<chmetcnv></chmetcnv>氢氧化钾溶于100ml水中。注：由于氢氧化钾含量仅为82%左右，按含量100%折算<chmetcnv wst="on" unitname="g" sourcevalue="53" hasspace="False" negative="False" numbertype="1" tcsc="0"></chmetcnv>53g<chmetcnv></chmetcnv>氢氧化钾应称取<chmetcnv wst="on" unitname="g" sourcevalue="64.4" hasspace="False" negative="False" numbertype="1" tcsc="0"></chmetcnv>64.4g<chmetcnv></chmetcnv>。

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7 蓝色标准液称取<chmetcnv wst="on" unitname="g" sourcevalue="62.45" hasspace="False" negative="False" numbertype="1" tcsc="0"></chmetcnv>62.45g<chmetcnv></chmetcnv>硫酸铜（CuSO4·5H2O）用1%盐酸溶解，并用1%盐酸稀释至<chmetcnv wst="on" unitname="l" sourcevalue="1" hasspace="False" negative="False" numbertype="1" tcsc="0"></chmetcnv>1L<chmetcnv></chmetcnv>，过滤。8 标准色阶的配制取一组250ml专用溶氧瓶，每瓶中加入1.0ml浓盐酸，分别按表26加入个假色标准液，然后用蒸馏水装满，充分摇匀，并用蜡密封。此标准液如贮存在暗处，可用1个月。                                 标准色阶的配制                              表47<div align="center"><table class="MsoNormalTable" cellspacing="0" cellpadding="0" border="1" style="BORDER-RIGHT: medium none; BORDER-TOP: medium none; BORDER-LEFT: medium none; BORDER-BOTTOM: medium none; BORDER-COLLAPSE: collapse; mso-table-layout-alt: fixed; mso-padding-alt: 0cm 5.4pt 0cm 5.4pt; mso-border-alt: solid windowtext .5pt; mso-border-insideh: .5pt solid windowtext; mso-border-insidev: .5pt solid windowtext;"><tbody><tr style="HEIGHT: 16.1pt; mso-yfti-irow: 0; mso-yfti-firstrow: yes; page-break-inside: avoid;"><td width="98" rowspan="2" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 73.85pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 16.1pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext .5pt; mso-border-right-alt: solid windowtext .5pt;">瓶号</td><td width="108" rowspan="2" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 81pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 16.1pt; BACKGROUND-COLOR: transparent; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">溶解氧含量μg/L</td><td width="264" colspan="3" style="BORDER-RIGHT: #ece9d8; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 198pt; PADDING-TOP: 0cm; BORDER-BOTTOM: #ece9d8; HEIGHT: 16.1pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt;">配制溶液的加入体积，ml</td><td width="96" rowspan="2" style="BORDER-RIGHT: #ece9d8; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: windowtext 1pt solid; WIDTH: 72.15pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 16.1pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt;">溶液颜色</td></tr><tr style="HEIGHT: 14.75pt; mso-yfti-irow: 1; page-break-inside: avoid;"><td valign="top" width="88" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: windowtext 1pt solid; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 66pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 14.75pt; BACKGROUND-COLOR: transparent; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">黄色溶液</td><td valign="top" width="88" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 66pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 14.75pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">红色溶液</td><td width="88" style="BORDER-RIGHT: #ece9d8; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 66pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 14.75pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt;">蓝色溶液</td></tr><tr style="HEIGHT: 15.5pt; mso-yfti-irow: 2; mso-yfti-lastrow: yes;"><td width="98" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 73.85pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext .5pt; mso-border-right-alt: solid windowtext .5pt;">1234567891011121314</td><td valign="top" width="108" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 81pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">051015202530354050607080100</td><td width="88" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 66pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">26.2515.009.407.504.203.002.602.201.801.200.800.400.200.00</td><td width="88" style="BORDER-RIGHT: windowtext 1pt solid; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 66pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt; mso-border-alt: solid windowtext .5pt;">0.563.754.707.059.6010.8011.2011.4011.8013.6016.6019.8022.0022.40</td><td width="88" style="BORDER-RIGHT: #ece9d8; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: #ece9d8; WIDTH: 66pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt;">～～～～～～～1.001.606.0012.6016.4020.0034.00</td><td width="96" style="BORDER-RIGHT: #ece9d8; PADDING-RIGHT: 5.4pt; BORDER-TOP: #ece9d8; PADDING-LEFT: 5.4pt; PADDING-BOTTOM: 0cm; BORDER-LEFT: windowtext 1pt solid; WIDTH: 72.15pt; PADDING-TOP: 0cm; BORDER-BOTTOM: windowtext 1pt solid; HEIGHT: 15.5pt; BACKGROUND-COLOR: transparent; mso-border-top-alt: solid windowtext .5pt; mso-border-bottom-alt: solid windowtext .5pt; mso-border-left-alt: solid windowtext .5pt;">黄带绿色微绿黄色橙黄色橙黄带红色粉红色桔红色红色绛红色绛红色绛红微紫红紫色浅红紫色紫色深紫色</td></tr></tbody></table></div>附录：器皿的洗涤在分析工作之前，必须将所用的器皿仔细洗净。洗净的器皿的内壁应能被水均匀湿润而无条纹及水珠。 铬酸洗涤液的配制：<span style="FONT-SIZE: 12pt; COLOR: black; FONT-FAMILY: 宋体; mso-ascii-font-family: 仿宋_GB2312; mso-font-kerning: 1.0pt; mso-bidi-font-family: "Times New Roman"; mso-ansi-language: EN-US; mso-fareast-language: ZH-CN; mso-bidi-language: AR-SA;">称取研细的重铬酸钾<chmetcnv wst="on" tcsc="0" numbertype="1" negative="False" hasspace="False" sourcevalue="5" unitname="g"><span lang="EN-US" style="FONT-SIZE: 12pt; COLOR: black; FONT-FAMILY: 仿宋_GB2312; mso-hansi-font-family: 宋体; mso-fareast-font-family: 宋体; mso-font-kerning: 1.0pt; mso-bidi-font-family: "Times New Roman"; mso-ansi-language: EN-US; mso-fareast-language: ZH-CN; mso-bidi-language: AR-SA;">5g</chmetcnv><span style="FONT-SIZE: 12pt; COLOR: black; FONT-FAMILY: 宋体; mso-ascii-font-family: 仿宋_GB2312; mso-font-kerning: 1.0pt; mso-bidi-font-family: "Times New Roman"; mso-ansi-language: EN-US; mso-fareast-language: ZH-CN; mso-bidi-language: AR-SA;">置于<span lang="EN-US" style="FONT-SIZE: 12pt; COLOR: black; FONT-FAMILY: 仿宋_GB2312; mso-hansi-font-family: 宋体; mso-fareast-font-family: 宋体; mso-font-kerning: 1.0pt; mso-bidi-font-family: "Times New Roman"; mso-ansi-language: EN-US; mso-fareast-language: ZH-CN; mso-bidi-language: AR-SA;">250ml<span style="FONT-SIZE: 12pt; COLOR: black; FONT-FAMILY: 宋体; mso-ascii-font-family: 仿宋_GB2312; mso-font-kerning: 1.0pt; mso-bidi-font-family: "Times New Roman"; mso-ansi-language: EN-US; mso-fareast-language: ZH-CN; mso-bidi-language: AR-SA;">烧杯中，加水<span lang="EN-US" style="FONT-SIZE: 12pt; COLOR: black; FONT-FAMILY: 仿宋_GB2312; mso-hansi-font-family: 宋体; mso-fareast-font-family: 宋体; mso-font-kerning: 1.0pt; mso-bidi-font-family: "Times New Roman"; mso-ansi-language: EN-US; mso-fareast-language: ZH-CN; mso-bidi-language: AR-SA;">10ml<span style="FONT-SIZE: 12pt; COLOR: black; FONT-FAMILY: 宋体; mso-ascii-font-family: 仿宋_GB2312; mso-font-kerning: 1.0pt; mso-bidi-font-family: "Times New Roman"; mso-ansi-language: EN-US; mso-fareast-language: ZH-CN; mso-bidi-language: AR-SA;">加热使之溶解，冷却后，再慢慢加入<span lang="EN-US" style="FONT-SIZE: 12pt; COLOR: black; FONT-FAMILY: 仿宋_GB2312; mso-hansi-font-family: 宋体; mso-fareast-font-family: 宋体; mso-font-kerning: 1.0pt; mso-bidi-font-family: "Times New Roman"; mso-ansi-language: EN-US; mso-fareast-language: ZH-CN; mso-bidi-language: AR-SA;">80ml<span style="FONT-SIZE: 12pt; COLOR: black; FONT-FAMILY: 宋体; mso-ascii-font-family: 仿宋_GB2312; mso-font-kerning: 1.0pt; mso-bidi-font-family: "Times New Roman"; mso-ansi-language: EN-US; mso-fareast-language: ZH-CN; mso-bidi-language: AR-SA;">粗浓硫酸（应注意，切不可把水加入浓硫酸中），边加边搅拌，配好的洗液应为深褐色。贮于磨口塞小口瓶中密塞备用。使用时防止被水稀释。

[此贴子已经被作者于2007-10-19 14:07:13编辑过]

desk8347 · 发表于 2007-11-21 09:12:23

不全？？ [em03][em03]

irisyang_05 · 发表于 2007-12-9 10:35:18

佩服

lihong · 发表于 2008-1-3 11:29:25

huifu看看化验

lihong · 发表于 2008-1-3 11:33:51

huayan方法

lpas · 发表于 2008-4-12 10:36:39

挺不错的我支持！！！！！！！！！！！

中尉 · 发表于 2008-5-13 14:24:11

挺不错的我支持

ygrdfxf · 发表于 2008-6-23 08:52:37

[em01]

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