CN102141487A - Method for separating and enriching trace lead in substrate - Google Patents
Method for separating and enriching trace lead in substrate Download PDFInfo
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- CN102141487A CN102141487A CN 201110001498 CN201110001498A CN102141487A CN 102141487 A CN102141487 A CN 102141487A CN 201110001498 CN201110001498 CN 201110001498 CN 201110001498 A CN201110001498 A CN 201110001498A CN 102141487 A CN102141487 A CN 102141487A
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Abstract
The invention discloses a method for separating and enriching trace lead in a substrate, which comprises the following steps: adding an alkaline precipitator into the substrate with shaking till the pH value of the solution is 7 to 9 and gelatinous precipitate appears in the solution; centrifuging the solution to obtain separated precipitate and supernate and removing the supernate; and according to test requirements, dissolving the precipitate in acid, fixing volume, and performing quantitative or fingerprint analysis on the lead in the solution. In the invention, a precipitation-centrifugation process is used to remove a large amount of Na, K and other ions which are not precipitated in the substrate from the supernate, the trace lead ions are separated and enriched at one step, the operation is simple and convenient, the repeatability is high, the recovery rate is high, fewer pollutants are introduced, and the method can be used for samples in which the substrate has high concentration and complex components.
Description
Technical field
The present invention relates to the separation method of trace lead, relate in particular to the method for separating and concentrating of trace lead in the sample of a kind of matrix concentration height and complicated component.
Background technology
When carrying out lead and plumbous fingerprint detection, traditional detection method is directly to detect after sample is cleared up.And for samples such as biology, food, environment, low and the relative matrix concentration height of lead content, element complexity, in mensuration, sensitivity, precision and the accuracy of the serious interference Instrument test of matrix effect meeting also can cause problems such as baseline wander, injection port pollution even obstruction simultaneously.
In order to overcome the variety of problems that traditional detection method is brought, further improve sensitivity, precision and the accuracy of assay method, produced the lead in the Specimen eliminating liquid has been separated technology with enrichment in advance.This technology can make analyzes detection limit, precision and effectively improvement of accuracy acquisition, through after the separation and concentration, but up to a hundred samples of instrument METHOD FOR CONTINUOUS DETERMINATION, and state is very stable.
At present at the various method for separating and concentrating of lead mainly leadedly recycle used batteries, industrial circles such as mining, wastewater treatment.What also be primarily aimed in the analytical chemistry field is the enrichment of the lead of ppm level (mcg/ml) concentration, and commonly used has Sulfhydryl Cotton post, the cotton post of xanthan ester, sulfhydryl dextran gel or chelating resin post and organic and inorganic mesoporous material, liquid film, molecular sieve and add coprecipitator etc.
The defective that above-mentioned separation and concentration technology exists is: step is comparatively loaded down with trivial details, concentration and separation is subjected to a lot of condition influence; Different samples, the condition of enrichment and wash-out all need be groped separately, and the plumbous recovery and reappearance all can not guarantee, even also can introduce new pollution (such as initiate coprecipitator, eluant, eluent etc.); This, is difficult to realize with regard to the plumbous separation and concentration of the ppb level (nanograms/milliliter) of trace very for content own; If sample type differs greatly, and matrix situation complexity, just more cannot say for sure to demonstrate,prove the separation and concentration effect.
Summary of the invention
The object of the present invention is to provide the method for separating and concentrating of trace lead in a kind of matrix.Based on the present invention, can one the step with the lead ion separation and concentration, satisfy the detection requirement of trace lead and plumbous fingerprint in the complicated substrate.
The method for separating and concentrating of trace lead comprises the steps: at room temperature in a kind of matrix of the present invention, adds alkaline precipitating agent in matrix, and the limit edged shakes up, and is 7～9 until the pH value of solution value, occurs the colloidal precipitation simultaneously in the solution; The solution that forms the colloidal precipitation is carried out centrifugally operated, form the precipitation and the supernatant of layering, supernatant is discarded; According to measuring requirement, described precipitation with acid dissolving and constant volume, is carried out quantitatively or fingerprint analysis wherein lead afterwards.
Above-mentioned method for separating and concentrating, preferred described precipitation agent adds in the step, and described precipitation agent is NH
3H
2O.
Above-mentioned method for separating and concentrating, preferred described precipitation agent adds in the step, and described precipitation agent is NaOH or KOH.
Above-mentioned method for separating and concentrating, in the preferred described separating step, the centrifugal revolution of described centrifugally operated is (3000～8000) rev/min; The time that centrifugally operated continues was greater than 3 minutes.
Above-mentioned method for separating and concentrating, in the preferred described determination step, described acid is that mass percent concentration is the HNO of (1+q) %
3, q is the natural number of 1-40.
In terms of existing technologies, the present invention has following advantage: the first, Pb recovery height, favorable reproducibility, the plumbous recovery is up to more than 99%, even the ultratrace lead of ppb level (ng/mL) also well separation and concentration come out, measure through actual sample, reappearance is very good; The second, easy and simple to handle, use method of the present invention can realize a step precipitation, other equipment and process engineering need not be increased and just concentration and separation can be effectively carried out; Three, cost is low, and used precipitation dosage is few and cheap, buys easily, and test is realized easily; Four, introduce pollution and lack, do not contact organic reagent, avoid introducing in the operating process too much ion or pollution simultaneously; Five, matrix ion remaval rate height: can remove the Na, the K plasma that occupy the proportion maximum in the digestive juice preferably, effectively reduce matrix effect, avoid of the interference of high concentration matrix to measured signal; Six, applied range: desire be can be widely used in and plumbous and isotopic various complicated substrate sample detected, and can leaded per sample situation, concentrate, measure requirement to satisfy.For analytical test work provides better sample-pretreating method, can improve sensitivity, precision and the accuracy of mensuration greatly.
In sum, the present invention is a kind of easy trace lead method for separating and concentrating, this method adopts precipitation-centrifugation method, supernatant is removed a large amount of non-setting Na, K plasma in the digestion solution, the lead ion separation and concentration of one step with trace comes out, easy and simple to handle and favorable reproducibility, recovery height, introduce pollute few; The sample that can be used for matrix concentration height and complicated component.
Description of drawings
Fig. 1 is the flow chart of steps of the method for separating and concentrating embodiment of trace lead in the matrix of the present invention;
Fig. 2 is the process flow diagram of the method for separating and concentrating preferred embodiment of trace lead in the matrix of the present invention.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, the present invention is further detailed explanation below in conjunction with the drawings and specific embodiments.
At first, plumbous fingerprint, digestion solution and matrix are explained.
● the lead of plumbous fingerprint occurring in nature with
204Pb,
206Pb,
207Pb,
208Four kinds of isotope forms of Pb exist, and the lead of separate sources has different isotopics, and can not change with the variation of physics, chemistry and biotic factor.Compare by four kinds of isotopic abundances and can constitute three independently isotopic ratios, be referred to as " plumbous fingerprint ".
● digestion solution: clearing up is to destroy the organism in the sample or the method for reducing substances with acid solution or alkali lye and under heating condition.This method can all be destroyed the organism in the various samples and reducing substances and heat-labile material etc., and resulting supernatant liquid is called digestion solution.
● matrix: be all non-test substances of other except that element to be measured in the sample.Therefore, in the multielement system, the matrix of same sample is different for each element to be measured in the sample.
With reference to Fig. 1, Fig. 1 is the flow chart of steps of the method for separating and concentrating embodiment of trace lead in the matrix of the present invention, comprise the steps: that precipitation agent adds step S110, at room temperature, in matrix, add alkaline precipitating agent, the limit edged shakes up, and is 7～9 until the pH value of solution value, occurs the colloidal precipitation simultaneously in the solution; Separating step S120 carries out centrifugally operated to the solution that forms the colloidal precipitation, forms the precipitation and the supernatant of layering, supernatant is discarded, farthest to discard in the complicated substrate the non-precipitating ion based on Na, K ion.Determination step S130 according to measuring requirement, with acid dissolving and constant volume, carries out described precipitation quantitatively or fingerprint analysis wherein lead afterwards.
In the present embodiment, adopt the precipitation method, a step is come out the trace lead ion isolation enrichment in the matrix, and lead ion can reach ppb level (ng/mL) concentration; And, during resolution of precipitate, can require constant volume according to measuring, reach the concentrated purpose of trace lead; Simple to operate, can realize separation and concentration with single precipitation agent, need not to introduce organic reagent.
The foregoing description mainly is by a step precipitation trace lead separation and concentration to be come out.Need to prove that the selection of precipitation agent has multiple scheme, can select NH
3H
2O can avoid introducing metallic ion like this in system, increase the complicacy of matrix.But under the situation of control pH value, also can be used as precipitation agent as alkaline reagents such as NaOH, KOH; In addition, within protection scope of the present invention, the present invention does not do concrete qualification for the selection of precipitation agent to other known for those skilled in the art alkaline reagents yet.
With reference to Fig. 2, Fig. 2 is the process flow diagram of the method for separating and concentrating preferred embodiment of trace lead in the matrix of the present invention, and detailed process is as follows:
At room temperature, in matrix, directly add NH
3H
2The O precipitation agent, attention will slowly add, and the limit edged shakes up, and notices that pH value changes, and reaches neutrality or alkalescent with pH value and is (pH 7～9) well, and can observe at this moment has colloidal to precipitate appearance in the solution.NH
3H
2The O precipitation agent is not introduce metallic ion with respect to the advantage of highly basic such as NaOH, KOH.Then, above-mentioned solution is carried out centrifugal, centrifugal condition is, revolution is (3000～8000) rev/min; The time that centrifugally operated continues was greater than 3 minutes.After centrifugal, precipitation and supernatant layering, abandoning supernatant, the liquid above will precipitate as far as possible blots, and farthest discards in the complicated substrate the non-precipitating ion based on Na, K ion.At last, according to measuring requirement, with (1+q) %HNO
3Dissolution precipitation and constant volume carry out quantitatively or fingerprint analysis wherein lead afterwards.Present embodiment is by using single precipitation agent NH
3H
2O, control solution is alkalescent, a step is realized the concentration and separation of ppb level concentration trace lead; NH
3H
2O can not pollute precipitation to be measured, does not introduce metallic ion; Easy and simple to handle, the method favorable reproducibility; And owing to do not need to carry out the wash-out operation, the absorption, the elution requirement that need not at different samples are groped, and can not introduce other pollutions such as eluant, eluent; In addition, because NH
3H
2O is not an organic reagent, can not introduce new metallic ion yet, causes difficulty can for the separation and concentration of trace lead.
More than the method for separating and concentrating of trace lead in a kind of matrix provided by the present invention is described in detail, used specific embodiment herein principle of the present invention and embodiment are set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof; Simultaneously, for one of ordinary skill in the art, according to thought of the present invention, part in specific embodiments and applications all can change.In sum, this description should not be construed as limitation of the present invention.
Claims (5)
1. the method for separating and concentrating of trace lead in the matrix is characterized in that, comprises the steps:
Precipitation agent adds step: at room temperature, add alkaline precipitating agent in matrix, the limit edged shakes up, and is 7～9 until the pH value of solution value, occurs the colloidal precipitation simultaneously in the solution;
Separating step: the solution that forms the colloidal precipitation is carried out centrifugally operated, form the precipitation and the supernatant of layering, supernatant is discarded;
Determination step: according to measuring requirement, described precipitation with acid dissolving and constant volume, is carried out quantitatively or fingerprint analysis wherein lead afterwards.
2. method for separating and concentrating according to claim 1 is characterized in that, described precipitation agent adds in the step, and described precipitation agent is NH
3H
2O.
3. method for separating and concentrating according to claim 1 is characterized in that, described precipitation agent adds in the step, and described precipitation agent is NaOH or KOH.
4. according to each described method for separating and concentrating in the claim 1 to 3, it is characterized in that in the described separating step, the centrifugal revolution of described centrifugally operated is (3000～8000) rev/min; The time that centrifugally operated continues was greater than 3 minutes.
5. method for separating and concentrating according to claim 4 is characterized in that, in the described determination step, described acid is that mass percent concentration is the HNO of (1+q) %
3, q is the natural number of 1-40.
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| CN 201110001498 CN102141487B (en) | 2010-12-16 | 2011-01-06 | Method for separating and enriching trace lead in substrate |
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| CN201010591493 | 2010-12-16 | ||
| CN201010591493.2 | 2010-12-16 | ||
| CN 201110001498 CN102141487B (en) | 2010-12-16 | 2011-01-06 | Method for separating and enriching trace lead in substrate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102814196A (en) * | 2012-09-18 | 2012-12-12 | 济南大学 | Preparation method and application of dextrangel-supported nanogold catalyst |
| CN103645085A (en) * | 2013-12-26 | 2014-03-19 | 中南大学 | Device and method for settling high-temperature thick complex feed liquid base body on line |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1427298A1 (en) * | 1986-10-02 | 1988-09-30 | Киргизский Государственный Университет Им.50-Летия Ссср | Method of detecting humic acids in natural water |
| KR20070027154A (en) * | 2005-09-06 | 2007-03-09 | 현대자동차주식회사 | Sample pre-treatment method for pb analysis of break lining |
| CN101042349A (en) * | 2007-04-28 | 2007-09-26 | 云南出入境检验检疫局检验检疫技术中心 | Measuring method for harmful elements including lead, copper, chromium and cadmium in lotus root |
| CN101055252A (en) * | 2007-05-31 | 2007-10-17 | 中国铝业股份有限公司 | Method for determining minim plumbum of aluminium ingot |
| US20090263907A1 (en) * | 2006-08-28 | 2009-10-22 | Kowa Co., Ltd. | Reagent for lead concentration determination and method of determining lead concentration |
| CN101713714A (en) * | 2009-12-29 | 2010-05-26 | 南京工业大学 | Method for separating cadmium ion and lead ion from enrichment environmental water body by using bulk liquid membrane |
-
2011
- 2011-01-06 CN CN 201110001498 patent/CN102141487B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1427298A1 (en) * | 1986-10-02 | 1988-09-30 | Киргизский Государственный Университет Им.50-Летия Ссср | Method of detecting humic acids in natural water |
| KR20070027154A (en) * | 2005-09-06 | 2007-03-09 | 현대자동차주식회사 | Sample pre-treatment method for pb analysis of break lining |
| US20090263907A1 (en) * | 2006-08-28 | 2009-10-22 | Kowa Co., Ltd. | Reagent for lead concentration determination and method of determining lead concentration |
| CN101042349A (en) * | 2007-04-28 | 2007-09-26 | 云南出入境检验检疫局检验检疫技术中心 | Measuring method for harmful elements including lead, copper, chromium and cadmium in lotus root |
| CN101055252A (en) * | 2007-05-31 | 2007-10-17 | 中国铝业股份有限公司 | Method for determining minim plumbum of aluminium ingot |
| CN101713714A (en) * | 2009-12-29 | 2010-05-26 | 南京工业大学 | Method for separating cadmium ion and lead ion from enrichment environmental water body by using bulk liquid membrane |
Non-Patent Citations (2)
| Title |
|---|
| 《Clean-Soil, Air, Water》 20101130 Nagihan M. Karaaslan et al. Novel Polymeric Resin for Solid Phase Extraction and Determination of Lead in Waters 1047-1054 1-5 第38卷, 第11期 * |
| 《中国食品学报》 20100428 赵广英等 微型DPSA-1仪-SPCE微分电位溶出法快速检测茶叶中的微量铅 187-194 1-5 第10卷, 第2期 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102814196A (en) * | 2012-09-18 | 2012-12-12 | 济南大学 | Preparation method and application of dextrangel-supported nanogold catalyst |
| CN102814196B (en) * | 2012-09-18 | 2014-05-07 | 济南大学 | Preparation method and application of dextrangel-supported nanogold catalyst |
| CN103645085A (en) * | 2013-12-26 | 2014-03-19 | 中南大学 | Device and method for settling high-temperature thick complex feed liquid base body on line |
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| CN102141487B (en) | 2012-10-17 |
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Inventor after: Wu Jing Inventor after: Wang Jingyu Inventor after: Yan Lailai Inventor after: Tang Xiaoping Inventor before: Wu Jing Inventor before: Wang Jingyu Inventor before: Yan Lailai |
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Effective date of registration: 20111101 Address after: 100871 Zhongguancun the Summer Palace Road, Beijing, No. 5, No. Applicant after: Peking University Co-applicant after: Beijing Entry-exit Inspection and Quarantine Bureau, the People's Republic of China Address before: 100871 Zhongguancun the Summer Palace Road, Beijing, No. 5, No. Applicant before: Peking University |
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