CN107421896A - The separation and concentration and detection method of micro cadmium ion in seawater - Google Patents
The separation and concentration and detection method of micro cadmium ion in seawater Download PDFInfo
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- CN107421896A CN107421896A CN201710304266.9A CN201710304266A CN107421896A CN 107421896 A CN107421896 A CN 107421896A CN 201710304266 A CN201710304266 A CN 201710304266A CN 107421896 A CN107421896 A CN 107421896A
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Abstract
The invention discloses the separation and concentration and detection method of micro cadmium ion in seawater, utilize the characterization of adsorption of strong-base anion-exchange resin, the selective Adsorption of Cadmium from seawater in 1 mol/L hydrochloric acid mediums, cadmium ion is washed down from resin with dilute nitric acid solution again, the separation and concentration of cadmium is realized, then is detected with atomic absorption spectrum.The present invention spectra1 interfer- caused by eliminating a large amount of sodium chloride, makes follow-up detection become relatively simple, Matrix effects can be completely eliminated in this method, and the rate of recovery, precision are preferable by the way that object is separated with high salt matrix.
Description
Technical field
The present invention relates to the method for measure cadmium in seawater ion concentration, and in particular to separation and concentration cadmium ion is again from seawater
The method detected with atomic absorption spectrum.
Background technology
Substantial amounts of sodium chloride be present in the high salt sample such as salt, seawater, in the presence of a large amount of sodium salts, the survey of micro heavy
Surely it is analytical chemistry recognized problem, such as when detecting the heavy metal element of trace therein with AAS, sodium chloride can influence electric arc
Temperature and very big ambient interferences are produced, cause some trace heavy metals can not Accurate Determining.Examined with ICP or ICP-MS
During survey, substantial amounts of sodium chloride can also block atomizer or be deposited on torch pipe, sampling spiroid, so as to influence the normal use of instrument.
The method of detection cadmium in seawater pollution residual, or using organic solvent both at home and abroad at present, or need to make complexing agent by oneself,
Or using special installation, it is not easy to promote in common lab, organic solvent is harmful, homemade complexing agent short life, nothing
Method is reused for a long time.More is matrix modifier method, such as：Ammonium dihydrogen phosphate, magnesium nitrate, palladium nitrate etc., but it is real
Verify that the improved capacity of bright matrix modifier is very limited, the sodium chloride content of system is preferably controlled within 5/1000ths, is met
The seawater or saturated aqueous common salt higher to salt content, can not overcome ambient interferences, while cadmium in seawater is trace, is taken at all
Dilution means are inadvisable to reduce the method for sodium chloride content, so the method for the addition matrix modifier used at present is one
The individual method that can not be tackled the problem at its root of taking stopgap measures.Matrix phase, actually or matrix modifier is relied on, use matrix
The limitation that modifier eliminates sodium chloride interference is still present, and high salt sample still can not be detected accurately.
The content of the invention
It is an object of the invention to：The separation and concentration and detection method of micro cadmium ion in a kind of seawater are provided, will be micro
Cadmium ion is enriched with again after being separated with sodium chloride matrix, realizes the separation of cadmium ion and seawater, eliminates light caused by a large amount of sodium chloride
Spectrum interference, makes follow-up detection become relatively simple.
The present invention technical solution be：It is selective in hydrochloric acid medium using strong-base anion-exchange resin
The Adsorption of Cadmium from seawater, sodium ion is not adsorbed, recycle dilute nitric acid solution to wash down cadmium ion from resin, by object
It is enriched with again after being separated with high salt matrix, and carries out atomic absorption spectrum detection；It comprises the following steps：
（1）Seawater sample is acidified：Clear liquid is taken after measuring clarification seawater 50mL, or the muddy just centrifugation of seawater, adds 10mL 6mol/L
Hydrochloric acid, mix, the concentration of hydrochloric acid for making system is 1mol/L；
（2）The preparation of small ion exchange column：（1）Make：Small ion exchange column is made from 5mL acid burettes；（2）Dress
Post：First pad dacron thread in column bottom；Then 5.0g strong-base anion-exchange resins are placed in 100mL beakers, add 20mL water, used
After glass bar stirring, resin is transferred in post with suction pipe；Finally plus the high dacron threads of 0.5cm are compressed with glass bar, make resin bed
Highly it is 5cm, resin bed volume is 1.0mL；（3）Post pre-processes：Washed down with 10mL 0.16mol/L nitric acid liquids and be adsorbed in resin
Metal ion, then wash lower nitric acid twice with 10mL moisture, with the mL balance columns of 1 mol/L hydrochloric acid 10, make column regeneration；
（3）Separation and concentration：Draw 10-20mL acidifying sea water solutions and cross post, discarded with 1mL/min flow velocity by post, efflux；
Eluted twice with 10mL moisture, efflux discards；Eluted with 10mL 0.16mol/L nitric acid liquids, collect eluent 10mL, mixed
It is to be measured；Post is crossed with 10mL water and washes lower nitric acid, then crosses post with the mL of 1 mol/L hydrochloric acid 10, and post reactivates；
（4）Detection：Detected using graphite furnace atomic absorption spectrophotometer；Parameter during detection：Cadmium, Detection wavelength 228.8nm, slit
0.7nm, Zeeman deduction background, standard series：0、2、4、6、8、10µg/L；
（5）As a result calculate：Using absorbance as abscissa, concentration is ordinate, draws the standard curve of cadmium ion respectively, passes through survey
Determine the absorbance of cadmium in eluent, cadmium content in sample is calculated with reference to extension rate.
Wherein, it is strong-base anion-exchange resin cadmium separation and the material of sodium to be used in the small ion exchange column,
Specification is 100-200 mesh.
Wherein, the cylinder top of described small ion exchange column uses trumpet type enlarging, and bottom uses flat nick water conservancy diversion.
It is an advantage of the invention that：First, be filled into small ion exchange column with strong-base anion-exchange resin, using strong
The characterization of adsorption of alkalescence anion-exchange resin, in 1 mol/L hydrochloric acid mediums, cadmium ion is by strong-base anion-exchange resin
Selective absorption, and sodium ion is not adsorbed, and recycles dilute nitric acid solution to wash down cadmium from resin, realizes cadmium and seawater matrix
Separation, and carry out atomic absorption method detection, this method eliminates spectra1 interfer- problem existing for conventional method, can accurately detect
The content of cadmium in seawater ion；Second, ion exchange column is minimized, using the amount of resin of about 1mL volumes, lock out operation is easy,
The speed of separation is greatly improved, it is environment-friendly without using harmful organic solvent using only pure water and dilute acid soln；Third,
The strongly basic anionic resin of use may be reused, and analysis cost is cheap.
Brief description of the drawings
Fig. 1 is the elution curve of cadmium and sodium.
Fig. 2 is the small ion exchange column schematic diagram of the present invention.
Embodiment
The technical solution of the present invention is further illustrated with reference to instantiation, but example is not to be construed as to skill
The limitation of art scheme.
First, instrument and reagent：Atomic Absorption Spectrometer（Shimadzu A6300C, PE AA800）；Ultra-pure water instrument（Mi Libo
Milli-Q）；Cadmium standard liquid（State Standard Matter Research Centre）；DOWEX 1-X8 type resin anion (R.A.)s（100 ~ 200 mesh）；
Small ion exchange column（Self-control）；
2nd, experimentation：
1. small ion exchange column makes：Using 5mL acid burettes, the flare that 5cm grows is arranged at post top, such as Fig. 1 institutes
Show；
2. fill post：Pad dacron thread in column bottom；5.0gDOWEX 1-X8 type resin anion (R.A.)s are placed in 100mL beakers, add 20mL
Water, after being stirred with glass bar, resin is transferred in post with suction pipe；Again plus the high dacron threads of 0.5cm, slightly compressed, made with glass bar
Resin layer height is 5cm, and resin bed volume is 1mL；
3. post pre-processes：Wash down the metal ion for being adsorbed in resin with 10mL 0.16mol/L nitric acid liquids, then with 10mL moisture two
It is secondary to wash lower nitric acid, with the mL balance columns of 1 mol/L hydrochloric acid 10, make column regeneration；
4. analytical procedure：Measure clarification seawater 50mL（If seawater is muddy, 4000 revs/min, centrifuge 5 minutes）, add 10mL
6mol/L hydrochloric acid, mix, the concentration of hydrochloric acid for making system is 1mol/L；10-20mL acidifying sea water solutions are drawn, with 1mL/min
Flow velocity discarded by post, efflux；Eluted twice with 10mL moisture, efflux discards；With 10mL 0.16mol/L nitric acid liquids
Elution, eluent 10mL is collected, mixed to be measured；Do blank assay simultaneously；Post, which is crossed, with 10mL water washes lower nitric acid, then with 1 mol/L
The mL of hydrochloric acid 10 crosses post, and post reactivates；
5. detection：Detected using graphite furnace atomic absorption spectrophotometer；Parameter during detection：Cadmium, Detection wavelength 228.8nm, slit
0.7nm, Zeeman deduction background, standard series：0、2、4、6、8、10µg/L.
3rd, result and discussion：
1. in hydrochloric acid medium, the distribution coefficient of cadmium, sodium on DOWEX 1-X8 type resin anion (R.A.)s（Kd）：Distribution coefficient Kd from
Son, which is exchanged in separation, extremely important meaning, and it is metal adsorption capacity on ion exchange resin under the conditions of a certain
Mark；Respectively add dried resin 0.50g in 6 100mL conical flasks, then add 0.1,0.5,1.0,2.0,3.0,4.0 mol/ respectively
The mL of L hydrochloric acid 48, respectively plus concentration is 1000 μ g/mL cadmium standard liquid and the mL of sodium standard solution 1.0, adds magnetic stir bar,
Often stir 2min and place 1h, repeat totally 3 times, filtered after standing overnight, the content of cadmium/sodium in solution is determined, then by following public affairs
Formula calculates adsorption coefficient (Kd) of the cadmium/sodium in different content hydrochloric acid solution, and result of calculation is shown in Table 1.
The cadmium of table 1 and sodium are in HCl media in the distribution coefficient on DOWEX1-X8 anion exchange resin（Kd）
By determining distribution coefficient, the separation condition of element is then determined again, and this is most scientific, most easy method；Kd values are big,
Represent strong in certain adsorption capacity of medium ion over the resin, vice versa；Kd ＞ 40, are adsorbed in by force resin；Kd ＜ 10,
It is not adsorbed in resin；According to the difference of element to be separated and matrix distribution coefficient, suitably select separation condition, realize measured object with
Matrix efficiently separates；Found out by table 1, more than 1mol/L hydrochloric acid mediums, acid resin for cadmium is adsorbed by force, and sodium is not adsorbed, it is contemplated that
Practical application, 1 mol/L hydrochloric acid mediums are selected as adsorbing medium.
2. in nitric acid medium, the distribution coefficient of cadmium, sodium on DOWEX 1-X8 type resin anion (R.A.)s（Kd）：Using same
Method determines the distribution coefficient Kd of Na+ and Cd2+ in nitric acid medium（It is shown in Table 2）；In nitric acid medium, Cd2+ and Na+'s
Kd values are respectively less than 10, i.e., are not adsorbed in resin, therefore elute the Cd2+ adsorbed on resin using salpeter solution；In view of reality
Border application effect, the mol/L salpeter solutions of 10 mL 0.16 are selected as eluent.
The cadmium of table 2 and sodium are in HNO3 media in the distribution coefficient on anion exchange resin（Kd）
3.DOWEX 1-X8 types resin anion (R.A.) adsorbs the measure of cadmium capacity：Carried out using DOWEX 1-X8 types resin anion (R.A.) molten
In liquid during the absorption of cadmium ion, to ensure all to adsorb cadmium ion, adsorption saturation is prevented, it is necessary to determine it to metal
The adsorption capacity of ion, this is significant to cadmium content in accurate determination sample；It is cloudy to weigh a certain amount of DOWEX 1-X8 types
Ion exchange resin dried resin, with a small amount of ultrapure water infiltration, enough cadmium standard liquids known to addition, in 1 mol/L hydrochloric acid mediums,
Constant volume, shake up, vibrated on shaking table, vibrated 1 time per hour, overnight, then determine the concentration of cadmium ions in solution；With total addition
Subtract the cadmium content measured in solution, calculate the cadmium content on resin, then divided by resin weight, draw a resin adsorption huge sum of money
The capacity of category；Calculation formula is as follows：
Ac：Adsorption capacity adsorption capacity（µg/g）
mAdd：Add the quality (μ g) of heavy metal；
c：The concentration (μ g/mL) of heavy metal in solution；
v：Constant volume（mL）；
mResin：Dried resin quality（g）.
Experiment has weighed 0.1g dried resins, is respectively placed in three small beakers, adds 1000 μ g cadmium, constant volume 100mL, treats
After adsorption equilibrium, using concentration of cadmium ions in Flame Atomic Absorption Spectrometry Determination solution；DOWEX is calculated with above-mentioned formula
Adsorption capacity such as table 3 of the 1-X8 types resin anion (R.A.) to cadmium.
Adsorption capacity of the DOWEX 1-X8 types resin anion (R.A.)s of table 3 to cadmium
From table 3 it can be seen that DOWEX 1-X8 types resin anion (R.A.)s are very big to the adsorption capacity of cadmium, it is assumed that only with 0.1g dried resins
Small ion exchange column is filled into, seawater sampling amount is 50mL, post is all crossed after processing, even if the cadmium content of the seawater is
10mg/L, also it is unlikely to make post saturation；General cadmium in seawater content is trace level or trace level mostly, and actually fills post and use
Dried resin weight be generally 0.5g or so, it can be ensured that will not adsorption saturation in detection.
4. the column behavior and elution curve of cadmium, sodium on DOWEX 1-X8 type resin anion (R.A.)s：To observe Cd2+ and Na+
Behavior on anion-exchange resin column, experiment are as follows：1 mg Na+ and 0.1 mg Cd2+ are added in 10 mL solution, will
Sample crosses post, and every 1 mL is collected 1 time；Then with the mL of HCl solution 10 elution posts, every 1 mL is collected 1 time, then with 0.16 mol/
The Cd2+ on post is adsorbed in the elution of L HNO3 solution, and every 1 mL is collected 1 time；The solution of collection is diluted to 10mL and uses ICP- respectively
AES is determined, and observes Cd2+ and Na+ whereabouts, and experiment finds that in 1 mol/L hydrochloric acid mediums, Cd2+ can be adsorbed in the moon by force
Ion exchange resin, show as collect sample liquid and HCl leacheates in all do not detect Cd2+ values；And 0.16 mol/L HNO3
Solution can elute Cd2+ rapidly, that is, Cd2+ reaches maximum in the 3rd mL eluents collected, and sees Fig. 1；For Na+, it is 1
Substantially without absorption in mol/L hydrochloric acid medium.
5. actual sample determines and added recovery：The seawater sample being collected into is separated and surveyed according to experimental method
It is fixed, and add a certain amount of standard liquid thereto respectively, investigate whole experiment process whether there is sample loss, acquired results are shown in Table
4；As a result the recovery of standard addition for showing this method is 90%-95%, and experimentation is reliable and stable.
The measure of the seawater sample of table 4 and addition recovery
To sum up, the degree of accuracy of the present invention is high, and precision is good；The method can solve the problem that the interference that seawater matrix determines to cadmium, operation difficulty
Less；Using commercialization resin, method is reliable and practical, easily promotes.
Claims (3)
1. the separation and concentration and detection method of micro cadmium ion in seawater, it is characterized in that：Utilize strong-base anion-exchange resin
Characterization of adsorption, the selective Adsorption of Cadmium from sea water solution, does not adsorb sodium ion in 1 mol/L hydrochloric acid mediums, then
Cadmium ion is washed down from resin using dilute nitric acid solution, after object is separated with high salt matrix, then carries out atomic absorption light
Spectrum detection；It comprises the following steps：
（1）Seawater sample is acidified：Clarification seawater 50mL is measured, 10mL 6mol/L hydrochloric acid is added, mixes, make the hydrochloric acid of system
Concentration is 1mol/L；
（2）The preparation of small ion exchange column：（1）Make：Small ion exchange column is made from 5mL acid burettes；（2）Dress
Post：First pad dacron thread in column bottom；Then 5.0g strong-base anion-exchange resins are placed in 100mL beakers, add 20mL water, used
After glass bar stirring, resin is transferred in post with suction pipe；Finally plus the high dacron threads of 0.5cm are compressed with glass bar, make resin bed
Highly it is 5cm, resin bed volume is 1.0mL；（3）Post pre-processes：Washed down with 10mL 0.16mol/L nitric acid liquids and be adsorbed in resin
Metal ion, then wash lower nitric acid twice with 10mL moisture, with the mL balance columns of 1 mol/L hydrochloric acid 10, make column regeneration；
（3）Separation and concentration：The sea water solution for drawing 10-20mL acidifyings crosses post, is abandoned with 1mL/min flow velocity by post, efflux
Go；Eluted twice with 10mL moisture, efflux discards；Eluted with 10mL 0.16mol/L nitric acid liquids, collect eluent 10mL, mixed
It is even to be measured；Post is crossed with 10mL water and washes lower nitric acid, then crosses post with the mL of 1 mol/L hydrochloric acid 10, and post reactivates；
（4）Detection：Detected using graphite furnace atomic absorption spectrophotometer；Parameter during detection：Cadmium, Detection wavelength 228.8nm, slit
0.7nm, Zeeman deduction background, standard series：0、2、4、6、8、10µg/L；
（5）As a result calculate：Using absorbance as abscissa, concentration is ordinate, draws the standard curve of cadmium ion respectively, passes through survey
Determine the absorbance of cadmium in eluent, cadmium in seawater content is calculated with reference to extension rate.
2. the separation and concentration and detection method of micro cadmium ion in seawater according to claim 1, it is characterized in that：Using small
Type ion exchange column carries out separation and concentration, the material that cadmium separation and sodium are used in the small ion exchange column be strong basicity the moon from
Sub-exchange resin, specification are 100-200 mesh.
3. the separation and concentration and detection method of micro lead cadmium ion in seawater according to claim 1, it is characterized in that：It is described
The cylinder top of small ion exchange column use flare, bottom uses flat nick water conservancy diversion.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108195781A (en) * | 2018-01-23 | 2018-06-22 | 山东省食品药品检验研究院 | The detection method of lead content in a kind of grape wine |
| CN108896534A (en) * | 2018-05-10 | 2018-11-27 | 中国地质科学院矿产综合利用研究所 | Determination method for detecting chromium element in fish feed product by melting-plasma spectrometry |
| CN109975386A (en) * | 2018-12-19 | 2019-07-05 | 核工业北京地质研究院 | A kind of efficient separation method for cadmium isotope measurement |
| CN110596022A (en) * | 2019-08-28 | 2019-12-20 | 广东工业大学 | Atomization device and atomization method |
| CN111707651A (en) * | 2020-06-22 | 2020-09-25 | 自然资源部第二海洋研究所 | In-situ seawater nutrition enrichment experiment device and application method thereof |
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Cited By (7)
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|---|---|---|---|---|
| CN108195781A (en) * | 2018-01-23 | 2018-06-22 | 山东省食品药品检验研究院 | The detection method of lead content in a kind of grape wine |
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| CN111707651B (en) * | 2020-06-22 | 2023-05-23 | 自然资源部第二海洋研究所 | In-situ seawater nutrition enrichment experimental device and application method thereof |
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Address after: No. 51, Second Avenue, Tianjin Binhai New Area Development Zone, 300450 Applicant after: Tianjin Customs Animal, Plant and Food Inspection Center Address before: No. 51 Second Avenue, Tianjin Binhai New Area Development Zone, 300461 Applicant before: Animal-Plant and food Detecting Center, Tianjin Exit-Entery Inspection & Quarant |
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| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171201 |