CN1033321A - 简易快速测定水中有害金属铜检测管 - Google Patents

简易快速测定水中有害金属铜检测管 Download PDF

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CN1033321A
CN1033321A CN 87106810 CN87106810A CN1033321A CN 1033321 A CN1033321 A CN 1033321A CN 87106810 CN87106810 CN 87106810 CN 87106810 A CN87106810 A CN 87106810A CN 1033321 A CN1033321 A CN 1033321A
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ddtc
detector tube
water
aqueous solution
concentration
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CN1004583B (zh
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许维光
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Beijing Physichemistry Analysis & Measurment Centre
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Beijing Physichemistry Analysis & Measurment Centre
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Abstract

本发明为一种简易快速测定水中有害金属铜检 测管。
检测管内的检知剂为二乙基氨荒酸铅 (DDTC-Pb)螯合化树脂。其测定水中含铜量准确度 高、精密度好。
本检测管价格低廉、使用方便、易于随身携带,测 量使用中不需要动力,适合于工厂、企业废水处理的 自我控制检测。

Description

本发明涉及的是一种简易快速测定水中有害金属铜检测管。
测定水中有害金属铜的含量,一般有仪器分析方法和化学分析方法。仪器分析方法中常用的有原子吸收法、等离子发射光谱法等;化学分析方法中用的最多的是分光光度法。这些方法都需要专门的实验室、昂贵的仪器、技术人员,手续繁复,多有不变。日本出版的“电气化学”杂誌39    No1(1971)曾报导了用检测管法快速测定水中的含铜量。其检知剂为二乙基氨荒酸钠螯合树脂;检测范围为2~150PPm;这种铜检测管当水中同时存在锰(Mn)、锌(Zn)、铁(Fe)、铅(Pb)等离子时,对含铜量的测定有严重影响。
本发明的目的在于寻找一种新的检知剂制成一种使用方便、简易快速测定水中含铜量的检测管,使之能够不受被测水中同时存在的其它一些杂质,如铁(Fe)、锰(Mn)、锌(Zn)、铅(Pb)等离子的影响,并且提高测定被测水中含铜量的准确度和精密度。
本专利发明的铜检测管的结构是一根两端熔封,下端拉细的玻璃管内装有二乙基氨荒酸铅〔DDTC-Pb〕螯合化树脂检知剂,并在此检知剂的两端塞堵着脱脂棉所构成的。二乙基氨荒酸铅〔DDTC-Pb〕螯合化树脂合成方法如下:在100~200毫升的蒸馏水中加入1克其粒度为100~200目的粉末状强碱阴离子交换树脂〔201×8〕,置于24°~26℃的水浴中,并以380~410转/分的速度连续搅拌10~12分钟,然后加入1.5~5毫升1%浓度的二乙基氨荒酸钠〔DDTC-Na〕水溶液,至少搅拌30分钟后再加入1%浓度的硝酸铅水溶液1~3毫升,继续反应10~20分钟,停止搅拌,取出过滤、洗净,在50℃以下的温度范围内干燥至含水量为20~30%,置暗处保存。使用时按上述结构装入玻璃管。测量水样中含铜量时,先将管的两端切断,用乳胶管将粗端与玻璃小漏斗连接在一起,垂直放在试管架上,检测管的下端插入底部放有脱脂棉的玻璃小烧杯内并使其接触脱脂棉。用移液管取待测水样品加入玻璃小漏斗内,样品靠自重和脱脂棉的毛吸作用自动流过检测管,待样品自动流完,测量自动结束。样品中的铜离子与管内的白黄色检知剂发生化学反应,生成深棕褐色色带,色带长度与样品中含铜量成比例,测量色带长度并查标准曲线,就能得出样品中的含铜量。
本发明铜检测管价格低廉,一只铜检测管成本才几角钱。被测水样适应范围宽,只要水样的PH值在1.5~7的范围内均可准确地测出水样中的含铜量。测量过程不需要动力,也不需要专人看管与操作,样品自行通过检测管后,测量结果可在48小时内的任何时候读取。检测管本身与其它所用的用具体积都很小,总重量不会超过1公斤,易于随身携带。
本发明检测管是基于测量所产生的色带长度进行定量的。本发明采用二乙基氨荒酸铅螯合化树脂做检知剂,其颜色为白黄色,与样品中的铜离子发生化学反应后生成深棕褐色色带,色带鲜明、层界清楚、整齐,因此,测定被测水中的含铜量的准确度、精密度都高于前文日本报导的检测管。
本发明铜检测管灵敏度高,含铜量的检测范围为0.5~40PPm,最小检测量为0.5PPm,适合于工厂、企业废水处理的自我控制性检测。
本发明铜检测管对于常见的阴离子SO 4、NO- 3、Cl-、F-、CO 3、PO 4、CH3COO-和常见的阳离子K+、Na+、Ca++、Mg++、Al+++、Fe++、Mn++、Pb++、Zn++、Cd++等其共存量高达1000微克/毫升时对含铜量的测定均未发现影响。
实施例:
本发明铜检测管的结构如附图所示,一根两端熔封、内径2.5毫米、总长120毫米、下端拉细的玻璃管1,管内较粗段内装有180毫克铜检知剂2,在检知剂的两端塞堵有脱脂棉3,铜检知剂为二乙基氨荒酸铅〔DDTC-Pb〕螯合化树脂,其合成方法如下:在500毫升的玻璃烧杯中加入180毫升的蒸馏水,再加入1克其粒度为100~200目的粉末状强碱阴离子交换树脂〔201×8〕,置于25℃的水浴中以380转/分的速度连续搅拌10分钟后加入2.8毫升1%浓度的二乙基氨荒酸钠〔DDTC-Na〕水溶液,30分钟后再加入2.8毫升1%浓度的硝酸铅水溶液,继续反应20分钟,停止搅拌,取出过滤、洗净,在45℃干燥至含水量为25%。称取此检知剂180毫升装入玻璃管内,同时先后塞堵脱脂棉,然后熔封。使用时先将检测管的两端切断,用乳胶管将粗端与直径30毫米的玻璃小漏斗连接在一起,垂直放在试管架上,检测管的下端插入底部有脱脂棉的玻璃小烧杯中并使其接触脱脂棉,用移液管量取2毫升待测水样,加入玻璃小漏斗内,样品靠自重和脱脂棉的毛吸作用自动流过检测管,30分钟内样品流完,测量自动结束。在样品流经检测管时,样品中的铜离子与管内的白黄色检知剂发生化学反应,生成深棕褐色色带,测量色带长度并查标准曲线,就得出样品中的含铜量。
曾用本发明铜检测管按上述方法步骤测定含铜量为40微克/毫升的水样,共做10次,其色带长度测量的标准偏差为0.53,精密度为3.2%。用含铜量为40微克/毫升的水样品进行8次测量,其含铜量测量的相对误差和精密度均优于5%。

Claims (3)

1、本发明所涉及的是一种测定水中有害金属铜检测管,其特征在于检测管是一根两端熔封、下端拉细的玻璃管内装有二乙基氨荒酸铅[DDTC-Pb]螯合化树脂检知剂并在此检知剂的两端塞堵有脱脂棉所构成的。
2、按照权利要求1所述的测定水中有害金属铜的检测管,其特征在于二乙基氨荒酸铅〔DDTC-Pb〕螯合化树脂在合成过程中,强碱阴离子交换树脂〔201×8〕、1%浓度的二乙基氨荒酸钠〔DDTC-Na〕水溶液、1%浓度的硝酸铅水溶液之比为:
强碱阴离子交换树脂〔201×8〕:1克
1%浓度的二乙基氨荒酸钠水溶液:1.5~5毫升。
1%浓度的硝酸铅水溶液:1~3毫升
3、按照权利要求1所述的测定水中有害金属铜的检测管,其特征在于二乙基氨荒酸铅〔DDTC-Pb〕螯合化树脂在合成过程中,强碱阴离子交换树脂〔201×8〕首先置于蒸馏水中,然后在24°~26℃的水浴中以380~410转/分的速度连续搅拌10~12分钟,再加入1%浓度的二乙基氨荒酸钠〔DDTC-Na〕水溶液,连续搅拌至少30分钟后再加入1%浓度的硝酸铅水溶液,继续反应10~20分钟,停止搅拌,取出过滤、洗净,在50℃以下的温度范围内干燥至含水量为20~30%,置暗处保存。
CN87106810.9A 1987-10-14 1987-10-14 简易快速测定水中有害金属铜检测管 Expired CN1004583B (zh)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100465618C (zh) * 2007-02-05 2009-03-04 同济大学 光吸收比差-连续流动测定痕量铜离子的方法
CN101435778B (zh) * 2007-11-12 2011-05-11 国家纳米科学中心 一种直接用眼睛定性检测溶液中Cu2+的方法
CN103018235A (zh) * 2012-11-23 2013-04-03 沈阳理工大学 一种镍的分离富集显色测定柱及其制备方法

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100465618C (zh) * 2007-02-05 2009-03-04 同济大学 光吸收比差-连续流动测定痕量铜离子的方法
CN101435778B (zh) * 2007-11-12 2011-05-11 国家纳米科学中心 一种直接用眼睛定性检测溶液中Cu2+的方法
CN103018235A (zh) * 2012-11-23 2013-04-03 沈阳理工大学 一种镍的分离富集显色测定柱及其制备方法
CN103018235B (zh) * 2012-11-23 2015-04-08 沈阳理工大学 一种镍的分离富集显色测定柱的制备方法

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