CN103926133A - Solid-phase extraction method for separating aluminum from trace cadmium, copper and zinc - Google Patents
Solid-phase extraction method for separating aluminum from trace cadmium, copper and zinc Download PDFInfo
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- CN103926133A CN103926133A CN201410169403.9A CN201410169403A CN103926133A CN 103926133 A CN103926133 A CN 103926133A CN 201410169403 A CN201410169403 A CN 201410169403A CN 103926133 A CN103926133 A CN 103926133A
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- zinc
- copper
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- cadmium
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- 239000010949 copper Substances 0.000 title claims abstract description 33
- 239000011701 zinc Substances 0.000 title claims abstract description 32
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 31
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 27
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 26
- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 25
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 24
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 24
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002414 normal-phase solid-phase extraction Methods 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 title abstract description 8
- 239000000835 fiber Substances 0.000 claims abstract description 37
- 239000012488 sample solution Substances 0.000 claims abstract description 8
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052921 ammonium sulfate Inorganic materials 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
- 239000004411 aluminium Substances 0.000 claims description 22
- 239000003480 eluent Substances 0.000 claims description 12
- 239000000523 sample Substances 0.000 claims description 12
- 150000001450 anions Chemical class 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000005342 ion exchange Methods 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
- 239000000284 extract Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 18
- 238000005349 anion exchange Methods 0.000 abstract description 2
- 238000001675 atomic spectrum Methods 0.000 abstract 1
- 238000005259 measurement Methods 0.000 abstract 1
- 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
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 5
- 235000011114 ammonium hydroxide Nutrition 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
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000000559 atomic spectroscopy Methods 0.000 description 2
- 238000005516 engineering process 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
- 239000005030 aluminium foil Substances 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
- 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
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a solid-phase extraction method for separating aluminum from trace cadmium, copper and zinc. The method comprises the following steps: adding strongly basic anion exchange fibers into an aluminum sample solution containing ammonium thiocyanate for extracting cadmium, copper and zinc, oscillating and eluting the loaded fibers by using an ammonium sulfate solution, and measuring the cadmium, copper and zinc through an atomic spectrum provided by eluant. The concentration of residual Al in the eluant obtained by the method is only 0.09-0.13 percent of the original aluminum sample solution, and accurate measurement of the cadmium, copper and zinc is not interfered. Moreover, the recovery rate of Cd is 98.2-100 percent, the recovery rate of Cu is 97.1-100 percent, and the recovery rate of Zn is 97.9-100 percent.
Description
Technical field
The invention belongs to a kind of by aluminium and Determination of Trace Amount Cadmium, copper, the separated solid phase extraction of zinc.
Background technology
In aluminium and goods thereof, often contain the heavy metal elements such as trace Cd, Cu, Zn, aluminum products with Food Contact, as the 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, owing to directly affecting the healthy of people, receive much attention.Measure trace heavy metals and conventionally adopt atomic spectroscopy, but because the accuracy of this class measuring method affected by the existence of aluminium in tested test solution very large, the mensuration to trace element in those raffinals and goods thereof especially.Therefore, need set up the effective separation method of a kind of green, aluminium is separated with trace element to be measured, the interference of trace element being measured to eliminate aluminium.
There is bibliographical information, adopt APDC (pyrrolidine curing aminoquinoxaline)-MIBK (methyl isobutyl ketone) system, extract trace Co, Ni, Cu, Mo, Cd, Pb and Bi from aluminium sample solution after, with inductively coupled plasma mass spectrometry Accurate Determining these trace elements.The greatest drawback of this class liquid-liquid extraction method is: for the organic solvent extracting, can have a negative impact to environment and operating personnel.In order to overcome this defect of liquid-liquid extraction, someone adopts charcoal absorption to contain PAN[1-(2-pyridylazo)] aluminium sample solution in trace Fe, Cu, Mn and Zn, after making them separated with aluminium in test solution, with these elements that adsorb on hydrochloric acid wash-out activated charcoal, supply Accurate Determining again, although this method has been avoided the use of organic solvent, but the absorption property of activated charcoal is unstable, and be difficult to reclaim and again utilize with the activated charcoal of crossing.
Summary of the invention
The technical problem to be solved in the present invention is: provide a kind of with anion-exchange fibre as solid extracting agent, by wash-out again after cadmium in aluminium sample solution, copper and zinc extraction, more green, more economical by aluminium and Determination of Trace Amount Cadmium, copper, the separated solid phase extraction of zinc.
The present invention solves the problems of the technologies described above with following technical scheme:
Strongly basic anion ion exchange fibre is added in the aluminium sample solution that contains ammonium thiocyanate and extracts cadmium, copper and zinc, then with ammonium sulfate to the carrying fiber wash-out that vibrates, eluent can be measured cadmium, copper and zinc for atomic spectroscopy.
Concrete grammar is:
1. accurately take 0.5～0.6g aluminium sample, add 15～20mL wang aqueous solution, be heated to sample and all dissolve, add 20mL5.00molL after cooling
-1nH
4sCN solution, deionized water constant volume.
2. take 0.2～0.25g strongly basic anion ion exchange fibre, add the 1. solution 20mL of gained of step, at 20～30 ℃, oscillation extraction 30～40min.
3. by the 2. fiber taking-up of gained of step, this fiber is washed with 20mL deionized water in filtration limit, limit, and to the carrying fiber that washs and be filtered dry, adding 20mL pH=8～8.5, concentration is 2molL
-1(NH
4)
2sO
4solution, after fiber is fully infiltrated by solution, at 60～75 ℃, vibration wash-out 40～60min, the eluent obtaining is for atomic absorption spectrometry cadmium, copper and zinc.
Through measuring, the eluent that uses the inventive method to obtain 3. in, Al residual concentration is only 0.09～0.13% of original aluminium sample solution, has not disturbed the Accurate Determining to cadmium, copper and zinc; The recovery of Cd is 98.2～100%; The recovery of Cu is 97.1～100%; The recovery of Zn is 97.9～100%.
Embodiment
Embodiment 1:
1. accurately take 0.6g aluminium sample to beaker, add 20mL50% (V/V) wang aqueous solution, be heated to sample and all dissolve, in cooling rear quantitative immigration 100mL volumetric flask, add 20.00mL5.00molL
-1nH
4sCN solution, deionized water constant volume.
2. take 0.25g strongly basic anion ion exchange fibre in 200mL iodine flask, then the solution 20.00mL that adds step 1. to prepare, at 20 ℃, oscillation extraction 40min.
3. by the 2. carrying fiber taking-up of gained of step, this fiber is washed 3 times with 20mL deionization moisture in filtration limit, limit, and the carrying fiber that washs and be filtered dry is put into the dry iodine flask of another, accurately adds 20.00mL through ammoniacal liquor, to be adjusted to the 2.00molL of pH=8
-1(NH
4)
2sO
4solution, shakes iodine flask, after fiber is fully infiltrated by solution, and at 70 ℃, vibration wash-out 1h, eluent is for atomic absorption spectrometry cadmium, copper and zinc.
After measured, in eluent, Al residual concentration is only 0.11% of original concentration, has not disturbed the Accurate Determining to cadmium, copper and zinc; The recovery 98.2% of Cd; The recovery 100% of Cu; The recovery 98.7% of Zn.
Embodiment 2:
1. accurately take 0.5g aluminium sample to 100mL beaker, add 15mL50% (V/V) wang aqueous solution, be heated to sample and all dissolve, in cooling rear quantitative immigration 100mL volumetric flask, add 20.00mL5.00molL
-1nH
4sCN solution, deionized water constant volume.
2. take 0.2g strongly basic anion ion exchange fibre in 200mL iodine flask, then add 1. prepared solution 20.00mL of step, at 25 ℃, oscillation extraction 30min.
3. by step 2. gained carrying fiber take out, this fiber is washed 3 times with 20mL deionization moisture in filtration limit, limit, the carrying fiber that washs and be filtered dry is put into another and be dried iodine flask, accurately adds 20.00mL through ammoniacal liquor, to be adjusted to the 2.00molL of pH=8.5
-1(NH
4)
2sO
4solution, shakes iodine flask, after fiber is fully infiltrated by solution, and at 65 ℃, vibration wash-out 1h, eluent is for atomic absorption spectrometry cadmium, copper and zinc.
After measured, in eluent, Al residual concentration is only 0.09% of original concentration, has not disturbed the Accurate Determining to cadmium, copper and zinc; The recovery 100% of Cd; The recovery 97.1% of Cu; The recovery 100% of Zn.
Embodiment 3:
1. accurately take 0.6g aluminium sample to 100mL beaker, add 20mL50% (V/V) wang aqueous solution, be heated to sample and all dissolve, in cooling rear quantitative immigration 100mL volumetric flask, add 20.00mL5.00molL
-1nH
4sCN solution, deionized water constant volume.
2. take 0.25g strongly basic anion ion exchange fibre in 200mL iodine flask, then add 1. prepared solution 20.00mL of step, at 28 ℃, oscillation extraction 40min.
3. by the 2. carrying fiber taking-up of gained of step, this fiber is washed 3 times with 20mL deionization moisture in filtration limit, limit, and the carrying fiber that washs and be filtered dry is put into the dry iodine flask of another, accurately adds 20.00mL through ammoniacal liquor, to be adjusted to the 2.00molL of pH=8
-1(NH
4)
2sO
4solution, shakes iodine flask, after fiber is fully infiltrated by solution, and at 75 ℃, vibration wash-out 40min, eluent is for atomic absorption spectrometry cadmium, copper and zinc.
After measured, in eluent, Al residual concentration is only 0.13% of original concentration, has not disturbed the Accurate Determining to cadmium, copper and zinc; The recovery 99.3% of Cd; The recovery 98.6% of Cu; The recovery 97.9% of Zn.
Embodiment 4:
1. accurately take 0.5g aluminium sample to 100mL beaker, add 18mL50% (V/V) wang aqueous solution, be heated to sample and all dissolve, in cooling rear quantitative immigration 100mL volumetric flask, add 20.00mL5.00molL
-1nH
4sCN solution, deionized water constant volume.
2. take 0.2g strongly basic anion ion exchange fibre in 200mL iodine flask, then add 1. prepared solution 20.00mL of this example, at 30 ℃, oscillation extraction 30min.
3. carrying fiber is taken out, this fiber is washed 3 times with 20mL deionization moisture in filtration limit, limit, and the carrying fiber that washs and be filtered dry is put into the dry iodine flask of another, accurately adds 20.00mL through ammoniacal liquor, to be adjusted to the 2.00molL of pH=8.5
-1(NH
4)
2sO
4solution, shakes iodine flask, after fiber is fully infiltrated by solution, and at 60 ℃, vibration wash-out 50min, eluent is for atomic absorption spectrometry cadmium, copper and zinc.
After measured, in eluent, Al residual concentration is only 0.1% of original concentration, has not disturbed the Accurate Determining to cadmium, copper and zinc; The recovery 99.5% of Cd; The recovery 98.9% of Cu; The recovery 99.4% of Zn.
Claims (2)
1. one kind by aluminium and Determination of Trace Amount Cadmium, copper, the separated solid phase extraction of zinc, it is characterized in that strongly basic anion ion exchange fibre to add in the aluminium sample solution that contains ammonium thiocyanate and extract cadmium, copper and zinc, again with ammonium sulfate to the carrying fiber wash-out that vibrates, obtain the eluent for aas determination.
2. as claimed in claim 1 a kind of by aluminium and Determination of Trace Amount Cadmium, copper, the separated solid phase extraction of zinc, it is characterized in that concrete grammar is:
1. accurately take 0.5～0.6g aluminium sample, add 15～20mL wang aqueous solution, be heated to sample and all dissolve, add 20mL5.00molL after cooling
-1nH
4sCN solution, deionized water constant volume;
2. take 0.2～0.25g strongly basic anion ion exchange fibre, add 1. gained solution 20mL of step, at 20～30 ℃, oscillation extraction 30～40min;
3. by step 2. the carrying fiber of gained take out, this fiber is washed with 20mL deionized water in filtration limit, limit, to after washing and the carrying fiber being filtered dry to add 20mL pH=8～8.5, concentration be 2molL
-1(NH
4)
2sO
4solution, after fiber is fully infiltrated by solution, at 60～75 ℃, vibration wash-out 40～60min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410169403.9A CN103926133B (en) | 2014-04-25 | 2014-04-25 | A kind of solid phase extraction that aluminum is separated with Determination of Trace Amount Cadmium, copper, zinc |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410169403.9A CN103926133B (en) | 2014-04-25 | 2014-04-25 | A kind of solid phase extraction that aluminum is separated with Determination of Trace Amount Cadmium, copper, zinc |
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| Publication Number | Publication Date |
|---|---|
| CN103926133A true CN103926133A (en) | 2014-07-16 |
| CN103926133B CN103926133B (en) | 2016-07-06 |
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|---|---|---|---|
| CN201410169403.9A Expired - Fee Related CN103926133B (en) | 2014-04-25 | 2014-04-25 | A kind of solid phase extraction that aluminum is separated with Determination of Trace Amount Cadmium, copper, zinc |
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| Country | Link |
|---|---|
| CN (1) | CN103926133B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080092629A1 (en) * | 2006-10-20 | 2008-04-24 | Masao Suga | Gas component collector, gas component collecting device, filter producing method, and gas component analyzing apparatus |
| CN202141627U (en) * | 2011-03-14 | 2012-02-08 | 国家海洋局第一海洋研究所 | 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 |
-
2014
- 2014-04-25 CN CN201410169403.9A patent/CN103926133B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080092629A1 (en) * | 2006-10-20 | 2008-04-24 | Masao Suga | Gas component collector, gas component collecting device, filter producing method, and gas component analyzing apparatus |
| CN202141627U (en) * | 2011-03-14 | 2012-02-08 | 国家海洋局第一海洋研究所 | 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 (5)
| Title |
|---|
| A.K.MAJUMADR ET AL: "Ion exchange seperation of metal ions with thiocyanate", 《FRESENIUS" ZEITSCHRIFT FÜR ANALYTISCHE CHEMIE》 * |
| 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》 * |
| 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》 * |
| 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》 * |
| 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》 * |
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| Publication number | Publication date |
|---|---|
| CN103926133B (en) | 2016-07-06 |
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