CN106053359A - Method using static adsorption ion exchange technology to separate and measure copper ions in salt - Google Patents
Method using static adsorption ion exchange technology to separate and measure copper ions in salt Download PDFInfo
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- CN106053359A CN106053359A CN201610328202.8A CN201610328202A CN106053359A CN 106053359 A CN106053359 A CN 106053359A CN 201610328202 A CN201610328202 A CN 201610328202A CN 106053359 A CN106053359 A CN 106053359A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
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Abstract
The invention discloses a method using a static adsorption ion exchange technology to separate and measure copper ions in salt. According to the method, an iminodiacetic acid type chelate resin is used to adsorb copper ions in a sodium chloride water solution through static adsorption; then a diluted nitric acid solution is used to wash copper ions from the resin; and after copper ions and the high salinity matrix are separated, the copper ions can be detected by atomic absorption spectrum. The static adsorption is realized through a cage shaped adsorption device; the artificial filtering is not needed, the separation is simplified, a large amount of spectrum interference caused by sodium chloride is eliminated, the subsequent detection is very simple, the results are accurate and reliable, the sensitivity is high, the selectivity is good, and the recovery rate and precision are both good.
Description
Technical field
The present invention relates to measure the method for content of copper ion in Sal, be specifically related to from Sal separation and concentration copper ion again
The method carrying out detecting with atomic absorption spectrum.
Background technology
There is substantial amounts of sodium chloride in the high salt samples such as cure foods, soy sauce, Sal, salt, in the presence of a large amount of sodium salts,
The mensuration of micro heavy is analytical chemistry recognized problem, such as when detecting the heavy metal element of trace therein with AAS, and chlorine
Change sodium to affect arc temperature and produce the biggest ambient interferences, cause some trace heavy metals cannot Accurate Determining.Fortune
When detecting with ICP or ICP-MS, substantial amounts of sodium chloride also can block nebulizer or deposit on torch pipe, sampling spiroid, thus affects
The normal use of instrument.
The method of heavy metal pollution residual in the most domestic and international detection high salt sample, or use organic solvent, or need certainly
Chelating agent processed, or use special installation, it being difficult to promote in common lab, organic solvent enrichment times is low and harmful,
The homemade chelating agent life-span is short, it is impossible to reuse for a long time.More be matrix modifier method, such as: ammonium dihydrogen phosphate, nitre
Acid magnesium, Palladous nitrate. etc., but the improved capacity that experiment proves matrix modifier is very limited, and the sodium chloride content of system is preferably controlled
System, within 5/1000ths, runs into the higher sample of salinity (such as saturated aqueous common salt), cannot overcome ambient interferences at all, with
Time food in heavy metal be trace, take dilution means inadvisable to the method reducing sodium chloride content, so using at present
Add matrix modifier way be a way that can not tackle the problem at its root of taking stopgap measures.Matrix phase, actual
On be also intended to rely on matrix modifier, the limitation eliminating sodium chloride interference with matrix modifier still exists, to high salt sample
Or cannot accurately detect.
Summary of the invention
It is an object of the invention to: the side of copper ion in a kind of static adsorption ion exchange technique separation determination Sal is provided
Method, uses static adsorption technology to complete to separate, it is achieved object separates with high salt matrix, eliminates the light that a large amount of sodium chloride causes
Spectrum interference, makes follow-up detection become extremely simple.
The technical solution of the present invention is: utilize iminodiacetic acid (salt) acid type chelating resin, quiet from sodium-chloride water solution
State absorbing copper ion；Copper ion is washed down from resin by recycling dilute nitric acid solution, separates laggard by copper ion with high salt matrix
Row atomic absorption spectrum detects；Specifically include following steps:
(1) preparation of cage type adsorbent equipment:Make: diameter 3cm height 5cm cylindrical plastic cage type skeleton bottom and
Side, closes with 200 mesh nylon wires, and top adds vinyl cover, and the circular hole of a diameter of 0.6cm is opened at the center of vinyl cover, glue in circular hole
The plastic round tube of the band centre bore of knot external diameter 0.6cm height 2.5cm；Filling: close to nylon wire from the centre bore of plastic round tube
Cage type skeleton in add the iminodiacetic acid (salt) acid type chelating resin of 0.1g and magnetic stir bar；Activation: cage type adsorbent equipment
It being immersed in 5%(V/V) in aqueous solution of nitric acid, magnetic agitation activates, and embathes with deionized water before use；
(2) salt sample dissolves: weighs 5g salt sample and puts in beaker, with the deionized water dissolving of 50mL；
(3) separation and concentration: in the beaker having dissolved salt solution 50mL, puts by filling and through the cage type adsorbent equipment of overactivation
Enter wherein, magnetic agitation 5 minutes；Then by cage type adsorbent equipment lift-off beaker, embathe with deionized water；Take a beaker again, will
5%(V/V) aqueous solution of nitric acid is poured into wherein, and the cage type adsorbent equipment after being embathed by deionized water is put in beaker, and magnetic agitation is washed
De-, eluent is to be measured；Finally with 5%(V/V) aqueous solution of nitric acid, deionized water embathe cage type adsorbent equipment successively, reactivate；
(4) detection: use graphite furnace atomic absorption spectrophotometer detection；Parameter: copper, detects wavelength 324.8nm, slit 0.7nm, plug
Graceful buckle back scape, standard series: 0,10,20,30,40,50 g/L.
(5) result calculates: with absorbance as abscissa, concentration is vertical coordinate, draws the standard curve of copper ion；By surveying
Determine the absorbance of copper ion in eluent, calculate copper content in sample.
Wherein, described iminodiacetic acid (salt) acid type chelating resin uses commercialization chelating resin, and resin title is sub-
Aminoacetaldehyde diethyl acid resin, has another name called ammonia carboxylic resin, and specification is 100-200 mesh.
The invention have the advantage that one is the characterization of adsorption utilizing iminodiacetic acid (salt) acid type chelating resin, be i.e. situated between at weakly acidic pH
In matter, iminodiacetic acid (salt) acid type chelating resin optionally static strong absorbing copper ion from sodium-chloride water solution, recycle dilute
Heavy metal is washed down from resin by salpeter solution, it is achieved copper ion and the sharp separation of sodium chloride, and carries out atomic absorption method inspection
Survey, eliminate the spectral interference problem that conventional method exists, accurately detect the content of the high salt copper ions in samples such as Sal；Two are
The utilization of cage type adsorbent equipment, quickly realizes static adsorption, without artificial filter, compares column chromatography, can realize copper ion with
The sharp separation of sodium chloride, simplifies separation process, greatly improves the speed of separation, only uses pure water and dust technology liquid,
Do not use hazardous solvent, environmental friendliness；Three is that the chelating resin used can be reused, and analysis cost is cheap；Four is this
Bright accuracy is high, and precision is good, it is possible to solve the interference that copper is measured by high salt matrix, and operation easier is little, uses commodity
Changing resin, method is reliable and practical, easily promotes.
Accompanying drawing explanation
Fig. 1 is the cage type adsorbent equipment schematic diagram of the present invention.
In figure: 1 centre bore, 2 plastic round tube, 3 vinyl covers, 4 nylon wires, 5 cage type skeletons.
Detailed description of the invention
Further illustrate the technical solution of the present invention below in conjunction with specific embodiment, these embodiments it is not intended that
It it is the restriction to technical scheme.
One, instrument and reagent: Atomic Absorption Spectrometer (Shimadzu A6300C, PE AA800)；Ultra-pure water instrument (Mi Libo
Milli-Q)；Copper standard solution (State Standard Matter Research Centre)；Iminodiacetic acid resin (100 ~ 200 mesh)；Cage type is inhaled
Adsorption device (is made by oneself)；
Two, experimentation:
1. the preparation of cage type adsorbent equipment:
Make: in the bottom of cylindrical plastic cage type skeleton 5 and the side of diameter 3cm height 5cm, by 200 mesh nylon wire 4 envelopes
Closing, top adds vinyl cover 3, and the circular hole of a diameter of 0.6cm is opened at the center of vinyl cover 3, cementing external diameter 0.6cm height 2.5cm in circular hole
The plastic round tube 2 of band centre bore 1；
Filling: from the centre bore 1 of plastic round tube 2 to the imino-diacetic adding 0.1g in the cage type skeleton 5 that nylon wire 4 is closed
Acetic acid type chelating resin and magnetic stir bar；
Activation: cage type adsorbent equipment is immersed in 5%(V/V) in aqueous solution of nitric acid, magnetic agitation activates, and uses deionization before use
Water logging is washed.
2. analytical procedure:
(1) salt sample dissolves: weighs 5g salt sample and is placed in beaker, with the deionized water dissolving of 50mL；
(2) separation and concentration: in the beaker having dissolved salt solution 50mL, puts by filling and through the cage type adsorbent equipment of overactivation
Enter wherein, magnetic agitation 5 minutes；Then by cage type adsorbent equipment lift-off beaker, embathe with deionized water；Take a beaker again, will
5%(V/V) aqueous solution of nitric acid is poured into wherein, and the cage type adsorbent equipment after being embathed by deionized water is put in beaker, and magnetic agitation is washed
De-, eluent is to be measured；Finally with 5%(V/V) aqueous solution of nitric acid, deionized water embathe cage type adsorbent equipment successively, reactivate；
(3) detection: use graphite furnace atomic absorption spectrophotometer detection；Parameter: copper, detects wavelength 324.8nm, slit 0.7nm, plug
Graceful buckle back scape, standard series: 0,10,20,30,40,50 g/L.
(4) result calculates: with absorbance as abscissa, concentration is vertical coordinate, draws the standard curve of copper ion；By surveying
Determine the absorbance of copper ion in eluent, calculate copper content in sample.
Three, result and discussion:
1., in different pH value, copper, the sodium partition coefficient (Kd) on iminodiacetic acid resin, partition coefficient Kd is at ion
Exchange has extremely important meaning in separating, and it is under the conditions of a certain, and metal is the mark of absorbability on ion exchange resin
Will；Method with reference to Strelow: respectively add dried resin 0.50g in 8 100mL conical flasks, is separately added into the solution of different pH value
48mL(pH value is regulated by hydrochloric acid, potassium hydroxide, stands overnight, accurate adjustment again in second day after regulation pH), respectively add 1.0mg (at 1mL
In) copper/sodium standard solution, add magnetic stir bar, often stirring 2min places 1h, repeats totally 3 times, filters after standing overnight, and surveys
Determine the content of copper/sodium in solution, calculate copper/sodium adsorption coefficient (Kd) in different pH value by formula below, calculate knot
Fruit is shown in Table 1.
M is absorption quality (mg) of copper on resin；
M ' is the quality (mg) of copper in solution；
V is overall solution volume, is 50mL in test；
mResinFor resin quality, test is 0.5g.
Copper under table 1 different acidity system/sodium KdValue
By measuring partition coefficient, then determining the separation condition of element, this is most scientific, the easiest method；Kd value is big, represents
Certain medium ion high adsorption capacity over the resin, vice versa；Kd ＞ 40, is adsorbed in by force resin；Kd ＜ 10, does not adsorbs
In resin；According to element to be separated and the difference of matrix partition coefficient, suitably select separation condition, it is achieved measured object and matrix
Efficiently separate；Find out by table 1, more than pH3.0 that sodium ion is not adsorbed by resin absorption strong to copper ion.
2. the solution ph impact on polluted by copper effect: iminodiacetic acid resin absorbing copper is chelatropic reaction, so pH
Resin absorption ability is had a great impact by value, draws pH and LogK in conjunction with table 1dCurve, along with the increase of pH value, adsorption coefficient
Kd value becomes larger, and copper is adsorbed in by force on resin, common salt aqueous solution general pH ≈ 6, it is ensured that copper therein adsorbs by force on resin.
3. the mensuration of iminodiacetic acid resin absorbing copper capacity: utilize iminodiacetic acid resin to carry out a huge sum of money in solution
When belonging to the absorption of ion, for guaranteeing all to adsorb heavy metal ion, prevent absorption saturated, need to measure its to metal from
The adsorption capacity of son, this is significant to the content of heavy metal in Accurate Determining food；Weigh a certain amount of iminodiacetic acid (salt)
Acid dried resin, infiltrates with a small amount of ultra-pure water, adds known enough heavy metal standard solution, regulates pH weakly acidic pH, constant volume, shakes
Even, shaking table vibrates, per hour vibration 1 time, overnight, then measure the concentration of heavy metal ion in solution；Subtract by total addition
Remove the content of beary metal measured in solution, calculate the content of beary metal on resin, then the weight divided by resin, show that resin is inhaled
The capacity of attached heavy metal；Computing formula is as follows:
Ac=
Ac: adsorption capacity adsorption capacity(g/g)
mAdd: add the quality (g) of heavy metal；
C: the concentration (g/mL) of heavy metal in solution；
V: constant volume (mL)；
mResin: iminodiacetic acid dried resin quality (g).
Experiment has respectively weighed 0.1g dried resin, is respectively placed in three small beakers, respectively the copper of each addition 1000 g, constant volume
100mL, after balance upon adsorption, uses copper ion concentration in Flame Atomic Absorption Spectrometry Determination solution；Use above-mentioned formula meter
Calculate the iminodiacetic acid resin adsorption capacity such as table 2 to copper.
Table 2 iminodiacetic acid resin adsorption capacity to copper
From table 2 it can be seen that iminodiacetic acid resin is the biggest to the adsorption capacity of copper, it is assumed that only inhale with 0.1g dried resin
Adhesion test, sample sample weighting amount is 1g, is settled to 50mL and adsorbs, even if the content of beary metal of this sample is 900mg/kg, also
It is unlikely to make post saturated；In general Sal, mostly copper content is trace level or trace level, it can be ensured that in detection Sal during copper not
Can adsorb saturated.
4. sample detection and recovery testu: use said method, the former halogen of salt mine, Sal are detected, and mark-on returns
Yield: 95.1% ~ 99.3%, RSD:0.8%～3.7%, is detected soy sauce Quality Control sample, and result is accurate；Testing result is shown in Table
3。
Table 3 sample detection result and recovery of standard addition and Precision Experiment
Claims (2)
1. the method for copper ion in static adsorption ion exchange technique separation determination Sal, is characterized in that: utilize iminodiacetic acid (salt)
Acid type chelating resin, static adsorption copper ion from sodium-chloride water solution；Recycling dilute nitric acid solution by copper ion from resin
Wash down, after being separated with high salt matrix by copper ion, carry out atomic absorption spectrum detection；Specifically include following steps:
(1) preparation of cage type adsorbent equipment:Make: in the bottom of cylindrical plastic cage type skeleton (5) of diameter 3cm height 5cm
And side, to close with 200 mesh nylon wires (4), top adds vinyl cover (3), and the circle of a diameter of 0.6cm is opened at the center of vinyl cover (3)
Hole, the plastic round tube (2) of the band centre bore (1) of cementing external diameter 0.6cm height 2.5cm in circular hole；Filling: from plastic round tube (2)
Centre bore (1) in the cage type skeleton (5) that nylon wire (4) is closed, add iminodiacetic acid (salt) acid type chelating resin and the magnetic of 0.1g
Power stirrer；Activation: cage type adsorbent equipment is immersed in 5%(V/V) in aqueous solution of nitric acid, magnetic agitation activates, and uses before use
Deionized water embathes；
(2) salt sample dissolves: weighs 5g salt sample and is placed in beaker, with the deionized water dissolving of 50mL；
(3) separation and concentration: in the beaker having dissolved salt solution 50mL, puts by filling and through the cage type adsorbent equipment of overactivation
Enter wherein, magnetic agitation 5 minutes；Then by cage type adsorbent equipment lift-off beaker, embathe with deionized water；Take a beaker again, will
5%(V/V) aqueous solution of nitric acid is poured into wherein, and the cage type adsorbent equipment after being embathed by deionized water is put in beaker, and magnetic agitation is washed
De-, eluent is to be measured；Finally with 5%(V/V) aqueous solution of nitric acid, deionized water embathe cage type adsorbent equipment successively, reactivate；
(4) detection: use graphite furnace atomic absorption spectrophotometer detection；Parameter: copper, detects wavelength 324.8nm, slit 0.7nm, plug
Graceful buckle back scape, standard series: 0,10,20,30,40,50 g/L；
(5) result calculates: with absorbance as abscissa, concentration is vertical coordinate, draws the standard curve of copper ion；Washed by mensuration
In de-liquid, the absorbance of copper ion, calculates copper content in sample.
The method of copper ion in static adsorption ion exchange technique separation determination Sal the most according to claim 1, it is special
Levy and be: described iminodiacetic acid (salt) acid type chelating resin uses commercialization chelating resin, and resin title is iminodiacetic acid (salt)
Acid resin, has another name called ammonia carboxylic resin, and specification is 100-200 mesh.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106404698A (en) * | 2016-11-30 | 2017-02-15 | 大工（青岛）新能源材料技术研究院有限公司 | Beneficiation method for detecting low-concentration copper in wastewater |
| CN107367472A (en) * | 2017-06-30 | 2017-11-21 | 益盐堂（应城）健康盐制盐有限公司 | A kind of method of multiple element content in rapid sensitive detection salt |
| CN115108648A (en) * | 2022-05-23 | 2022-09-27 | 西南交通大学 | Water body in-situ phosphate enrichment device |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106404698A (en) * | 2016-11-30 | 2017-02-15 | 大工（青岛）新能源材料技术研究院有限公司 | Beneficiation method for detecting low-concentration copper in wastewater |
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| CN115108648A (en) * | 2022-05-23 | 2022-09-27 | 西南交通大学 | Water body in-situ phosphate enrichment device |
| CN115108648B (en) * | 2022-05-23 | 2023-10-20 | 西南交通大学 | Water normal position enrichment phosphate device |
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Application publication date: 20161026 |