CN103926133B - A kind of solid phase extraction that aluminum is separated with Determination of Trace Amount Cadmium, copper, zinc - Google Patents
A kind of solid phase extraction that aluminum is separated with Determination of Trace Amount Cadmium, copper, zinc Download PDFInfo
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- CN103926133B CN103926133B CN201410169403.9A CN201410169403A CN103926133B CN 103926133 B CN103926133 B CN 103926133B CN 201410169403 A CN201410169403 A CN 201410169403A CN 103926133 B CN103926133 B CN 103926133B
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- copper
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- cadmium
- aluminum
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- 239000010949 copper Substances 0.000 title claims abstract description 32
- 239000011701 zinc Substances 0.000 title claims abstract description 31
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 30
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 26
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 25
- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 23
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 23
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002414 normal-phase solid-phase extraction Methods 0.000 title claims abstract description 6
- 239000000835 fiber Substances 0.000 claims abstract description 37
- 239000003480 eluent Substances 0.000 claims abstract description 14
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 9
- 150000001450 anions Chemical class 0.000 claims abstract description 9
- 238000005342 ion exchange Methods 0.000 claims abstract description 9
- 239000012488 sample solution Substances 0.000 claims abstract description 8
- 239000000284 extract Substances 0.000 claims abstract description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 3
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 3
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 24
- 239000000523 sample Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- 238000001479 atomic absorption spectroscopy Methods 0.000 abstract description 6
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 12
- 239000011630 iodine Substances 0.000 description 12
- 229910052740 iodine Inorganic materials 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 238000002242 deionisation method Methods 0.000 description 4
- 239000011573 trace mineral Substances 0.000 description 4
- 235000013619 trace mineral Nutrition 0.000 description 4
- RWRDLPDLKQPQOW-UHFFFAOYSA-N Pyrrolidine Chemical compound C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000000559 atomic spectroscopy Methods 0.000 description 2
- 238000000622 liquid--liquid extraction Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 1
- 239000005030 aluminium foil Substances 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- MDDIUTVUBYEEEM-UHFFFAOYSA-N azane;pyrrolidine-1-carbodithioic acid Chemical compound N.SC(=S)N1CCCC1 MDDIUTVUBYEEEM-UHFFFAOYSA-N 0.000 description 1
- 235000021168 barbecue Nutrition 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229940043265 methyl isobutyl ketone Drugs 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- YOWAEZWWQFSEJD-UHFFFAOYSA-N quinoxalin-2-amine Chemical compound C1=CC=CC2=NC(N)=CN=C21 YOWAEZWWQFSEJD-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
A kind of solid phase extraction that aluminum is separated with Determination of Trace Amount Cadmium, copper, zinc, strongly basic anion ion exchange fibre is added in the aluminum sample solution containing ammonium thiocyanate and extract cadmium, copper and zinc, carrying fiber being vibrated eluting with ammonium sulfate, eluent is for atomic absorption spectrometry cadmium, copper and zinc again.It is only the 0.09～0.13% of original aluminum sample solution with Al residual concentration in the eluent of the method gained of the present invention, does not disturb the Accurate Determining to cadmium, copper and zinc；The response rate of Cd is 98.2～100%；The response rate of Cu is 97.1～100%；The response rate of Zn is 97.9～100%.
Description
Technical field
The invention belongs to a kind of solid phase extraction separated by aluminum with Determination of Trace Amount Cadmium, copper, zinc.
Background technology
Often containing the heavy metal element such as trace Cd, Cu, Zn in aluminum and goods thereof, aluminum products with Food Contact, contents of heavy metal elements in the aluminum products such as aluminum pot, aluminum easy open can, packaging for foodstuff and aluminium foil used for barbecue, receives much attention owing to directly affecting the healthy of people.Measure trace heavy metals and generally adopt atomic spectroscopy, but the accuracy being because this kind of measuring method is affected by the existence of aluminum in tested test solution very big, especially to the mensuration of trace element in those raffinals and goods thereof.Therefore, a kind of green need to be set up and efficiently separate method, aluminum be separated with trace element to be measured, to eliminate the interference that trace element is measured by aluminum.
There is bibliographical information, adopt APDC (pyrrolidine curing aminoquinoxaline)-MIBK (methyl iso-butyl ketone (MIBK)) system, extract after trace Co, Ni, Cu, Mo, Cd, Pb and Bi from aluminum sample solution, these trace elements with inductively coupled plasma mass spectrometry Accurate Determining.The greatest drawback of this kind of liquid-liquid extraction method is: environment and operator can be had a negative impact by the organic solvent for extracting.In order to overcome this defect of liquid-liquid extraction, someone adopts activated carbon adsorption to contain trace Fe, Cu, Mn and Zn in the aluminum sample solution of PAN [1-(2-pyridylazo)], after making them separate with the aluminum in test solution, again with these elements of absorption on the activity eluted charcoal of hydrochloric acid for Accurate Determining, although The method avoids the use of organic solvent, but the absorption property of activated carbon is unstable, and used activated carbon is difficult to reclaim and again with.
Summary of the invention
The technical problem to be solved in the present invention is: provide one anion-exchange fibre as solid extracting agent, by eluting, more green, the more economical solid phase extraction separated with Determination of Trace Amount Cadmium, copper, zinc by aluminum again after cadmium, copper and zinc extraction in aluminum sample solution.
The present invention solves above-mentioned technical problem with following technical scheme:
Being added by strongly basic anion ion exchange fibre in the aluminum sample solution containing ammonium thiocyanate and extract cadmium, copper and zinc, then carrying fiber vibrated eluting with ammonium sulfate, eluent is available for atomic spectroscopy and measures cadmium, copper and zinc.
Method particularly includes:
1. accurately weigh 0.5～0.6g aluminum sample, add 15～20mL wang aqueous solution, heat and all dissolve to sample, after cooling, add 20mL5.00mol L-1NH4SCN solution, deionized water constant volume.
2. weigh 0.2～0.25g strongly basic anion ion exchange fibre, add the solution 20mL of step 1. gained, at 20～30 DEG C, oscillation extraction 30～40min.
3. the fiber of step 2. gained is taken out, filtration limit, limit this fiber of 20mL deionized water wash, be 2mol L to carrying fiber addition 20mLpH=8～8.5 washed and be filtered dry, concentration-1(NH4)2SO4Solution, after fiber is fully infiltrated by solution, at 60～75 DEG C, vibrate eluting 40～60min, and the eluent obtained is for atomic absorption spectrometry cadmium, copper and zinc.
Through measuring, the eluent using the inventive method to obtain 3. in, Al residual concentration is only the 0.09～0.13% of original aluminum sample solution, has not disturbed the Accurate Determining to cadmium, copper and zinc；The response rate of Cd is 98.2～100%；The response rate of Cu is 97.1～100%；The response rate of Zn is 97.9～100%.
Detailed description of the invention
Embodiment 1:
1. accurately weigh 0.6g aluminum sample to beaker, add 20mL50% (V/V) wang aqueous solution, heat and all dissolve to sample, quantitatively move in 100mL volumetric flask after cooling, add 20.00mL5.00mol L-1NH4SCN solution, deionized water constant volume.
2. weigh 0.25g strongly basic anion ion exchange fibre in 200mL iodine flask, add the solution 20.00mL that 1. step is prepared, at 20 DEG C, oscillation extraction 40min.
3. being taken out by the carrying fiber of step 2. gained, filtration limit, limit 20mL deionization moisture washs this fiber 3 times, is put into by the carrying fiber washed and be filtered dry in the dry iodine flask of another, accurately adds 20.00mL and is adjusted to the 2.00mol L of pH=8 through ammonia-1(NH4)2SO4Solution, shakes iodine flask, and after fiber is fully infiltrated by solution, at 70 DEG C, vibrate eluting 1h, and eluent is for atomic absorption spectrometry cadmium, copper and zinc.
After measured, in eluent, Al residual concentration is only the 0.11% of original concentration, has not disturbed the Accurate Determining to cadmium, copper and zinc；The response rate 98.2% of Cd；The response rate 100% of Cu；The response rate 98.7% of Zn.
Embodiment 2:
1. accurately weigh 0.5g aluminum sample to 100mL beaker, add 15mL50% (V/V) wang aqueous solution, heat and all dissolve to sample, quantitatively move in 100mL volumetric flask after cooling, add 20.00mL5.00mol L-1NH4SCN solution, deionized water constant volume.
2. weigh 0.2g strongly basic anion ion exchange fibre in 200mL iodine flask, add the solution 20.00mL that step is 1. prepared, at 25 DEG C, oscillation extraction 30min.
3. by step 2. gained carrying fiber take out, filtration limit, limit 20mL deionization moisture washs this fiber 3 times, washing the carrying fiber that is filtered dry is put in the dry iodine flask of another, accurately adds 20.00mL and is adjusted to the 2.00mol L of pH=8.5 through ammonia-1(NH4)2SO4Solution, shakes iodine flask, and after fiber is fully infiltrated by solution, at 65 DEG C, vibrate eluting 1h, and eluent is for atomic absorption spectrometry cadmium, copper and zinc.
After measured, in eluent, Al residual concentration is only the 0.09% of original concentration, has not disturbed the Accurate Determining to cadmium, copper and zinc；The response rate 100% of Cd；The response rate 97.1% of Cu；The response rate 100% of Zn.
Embodiment 3:
1. accurately weigh 0.6g aluminum sample to 100mL beaker, add 20mL50% (V/V) wang aqueous solution, heat and all dissolve to sample, quantitatively move in 100mL volumetric flask after cooling, add 20.00mL5.00mol L-1NH4SCN solution, deionized water constant volume.
2. weigh 0.25g strongly basic anion ion exchange fibre in 200mL iodine flask, add the solution 20.00mL that step is 1. prepared, at 28 DEG C, oscillation extraction 40min.
3. being taken out by the carrying fiber of step 2. gained, filtration limit, limit 20mL deionization moisture washs this fiber 3 times, is put into by the carrying fiber washed and be filtered dry in the dry iodine flask of another, accurately adds 20.00mL and is adjusted to the 2.00mol L of pH=8 through ammonia-1(NH4)2SO4Solution, shakes iodine flask, and after fiber is fully infiltrated by solution, at 75 DEG C, vibrate eluting 40min, and eluent is for atomic absorption spectrometry cadmium, copper and zinc.
After measured, in eluent, Al residual concentration is only the 0.13% of original concentration, has not disturbed the Accurate Determining to cadmium, copper and zinc；The response rate 99.3% of Cd；The response rate 98.6% of Cu；The response rate 97.9% of Zn.
Embodiment 4:
1. accurately weigh 0.5g aluminum sample to 100mL beaker, add 18mL50% (V/V) wang aqueous solution, heat and all dissolve to sample, quantitatively move in 100mL volumetric flask after cooling, add 20.00mL5.00mol L-1NH4SCN solution, deionized water constant volume.
2. weigh 0.2g strongly basic anion ion exchange fibre in 200mL iodine flask, add the solution 20.00mL that this example is 1. prepared, at 30 DEG C, oscillation extraction 30min.
3. being taken out by carrying fiber, filtration limit, limit 20mL deionization moisture washs this fiber 3 times, is put into by the carrying fiber washed and be filtered dry in the dry iodine flask of another, accurately adds 20.00mL and is adjusted to the 2.00mol L of pH=8.5 through ammonia-1 (NH4)2SO4Solution, shakes iodine flask, and after fiber is fully infiltrated by solution, at 60 DEG C, vibrate eluting 50min, and eluent is for atomic absorption spectrometry cadmium, copper and zinc.
After measured, in eluent, Al residual concentration is only the 0.1% of original concentration, has not disturbed the Accurate Determining to cadmium, copper and zinc；The response rate 99.5% of Cd；The response rate 98.9% of Cu；The response rate 99.4% of Zn.
Claims (1)
1. the solid phase extraction that aluminum is separated with Determination of Trace Amount Cadmium, copper, zinc, it is characterized in that adding strongly basic anion ion exchange fibre the aluminum sample solution containing ammonium thiocyanate extracts cadmium, copper and zinc, carrying fiber vibrated eluting with ammonium sulfate again, obtain the eluent for aas determination；
Concrete grammar is:
1. accurately weigh 0.5～0.6g aluminum sample, add 15～20mL wang aqueous solution, heat and all dissolve to sample, after cooling, add 20mL5.00mol L-1NH4SCN solution, deionized water constant volume；
2. weigh 0.2～0.25g strongly basic anion ion exchange fibre, add step 1. gained solution 20mL, at 20～30 DEG C, oscillation extraction 30～40min；
3. the carrying fiber of step 2. gained is taken out, filtration limit, limit this fiber of 20mL deionized water wash, after washing and the carrying fiber that is filtered dry adds 20mLpH=8～8.5, concentration is 2mol L-1(NH4)2SO4Solution, after fiber is fully infiltrated by solution, at 60～75 DEG C, vibrate eluting 40～60min.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202141627U (en) * | 2011-03-14 | 2012-02-08 | 国家***第一海洋研究所 | Low-temperature carrier gas cold-trapping and thermal-desorption device |
| CN103674669A (en) * | 2013-06-18 | 2014-03-26 | 宁波检验检疫科学技术研究院 | Device and method for determining each element in filament sample by adopting LA-ICP-MS (Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry) method |
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| JP4856514B2 (en) * | 2006-10-20 | 2012-01-18 | 株式会社日立製作所 | Exhalation component collector, exhalation component collection device, exhalation component collector manufacturing method, exhalation component analysis device, and exhalation component analysis method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202141627U (en) * | 2011-03-14 | 2012-02-08 | 国家***第一海洋研究所 | Low-temperature carrier gas cold-trapping and thermal-desorption device |
| CN103674669A (en) * | 2013-06-18 | 2014-03-26 | 宁波检验检疫科学技术研究院 | Device and method for determining each element in filament sample by adopting LA-ICP-MS (Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry) method |
Non-Patent Citations (4)
| Title |
|---|
| Chunhua Xiong et al.Preparation and application of acrylic acid grafted polytetrafluoroethylene fiber as a weak acid cation exchanger for adsorption of Er(Ⅲ).《Journal of Hazardous Materials》.2009,第170卷 * |
| 伍娟 等.铬（Ⅲ）和铬（Ⅵ）的离子交换纤维柱分离和电感耦合等离子体原子发射光谱法测定.《冶金分析》.2010,第30卷(第2期), * |
| 潘雪珍 等.强酸阳离子交换纤维柱分离-石墨炉原子吸收光谱法测定金属铟及其盐中镉.《冶金分析》.2010,第30卷(第4期), * |
| 赵燕 等.新型阴离子交换纤维对铬（Ⅵ）的静态吸附的研究.《中国皮革》.2007,第36卷(第13期), * |
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