CN103512796B - Flame atomic absorption spectrometry method for separating, enriching and detecting trace plumbum and cadmium in water sample by utilizing thiourea-modified silica gel - Google Patents
Flame atomic absorption spectrometry method for separating, enriching and detecting trace plumbum and cadmium in water sample by utilizing thiourea-modified silica gel Download PDFInfo
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Abstract
The invention discloses a flame atomic absorption spectrometry method for separating, enriching and detecting trace plumbum and cadmium in a water sample by utilizing thiourea-modified silica gel. Macroporous silica gel is used as a carrier to prepare the thiourea-modified silica gel, the thiourea-modified silica gel is used as an adsorbent to carry out microcolumn separation and enrichment of plumbum and cadmium, and a flame atomic absorption spectrometry detecting method is established. Within the concentration range of 0.5-10.0 <mu>g/mL, absorbance and the concentration of Pb (II) in the sample liquid are in a good linear relation: A=0.0122*C-0.0006(C: <mu>g/mL). Within the concentration range of 0.1-5.0 <mu>g/mL, the absorbance and the concentration of Cd (II) in the sample liquid are in a good linear relation: A=0.1943*C+0.0125 (C: <mu>g/mL). The detection limits of the method for detecting Pb (II) and Cd (II) are respectively 40.44 and 1.28 ng/mL. The method improves detection sensitivity and selectivity and is easy in automation for detecting low-concentration Pb (II) and Cd (II).
Description
Technical field
The present invention relates to a kind of method utilizing chemical modification adsorbent concentration and separation and atomic absorption spectrum coupling Rapid Determination of Trace Lead, cadmium.
Background technology
Along with global industry development, plumbous, cadmium pollution causes great threat to the mankind, therefore, in the urgent need to research and develop sensitive, fast, plumbous, cadmium separation and concentration technology easily, to meet the needs of the aspects such as environment measuring.
At present, method that is plumbous in separation and concentration water, cadmium has precipitation, ion-exchange, absorption etc.Wherein, absorption method is widely used with recycling because easy, efficient and adsorbent is renewable.In various solid adsorption material, silica gel adsorption performance is good, stable in properties.Direct use silica gel is as adsorbent for separating of enrichment, and its selectivity is not high, therefore, Silica Surface silicone hydroxyl must be utilized to carry out chemical modification and prepare selective absorbent, then detects after carrying out separation and concentration plumbous in sample solution, cadmium.
The flame atomic absorption spectrometry method of trace lead, cadmium in thiourea modified silica gel separation and concentration-mensuration water sample is utilized not have correlative study temporarily at present.
Summary of the invention
The invention reside in the flame atomic absorption spectrometry method that trace lead, cadmium in a kind of high selectivity separation and concentration-mensuration water sample are provided.
Conceive as follows: although silica gel adsorption performance is good, stable in properties, directly use silica gel as adsorbent for separating of enrichment, its selectivity is not high, therefore, usually utilizes Silica Surface silicone hydroxyl to carry out modification.Arrive Cyanuric Chloride Silica Surface by substitution reaction by thiourea modified, thus improve the selectivity of silica gel enriched lead, cadmium, the sensitivity of raising Flame Atomic Absorption Spectrometry Determination trace lead, cadmium and antijamming capability.In this experiment, utilize thiourea modified silica gel as microtrabeculae adsorbent, plumbous in complicated substrate sample solution, cadmium can be carried out dynamic enrichment and be separated, reduce manual steps, improve the reappearance and precision that measure.
The present invention relates to dynamic microcolumn separation and enrichment and the coupling of atomic absorption light spectral method.When plumbous in testing sample solution, cadmium is by the microtrabeculae that is loaded with adsorbent, plumbous, cadmium and Silica Surface thiourea group generation Absorptive complex wave, then with eluent by lead, cadmium wash-out carry out Atomic Absorption Spectrometry.
Concrete steps are as follows:
(1) thiourea modified silica gel preparation:
Take 30-70 order microsphere silica gel 30g, be placed in 250mL there-necked flask, install condenser pipe, add the hydrochloric acid that 150.0mL concentration is 6.0mol/L, heating makes solution return and mechanical raking 5-6 hour, cooled and filtered goes out silica gel, and washing to wash solution with distilled water by silica gel is neutral (whether having chlorion with the silver nitrate inspection wash solution that mass percent is 2%), and vacuum drying obtains activated silica gel.
Take the above-mentioned activated silica gel of 30.0g, be placed in 250ml there-necked flask, add the chemical pure gamma-aminopropyl-triethoxy-silane (KH550) after 100.0mL analysis pure toluene and 10.0-15.0mL distilation respectively, mechanical raking also adds hot reflux 6 hours, cooled and filtered solid product, respectively wash solid product 3 times with analysis pure toluene, absolute ethyl alcohol, after vacuum drying, obtain γ-Aminopropyl silica gel (APSG).
Take 8.0-10.0g to analyze pure Cyanuric Chloride and be dissolved in 250ml there-necked flask, add 150mL and analyze pure toluene and the above-mentioned γ-Aminopropyl silica gel of 20.0g, potpourri mechanical raking 2 hours in ice-water bath, filtering solids product, respectively wash 5 times with analysis pure toluene, ethanol respectively, the drying of suction filtration final vacuum obtains Cyanuric Chloride modified silica-gel (CCSG).
Take 10.0g and analyze bright sulfur urea in 250ml there-necked flask, install condenser pipe, add 100ml and analyze pure N, dinethylformamide (DMF) makes thiocarbamide dissolve, add 20.0g Cyanuric Chloride modified silica-gel again, at 80 DEG C, mechanical raking refluxes 4 hours, and cooled and filtered solid product also washs 5 times with the pure DMF of analysis, and the drying of suction filtration final vacuum obtains thiourea modified silica gel (TUSG).
(2) thiourea modified silica gel separation and concentration lead, cadmium:
By peristaltic pump, self-made miniature post, ((7cm × 0.5mm i.d.), polyfluortetraethylene pipe (0.8mm i.d) and jointing are formed separation and concentration device.First a small amount of glass wool beyond the Great Wall in pillar one end before dress post, upper prop loads thiourea modified silica gel absorber prepared by step (1) in a wet process, then fills in a small amount of glass wool, and compacting also connects, utilize peristaltic pump that redistilled water is pumped into micro-column, for subsequent use after washing; The separation and concentration step of Pb (II) is as follows: Pb (II) solution of pH=5.0 is passed through micro-column with 2.4mL/min flow velocity, then wash away not by the ion adsorbed in micro-column with the blank solution of 5.0mL pH=5.0 with 2.4mL/min flow velocity, with 10.0mL 1.0mol/L HCl with the reverse wash-out of 4.2mL/min flow velocity by the Pb (II) adsorbed; The separation and concentration step of Cd (II) is as follows: Cd (II) solution of pH=6.0 is passed through micro-column with 2.4mL/min flow velocity, then wash away not by the ion adsorbed in micro-column with the blank solution of 5.0mL pH=6.0 with 2.4mL/min flow velocity, with 10.0mL 1.0mol/L HCl with the reverse wash-out of 4.2mL/min flow velocity by the Cd (II) adsorbed.Elute soln is used 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 the Pb (II) in Flame Atomic Absorption Spectrometry Determination above-mentioned steps (2) gained eluent or Cd (II) concentration.
(4) drafting of standard working curve:
Pb (II) standard solution of 10.0mL pH=5.0 or Cd (II) standard solution of pH=6.0 are carried out separation and concentration and Atomic Absorption Spectrometry according to step (2) and step (3); In 0.5-10.0 μ g/mL concentration range, in absorbance and sample liquid, Pb (II) concentration is good linear relationship: A=0.0122*C-0.0006, C are concentration, and its unit is μ g/mL, linearly dependent coefficient r=0.9994; In 0.1-5.0 μ g/mL concentration range, in absorbance and sample liquid, Cd (II) concentration is good linear relationship: A=0.1943*C+0.0125, C are concentration, and its unit is μ g/mL, linearly dependent coefficient r=0.9993.
(5) mensuration that is plumbous in test sample, cadmium content is treated:
Pb (II) sample solution of pH=5.0 or Cd (II) sample solution of pH=6.0 are carried out separation and concentration and Atomic Absorption Spectrometry according to step (2) and step (3), obtains absorbance A; Finally calculate Pb in sample solution (II) or Cd (II) concentration according to calibration curve.
Instant invention overcomes the complex operation that existing static separation technology exists, the shortcomings such as step is complicated, reappearance is bad, improve sensitivity and the selectivity of detection better, and detection that is plumbous for super low concentration, cadmium is easy to robotization.
Accompanying drawing explanation
Fig. 1 is the preparation flow figure of thiourea modified silica gel in the present invention.
Embodiment
Embodiment:
(1) thiourea modified silica gel preparation:
Take 30-70 order microsphere silica gel 30g, be placed in 250mL there-necked flask, install condenser pipe, add the hydrochloric acid that 150.0mL concentration is 6.0mol/L, heating makes solution return and mechanical raking 6 hours, cooled and filtered goes out silica gel, and washing to wash solution with distilled water by silica gel is neutral (whether having chlorion with the silver nitrate inspection wash solution that mass percent is 2%), and vacuum drying obtains activated silica gel.
Take the above-mentioned activated silica gel of 30.0g, be placed in 250ml there-necked flask, add the chemical pure gamma-aminopropyl-triethoxy-silane (KH550) after 100.0mL analysis pure toluene and 12.0mL distilation respectively, mechanical raking also adds hot reflux 6 hours, cooled and filtered solid product, respectively wash solid product 3 times with analysis pure toluene, absolute ethyl alcohol, after vacuum drying, obtain γ-Aminopropyl silica gel (APSG).
Take 9.0g to analyze pure Cyanuric Chloride and be dissolved in 250ml there-necked flask, add 150mL and analyze pure toluene and the above-mentioned γ-Aminopropyl silica gel of 20.0g, potpourri mechanical raking 2 hours in ice-water bath, filtering solids product, respectively wash 5 times with analysis pure toluene, absolute ethyl alcohol respectively, the drying of suction filtration final vacuum obtains Cyanuric Chloride modified silica-gel (CCSG).
Take 10.0g and analyze bright sulfur urea in 250ml there-necked flask, install condenser pipe, add 100ml and analyze pure N, dinethylformamide (DMF) makes thiocarbamide dissolve, add 20.0g Cyanuric Chloride modified silica-gel again, at 80 DEG C, mechanical raking refluxes 4 hours, and cooled and filtered solid product also washs 5 times with the pure DMF of analysis, and the drying of suction filtration final vacuum obtains thiourea modified silica gel (TUSG).Absorbent preparation flow process is as Fig. 1.
(2) thiourea modified silica gel separation and concentration lead, cadmium:
By peristaltic pump, self-made miniature post, ((7cm × 0.5mm i.d.), polyfluortetraethylene pipe (0.8mm i.d) and jointing are formed separation and concentration device.First a small amount of glass wool beyond the Great Wall in pillar one end before dress post, upper prop loads thiourea modified silica gel absorber prepared by step (1) in a wet process, then fills in a small amount of glass wool, and compacting also connects, utilize peristaltic pump that redistilled water is pumped into micro-column, for subsequent use after washing; The separation and concentration step of Pb (II) is as follows: Pb (II) solution of pH=5.0 is passed through micro-column with 2.4mL/min flow velocity, then wash away not by the ion adsorbed in micro-column with the blank solution of 5.0mL pH=5.0 with 2.4mL/min flow velocity, with 10.0mL 1.0mol/L HCl with the reverse wash-out of 4.2mL/min flow velocity by the Pb (II) adsorbed; The separation and concentration step of Cd (II) is as follows: Cd (II) solution of pH=6.0 is passed through micro-column with 2.4mL/min flow velocity, then wash away not by the ion adsorbed in micro-column with the blank solution of 5.0mL pH=6.0 with 2.4mL/min flow velocity, with 10.0mL 1.0mol/L HCl with the reverse wash-out of 4.2mL/min flow velocity by the Cd (II) adsorbed.Elute soln is used 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 the Pb (II) in Flame Atomic Absorption Spectrometry Determination above-mentioned steps (2) gained eluent or Cd (II) concentration.
(4) drafting of standard working curve:
Pb (II) standard solution of 10.0mL pH=5.0 or Cd (II) standard solution of pH=6.0 are carried out separation and concentration and Atomic Absorption Spectrometry according to step (2) and step (3); In 0.5-10.0 μ g/mL concentration range, in absorbance and sample liquid, Pb (II) concentration is good linear relationship: A=0.0122*C-0.0006, C are concentration, and its unit is μ g/mL, linearly dependent coefficient r=0.9994; In 0.1-5.0 μ g/mL concentration range, in absorbance and sample liquid, Cd (II) concentration is good linear relationship: A=0.1943*C+0.0125, C are concentration, and its unit is μ g/mL, linearly dependent coefficient r=0.9993.
(5) mensuration that is plumbous in test sample, cadmium content is treated:
Pb (II) sample solution of pH=5.0 or Cd (II) sample solution of pH=6.0 are carried out separation and concentration and Atomic Absorption Spectrometry according to step (2) and step (3), obtains absorbance A; Finally calculate Pb in sample solution (II) or Cd (II) concentration according to calibration curve, calculate the recovery, result is as shown in table 1.
Table 1 sample determination and mark-on recovery test result
Claims (1)
1. the flame atomic absorption spectrometry method of trace lead, cadmium in thiourea modified silica gel separation and concentration-mensuration water sample, is characterized in that concrete steps are as follows:
(1) thiourea modified silica gel 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 makes solution return and mechanical raking 5-6 hour, and cooled and filtered goes out silica gel, and it is neutral for washing silica gel to wash solution with distilled water, whether have chlorion with the silver nitrate inspection wash solution that mass percent is 2%, vacuum drying obtains activated silica gel;
Take the above-mentioned activated silica gel of 30.0g, be placed in 250ml there-necked flask, add the chemical pure gamma-aminopropyl-triethoxy-silane after 100.0mL analysis pure toluene and 10.0-15.0 mL distilation and KH550 respectively, mechanical raking also adds hot reflux 6 hours, cooled and filtered solid product, respectively wash solid product 3 times with analysis pure toluene, absolute ethyl alcohol, after vacuum drying, obtain γ-Aminopropyl silica gel and APSG;
Take 8.0-10.0 g to analyze pure Cyanuric Chloride and be dissolved in 250ml there-necked flask, add 150 mL and analyze pure toluene and the above-mentioned γ-Aminopropyl silica gel of 20.0g, potpourri mechanical raking 2 hours in ice-water bath, filtering solids product, respectively wash 5 times with analysis pure toluene, absolute ethyl alcohol respectively, the drying of suction filtration final vacuum obtains Cyanuric Chloride modified silica-gel and CCSG;
Take 10.0g and analyze bright sulfur urea in 250ml there-necked flask, install condenser pipe, add 100 ml and analyze pure N, dinethylformamide and DMF make thiocarbamide dissolve, add 20.0g Cyanuric Chloride modified silica-gel again, at 80 DEG C, mechanical raking refluxes 4 hours, and cooled and filtered solid product also washs 5 times with the pure DMF of analysis, and the drying of suction filtration final vacuum obtains thiourea modified silica gel and TUSG;
(2) thiourea modified silica gel separation and concentration lead, cadmium:
Separation and concentration device is made up of peristaltic pump, self-made miniature post, polyfluortetraethylene pipe and jointing; First a small amount of glass wool beyond the Great Wall in pillar one end before dress post, upper prop loads thiourea modified silica gel absorber prepared by step (1) in a wet process, then fills in a small amount of glass wool, and compacting also connects, and utilizes peristaltic pump that redistilled water is pumped into micro-column, for subsequent use after washing; The separation and concentration step of Pb (II) is as follows: by Pb (II) solution of pH=5.0 with 2.4 mL
/min flow velocity, by micro-column, then uses the blank solution of 5.0mL pH=5.0 with 2.4 mL
/min flow velocity washes away not by the ion adsorbed in micro-column, with 10.0mL 1.0 mol
/l HCl is with 4.2 mL
/the reverse wash-out of min flow velocity is by the Pb (II) adsorbed; The separation and concentration step of Cd (II) is as follows: by Cd (II) solution of pH=6.0 with 2.4 mL
/min flow velocity, by micro-column, then uses the blank solution of 5.0mL pH=6.0 with 2.4 mL
/min flow velocity washes away not by the ion adsorbed in micro-column, with 10.0mL 1.0 mol
/l HCl is with 4.2 mL
/the reverse wash-out of min flow velocity is by the Cd (II) adsorbed; Elute soln is used 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 the Pb (II) in Flame Atomic Absorption Spectrometry Determination above-mentioned steps (2) gained eluent or Cd (II) concentration;
(4) drafting of standard working curve:
Pb (II) standard solution of 10.0mL pH=5.0 or Cd (II) standard solution of pH=6.0 are carried out separation and concentration and Atomic Absorption Spectrometry according to step (2) and step (3); In 0.5-10.0 μ g/mL concentration range, in absorbance and sample liquid, Pb (II) concentration is good linear relationship: A=0.0122*C-0.0006, C are concentration, and its unit is μ g/mL, linearly dependent coefficient
r=0.9994; In 0.1-5.0 μ g/mL concentration range, in absorbance and sample liquid, Cd (II) concentration is good linear relationship: A=0.1943*C+0.0125, C are concentration, and its unit is μ g/mL, linearly dependent coefficient
r=0.9993;
(5) mensuration that is plumbous in test sample, cadmium content is treated:
Pb (II) sample solution of pH=5.0 or Cd (II) sample solution of pH=6.0 are carried out separation and concentration and Atomic Absorption Spectrometry according to step (2) and step (3), obtains absorbance A; Finally calculate Pb in sample solution (II) or Cd (II) concentration according to calibration curve.
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