CN103528980A - Flame atomic absorption spectrum method for separating, enriching and determining trace lead and cadmium in water sample by using thiomalamic acid modified silica gel - Google Patents
Flame atomic absorption spectrum method for separating, enriching and determining trace lead and cadmium in water sample by using thiomalamic acid modified silica gel Download PDFInfo
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Abstract
The invention discloses a flame atomic absorption spectrum method for separating, enriching and determining trace lead and cadmium in a water sample by using thiomalamic acid modified silica gel. The flame atomic absorption spectrum method comprises the following steps: taking macro-porous silica gel as a carrier and taking thiomalamic acid as a functional molecule to prepare the thiomalamic acid modified silica gel; taking the thiomalamic acid modified silica gel as an adsorbent to dynamically separate and enrich the lead and the cadmium, and establishing the flame atomic absorption spectrum method. In a concentration range of 0.5-10.0 micrograms/milliliter, a Pb (II) absorbance in an eluting solution and the concentration form a good linear relation: A=0.0122*C-0.0011 (C: micrograms/milliliter); in a concentration range of 0.1-5.0 micrograms/milliliter, a Cb (II) absorbance in the eluting solution and the concentration form a good linear relation: A=0.1898*C+0.001 (C: micrograms/milliliter); the detection limits of the Pb (II) and the Cd(II) are 12.41ng/mL and 0.79ng/mL. According to the flame atomic absorption spectrum method, the sensitivity and the selectivity of the detection are improved and the detection of low-concentration Pb (II) and Cd(II) is easy to be automatic.
Description
Technical field
The present invention relates to a kind of method of utilizing chemical modification to prepare adsorbent concentration and separation and atomic absorption spectrum coupling Rapid Determination of Trace Lead, cadmium.
Background technology
Along with the propelling of global process of industrialization, heavy metal lead, cadmium pollution have caused great threat to the mankind, therefore, sensitive in the urgent need to researching and developing, fast, plumbous, cadmium separation and concentration technology easily, to meet the needs of the aspects such as environment measuring.
At present, method plumbous in separation and concentration water, cadmium has chemical precipitation method, chemical reduction method, ion exchange process, biological treatment and absorption method etc.Wherein, absorption method because it is easy, efficient and adsorbent is renewable is widely used with recycling.And in various solid adsorption materials, silica gel adsorption performance is good, stable chemical nature.Directly use silica gel as adsorbent for separating of enrichment, its selectivity is not high, therefore, must utilize the silicon hydroxyl of Silica Surface to carry out chemical modification and prepare selective absorbent, then plumbous in sample solution, cadmium is carried out detecting after separation and concentration.
Utilize at present the flame atomic absorption spectrometry method of trace lead, cadmium in thiomalic acid modified silica-gel separation and concentration-mensuration water sample not have temporarily correlative study.
Summary of the invention
The invention reside in a kind of flame atomic absorption spectrometry method that trace lead, cadmium in high selectivity separation and concentration-mensuration water sample are provided.
Conceive as follows: although silica gel adsorption performance is good, stable chemical nature, directly use silica gel as adsorbent for separating of enrichment, its selectivity is not high, therefore, conventionally utilizes the silicon hydroxyl of Silica Surface to carry out modification.By amidation process, thiomalic acid is modified to ammonification Silica Surface, thereby improve the selectivity of silica gel absorber enriched lead, cadmium, improve sensitivity and the antijamming capability of Flame Atomic Absorption Spectrometry Determination trace lead, cadmium.In this experiment, utilize thiomalic acid modified silica-gel as microtrabeculae adsorbent, plumbous in complicated substrate sample solution, cadmium can be carried out to dynamic enrichment with separated, reduce manual steps, improve reappearance and the precision measured.
The present invention relates to dynamic microcolumn separation and enrichment and the coupling of atomic absorption light spectral method.Plumbous in testing sample solution, cadmium is when having loaded the microtrabeculae of adsorbent, and plumbous, cadmium adsorbs with Silica Surface thiomalic acid generation complexing, then with eluent by lead, cadmium wash-out and carry out Atomic Absorption Spectrometry.
Concrete steps are as follows:
(1) thiomalic acid modified silica-gel absorbent preparation:
Take 30-70 order microsphere silica gel 30g, be placed in 250mL there-necked flask, install condenser pipe, adding 150.0mL concentration is the hydrochloric acid of 6.0mol/L, heating refluxes solution and mechanical raking 5-6 hour, cooled and filtered goes out silica gel, with distilled water by silica gel wash to wash solution be neutral (silver nitrate that is 2% with mass percent checks wash solution whether to have chlorion), vacuum drying obtains activated silica gel.
Take the above-mentioned activated silica gel of 30.0g, be placed in 250ml there-necked flask, add respectively 100.0mL to analyze the chemical pure gamma-aminopropyl-triethoxy-silane (KH550) after pure toluene and 10.0-15.0mL distilation, mechanical raking also adds hot reflux 6 hours, cooled and filtered solid product, with analysis pure toluene, absolute ethyl alcohol, respectively wash solid product 3 times, after vacuum drying, obtain γ-aminopropyl silica gel (APSG).
Take 4.5-6.0g thiomalic acid, be dissolved in 150ml and analyze pure N, in dinethylformamide (DMF), then add successively 1.0-1.5g to analyze pure N-hydroxy-succinamide (NHS), 8.5-9.0g analyzes pure 1-ethyl-(3-dimethylamino-propyl) carbodiimide hydrochloride (EDCHCl) and makes it and dissolves, finally add the above-mentioned γ-aminopropyl of 30.0g silica gel, stirring at normal temperature filtered out solid product after 24 hours, respectively with analyzing pure N, dinethylformamide (DMF), absolute ethanol washing solid product each 5 times, the dry thiomalic acid modified silica-gel (TMSG) that obtains of suction filtration final vacuum.
(2) thiomalic acid modified silica-gel separation and concentration lead, cadmium:
Separation and concentration device by peristaltic pump, self-control micro-column ((7cm * 0.5mm i.d.), polyfluortetraethylene pipe (0.8mm i.d) and joint connect into formation.First a small amount of glass wool beyond the Great Wall in pillar one end before dress post, with wet method upper prop, pack adsorbent thiomalic acid modified silica-gel prepared by step (1) into, then fill in a small amount of glass wool, compacting also connects, utilize peristaltic pump that redistilled water is pumped into micro-column, standby after washing; The separation and concentration step of Pb (II) is as follows: the Pb of pH=6.0 (II) solution is passed through to micro-column with 1.8mL/min flow velocity, then with the blank solution of 5.0mL pH=6.0, with 1.8mL/min flow velocity, wash away the ion not being adsorbed in micro-column, the Pb (II) being adsorbed with the reverse wash-out of 3.0mL/min flow velocity with 10.0mL1.0mol/L HCl; The separation and concentration step of Cd (II) is as follows: the Cd of pH=8.0 (II) solution is passed through to micro-column with 1.8mL/min flow velocity, then with the blank solution of 5.0mL pH=8.0, with 1.8mL/min flow velocity, wash away the ion not being adsorbed in micro-column, the Cd (II) being adsorbed with the reverse wash-out of 3.6mL/min flow velocity with 10.0mL1.0mol/L HCl.Elute soln is for follow-up Atomic Absorption Spectrometry.
(3) detection method:
Determining instrument: atomic absorption spectrophotometer (AAS) (Beijing Puxi General Instrument Co., Ltd); Measure the instrument condition of Pb element: wavelength 283.3nm, slit 0.5nm, lamp current 2.0mA, burner height 5.0mm, acetylene flow 1500mL/min, air mass flow 5000mL/min; Measure the instrument condition of Cd element: wavelength 228.8nm, slit 0.5nm, lamp current 2.0mA, burner height 5.0mm, acetylene flow 1500mL/min, air mass flow 5000mL/min; Utilize Pb (II) or Cd (II) concentration in Flame Atomic Absorption Spectrometry Determination above-mentioned steps (2) gained eluent.
(4) drafting of standard working curve:
Cd (II) standard solution of the Pb of 10.0mL pH=6.0 (II) standard solution or pH=8.0 is carried out to separation and concentration and Atomic Absorption Spectrometry according to step (2) and step (3); In 0.5-10.0 μ g/mL concentration range, (II) absorbance of Pb in eluent and its concentration are good linear relationship: A=0.0122*C-0.0011, and C is that concentration ，Qi unit is μ g/mL, linearly dependent coefficient r=0.9993; In 0.1-5.0 μ g/mL concentration range, (II) absorbance of Cd in eluent and its concentration are good linear relationship: A=0.1898*C+0.01, and C is that concentration ，Qi unit is μ g/mL, linearly dependent coefficient r=0.9994.
(5) treat mensuration plumbous in test sample, cadmium content:
Cd (II) sample solution of the Pb of pH=6.0 (II) sample solution or pH=8.0 is carried out to separation and concentration and Atomic Absorption Spectrometry according to step (2) and step (3), obtain absorbance A; Finally according to calibration curve, calculate Pb in sample solution (II) or Cd (II) concentration C.
The shortcomings such as the present invention has overcome the complex operation that existing static separation technology exists, and step is complicated, reappearance is bad, have improved the sensitivity and the selectivity that detect better, and detection plumbous for super low concentration, cadmium is easy to robotization.
Accompanying drawing explanation
Fig. 1 is the preparation flow figure of thiomalic acid modified silica-gel in the present invention.
Embodiment
Embodiment:
(1) thiomalic acid modified silica-gel absorbent preparation:
Take 30-70 order microsphere silica gel 30g, be placed in 250mL there-necked flask, install condenser pipe, adding 150.0mL concentration is the hydrochloric acid of 6.0mol/L, heating refluxes solution and mechanical raking 5 hours, cooled and filtered goes out silica gel, with distilled water by silica gel wash to wash solution be neutral (silver nitrate that is 2% with mass percent checks wash solution whether to have chlorion), vacuum drying obtains activated silica gel.
Take the above-mentioned activated silica gel of 30.0g, be placed in 250ml there-necked flask, add respectively 100.0mL to analyze the chemical pure gamma-aminopropyl-triethoxy-silane (KH550) after pure toluene and 13.0mL distilation, mechanical raking also adds hot reflux 6 hours, cooled and filtered solid product, with analyzing pure toluene, absolute ethanol washing solid product each 3 times, after vacuum drying, obtain γ-aminopropyl silica gel (APSG).
Take 5.0g thiomalic acid, be dissolved in 150ml and analyze pure N, in dinethylformamide (DMF), then adding successively 1.2g to analyze pure N-hydroxy-succinamide (NHS), 9g analyzes pure 1-ethyl-(3-dimethylamino-propyl) carbodiimide hydrochloride (EDCHCl) and makes it and dissolve, finally add the above-mentioned γ-aminopropyl of 30.0g silica gel, stirring at normal temperature filtered out solid product after 24 hours, with analyzing pure DMF, absolute ethanol washing solid product each 5 times, suction filtration final vacuum is dried and obtains thiomalic acid modified silica-gel (TMSG) respectively.Absorbent preparation flow process is as Fig. 1.
(2) thiomalic acid modified silica-gel separation and concentration lead, cadmium:
Separation and concentration device by peristaltic pump, self-control micro-column ((7cm * 0.5mm i.d.), polyfluortetraethylene pipe (0.8mm i.d) and joint connect into formation.First a small amount of glass wool beyond the Great Wall in pillar one end before dress post, with wet method upper prop, pack adsorbent thiomalic acid modified silica-gel prepared by step (1) into, then fill in a small amount of glass wool, compacting also connects, utilize peristaltic pump that redistilled water is pumped into micro-column, standby after washing; The separation and concentration step of Pb (II) is as follows: the Pb of pH=6.0 (II) solution is passed through to micro-column with 1.8mL/min flow velocity, then with the blank solution of 5.0mL pH=6.0, with 1.8mL/min flow velocity, wash away the ion not being adsorbed in micro-column, the Pb (II) being adsorbed with the reverse wash-out of 3.0mL/min flow velocity with 10.0mL1.0mol/L HCl; The separation and concentration step of Cd (II) is as follows: the Cd of pH=8.0 (II) solution is passed through to micro-column with 1.8mL/min flow velocity, then with the blank solution of 5.0mL pH=8.0, with 1.8mL/min flow velocity, wash away the ion not being adsorbed in micro-column, the Cd (II) being adsorbed with the reverse wash-out of 3.6mL/min flow velocity with 10.0mL1.0mol/L HCl.Elute soln is for follow-up Atomic Absorption Spectrometry.
(3) detection method:
Determining instrument: atomic absorption spectrophotometer (AAS) (Beijing Puxi General Instrument Co., Ltd); Measure the instrument condition of Pb element: wavelength 283.3nm, slit 0.5nm, lamp current 2.0mA, burner height 5.0mm, acetylene flow 1500mL/min, air mass flow 5000mL/min; Measure the instrument condition of Cd element: wavelength 228.8nm, slit 0.5nm, lamp current 2.0mA, burner height 5.0mm, acetylene flow 1500mL/min, air mass flow 5000mL/min; Utilize Pb (II) or Cd (II) concentration in Flame Atomic Absorption Spectrometry Determination above-mentioned steps (2) gained eluent.
(4) drafting of standard working curve:
Cd (II) standard solution of the Pb of 10.0mL pH=6.0 (II) standard solution or pH=8.0 is carried out to separation and concentration and Atomic Absorption Spectrometry according to step (2) and step (3); In 0.5-10.0 μ g/mL concentration range, (II) absorbance of Pb in eluent and its concentration are good linear relationship: A=0.0122*C-0.0011, and C is that concentration ，Qi unit is μ g/mL, linearly dependent coefficient r=0.9993; In 0.1-5.0 μ g/mL concentration range, (II) absorbance of Cd in eluent and its concentration are good linear relationship: A=0.1898*C+0.01, and C is that concentration ，Qi unit is μ g/mL, linearly dependent coefficient r=0.9994.
(5) treat mensuration plumbous in test sample, cadmium content:
Cd (II) sample solution of the Pb of 100ml pH=6.0 (II) sample solution or pH=8.0 is carried out to separation and concentration and Atomic Absorption Spectrometry according to step (2) and step (3), obtain absorbance A; Finally according to calibration curve, calculate Pb in sample solution (II) or Cd (II) concentration C, calculate recovery rate, result is as shown in table 1.
Table 1: sample determination and mark-on recovery test data
Claims (1)
1. a flame atomic absorption spectrometry method for trace lead, cadmium in thiomalic acid modified silica-gel separation and concentration-mensuration water sample, is characterized in that concrete steps are as follows:
(1) thiomalic acid modified silica-gel absorbent preparation:
Take 30-70 order microsphere silica gel 30g, be placed in 250mL there-necked flask, install condenser pipe, adding 150.0mL concentration is 6.0 mol
/the hydrochloric acid of L, heating refluxes solution and mechanical raking 5-6 hour, and cooled and filtered goes out silica gel, and it is neutral with distilled water, silica gel being washed to wash solution, whether the silver nitrate that is 2% by mass percent check wash solution has chlorion, and vacuum drying obtains activated silica gel;
Take the above-mentioned activated silica gel of 30.0g, be placed in 250ml there-necked flask, the chemical pure gamma-aminopropyl-triethoxy-silane that adds respectively 100.0mL to analyze after pure toluene and 10.0-15.0 mL distilation is KH550, mechanical raking also adds hot reflux 6 hours, cooled and filtered solid product, with analysis pure toluene, absolute ethyl alcohol, wash successively solid product 3 times, after vacuum drying, obtaining γ-aminopropyl silica gel is APSG;
Take 4.5-6.0 g thiomalic acid, be dissolved in 150 ml and analyze pure N, dinethylformamide is in DMF, then adding successively 1.0-1.5 g to analyze pure N-hydroxy-succinamide is NHS, 8.5-9.0 g analyzes pure 1-ethyl-(3-dimethylamino-propyl) carbodiimide hydrochloride to be EDCHCl and to make it to dissolve, finally add the above-mentioned γ-aminopropyl of 30.0 g silica gel, stirring at normal temperature filtered out solid product after 24 hours, respectively with analyzing pure N, dinethylformamide, absolute ethanol washing solid product each 5 times, suction filtration final vacuum is dried and obtains thiomalic acid modified silica-gel is TMSG,
(2) thiomalic acid modified silica-gel separation and concentration lead, cadmium:
Separation and concentration device is connected into and is formed by peristaltic pump, self-control micro-column, polyfluortetraethylene pipe and joint; First a small amount of glass wool beyond the Great Wall in pillar one end before dress post, with wet method upper prop, pack adsorbent thiomalic acid modified silica-gel prepared by step (1) into, then fill in a small amount of glass wool, compacting also connects, utilize peristaltic pump that redistilled water is pumped into micro-column, standby after washing; The separation and concentration step of Pb (II) is as follows: the Pb of pH=6.0 (II) solution is passed through to micro-column with 1.8 mL/min flow velocitys, then with the blank solution of 5.0mL pH=6.0, with 1.8 mL/min flow velocitys, wash away the ion not being adsorbed in micro-column, the Pb (II) being adsorbed with the reverse wash-out of 3.0 mL/min flow velocity with 10.0mL 1.0 mol/L HCl; The separation and concentration step of Cd (II) is as follows: the Cd of pH=8.0 (II) solution is passed through to micro-column with 1.8 mL/min flow velocitys, then with the blank solution of 5.0mL pH=8.0, with 1.8 mL/min flow velocitys, wash away the ion not being adsorbed in micro-column, the Cd (II) being adsorbed with the reverse wash-out of 3.6 mL/min flow velocity with 10.0mL 1.0 mol/L HCl; Elute soln is for follow-up Atomic Absorption Spectrometry;
(3) detection method:
Determining instrument: atomic absorption spectrophotometer (AAS); Measure the instrument condition of Pb element: wavelength 283.3nm, slit 0.5nm, lamp current 2.0 mA, burner height 5.0mm, acetylene flow 1500mL/min, air mass flow 5000mL/min; Measure the instrument condition of Cd element: wavelength 228.8 nm, slit 0.5nm, lamp current 2.0 mA, burner height 5.0mm, acetylene flow 1500mL/min, air mass flow 5000mL/min; Utilize Pb (II) or Cd (II) concentration in Flame Atomic Absorption Spectrometry Determination above-mentioned steps (2) gained eluent;
(4) drafting of standard working curve:
Cd (II) standard solution of the Pb of 10.0mL pH=6.0 (II) standard solution or pH=8.0 is carried out to separation and concentration and Atomic Absorption Spectrometry according to step (2) and step (3); In 0.5-10.0 μ g/mL concentration range, (II) absorbance of Pb in eluent and its concentration are good linear relationship: A=0.0122*C-0.0011, and C is that concentration ，Qi unit is μ g/mL, linearly dependent coefficient
r=0.9993; In 0.1-5.0 μ g/mL concentration range, (II) absorbance of Cd in eluent and its concentration are good linear relationship: A=0.1898*C+0.01, and C is that concentration ，Qi unit is μ g/mL, linearly dependent coefficient
r=0.9994;
(5) treat mensuration plumbous in test sample, cadmium content:
Cd (II) sample solution of the Pb of pH=6.0 (II) sample solution or pH=8.0 is carried out to separation and concentration and Atomic Absorption Spectrometry according to step (2) and step (3), obtain absorbance A; Finally according to calibration curve, calculate Pb in sample solution (II) or Cd (II) concentration.
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| CN107376872A (en) * | 2017-08-06 | 2017-11-24 | 桂林理工大学 | Preparation method for the chitosan soybean protein composite porous microspheres of lead absorption |
| CN107442073A (en) * | 2017-08-06 | 2017-12-08 | 桂林理工大学 | For the preparation method for the crosslinking soybean protein microballoon for adsorbing cadmium |
| CN108088804A (en) * | 2017-12-04 | 2018-05-29 | 武汉大学 | A kind of assay method of trace cadmium in water samples |
| CN115382900A (en) * | 2022-10-12 | 2022-11-25 | 成都理工大学 | Method for leaching and repairing heavy metal contaminated soil by using thiomalic acid |
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