CN103344629B - The ICP-AES measurement method of lead content in water - Google Patents
The ICP-AES measurement method of lead content in water Download PDFInfo
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- CN103344629B CN103344629B CN201310261597.0A CN201310261597A CN103344629B CN 103344629 B CN103344629 B CN 103344629B CN 201310261597 A CN201310261597 A CN 201310261597A CN 103344629 B CN103344629 B CN 103344629B
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Abstract
A kind of measuring method of metallic lead in water content, the method adopts ICP-AES method to measure the content of metallic lead in water, leaded aqueous sample is first dissolved by the method, carry out post bake after adding a certain amount of carbon sodium hydride solution, salpeter solution and citrate one potassium cyanide solution to clear up, it is possible to effectively metallic lead is dissolved；Then adopt ICP-AES spectrogrph to plumbous content measurement, adopt the method detection matrix interference little, it is possible to meet the needs of production.
Description
Technical field
The present invention relates to elementary analysis field, measure lead metal element especially with ICP-AES inductively coupled plasma atomic emission spectrum.
Background technology
Content plumbous in natural water is very micro-, and some river, when the mineral deposit flowed through containing plumbous matter or stratum, often contains the lead (0.04～0.08mg/L) of trace.The discharge of the industrial wastewaters such as accumulator, metallurgy, five metals, machinery, electroplating industry, is source plumbous in natural water.
Plumbous mensuration is generally adopted spectrophotography and atomic absorption spectrophotometry.But it is more complicated that these methods prepare solution, accuracy of measurement is not high.ICP-AES coupled plasma Plasma-Atomic Emission spectrographic method can measure the trace element in water accurately, effectively lead content in water is monitored.
Summary of the invention
In a kind of water, the ICP-AES plasmon coupling atomic emissions method measuring method of lead content, the steps include:
Step (1): weigh water sample 200ml to be measured in beaker, 3g carbon sodium hydride, in 90-110 degree Celsius temperature range: keep 5-7 minute at certain temperature, and then heating keeps 5-7 minute to another temperature；It is neutralized to appearance muddiness, stirring with nitric acid and citrate one potassium cyanide, adds the nitric acid 15ml of concentration (1+1), after cooling, move in 1L volumetric flask, be diluted with water to scale, shake up stand-by；
The plumbous standard solution of step (2): accurately weigh 1.0g in 200ml beaker, add 50ml water and 3g carbon sodium hydride, in 90-110 degree Celsius temperature range: keep 5-7 minute at certain temperature, and then heating keeps 5-7 minute to another temperature；It is neutralized to appearance muddiness, stirring with nitric acid and citrate one potassium cyanide, adds the nitric acid 10ml of concentration (1+1), after cooling, move in 1L volumetric flask, be diluted with water to scale, shake up；
Step (3) take out respectively again 0 μ L, 50 μ L, 100 μ L, 200 μ L, 400 μ L described plumbous standard solution mother solution be respectively placed in 10mL volumetric flask, be diluted to standard working solution respectively with high-purity water, it is thus achieved that 0 μ L, 50 μ L, 100 μ L, 200 μ L, 400 μ L standard working solution in the content of lead element correspond to 0 μ g/L, 5 μ g/L, 10 μ g/L, 20 μ g/L, 40 μ g/L respectively；
The standard working solution obtained according to step (2) and the Specimen eliminating solution obtained according to step (1) are measured: the Specimen eliminating solution that the plumbous standard solution obtain step (2) and step (1) obtain imports inductively coupled plasma atomic emission spectrometer, i.e. ICP-AES instrument, mixing before entering nebulizer；First measure plumbous standard solution, further according to the known content of lead element in standard solution and inductively coupled plasma atomic emission spectrometer, namely ICP-AES Instrument measuring to lead element response value draw the standard working curve of lead element respectively, then Specimen eliminating solution and the response value of blank digestion solution element are measured, the concentration value of concentration value and the Specimen eliminating solution lead element obtaining blank digestion solution lead element is calculated, thus obtaining underwater gold to belong to the content of Element Lead according to standard working curve.
Described inductively-coupled plasma spectrometer, running parameter is: radio-frequency power 1000W, plasma gas flow rate 12.0L/min, the time of integration 30s.Nebulizer flow 0.8L/min, assisted gas flow 1.5L/min, nebulizer pressure is 200kPa, and the rate of rise is 15kPa/s, and peristaltic pump rotating speed is 100r/min, number of repetition 3 times.
Can well preparing lead solution to be measured by the High Temperature High Pressure digestion procedure of above-mentioned record, this is cleared up the reagent adopted and can g of slag sample well be cleared up with parameter, to facilitate follow-up measurement.
Adopting ICP-AES method can also well solve the matrix interference of other element, accuracy is high.
The method that have employed post bake in the measurement process of this method, can well solve element in prior art and dissolve insufficient, the shortcoming that measurement error is big.
Specific embodiment
Embodiment 1
Step (1): weigh water sample 200ml to be measured in beaker, 3g carbon sodium hydride, keep 5 minutes under 90 degrees Celsius, and then heating keeps 5 minutes under 110 degrees Celsius；It is neutralized to appearance muddiness, stirring with nitric acid and citrate one potassium cyanide, adds the nitric acid 15ml of concentration (1+1), after cooling, move in 1L volumetric flask, be diluted with water to scale, shake up stand-by；
The plumbous standard solution of step (2): accurately weigh 1.0g in 200ml beaker, add 50ml water and 3g carbon sodium hydride, keep 5 minutes under 90 degree celsius temperature, and then heat under 110 degrees Celsius maintenance 5 minutes；It is neutralized to appearance muddiness, stirring with nitric acid and citrate one potassium cyanide, adds the nitric acid 15ml of concentration (1+1), after cooling, move in 1L volumetric flask, be diluted with water to scale, shake up；
Step (3) take out respectively again 0 μ L, 50 μ L, 100 μ L, 200 μ L, 400 μ L described plumbous standard solution mother solution be respectively placed in 10mL volumetric flask, be diluted to standard working solution respectively with high-purity water, it is thus achieved that 0 μ L, 50 μ L, 100 μ L, 200 μ L, 400 μ L standard working solution in the content of lead element correspond to 0 μ g/L, 5 μ g/L, 10 μ g/L, 20 μ g/L, 40 μ g/L respectively；
The standard working solution obtained according to step (2) and the Specimen eliminating solution obtained according to step (1) are measured: the Specimen eliminating solution that the plumbous standard solution obtain step (2) and step (1) obtain imports inductively coupled plasma atomic emission spectrometer, i.e. ICP-AES instrument, mixing before entering nebulizer；First measure plumbous standard solution, further according to the known content of lead element in standard solution and inductively coupled plasma atomic emission spectrometer, namely ICP-AES Instrument measuring to lead element response value draw the standard working curve of lead element respectively, then Specimen eliminating solution and the response value of blank digestion solution element are measured, the concentration value of concentration value and the Specimen eliminating solution lead element obtaining blank digestion solution lead element is calculated, thus obtaining underwater gold to belong to the content of Element Lead according to standard working curve.
Described inductively-coupled plasma spectrometer, running parameter is:
Radio-frequency power 1000W,
Plasma gas flow rate 12.0L/min,
The time of integration 30s.
Nebulizer flow 0.8L/min,
Assisted gas flow 1.5L/min,
Nebulizer pressure is 200kPa,
The rate of rise is 15kPa/s,
Peristaltic pump rotating speed is 100r/min,
Number of repetition 3 times.
Embodiment 2
Step (1): weigh water sample 200ml to be measured in beaker, 3g carbon sodium hydride, keep 7 minutes under 90 degrees Celsius, and then heating keeps 7 minutes under 105 degrees Celsius；It is neutralized to appearance muddiness, stirring with nitric acid and citrate one potassium cyanide, adds the nitric acid 15ml of concentration (1+1), after cooling, move in 1L volumetric flask, be diluted with water to scale, shake up stand-by；
The plumbous standard solution of step (2): accurately weigh 1.0g in 200ml beaker, add 50ml water and 3g carbon sodium hydride, keep 7 minutes under 90 degree celsius temperature, and then heat under 105 degrees Celsius maintenance 7 minutes；It is neutralized to appearance muddiness, stirring with nitric acid and citrate one potassium cyanide, adds the nitric acid 15ml of concentration (1+1), after cooling, move in 1L volumetric flask, be diluted with water to scale, shake up；
Step (3) take out respectively again 0 μ L, 50 μ L, 100 μ L, 200 μ L, 400 μ L described plumbous standard solution mother solution be respectively placed in 10mL volumetric flask, be diluted to standard working solution respectively with high-purity water, it is thus achieved that 0 μ L, 50 μ L, 100 μ L, 200 μ L, 400 μ L standard working solution in the content of lead element correspond to 0 μ g/L, 5 μ g/L, 10 μ g/L, 20 μ g/L, 40 μ g/L respectively；
The standard working solution obtained according to step (2) and the Specimen eliminating solution obtained according to step (1) are measured: the Specimen eliminating solution that the plumbous standard solution obtain step (2) and step (1) obtain imports inductively coupled plasma atomic emission spectrometer, i.e. ICP-AES instrument, mixing before entering nebulizer；First measure plumbous standard solution, further according to the known content of lead element in standard solution and inductively coupled plasma atomic emission spectrometer, namely ICP-AES Instrument measuring to lead element response value draw the standard working curve of lead element respectively, then Specimen eliminating solution and the response value of blank digestion solution element are measured, the concentration value of concentration value and the Specimen eliminating solution lead element obtaining blank digestion solution lead element is calculated, thus obtaining underwater gold to belong to the content of Element Lead according to standard working curve.
Described inductively-coupled plasma spectrometer, running parameter is:
Radio-frequency power 1000W,
Plasma gas flow rate 12.0L/min,
The time of integration 30s.
Nebulizer flow 0.8L/min,
Assisted gas flow 1.5L/min,
Nebulizer pressure is 200kPa,
The rate of rise is 15kPa/s,
Peristaltic pump rotating speed is 100r/min,
Number of repetition 3 times.
Lead content in water has been carried out effective measurement by this method creationary use ICP-AES inductively coupled plasma atomic emission spectrometer；And before measuring sample being performed twice at heating to clear up, the amount of temperature and solvent is accurately controlled by the method, so that clear up more abundant, it is simple to the measurement of subsequent optical spectrometer.
Claims (1)
1. an ICP-AES plasmon coupling atomic emissions method measuring method for lead content in aqueous solution, the steps include:
Step (1): weigh water sample 200ml to be measured in beaker, 3g carbon sodium hydride, keep 5 minutes under 95 degree celsius temperature, and then heating keeps 5 minutes to 110 degree celsius temperature；It is neutralized to appearance muddiness, stirring with nitric acid and citrate one potassium cyanide, adds the nitric acid 15ml of concentration (1+1), after cooling, move in 1L volumetric flask, be diluted with water to scale, shake up stand-by；
The plumbous standard solution of step (2): accurately weigh 1.0g in 200ml beaker, add 50ml water and 3g carbon sodium hydride, in 90-110 degree Celsius temperature range: keep 5-7 minute at certain temperature, and then heating keeps 5-7 minute to another temperature；It is neutralized to appearance muddiness, stirring with nitric acid and citrate one potassium cyanide, adds the nitric acid 10ml of concentration (1+1), after cooling, move in 1L volumetric flask, be diluted with water to scale, shake up；
Step (3) take out respectively again 0 μ L, 50 μ L, 100 μ L, 200 μ L, 400 μ L described plumbous standard solution mother solution be respectively placed in 10mL volumetric flask, be diluted to standard working solution respectively with high-purity water, it is thus achieved that 0 μ L, 50 μ L, 100 μ L, 200 μ L, 400 μ L standard working solution in the content of lead element correspond to 0 μ g/L, 5 μ g/L, 10 μ g/L, 20 μ g/L, 40 μ g/L respectively；
The standard working solution obtained according to step (2) and the Specimen eliminating solution obtained according to step (1) are measured: the Specimen eliminating solution that the plumbous standard solution obtain step (2) and step (1) obtain imports inductively coupled plasma atomic emission spectrometer, i.e. ICP-AES instrument, mixing before entering nebulizer；First measure plumbous standard solution, further according to the known content of lead element in standard solution and inductively coupled plasma atomic emission spectrometer, namely ICP-AES Instrument measuring to lead element response value draw the standard working curve of lead element respectively, then Specimen eliminating solution and the response value of blank digestion solution element are measured, the concentration value of concentration value and the Specimen eliminating solution lead element obtaining blank digestion solution lead element is calculated, thus obtaining underwater gold to belong to the content of Element Lead according to standard working curve；
Described inductively-coupled plasma spectrometer, running parameter is: radio-frequency power 1000W, plasma gas flow rate 12.0L/min, the time of integration 30s；Nebulizer flow 0.8L/min, assisted gas flow 1.5L/min, nebulizer pressure is 200kPa, and the rate of rise is 15kPa/s, and peristaltic pump rotating speed is 100r/min, number of repetition 3 times.
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| CN105067590A (en) * | 2015-07-16 | 2015-11-18 | 西安航空动力股份有限公司 | Method for measuring content of lead and bismuth elements in depollution solution |
| CN105628684B (en) * | 2015-12-30 | 2019-10-08 | 河南省有色金属地质勘查总院 | A method of utilizing high-content lead in ICP-AES method measurement Pb-Zn deposits |
| CN106124484A (en) * | 2016-06-16 | 2016-11-16 | 重庆天原化工有限公司 | Sodium hypochlorite low content slaine ICP measures pre-treating method |
| US10890574B2 (en) * | 2018-11-05 | 2021-01-12 | Hach Company | Digestion of lead(0) and subsequent colorimetric detection of lead(II) |
| CN111337564A (en) * | 2018-12-18 | 2020-06-26 | 海南先声药业有限公司 | ICP-MS (inductively coupled plasma-mass spectrometry) detection method for content of soluble lead in montmorillonite powder |
| CN111999283A (en) * | 2020-08-14 | 2020-11-27 | 贵州省产品质量检验检测院 | Method for detecting metal ions in methanol fuel |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2291184A (en) * | 1994-07-02 | 1996-01-17 | Natural Environment Res | Inductively-coupled plasma atomic emission spectrometer |
| CN101914059A (en) * | 2010-08-18 | 2010-12-15 | 云南烟草科学研究院 | Analytical reagent for detecting trace lead as well as preparation method and application thereof |
| CN102749298A (en) * | 2012-07-10 | 2012-10-24 | 上海海洋大学 | Determination method for lead in shrimp |
-
2013
- 2013-06-26 CN CN201310261597.0A patent/CN103344629B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2291184A (en) * | 1994-07-02 | 1996-01-17 | Natural Environment Res | Inductively-coupled plasma atomic emission spectrometer |
| CN101914059A (en) * | 2010-08-18 | 2010-12-15 | 云南烟草科学研究院 | Analytical reagent for detecting trace lead as well as preparation method and application thereof |
| CN102749298A (en) * | 2012-07-10 | 2012-10-24 | 上海海洋大学 | Determination method for lead in shrimp |
Non-Patent Citations (4)
| Title |
|---|
| ICP-AES法测定环境水样中的微量镉铬铜镍铅锌;白英彬等;《分析测试技术与仪器》;19990930;第5卷(第3期);第164-167页（具体参见"1.2试剂"、"1.3样品处理"、"分析测定"） * |
| 共聚物吸附剂富集用ICP-AES法测定痕量铅;谢志海等;《分析试验室》;20130228;第32卷(第2期);第122-124页 * |
| 微波消解ICP-AES法同时测定化妆品中Pb、As、Hg;倪伟红等;《分析试验室》;20081231;第27卷;第326-328页 * |
| 微量铅的检测方法综述;潘微平;《广东化工》;20080430;第35卷(第4期);第97-99页（具体参见第1页右栏第2段） * |
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