哈希COD测定方法
哈希COD测定法
原理:用一定量的重铬酸钾在强酸性溶液中,加入硫酸汞去除氯离子干扰,在银催化下,经过高温消解反应后的溶液COD浓度与吸光度成线性关系,符合朗伯—比尔定律,在620nm处比色得出样品浓度。
仪器:HACH-DR 3900分光光度仪,HACH-DRB 200消解仪
试剂:
1、邻苯二甲酸标准贮备溶液,COD=5000mg/l
称取0.4251g邻苯二甲酸氢钾溶于水中,定容至100ml。
2、邻苯二甲酸标准使用溶液,COD=500mg/l
取10ml邻苯二甲酸氢钾标准贮备溶液溶于水中,定容至100ml。
现配现用。
3、重铬酸钾溶液,1/6ρ=1.50mol/l
称取73.5475重铬酸钾(预先在120℃烘干2小时)溶于水中,定容至1000ml。
由于重铬酸钾不易溶于冷水,可边加热边溶解。
4℃冷藏保存。
若用前有析出,可在60℃下加热使其溶解后再使用。
4、1% H2SO4-Ag2SO4溶液
于500ml浓硫酸中加入5g硫酸银,放置1~2天,不时摇动使其溶解。
5、硫酸汞
步骤:
1、标线的绘制
(1)配置标准样品
于6支HACH消解-比色管中依次加入0.04g硫酸汞,2.50ml 1% H2SO4-Ag2SO4溶液,0.5ml重铬酸钾溶液,0.00、0.40、0.80、1.20、1.60、2.00ml 邻苯二甲酸标准使用液,2.00、1.60、1.20、0.80、0.40、0.00ml水,密封后摇匀。
(2)HACH-DRB 200进行消解
打开HACH-DRB 200消解仪开关,轻按屏幕显示COD的下方按键。
待温度上升至150℃,消解仪会发出滴滴滴的声音。
打开消解仪塑料盖,将比色管置于消解孔中,关上塑料盖,轻按屏幕显示start的下方按键,消解开始。
消解仪在150℃下恒温消解120min,然后慢慢降温,待温度降至120℃,仪器又会发出滴
滴滴的声音。
此时关闭消解仪,拿出比色管并摇匀,冷却至室温。
(3)HACH-DR 3900分光光度仪测量
首先准备含有2/3体积蒸馏水的比色管作为空白。
然后打开HACH-DR 3900分光光度仪,确定除了圆孔外其他光路已被遮住。
按单波长键,待进入测定界面后设定发射波长为620nm。
将含有蒸馏水的比色管插入圆孔中,按调零键后拿出,再将其余比色管插入圆孔中,按读数,测定其吸光度,记录数据。
最后关闭分光光度仪。
2、水样的测定
于HACH消解-比色管中依次加入0.04g硫酸汞,2.50ml 1% H2SO4-Ag2SO4溶液,0.5ml重铬酸钾溶液,2ml水样(当水样COD浓度大于1000mg/l时减小水样体积,用蒸馏水补足至2ml),密封后摇匀。
按标准曲线法测定吸光度,由标准曲线查得相应COD含量。
化学需氧量(COD)的测定方法
化学需氧量(COD)的测定方法
1、分析仪器
哈希(HACH)恒温消解器DR200、哈希(HACH)多参数水质分光光度计DR3900
2、样品处理
1)打开加热器,选择“COD”程序,等待仪器加热至150°C。
2)取2个COD试剂瓶,去掉盖子。
3)使用移液枪取2ml待测试水样于一支COD试剂瓶中,另取2ml去离子水于另一支COD试剂瓶中。
4)两个瓶子上盖,并将瓶外壁擦拭干净。
5)振摇几次后,插入消解器中。
6)按下仪器上“start”键,开始加热2个小时。
7)加热完成后,关闭加热器,待试剂瓶冷却片刻后,取出并放入试管架上冷却至室温。
3、测试方法
1)选择430号程序,波长420nm。
2)清洁瓶壁,将瓶外壁擦拭干净。
3)把空白样放入仪器中。
4)按调零键,仪器调零。
5)取出空白样,放入待测试样品。
6)按读数键盘,读取待测样品的COD值。
哈希COD日常操作规程
电仪部内部资料哈希COD在线监测仪操作规程哈希COD在线监测仪操作规程一、设备工作原理设备工作原理:1、检测原理:水样、重铬酸钾、硫酸银溶液(催化剂)和浓硫酸的混合液在消解池中被加热到175℃,在此期间铬离子作为氧化剂从Cr6+价被还原成Cr3+而改变了颜色,颜色的改变度与样品中被氧化物质的含量成对应关系,仪器通过比色换算直接将样品的COD显示出来。
2.检测过程:(1)测试前仪器自动抽取新鲜的样品清洗进样管道;(2)仪器使用活塞泵进样,活塞泵不与样品、试剂直接接触;(3)试剂(硫酸汞、重铬酸钾、硫酸包括催化剂)也通过活塞泵吸入,(4)通过气泡的方式混合样品和试剂;(5)仪器关闭消解试管的两端的阀门后,加热电阻丝将样品和试剂的混合溶液迅速地加热至175℃;(6)测量系统按照仪器参数的设定值自动控制消解时间;(7)溶液冷却后,由活塞泵排出溶液。
(8)仪器按预设置的校准时间和清洗时间自动地对仪器进行校准和清洗。
(9)根据实际校准系数,微处理器单元计算出经过自动温度补偿后的COD值。
COD设备结构说明图试剂型号:LCW2401、硫酸溶液2.5升(强腐蚀);2、重铬酸钾溶液1升;3、硫酸汞溶液1升(剧毒);4、零点校准溶液0.5升;5、标准溶液0.25升V1:消解试管入口阀V2:空缺水平阀V3:样品阀V4:排放阀V5:重铬酸钾阀V6:消解阀V7:95硫酸阀V8:硫酸汞阀V9:标液阀V10:空气消解阀3.COD设定-SETTING项:(1)digest.time消解时间:30分钟;(2)Mea.intervall测量间隔时间:COD、NH3-N设定,4小时采样周期;(3)cur.range:1#COD:0~5000mg/L、2#COD:0~500mg/L、NH3-N:0~120mg/L;(4)cleaning清洗:三天一次;(5)calibration校准:自动校正周期三天一次;COD设定-SERVICE项:(1)flush冲洗:冲洗所有管路(60秒);(2)cleaning清洗:启动自动清洗,然后进行测量;(3)calibration校准:启动自动校准,然后进行测量(60分钟);(4)CONTROLUNIT控制单元:复位控制器列表,仅处理电子问题;注意:进入SERVICE项产生以下动作(轻易不要进入该项)COD测量仪立即停止测量;仪表回到初始状态,消解管释放压力,排空,冷却;存储最后一次的有效测量值;所有的输出都保持为他们的最后状态值。
HACH哈希COD快速测定方法
HACH哈希COD快速测定方法哈希 (Hash) 算法是一种将任意长度的数据映射为固定长度哈希值的函数。
它在数据安全领域中起着重要的作用,常被用于数据的完整性验证、数据的唯一标识、密码的存储和验证等。
COB (Collision‐Based) 快速测定方法是一种使用哈希算法来快速检测哈希冲突的方法。
哈希冲突是指不同的输入数据经过哈希函数计算后得到相同的哈希值。
COB方法通过一系列巧妙的技巧,可以高效地检测出哈希冲突,并找到冲突的原始输入数据。
它在密码学、计算机图形学、数据处理等领域有广泛应用。
COB方法通常包含以下几个步骤:1.选择合适的哈希函数:COB方法通常要求哈希函数具有良好的随机性和抗碰撞性。
常见的哈希函数有MD5、SHA-1、SHA-256等,根据实际需求选择合适的哈希函数。
2.构建哈希表:COB方法中需要构建一个哈希表,用于存储已经计算过的哈希值和对应的原始输入数据。
哈希表可以用数组、链表或者二叉树等数据结构实现。
3.输入数据哈希化:将待检测冲突的输入数据通过哈希函数计算得到哈希值。
4.哈希冲突检测:将计算得到的哈希值与哈希表中已有的哈希值进行比较,如果存在相同的哈希值,则说明发生了哈希冲突。
5.哈希冲突解决:如果检测到哈希冲突,可以通过拉链法、开放寻址法等方法来解决冲突。
具体的方法根据实际情况进行选择。
6.冲突原始输入寻找:通过哈希冲突解决方法,可以找到冲突的原始输入数据。
这一步需要根据具体实现来进行。
COB方法的核心思想是通过哈希函数将输入数据映射到哈希空间中,然后利用哈希冲突检测和解决方法来找到冲突的原始输入数据。
COB方法在时间复杂度和空间复杂度方面都能够达到较好的性能,因此在实际应用中被广泛使用。
总之,COB方法是一种使用哈希算法进行快速冲突检测和解决的方法。
它具有高效、可靠的特点,在数据安全领域有着重要的应用。
通过合理选择哈希函数以及巧妙的哈希冲突解决方法,可以实现高效准确地进行哈希冲突的快速测定。
(HACH专用)微回流比色法测定CODcr的试剂配方和测定方法1
微回流比色法测定COD cr的试剂配方和测定方法1.概述用美国哈希专用试剂和仪器测定COD,方法简单,结果准确。
但其试剂价格较为昂贵,监测机构不可能大量使用,按照哈希公司提供的试剂配方,在制备上难以掌握,至使哈希测定COD这一简单准确的方法,在使用上受到了一定的限制。
为解决这一问题,我们对哈希提供的COD试剂配方进行了适当的调整。
调整后的配方容易操作,测定结果符合监测要求。
2.仪器2.1 DR/2010分光光度计。
2.2 COD加热器。
2.3 哈希COD测定试管。
3.试剂及试剂配方3.1硫酸银,化学纯。
3.2硫酸汞,化学纯。
3.3硫酸,分析纯,ρ=1.84g/ml。
3.4硫酸-硫酸银试剂:向500ml硫酸(3.3)中,加入5g硫酸银(3.1),放置1~2天使之溶解,并摇匀。
3.5C=0.01225g/ml重铬酸钾标准溶液:将6.125g在105℃干燥2h后的基准重铬酸钾溶解于蒸馏水中,稀释至500ml。
3.6COD测定管试剂配方(量程为0~700mg/l):取清洁的哈希COD测定试剂管(2.3)若干支,每支分别依次加入0.03g硫酸汞(3.2)、3.00ml硫酸-硫酸银试剂(3.4)、1.00ml C=0.01225g/ml重铬酸钾标准溶液(3.5),盖上试管帽。
4.建立用户COD测定程序4.1 获取用户COD测定程序参数:取6支COD测定试管(3.6),分别加入2.00ml不同浓度的COD已知样,盖上试管帽,在COD加热器(2.2)上,于150℃下加热2h,冷至室温后,在DR/2010分光光度计上测定其吸光度。
测定结果见下表:COD浓度mg/l 0 25 50 75 125 250 600nm处吸光度E 0 0.009 0.020 0.030 0.051 0.105校准曲线相关系数:γ=0.9998 校准曲线方程:C=2367E+2.674.2 建立用户COD测定程序:将(4.1)测定的结果参数输入到DR/2010分光光度计的用户自建程序中,便获得了一个适合用户的COD测定程序。
HACH-COD测试操作说明
COD测试操作说明一、COD反应器操作1、确认将仪器电压选择钮调至230V。
2、仪器面板上时间开关置于TIMER一边,温度开关置于150o C。
3、接上电源,开机。
二、样品消解1、取100ml样品于混合器中搅拌30秒。
2、将时间开关置于∞一边,COD反应器预热至150 o C。
3、取一支COD试剂(选择合适量程的试剂),拧开盖。
4、将试剂管倾斜45度角,用移液管加入2.00ml样品。
(0-15000ml/L量程时加0.20ml样品)5、拧上盖,用纸巾擦干净试管外壁。
6、拿住试管盖,上下倒置轻轻混合几次,放入已预热的COD反应器中。
7、取2.00ml去离子水作空白样,重复3-6步骤。
8、将时间开关置于TIMER一边,将时间拧至120分钟,开始消解。
9、到120分钟时仪器自动停止加热。
等待20分钟左右,试管温度会降至120o C左右。
10、将试管上下倒置几次后放在试管架上冷至室温。
11、用HACH分光光度计测COD值。
三、分光光度计使用DR/890分光光度计测COD1、按EXIT/0键开机。
2、如用0-150ppm试剂,按PRGM键,输入16(如用0-1500、0-15000ppm试剂,输入17),按ENTER键,启动COD测量程序。
3、将COD适配器插入仪器样品室中。
4、将已冷至室温的空白样品外壁擦干净。
5、插入适配器中,将盖盖上。
(将有HACH标记的一面朝向键盘)6、按ZERO键,仪器回零。
7、将已冷至室温的测试样品外壁擦干净。
8、将空白样拿出,将测试样品插入适配器中,将盖盖上。
(将有HACH标记的一面朝向键盘)9、按READ键,读COD值。
哈希DR2400型COD分析仪回流比色法作业指导书
哈希DR2400型COD分析仪回流比色法作业指导书
标识:XXEMS ZY 5.3-05-10
哈希DR2400型COD分析仪
回流比色法作业指导书
编制:________________
审核:________________
批准:________________
生效:
HACH DR/2400型COD分析仪回流比色法操作规程
一、仪器: DR/2400分光光度计。
二、适用范围:地下水、地表水和废水COD的检测。
三、操作步骤:
1.高量程:称取适量HgSO4试剂放入10ml比色瓶中,加入1.00mol/L重铬酸钾溶液0.75ml, HgSO4—AgSO4溶液2.25ml,再加入2ml混合均匀的水样,同时用蒸馏水做空白,放入COD反应仪上加热回流2小时,冷却后使用DR/2400分光光度计并选择相应的波长测定,读数即为COD值。
记录实验结果。
2.低量程:称取适量HgSO4试剂放入10ml比色瓶中,加入0.05mol/L重铬酸钾溶液0.75ml, HgSO4—AgSO4溶液2.25ml,再加入2ml混合均匀的水样,同时用蒸馏水做空白,放入COD反应仪上加热回流2小时,冷却后使用DR/2400分光光度计并选择相应的波长测定,读数即为COD值。
记录实验结果。
说明
本作业指导书及其具体内容仅为个人搜集编写提供,只做范文使用。
其具体内容所涉及仪器型号、操作步棸方法、适用范围、测量范围、注意事项、参数、图表等可能与仪器生产商的仪器相关资料不完全相同,仅供参考。
由此产生的一切后果与编写上传者无关。
特此说明。
哈希COD_max_培训教材概要
(V2 V1 )*8*C*1000 CODcr(O2 ,mg/L)= V
1摩尔重铬酸钾相当于1.5摩尔COD。
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1. 托盘 2. 试剂 3. 安全面板 4. 进样管 5. 废液排放管 6. 电源线 7. 屏蔽电缆口 8. 仪器外壳 9. RS232界面 10. 液晶显示屏 11. 操作键盘 12. 仪器门 13. 试剂瓶(空)
CODmax的测量原理
相同的试剂
1. 2. 3. 4. 5. 硫酸溶液2.5升 重铬酸钾溶液1升 硫酸汞溶液1升 零点校准溶液0.5升 标准溶液0.25升
经 典 原 理
CODmax采用经典的测量原理
相同的消解方法
水样 重铬酸钾 硫酸银(催化剂) 浓硫酸
消解池
混 抗干扰 合 加入硫酸汞形成络合物去
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试剂的安装
1. 2. 3. 4. 5. 硫酸溶液2.5升 重铬酸钾溶液1升 硫酸汞溶液1升 零点校准溶液0.5升 标准溶液0.25升
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拆卸安全面板
• 给仪器供电;
• 打开仪器门,然后按住 F1-F4四个功能键中的 任意一个,保持3秒钟; • 显示屏切换到菜单状态;
• 按F4键移动当前的选择 (滚动条),指向+ SERVICE菜单,并按F2键 (选中此菜单); • 1分钟之后用户可以拆卸 安全面板。
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安装试剂
• 危险! • 为安全起见,请遵守下列各条: – ������ 穿上安全服(实验工作服) – ������ 戴上安全眼罩/面罩 – ������ 戴橡胶手套 – ������ 旋下试剂瓶的原有瓶盖,先安装2.5升的硫酸溶液, 将仪器上对应的试剂溶液摄取管路装入玻璃瓶,小心旋转 玻璃瓶上相应配备的瓶盖,注意不要旋转瓶盖而是旋转试 剂瓶。然后将试剂瓶放入分析仪的底部托盘上,按照图所 示顺序装好每个试剂瓶。 –
哈希cod低量程标准曲线
哈希COD低量程标准曲线的建立步骤如下:
1. 配置标准溶液:按照哈希试剂说明书配置标准溶液,设置浓度范围,一般包括0-150mg/L。
2. 取样:使用移液枪准确取样,注意放液时应慢慢的并重复两三次以致放液干净。
3. 消解:将取样的标准溶液加入消解管中并加盖密封,然后进行消解处理,一般消解时间为15分钟。
4. 比色:消解完成后进行比色处理。
5. 建立曲线:在比色过程中,需要建立标准曲线。
通常建议平行测定3-4个样品,一个样品也可以。
在测量时需要注意:
1. 哈希COD低量程适用于0-150mg/L的测量范围,超过此范围的测量值可能会不准确。
2. 在使用哈希COD低量程进行测量时,需要先确认量程是否正确,然后按照说明书进行操作。
3. 在取样时需要保证样品数量和代表性,同时注意放液干净,避免影响测量结果。
4. 在比色过程中需要保证比色皿的清洁和干燥,避免影响测量结果。
5. 在建立曲线时需要使用标准溶液进行校准,确保曲线的准确性和可靠性。
哈希COD使用说明书
DOC023.52.03233.Jan04CODmax 化学需氧量分析仪操作手册○C HACH LANGE 2004. All rights reserved.致力优质水质目录第一章技术规格 (4)第二章引言 (5)2.1 系统描述 (5)2.2 应用 (6)第三章拆箱和安装 (7)3.1 拆箱和安装…………………………………………………………………………‥ 73.1.1安装位置要求…………………………………………………………‥•‥‥ 73.2 MODBUS界面……………………………………………………………………‥•103.2.1 MODBUS协议 (11)3.2.2连接……………………………………………………………………………• 113.2.3 MODBUS网卡 (11)3.2.4输出特性表……………………………………………………………………• 12第四章校准与准备试剂…………………………………………………………………• 164.1 试剂成份 (16)4.1.1 硫酸汞溶液 (16)4.1.2 重铬酸钾溶液 (18)4.1.3 硫酸溶液 (18)4.1.4 零点标准溶液 (19)4.1.5 标准溶液 (19)4.1.5.1 标准溶液的化测试验 (19)4.2 危害信息 (20)第五章试运行分析仪 (22)5.1 拆卸安全面板 (22)5.2 安装试剂 (23)5.3 暂停操作 (25)第六章操作…………………………………………………………………………………• 266.1 基本原理 (26)6.2 测试范围 (26)6.3 测试步骤 (26)6.4 校准 (27)6.5 自动清洗 (27)6.6 手动清洗 (27)6.7 安全面板 (27)6.8 湿度传感器 (28)6.9 分析单元 (29)6.10 导管分布图…………………………………………………………………………• 306.11 样品泵操作…………………………………………………………………………• 32第七章软件菜单系统……………………………………………………………………• 327.1 主显示屏……………………………………………………………………………‥ 327.2 键盘使用……………………………………………………………………………‥ 337.2.1 图形功能 (34)7.3 菜单结构……………………………………………………………………………‥ 357.3.1 设置菜单 (35)7.3.2 信号菜单 (36)7.3.3 维修菜单 (38)测试功能菜单…………………………………………………………• 397.3.3.17.3.4 状态菜单 (40)7.4 记录COD数据 (40)第八章设备维护 (42)第九章故障维修 (47)9.1 警告 (47)9.2 错误 (47)第十章附件列表 (50)安全预防措施尤其注意所有有关危险和谨慎问题的说明。
HACH哈希COD快速测定方法
HACH哈希COD快速测定方法Oxygen Demand, ChemicalPage 1 of 12How to use instrument-specific informationThe Instrument-specific information table displays requirements that may vary betweeninstruments. To use this table, select an instrument then read across to find the corresponding information required to perform this testOxygen Demand, ChemicalDOC316.53.01099USEPA 1 Reactor Digestion Method 21Ranges 3 to 150 mg/L COD and 20 to 1500 mg/L COD are USEPA approved for wastewater analyses (Standard Method 5220 D), Federal Register , April 21, 1980, 45(78), 26811-26812.2Jirka, A.M.; Carter, M.J., Analytical Chemistry , 1975, 47(8), 1397Method 80000.7 to 40.03 mg/L COD; 3 to 150 mg/L COD; 20 to 1500 mg/L COD; 200 to 15,000 mg/L COD3The ULR range is not available on the DR 2700 or the DR/2400.Scope and Application:For water, wastewater; digestion is requiredTest preparationTable 1 Instrument-specific informationInstrument Light shieldAdapter DR 5000——DR 2800LZV646—DR 2700LZV646—DR/2500——DR/2400—5945700Before starting the test:DR 2800 and DR 2700: Install the light shield in Cell Compartment #2 before performing this test.DR 2700 and DR/2400: Ultra low range (0.7 to 40.0 mg/L) is not available.Some of the chemicals and apparatus used in this procedure may be hazardous to the health and safety of the user if inappropriately handled or accidentally misused. Please read all warnings and associated MSDS sheets.Run one blank with each set of samples. Run all tests (the samples and the blank) with the same lot of vials. The lot number appears on the container label. See Blanks for colorimetric determination .Spilled reagent will affect test accuracy and is hazardous to skin and other materials. Be prepared to wash spills with running water.Wear appropriate eye protection and clothing for adequate user protection. If contact occurs, flush the affected area with running water. Review and follow reagent MSDS safety instructions carefully.If high chloride samples are being tested, refer to the Alternate reagents section.Oxygen Demand, Chemical Page 2 of 12Oxygen Demand, ChemicalCollect the following items:Description QuantityBeaker, 250-mL 1Blender1COD Digestion Reagent vials variesDRB200 Reactor1Light Shield or adapter (see Instrument-specific information )1Magnetic stirrer and stir bar1Opaque shipping container for storage of unused, light-sensitive reagent vials varies Pipet, TenSette ?, 0.1 to 1.0 mL, with tips (for 200–15,000 mg/L range)1Pipet, volumetric, 2.00 mL 2Pipet Filler, safety bulb 1Test Tube Rack2See Consumables and replacement items for reorder information.Reactor digestion procedure1.Homogenize 100 mL of sample for 30 seconds in a blender. For samples containing large amounts of solids, increase the homogenization time.If the sample does not contain suspended solids, omit steps 1 and2.2.For the 200–15,000mg/L range or to improve accuracy and reproducibility of the other ranges, pour thehomogenized sample into a 250-mL beaker andgently stir with a magnetic stir plate.3.Turn on the DRB200 Reactor. Preheat to 150°C.See the DRB200 User Manual for selecting pre-programmed temperature applications.4.Remove the caps from two COD DigestionReagent Vials. (Be sure to use vials for the appropriate range.) Oxygen Demand, ChemicalOxygen Demand, ChemicalPage 3 of 125.Prepared Sample: Hold one vial at a45-degree angle. Use a clean volumetric pipet to add 2.00 mL of sample to the vial.For the 200–15,000 mg/L vials: Use a TenSette ? Pipet to add 0.20mL of sample to the vial.6.Blank Preparation: Hold a second vial at a 45-degree angle. Use a clean volumetric pipet to add 2.00mL of deionized water to the vial.For the 200–15,000 mg/L vials: Use a TenSette Pipet to add 0.20mL of sample to the vial.7.Cap the vials tightly. Rinse them with water and wipe witha clean paper towel.8.Hold the vials by the cap over a sink. Invert gently several times to mix. The sample vials become very hot during mixing.Insert the vials in the preheated DRB200 Reactor. Close the protective lid.9.Heat the vials for two hours.10.Turn the reactor off.Before removing the vials, wait about 20 minutes for the vials to cool to 120 °C or less.11.Invert each vial several times while still warm.12.Place the vials into a rack and cool to room temperature.Proceed to Colorimetric determination .Reactor digestion procedure (continued)Oxygen Demand, Chemical Page 4 of 12Oxygen Demand, Chemical Blanks for colorimetric determinationThe blank may be used repeatedly for measurements using the same lot of vials. Store the blank in the dark.1.Monitor decomposition by measuring the absorbance at the appropriate wavelength. Refer tothe Range-specific test wavelengths table. 2.Zero the instrument in the absorbance mode. Use a vial containing 5 mL of deionized waterand measure the absorbance of the blank. Record the value.3.Prepare a new blank when the absorbance has changed by about 0.01 absorbance units.Colorimetric determination1.Select the test.Insert an adapter or light shield if required (see Instrument-specific information ).Refer to the user manual for orientation.2.Clean the outside of the vials with a damp towel followed by a dry one.3.Insert the blank into the 16-mm cell holder.4.ZERO the instrument.The display will show:0 mg/L COD or0.0 mg/L COD5.Insert the sample vial into the 16-mm cell holder.6.READ the results in mg/L COD.7.If using High Range Plus COD DigestionReagent Vials, multiply the result by 10.For most accurate results with samples near 1500 or 15,000 mg/L COD, repeat the analysis with a diluted sample.431 COD ULR Stored ProgramsStart430 COD LR435 COD HRZeroReadOxygen Demand, ChemicalOxygen Demand, ChemicalPage 5 of 12InterferencesChloride is the primary interference when determining COD concentration. Each COD vial contains mercuric sulfate that will eliminate chloride interference up to the level specified in Column 1 of the Interfering substances table. Dilute samples with higher chloride concentrations. Dilute the sample enough to reduce the chloride concentration to the level given in Column 2.Note: For best results, use the low range and ultra-low range test for samples with high chlorideconcentrations (approaching maximum concentration) and low COD concentrations.If sample dilution will cause the COD concentration to be too low for accurate determination, add 0.50 g of mercuric sulfate (HgSO 4) to each COD vial before the sample is added.The additional mercuric sulfate will raise the maximum chloride concentration allowable to the level given in Column 3.Sample collection, preservation and storageCollect samples in glass bottles.Use plastic bottles only if they are known to be free of organic contamination. ?Test biologically active samples as soon as possible.Homogenize samples containing solids to assure representative samples.Samples treated with sulfuric acid * to a pH of less than 2 (about 2mL per liter) and refrigerated at 4 °C can be stored up to 28 days. ?Correct the test results for volume additions.Table 2 Interfering substancesVial rangeColumn 1(Maximum chloride concentration )Column 2(Suggested chloride concentration for diluted samples)Column 3(Maximum chloride concentration with mercuric sulfate)Ultra Low Range 1(0.7–40.0 mg/L)1Ultra Low Range is not available on the DR 2700 or the DR/2400.20001000N/A Low Range (3–150 mg/L)200010008000HighRange (20–1500 mg/L)200010004000High Range Plus (200–15,000 mg/L)20,00010,00040,000*See Optional reagents and apparatus .Oxygen Demand, ChemicalAccuracy checkStandard solution methodNote: Refer to the instrument user manual for specific software navigation instructions.Required for accuracy check:Potassium acid phthalate (KHP), dried overnight at 120 °CDeionized water, organic freeClass A volumetric flasksClass A volumetric pipet0.7 to 40.0 mg/L range1.Prepare a 30-mg/L COD standard solution as follows:a.Dissolve 850 mg of dried KHP in 1000-mL of organic-free deionized water to make a1000-mg/L standard.b.Pipet 3.00 mL of the 1000 mg/L standard into a 100-mL volumetric flask.c.Dilute to volume with deionized water and mix well.e 2 mL of the 30 mg/L COD solution in place of the sample. Follow the Colorimetricdetermination test procedure. The result should be 30 mg/L. Refer to the Standard adjustinstructions in this procedure to adjust the curve with the reading obtained from the standard.3 to 150 mg/L range1.Prepare a 100-mg/L COD standard solution as follows:a.Dissolve 85 mg of dried KHP in 1000-mL of organic-free deionized water to make a1000-mg/L standard.b.Pipet 10 mL of the 1000 mg/L standard into a 100-mL volumetric flask.c.Dilute to volume with deionized water and mix well.e 2 mL of the 100-mg/L solution in place of the sample. Follow the Colorimetricdetermination test procedure. The result should be 100 mg/L. Refer to the Standard adjustinstructions in this procedure to adjust the curve with the reading obtained from the standard20 to 1500 mg/L range1.Prepare a 500-mg/L COD standard solution as follows:a.Dissolve 425 mg of dried KHP in 1000-mL of organic-free deionized water to make a500-mg/L standard.b.Mix well.e 2 mL of the 500 mg/L COD solution in place of the sample. Follow the Colorimetricdetermination test procedure. The result should be 500 mg/L. Refer to the Standard adjustinstructions in this procedure to adjust the curve with the reading obtained from the standard.Note: Alternately, use 2 mL of 300 mg/L, 800 or 1000 mg/L COD standards for accuracy check. Oxygen Demand, Chemical Page 6 of 12Oxygen Demand, Chemical200 to 15,000 mg/L range1.Prepare a 10,000-mg/L COD standard solution as follows:a.Dissolve 8.500 g of dried KHP in 1000-mL of organic-free deionized water.e 0.2 mL of the 10,000 mg/L COD solution in place of the sample. Follow the Colorimetricdetermination test procedure. The result should be 10,000 mg/L (after multiplying by 10).Refer to the Standard adjust instructions in this procedure to adjust the curve with the readingobtained from the standard.Standard adjust1.To adjust the calibration curve using the reading obtained with the standard solution, navigateto Standard Adjust in the software.Instrument Navigate to:DR 5000OPTIONS>MORE>STANDARD ADJUSTDR 2800OPTIONS>MORE>STANDARD ADJUSTDR 2700OPTIONS>MORE>STANDARD ADJUSTDR/2500OPTIONS>STANDARD ADJUSTDR/2400OPTIONS>STANDARD ADJUST2.Turn on the Standard Adjust feature and accept the displayed concentration. If an alternateconcentration is used, enter the concentration and adjust the curve to that value. Alternate reagentsMercury-free COD2 Reagents can provide a mercury-free testing option for non-reportingpurposes. For process control applications, COD2 Reagents will eliminate mercury waste andsave on disposal costs. These reagents are fully compatiblewith test procedures and calibrationcurves programmed into the spectrophotometer. Determine chloride and ammonia foraccurate results.Important Note: COD2 reagents are not approved for USEPA reporting purposes. Because COD2 reagents do not contain mercury as a masking agent, they exhibit a positiveinterference from chloride. Request a copy of the COD Reagent Vial Information Brochure,Lit.No. 1356, for more information about specific applications.Oxygen Demand, ChemicalPage7 of 12Oxygen Demand, Chemical Page 8 of 12Oxygen Demand, ChemicalMethod performanceProgram Instrument StandardPrecision95% Confidence Limitsof DistributionSensitivityConcentration change per 0.010 Abs change430(Range, 3–150 mg/L)DR 500030 mg/L COD (Ultra Low Range);80 mg/L COD (Low Range);800mg/L COD (High Range);8000 mg/L COD (High Range Plus)77–83 mg/L COD 3 mg/L COD DR 280077–83 mg/L COD 3 mg/L COD DR 270077–83 mg/L COD3 mg/L CODDR/250030 mg/L COD (Ultra Low Range);80 mg/L COD (Low Range); 800mg/L COD (High Range); 10,000 mg/L COD (High Range Plus)77.6–82.4 mg/L COD 3 mg/L COD DR/240077.6–82.4 mg/L COD3 mg/L COD431(Range, 0.5–40.0 mg/L)DR 500030 mg/L COD (Ultra Low Range);80 mg/L COD (Low Range);800mg/L COD (High Range);8000 mg/L COD (High Range Plus)28.8–31.2 mg/L COD 0.5 mg/L COD DR 280028.8–31.2 mg/L COD0.5 mg/L COD431(Range, 0.7–40.0 mg/L)DR/250030 mg/L COD (Ultra Low Range);80 mg/L COD (Low Range); 800mg/L COD (High Range); 10,000 mg/L COD (High Range Plus)29.0–31.0 mg/L COD 0.7 mg/L COD435(Range,20–1500 mg/L)DR 500030 mg/L COD (Ultra Low Range);80 mg/L COD (Low Range);800mg/L COD (High Range);8000 mg/L COD (High Range Plus)785–815 mg/L COD 23 mg/L COD DR 2800785–815 mg/L COD 23 mg/L COD DR 2700785–815 mg/L COD23 mg/L CODDR/250030 mg/L COD (Ultra Low Range);80 mg/L COD (Low Range); 800mg/L COD (High Range); 10,000 mg/L COD (High Range Plus)778–822 mg/L COD 20 mg/L COD DR/2400778–822 mg/L COD20 mg/L COD435(Range,200–15,000 mg/L)DR 500030 mg/L COD (Ultra Low Range);80 mg/L COD (Low Range);800mg/L COD (HighRange);8000 mg/L COD (High Range Plus)7850–8150 mg/L COD 230 mg/L COD DR 28007850–8150 mg/L COD 230 mg/L COD DR 27007850–8150 mg/L COD230 mg/L CODDR/250030 mg/L COD (Ultra Low Range);80 mg/L COD (Low Range); 800mg/L COD (High Range); 10,000 mg/L COD (High Range Plus)9780–10,220 mg/L COD 200 mg/L COD DR/24009780–10,220 mg/L COD200 mg/L CODOxygen Demand, ChemicalOxygen Demand, ChemicalPage 9 of 12Summary of methodThe results in mg/L COD are defined as the milligrams of O 2 consumed per liter of sample under the conditions of this procedure. The sample is heated for two hours with sulfuric acid and a strong oxidizing agent, potassium dichromate. Oxidizable organic compounds react, reducing the dichromate ion (Cr 2O 72–) to green chromic ion (Cr 3+).When the 0.7–40.0 or the 3–150 mg/L colorimetric method is used, the amount of Cr 6+ remaining is determined. When the 20–1500 mg/L or 200–15,000 mg/L colorimetric method is used,the amount of Cr 3+ produced is determined. The COD reagent also contains silver and mercury ions. Silver is a catalyst, and mercury is used to complex chloride interferences. Test results are measured at the wavelengths specified in the Range-specific test wavelengths table.Table 3 Range-specific test wavelengthsRange in mg/L COD Wavelength 0.7 to 40.0 mg/L 11Not available on the DR/2400 or the DR 2700350 nm 3 to 150 mg/L 420nm 20 to 1500620nm 2000 to 15,000 mg/L620nmOxygen Demand, ChemicalConsumables and replacement itemsRequired reagentsDescription Quantity/Test Unit Catalog number Select the appropriate COD Digestion Reagent Vial:Ultra Low Range, 0.7 to 40 mg/L COD1–2 vials25/pkg2415825 Low Range, 3 to 150 mg/L COD1–2 vials25/pkg2125825 High Range, 20 to 1500 mg/L COD1–2 vials25/pkg2125925 High Range Plus, 200 to 15,000 mg/L COD1–2 vials25/pkg2415925 Water, deionized varies 4 L27256Alternate reagents1Description Quantity/Test Unit Catalog number Select the appropriate COD Digestion Reagent Vial:COD2, Low Range, 0 to 150 mg/L COD1–2 vials25/pkg2565025 COD2, High Range, 0 to 1500 mg/L COD1–2 vials25/pkg2565125 COD2, High Range, 0 to 1500 mg/L COD1–2 vials150/pkg2565115 COD2, High Range Plus, 0 to 15,000 mg/L COD1–2 vials25/pkg2834325 COD Digestion Reagent Vials, 3 to 150 mg/L COD—150/pkg2125815 COD Digestion Reagent Vials,200 to 1500 mg/L COD—150/pkg21259151These reagents are not approved for USEPA reporting purposes. Request a copy of the COD Reagent Vial Information Brochure,Lit. No. 1356, for more information about specific applications.Required apparatusDescription Quantity/Test Unit Catalog number Blender, 2-speed, 120 VAC1each2616100 Blender, 2-speed, 240 VAC1each2616102 DRB200 Reactor, 110 V, 15 x 16 mm1each LTV082.53.40001 DRB200 Reactor, 220 V, 15 x 16 mm1each LTV082.52.40001 Pipet Filler, safety bulb1each1465100 Pipet, Volumetric, Class A, 2.00 mL1each1451536Oxygen Demand, ChemicalPage 10 of 12Oxygen Demand, ChemicalOxygen Demand, ChemicalPage 11 of 12Recommended standards and apparatusDescription Unit Catalog numberBeaker, 250-mLeach 50046H COD Standard Solution, 300-mg/L 200 mL 1218629COD Standard Solution, 300-mg/L 500mL 1218649COD Standard Solution, 800-mg/L 200 mL 2672629COD Standard Solution, 1000-mg/L200 mL 2253929Oxygen Demand Standard (BOD, COD, TOC), 10-mL ampules 16/pkg 2833510Pipet, TenSette ?, 0.1 to 1.0 mL each 1970001Pipet Tips, for TenSette Pipet 1970001 50/pkg 2185696Pipet Tips, for TenSette Pipet 1970001 1000/pkg 2185628Potassium Acid Phthalate, ACS 500 g 31534Stir Bareach 2095352Stirrer, Electromagnetic, 120 VAC, with electrode stand each 4530001Stirrer, Electromagnetic, 230 VAC, with electrode stand each 4530002Test Tube Rack each 1864100Disposable wipes70/pkg2096900Optional reagents and apparatusDescriptionUnit Catalog numberBalance, analytical, 80 g capacity, 115 VAC each 2936701COD Digestion Reagent Vials, ULR 0.7-40.0 mg/L 150/pkg 2415815COD Digestion Reagent Vials, HR plus,200-25,000 mg/L 150/pkg 2415915Flask, volumetric, 1000 mL Class A each 1457453Flask, volumetric, 100-mL Class A each 1457442Mercuric Sulfate, 28 g—191520Pipet, volumetric, 3-mL, Class A each 1451503Pipet, volumetric, 10-mL, Class A each 1451538Sulfuric Acid, 500 mL —97949Wastewater Influent Standard for mixed parameters NH 3–N, NO 3–N, PO 4, COD, SO 4, TOC500mL 2833149Wastewater Effluent Standard, for mixed parameters NH 3–N, NO 3–N, PO 4, COD, SO 4, TOC500mL 2833249Weighing Paper, 76x76 mm 500/pkg 1473800Finger cots2/pkg 1464702Gloves, chemical resistant 9-9 ?”11Other sizes are available 1 pair 2410104Safety goggles, vented each 2550700EZ COD TM Recycling Service with 5-gal 2 bucket220 and 50 gal are available.each2895405Hach Company,2007. All rights reserved. Printed in the U.S.A.Updated February2008,Edition5。
