CN106769926A - Copper, cadmium in a kind of detection tea oil, the method for lead - Google Patents

Copper, cadmium in a kind of detection tea oil, the method for lead Download PDF

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CN106769926A
CN106769926A CN201611083050.6A CN201611083050A CN106769926A CN 106769926 A CN106769926 A CN 106769926A CN 201611083050 A CN201611083050 A CN 201611083050A CN 106769926 A CN106769926 A CN 106769926A
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carbon nano
walled carbon
phase extraction
solid phase
extraction column
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张帆
黄志强
张莹
颜鸿飞
吴波
李忠海
周文化
喻念念
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HUNAN ACADEMY OF INSPECTION AND QUARANTINE
Central South University of Forestry and Technology
Changsha Environmental Protection College
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HUNAN ACADEMY OF INSPECTION AND QUARANTINE
Central South University of Forestry and Technology
Changsha Environmental Protection College
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Abstract

The present invention passes through enrichment and separation of the hydroxyl multi-walled carbon nano-tube solid phase extraction column to the copper in the tea oil sample solution through clearing up, cadmium and the heavy metal species ion of lead three, by hydroxyl multi-walled carbon nano-tube to the strong selectivity adsorption capacity of these three heavy metal ion such that it is able to obtain relatively low detection lower bound and accumulation ability higher.Flame atomic absorption spectrophotometer can be made full use of to determine copper, cadmium and the lead ion of trace in tea oil, selectively good, strong adaptability, not only analyze speed is fast, and cost greatly reduces compared with other analytical instrument.

Description

Copper, cadmium in a kind of detection tea oil, the method for lead
Technical field
The present invention relates to it is a kind of detect edible oil in copper, cadmium, lead method, specially it is a kind of detect tea oil in copper, The method of cadmium, lead.
Background technology
Flame atomic absorption spectrometry（FAAS）It is cheap etc. excellent by its high selectivity, quick, easy to operate, analysis cost Gesture turns into widely used analysis method in trace metal ion monitoring.Due to content of these heavy metals in food generally all It is very low, it is difficult to directly determined with instrument, so as to the sensitivity and the degree of accuracy to analysis method are proposed requirement higher.Although Flame atomic absorption spectrometry has significant analysis ability to the metal of low concentration, but its detection lower bound is usually μ gl-1, phase For graphite oven atomic absorption and inductively coupled plasma emission spectrography etc., test limit is slightly higher, in order to further promote The detection sensitivity and selectivity entered required for method reaches analysis, generally require that sample is needed suitably to be pre-separated And enriching step.The abstraction techniques such as SPE, liquid-liquid extraction, cloud point extraction, SPME are that application at present is more to be divided From and enrichment method.SPE（SPE）Because its have quickly, preenrichment multiple is big, the good, sorbing material of selectivity can be repeated The advantages of being used for multiple times, increasingly receives an acclaim in the preceding treatment application of heavy metal analysis.
In SPE, filler is a very crucial factor for influenceing effect of extracting.As traditional absorption such as C18 Material, has the deficiency of the aspects such as pH is unstable and opposed polarity extract common extraction is more difficult, the new solid phase of exploitation Therefore extraction sorbing material turns into the focus of analysis scholar's research.With the fast development of nanometer technology, with big specific surface The application of product, the CNT that chemical stability is high, adsorptivity is strong in SPE is more and more extensive.This research uses hydroxyl , to the special absorption property of metal, self-control hydroxyl multi-walled carbon nano-tube glass solid phase extraction column is to tea for multi-walled carbon nano-tube Copper, cadmium and lead carry out preenrichment and separation in oil, with reference to flame atomic absorption spectrometry, establish a kind of quick, selectivity it is high, Accurately, in tea oil with low cost Cu, Cd and Pb detection method.
The content of the invention
It is an object of the invention to provide it is a kind of detect tea oil in copper, cadmium, lead method, the technology used in the present invention Scheme is as follows：
Copper, cadmium in a kind of detection tea oil, the method for lead, comprise the following steps：
(1) weigh tea oil to obtain treating test sample after pretreatment, prepare hydroxyl multi-walled carbon nano-tube solid phase extraction column, and to hydroxyl Base multi-walled carbon nano-tube solid phase extraction column is cleaned and activated, while doing reagent blank；
(2) test sample or hybrid standard sample are treated using hydroxyl multi-walled carbon nano-tube solid phase extraction column separation and concentration, uses eluent Wash-out hydroxyl multi-walled carbon nano-tube solid phase extraction column obtains treating the wash-out solution of test sample or hybrid standard sample；
(3) wash-out solution is measured through flame atomic absorption spectrophotometer.
The pretreated mode of tea oil is dry ashing method or Wet etc..
Preparing hydroxyl multi-walled carbon nano-tube solid phase extraction column step includes：
(1) through nitric acid dousing and solid phase extraction column is rinsed well；
(2) lower sieve plate, hydroxyl multi-walled carbon nano-tube filler are sequentially placed into, upper sieve plate is fixed and pressed by upper sieve plate, lower sieve plate Tight hydroxyl multi-walled carbon nano-tube packing layer.
Hydroxyl multi-walled carbon nano-tube solid phase extraction column carries out cleaning and activation step to be included：
(1) rinsed except residual in de-hydroxylated multi-walled carbon nano-tubes solid phase extraction column using absolute ethyl alcohol, salpeter solution successively Metal ion and other impurities；
(2) continue drip washing hydroxyl multi-walled carbon nano-tube solid phase extraction column with 10 ~ 15mL ultra-pure waters, complete many wall carbon of hydroxylating The cleaning and activation of nanotube solid phase extraction column.
Test sample or hybrid standard sample are treated using hydroxyl multi-walled carbon nano-tube solid phase extraction column separation and concentration, eluent is used Wash-out hydroxyl multi-walled carbon nano-tube solid phase extraction column obtains treating the wash-out solution of test sample or hybrid standard sample, including following step Suddenly：
（1）50.0 ~ 150mL is taken to treat test sample or contain Cu2+、Cd2+And Pb2+Hybrid standard sample（Cu2+、Cd2+And Pb2+Concentration point Other 0.2mg/L, 0.04mg/L, 0.2mg/L）, solution ph to 6.0- is adjusted with PBS or sodium hydroxide solution 8.0, it is solid by hydroxyl multi-walled carbon nano-tube with the flow velocity of 1.0-4.0mL/min under the control of solid-phase extraction device peristaltic pump Mutually extract pillar；
（2）Use 5-10mL concentration be 1-3mol/L hydrochloric acid solution with the flow velocity of 1.0-2.0mL/min to being enriched Cu2+、Cd2 +And Pb2+Hydroxyl multi-walled carbon nano-tube solid phase extraction column eluted, must treat that the wash-out of test sample or hybrid standard sample is molten Liquid.
The method that flame atomic absorption spectrophotometer is measured includes：
（1）Determining instrument：Atomic absorption spectrophotometer;Determine the instrument condition of copper：Wavelength 324.8nm, slit 0.5nm, lamp current 3.0mA, acetylene flow 2.0L/min, air mass flow 10L/min;Determine the instrument condition of cadmium element：Wavelength 228.8nm, slit 0.5nm, lamp current 4.0mA, acetylene flow 2.0L/min, air mass flow 11.0L/min;Determine lead element Instrument condition：Wavelength 283.3nm, slit 0.5nm, lamp current 5.0mA, acetylene flow 2.0L/min, air mass flow 10.0L/ min;The wash-out solution of test sample or hybrid standard sample is treated using Flame Atomic Absorption Spectrometry Determination；
（2）The drafting of standard working curve：In 0.5 ~ 4.0 μ g/mL concentration ranges, Cu in absorbance and hybrid standard sample2+It is dense Degree is in good linear relationship：Abs=0.13820*C+0.01048, C are concentration, and its unit is μ g/mL, linearly dependent coefficient r= 0.9996；In 0.05 ~ 0.5 μ g/mL concentration ranges, Cd in absorbance and hybrid standard sample2+Concentration is in good linear relationship： Abs=0.31387*C+0.00263, C are concentration, and its unit is μ g/mL, linearly dependent coefficient r=0.9998, in 0.5 ~ 4.0 μ g/ In mL concentration ranges, Pb in absorbance and hybrid standard sample2+Concentration is in good linear relationship：Abs=0.02833*C+ 0.00166, C is concentration, and its unit is μ g/mL, linearly dependent coefficient r=0.9999；
（3）Treat Cu in test sample2+、Cd2+And Pb2+The measure of content：Absorbance A bs is obtained by flame atomic absorption spectrophotometer；Most Cu in sample solution is calculated according to standard working curve afterwards2+、Cd2+And Pb2+Concentration.
As a kind of preferred：When solution ph is adjusted to 7.0 with PBS or sodium hydroxide solution, Cu2+、 Cd2+And Pb2+Preferable extraction yield can be obtained.
As a kind of preferred：Use 5mL concentration be 1mol/L hydrochloric acid solution with the flow velocity of 1.0mL/min to being enriched Cu2+、Cd2+And Pb2+Hydroxyl multi-walled carbon nano-tube solid phase extraction column eluted, average recovery rate and standard deviation difference Not Wei 94.0 ± 1.3,91.3 ± 2.5,90.5 ± 0.8, elution efficiency is more satisfactory.
As a kind of preferred：The pretreated mode of tea oil is Wet, copper in the sample in sample after treatment, Cadmium, lead element average recovery rate scope between 92% ~ 95%.
As a kind of preferred：Hydroxyl multi-walled carbon nano-tube, external diameter is 20-30nm, and length is 0.5-2 μm.
As a kind of preferred：When hydroxyl multi-walled carbon nano-tube consumption is 200mg, Cu2+、Cd2+And Pb2+Can obtain Highest extraction yield.
The present invention by hydroxyl multi-walled carbon nano-tube solid phase extraction column to the copper in the tea oil sample solution through clearing up, The enrichment and separation of cadmium and the heavy metal species ion of lead three, by hydroxyl multi-walled carbon nano-tube to the strong of these three heavy metal ion Selective adsorption capacity such that it is able to obtain relatively low detection lower bound and accumulation ability higher.Flame can be made full use of former Sub- absorption spectrometer determines copper, cadmium and the lead ion of trace in tea oil, good, the strong adaptability of selectivity, and not only analyze speed is fast, And cost greatly reduces compared with other analytical instrument.
Copper ion and lead ion are in the range of 0.5 ~ 4.0mg/kg, and cadmium ion is linear to close in the range of 0.05 ~ 0.5mg/kg System is good, and coefficient correlation is all higher than 0.999；Addition recovery experiment of three metal ion species in linear scope, average recovery rate It is that 90.5% ~ 94.0%, RSD is 2.1% ~ 3.8%, disclosure satisfy that the detection needs of copper, cadmium and lead ion in tea oil.
Specific embodiment
Embodiment 1
Copper, cadmium in a kind of detection tea oil, the method for lead, comprise the following steps：
(1) weigh tea oil to obtain treating test sample after pretreatment, prepare hydroxyl multi-walled carbon nano-tube solid phase extraction column, and to hydroxyl Base multi-walled carbon nano-tube solid phase extraction column is cleaned and activated, while doing reagent blank；
(2) test sample or hybrid standard sample are treated using hydroxyl multi-walled carbon nano-tube solid phase extraction column separation and concentration, uses eluent Wash-out hydroxyl multi-walled carbon nano-tube solid phase extraction column obtains treating the wash-out solution of test sample or hybrid standard sample；
The pretreated mode of tea oil is dry ashing method：
Weigh tea oil sample 1.00g（It is accurate to 0.01g）In 25mL porcelain crucibles, porcelain crucible is placed in less fire first adjustable Carbonized on formula electric furnace to smokeless, then porcelain crucible is transferred in Muffle furnace, 390 DEG C of 4 ~ 6h of ashing add 1mL after taking out cooling (nitric acid and perchloric acid, volume ratio are 1 to mixed acid：4), in continuing to heat ash content dissolving on electric hot plate up to digestion is complete, put After repeatedly washing porcelain crucible with 1% dust technology after cold, it is transferred in 50mL volumetric flasks, and dust technology with 1% is settled to scale.
Preparing hydroxyl multi-walled carbon nano-tube solid phase extraction column step includes：
(1) through nitric acid dousing and 6mL glass SPE pillars are rinsed well；
(2) sieve plate, 200mg hydroxyl multi-walled carbon nano-tube fillers under supporting 6mL are sequentially placed into SPE pillars, are sieved on 6mL Plate, fixes and compresses hydroxyl multi-walled carbon nano-tube packing layer by sieve plate under 6mL upper sieve plates, 6mL.
Hydroxyl multi-walled carbon nano-tube solid phase extraction column carries out cleaning and activation step to be included：
(1) rinsed except de-hydroxylated multi-walled carbon nano-tubes solid phase extracts using 6mL absolute ethyl alcohols, 4mL1mol/L salpeter solutions successively Take the metal ion and other impurities remained in pillar；
(2) continue drip washing hydroxyl multi-walled carbon nano-tube solid phase extraction column with 10 ~ 15mL ultra-pure waters, complete many wall carbon of hydroxylating The cleaning and activation of nanotube solid phase extraction column.
Test sample or hybrid standard sample are treated using hydroxyl multi-walled carbon nano-tube solid phase extraction column separation and concentration, eluent is used Wash-out hydroxyl multi-walled carbon nano-tube solid phase extraction column obtains treating the wash-out solution of test sample or hybrid standard sample, including following step Suddenly：
（1）50.0mL is taken to treat test sample or contain Cu2+、Cd2+And Pb2+Hybrid standard sample（Cu2+、Cd2+And Pb2+Concentration is distinguished 0.2mg/L、0.04mg/L、0.2mg/L）, solution ph to 7.0 is adjusted with PBS or sodium hydroxide solution, It is small by hydroxyl multi-walled carbon nano-tube SPE with the flow velocity of 3.0mL/min under the control of solid-phase extraction device peristaltic pump Post；
（2）Use 5mL concentration be 1mol/L hydrochloric acid solution with the flow velocity of 1.0mL/min to being enriched Cu2+、Cd2+And Pb2+'s Hydroxyl multi-walled carbon nano-tube solid phase extraction column is eluted, and must treat the wash-out solution of test sample or hybrid standard sample.
The method that flame atomic absorption spectrophotometer is measured includes：
（1）Determining instrument：Atomic absorption spectrophotometer;Determine the instrument condition of copper：Wavelength 324.8nm, slit 0.5nm, lamp current 3.0mA, acetylene flow 2.0L/min, air mass flow 10L/min;Determine the instrument condition of cadmium element：Wavelength 228.8nm, slit 0.5nm, lamp current 4.0mA, acetylene flow 2.0L/min, air mass flow 11.0L/min;Determine lead element Instrument condition：Wavelength 283.3nm, slit 0.5nm, lamp current 5.0mA, acetylene flow 2.0L/min, air mass flow 10.0L/ min;The wash-out solution of test sample or hybrid standard sample is treated using Flame Atomic Absorption Spectrometry Determination；
（2）The drafting of standard working curve：In 0.5 ~ 4.0 μ g/mL concentration ranges, Cu in absorbance and hybrid standard sample2+It is dense Degree is in good linear relationship：Abs=0.13820*C+0.01048, C are concentration, and its unit is μ g/mL, linearly dependent coefficient r= 0.9996；In 0.05 ~ 0.5 μ g/mL concentration ranges, Cd in absorbance and hybrid standard sample2+Concentration is in good linear relationship： Abs=0.31387*C+0.00263, C are concentration, and its unit is μ g/mL, linearly dependent coefficient r=0.9998, in 0.5 ~ 4.0 μ g/ In mL concentration ranges, Pb in absorbance and hybrid standard sample2+Concentration is in good linear relationship：Abs=0.02833*C+ 0.00166, C is concentration, and its unit is μ g/mL, linearly dependent coefficient r=0.9999；
（3）Treat Cu in test sample2+、Cd2+And Pb2+The measure of content：Absorbance A bs is obtained by flame atomic absorption spectrophotometer；Most Cu in sample solution is calculated according to standard working curve afterwards2+、Cd2+And Pb2+Concentration.
Embodiment 2
Copper, cadmium in a kind of detection tea oil, the method for lead, comprise the following steps：
(1) weigh tea oil to obtain treating test sample after pretreatment, prepare hydroxyl multi-walled carbon nano-tube solid phase extraction column, and to hydroxyl Base multi-walled carbon nano-tube solid phase extraction column is cleaned and activated, while doing reagent blank；
(2) test sample or hybrid standard sample are treated using hydroxyl multi-walled carbon nano-tube solid phase extraction column separation and concentration, uses eluent Wash-out hydroxyl multi-walled carbon nano-tube solid phase extraction column obtains treating the wash-out solution of test sample or hybrid standard sample；
The pretreated mode of tea oil is Wet：
Weigh 3.0g（It is accurate to 0.01g）Tea oil sample in 150mL conical flasks, add 45mL nitric acid, add a cover, make sample with The mixture soaked overnight together of acid.Then the conical flask that small funnel will be added a cover is put into several beades, is placed into electric heating Cleared up in heating at 160 DEG C on plate, as the nitric acid residue about 3 ~ 4mL or so in bottle, flask is removed somewhat from electric hot plate After cooling, then toward addition 45mL hydrogen peroxide, 15mL nitric acid in conical flask, then waited to disappear in 160 DEG C of heating on electric hot plate After solution vigorous reaction terminates, continue to heat after electric plate temperature is raised into 60 DEG C, constant temperature digestion is extremely clarified, after removing small funnel, Acid is caught up with 240 DEG C until closely doing, conical flask is removed, after repeatedly washing flask using 1% dust technology after cooling, is transferred to In 150mL volumetric flasks, and dust technology with 1% is settled to scale.
Preparing hydroxyl multi-walled carbon nano-tube solid phase extraction column step includes：
(1) through nitric acid dousing and 6mL glass SPE pillars are rinsed well；
(2) sieve plate, 200mg hydroxyl multi-walled carbon nano-tube fillers under supporting 6mL are sequentially placed into SPE pillars, are sieved on 6mL Plate, fixes and compresses hydroxyl multi-walled carbon nano-tube packing layer by sieve plate under 6mL upper sieve plates, 6mL.
Hydroxyl multi-walled carbon nano-tube solid phase extraction column carries out cleaning and activation step to be included：
(1) rinsed except de-hydroxylated multi-walled carbon nano-tubes solid phase extracts using 6mL absolute ethyl alcohols, 4mL1mol/L salpeter solutions successively Take the metal ion and other impurities remained in pillar；
(2) continue drip washing hydroxyl multi-walled carbon nano-tube solid phase extraction column with 10 ~ 15mL ultra-pure waters, complete many wall carbon of hydroxylating The cleaning and activation of nanotube solid phase extraction column.
Test sample or hybrid standard sample are treated using hydroxyl multi-walled carbon nano-tube solid phase extraction column separation and concentration, eluent is used Wash-out hydroxyl multi-walled carbon nano-tube solid phase extraction column obtains treating the wash-out solution of test sample or hybrid standard sample, including following step Suddenly：
（1）150.0mL is taken to treat test sample or contain Cu2+、Cd2+And Pb2+Hybrid standard sample（Cu2+、Cd2+And Pb2+Concentration is distinguished 0.2mg/L、0.04mg/L、0.2mg/L）, solution ph to 6.0 is adjusted with PBS or sodium hydroxide solution, It is small by hydroxyl multi-walled carbon nano-tube SPE with the flow velocity of 1.0mL/min under the control of solid-phase extraction device peristaltic pump Post；
（2）Use 10mL concentration be 3mol/L hydrochloric acid solution with the flow velocity of 2.0mL/min to being enriched Cu2+、Cd2+And Pb2+'s Hydroxyl multi-walled carbon nano-tube solid phase extraction column is eluted, and must treat the wash-out solution of test sample or hybrid standard sample.
The method that flame atomic absorption spectrophotometer is measured includes：
（1）Determining instrument：Atomic absorption spectrophotometer;Determine the instrument condition of copper：Wavelength 324.8nm, slit 0.5nm, lamp current 3.0mA, acetylene flow 2.0L/min, air mass flow 10L/min;Determine the instrument condition of cadmium element：Wavelength 228.8nm, slit 0.5nm, lamp current 4.0mA, acetylene flow 2.0L/min, air mass flow 11.0L/min;Determine lead element Instrument condition：Wavelength 283.3nm, slit 0.5nm, lamp current 5.0mA, acetylene flow 2.0L/min, air mass flow 10.0L/ min;The wash-out solution of test sample or hybrid standard sample is treated using Flame Atomic Absorption Spectrometry Determination；
（2）The drafting of standard working curve：In 0.5 ~ 4.0 μ g/mL concentration ranges, Cu in absorbance and hybrid standard sample2+It is dense Degree is in good linear relationship：Abs=0.13820*C+0.01048, C are concentration, and its unit is μ g/mL, linearly dependent coefficient r= 0.9996；In 0.05 ~ 0.5 μ g/mL concentration ranges, Cd in absorbance and hybrid standard sample2+Concentration is in good linear relationship： Abs=0.31387*C+0.00263, C are concentration, and its unit is μ g/mL, linearly dependent coefficient r=0.9998, in 0.5 ~ 4.0 μ g/ In mL concentration ranges, Pb in absorbance and hybrid standard sample2+Concentration is in good linear relationship：Abs=0.02833*C+ 0.00166, C is concentration, and its unit is μ g/mL, linearly dependent coefficient r=0.9999；
（3）Treat Cu in test sample2+、Cd2+And Pb2+The measure of content：Absorbance A bs is obtained by flame atomic absorption spectrophotometer；Most Cu in sample solution is calculated according to standard working curve afterwards2+、Cd2+And Pb2+Concentration.
Embodiment 3
Copper, cadmium in a kind of detection tea oil, the method for lead, comprise the following steps：
(1) weigh tea oil to obtain treating test sample after pretreatment, prepare hydroxyl multi-walled carbon nano-tube solid phase extraction column, and to hydroxyl Base multi-walled carbon nano-tube solid phase extraction column is cleaned and activated, while doing reagent blank；
(2) test sample or hybrid standard sample are treated using hydroxyl multi-walled carbon nano-tube solid phase extraction column separation and concentration, uses eluent Wash-out hydroxyl multi-walled carbon nano-tube solid phase extraction column obtains treating the wash-out solution of test sample or hybrid standard sample；
The pretreated mode of tea oil is dry ashing method：
Weigh tea oil sample 2.00g（It is accurate to 0.01g）In 25mL porcelain crucibles, porcelain crucible is placed in less fire first adjustable Carbonized on formula electric furnace to smokeless, then porcelain crucible is transferred in Muffle furnace, 390 DEG C of 4 ~ 6h of ashing add 2mL after taking out cooling (nitric acid and perchloric acid, volume ratio are 1 to mixed acid：4), in continuing to heat ash content dissolving on electric hot plate up to digestion is complete, put After repeatedly washing porcelain crucible with 1% dust technology after cold, it is transferred in 100mL volumetric flasks, and dust technology with 1% is settled to quarter Degree.
Preparing hydroxyl multi-walled carbon nano-tube solid phase extraction column step includes：
(1) through nitric acid dousing and 6mL glass SPE pillars are rinsed well；
(2) sieve plate, 200mg hydroxyl multi-walled carbon nano-tube fillers under supporting 6mL are sequentially placed into SPE pillars, are sieved on 6mL Plate, fixes and compresses hydroxyl multi-walled carbon nano-tube packing layer by sieve plate under 6mL upper sieve plates, 6mL.
Hydroxyl multi-walled carbon nano-tube solid phase extraction column carries out cleaning and activation step to be included：
(1) rinsed except de-hydroxylated multi-walled carbon nano-tubes solid phase extracts using 6mL absolute ethyl alcohols, 4mL1mol/L salpeter solutions successively Take the metal ion and other impurities remained in pillar；
(2) continue drip washing hydroxyl multi-walled carbon nano-tube solid phase extraction column with 10 ~ 15mL ultra-pure waters, complete many wall carbon of hydroxylating The cleaning and activation of nanotube solid phase extraction column.
Test sample or hybrid standard sample are treated using hydroxyl multi-walled carbon nano-tube solid phase extraction column separation and concentration, eluent is used Wash-out hydroxyl multi-walled carbon nano-tube solid phase extraction column obtains treating the wash-out solution of test sample or hybrid standard sample, including following step Suddenly：
（1）100.0mL is taken to treat test sample or contain Cu2+、Cd2+And Pb2+Hybrid standard sample（Cu2+、Cd2+And Pb2+Concentration is distinguished 0.2mg/L、0.04mg/L、0.2mg/L）, solution ph to 8.0 is adjusted with PBS or sodium hydroxide solution, It is small by hydroxyl multi-walled carbon nano-tube SPE with the flow velocity of 4.0mL/min under the control of solid-phase extraction device peristaltic pump Post；
（2）Use 7.5mL concentration be 2mol/L hydrochloric acid solution with the flow velocity of 1.5mL/min to being enriched Cu2+、Cd2+And Pb2+ Hydroxyl multi-walled carbon nano-tube solid phase extraction column eluted, the wash-out solution of test sample or hybrid standard sample must be treated.
The method that flame atomic absorption spectrophotometer is measured includes：
（1）Determining instrument：Atomic absorption spectrophotometer;Determine the instrument condition of copper：Wavelength 324.8nm, slit 0.5nm, lamp current 3.0mA, acetylene flow 2.0L/min, air mass flow 10L/min;Determine the instrument condition of cadmium element：Wavelength 228.8nm, slit 0.5nm, lamp current 4.0mA, acetylene flow 2.0L/min, air mass flow 11.0L/min;Determine lead element Instrument condition：Wavelength 283.3nm, slit 0.5nm, lamp current 5.0mA, acetylene flow 2.0L/min, air mass flow 10.0L/ min;The wash-out solution of test sample or hybrid standard sample is treated using Flame Atomic Absorption Spectrometry Determination；
（2）The drafting of standard working curve：In 0.5 ~ 4.0 μ g/mL concentration ranges, Cu in absorbance and hybrid standard sample2+It is dense Degree is in good linear relationship：Abs=0.13820*C+0.01048, C are concentration, and its unit is μ g/mL, linearly dependent coefficient r= 0.9996；In 0.05 ~ 0.5 μ g/mL concentration ranges, Cd in absorbance and hybrid standard sample2+Concentration is in good linear relationship： Abs=0.31387*C+0.00263, C are concentration, and its unit is μ g/mL, linearly dependent coefficient r=0.9998, in 0.5 ~ 4.0 μ g/ In mL concentration ranges, Pb in absorbance and hybrid standard sample2+Concentration is in good linear relationship：Abs=0.02833*C+ 0.00166, C is concentration, and its unit is μ g/mL, linearly dependent coefficient r=0.9999；
（3）Treat Cu in test sample2+、Cd2+And Pb2+The measure of content：Absorbance A bs is obtained by flame atomic absorption spectrophotometer；Most Cu in sample solution is calculated according to standard working curve afterwards2+、Cd2+And Pb2+Concentration.
Embodiment 4
Copper, cadmium in a kind of detection tea oil, the method for lead, comprise the following steps：
(1) weigh tea oil to obtain treating test sample after pretreatment, prepare hydroxyl multi-walled carbon nano-tube solid phase extraction column, and to hydroxyl Base multi-walled carbon nano-tube solid phase extraction column is cleaned and activated, while doing reagent blank；
(2) test sample or hybrid standard sample are treated using hydroxyl multi-walled carbon nano-tube solid phase extraction column separation and concentration, uses eluent Wash-out hydroxyl multi-walled carbon nano-tube solid phase extraction column obtains treating the wash-out solution of test sample or hybrid standard sample；
The pretreated mode of tea oil is dry ashing method：
Weigh tea oil sample 1.00g（It is accurate to 0.01g）In 25mL porcelain crucibles, porcelain crucible is placed in less fire first adjustable Carbonized on formula electric furnace to smokeless, then porcelain crucible is transferred in Muffle furnace, 390 DEG C of 4 ~ 6h of ashing add 1mL after taking out cooling (nitric acid and perchloric acid, volume ratio are 1 to mixed acid：4), in continuing to heat ash content dissolving on electric hot plate up to digestion is complete, put After repeatedly washing porcelain crucible with 1% dust technology after cold, it is transferred in 50mL volumetric flasks, and dust technology with 1% is settled to scale.
Preparing hydroxyl multi-walled carbon nano-tube solid phase extraction column step includes：
(1) through nitric acid dousing and 6mL glass SPE pillars are rinsed well；
(2) sieve plate, 200mg hydroxyl multi-walled carbon nano-tube fillers under supporting 6mL are sequentially placed into SPE pillars, are sieved on 6mL Plate, fixes and compresses hydroxyl multi-walled carbon nano-tube packing layer by sieve plate under 6mL upper sieve plates, 6mL.
Hydroxyl multi-walled carbon nano-tube solid phase extraction column carries out cleaning and activation step to be included：
(1) rinsed except de-hydroxylated multi-walled carbon nano-tubes solid phase extracts using 6mL absolute ethyl alcohols, 4mL1mol/L salpeter solutions successively Take the metal ion and other impurities remained in pillar；
(2) continue drip washing hydroxyl multi-walled carbon nano-tube solid phase extraction column with 10 ~ 15mL ultra-pure waters, complete many wall carbon of hydroxylating The cleaning and activation of nanotube solid phase extraction column.
Test sample or hybrid standard sample are treated using hydroxyl multi-walled carbon nano-tube solid phase extraction column separation and concentration, eluent is used Wash-out hydroxyl multi-walled carbon nano-tube solid phase extraction column obtains treating the wash-out solution of test sample or hybrid standard sample, including following step Suddenly：
（1）50.0mL is taken to treat test sample or contain Cu2+、Cd2+And Pb2+Hybrid standard sample（Cu2+、Cd2+And Pb2+Concentration is distinguished 0.2mg/L、0.04mg/L、0.2mg/L）, solution ph to 7.5 is adjusted with PBS or sodium hydroxide solution, It is small by hydroxyl multi-walled carbon nano-tube SPE with the flow velocity of 2.0mL/min under the control of solid-phase extraction device peristaltic pump Post；
（2）Use 8mL concentration be 1.5mol/L hydrochloric acid solution with the flow velocity of 1.5mL/min to being enriched Cu2+、Cd2+And Pb2+ Hydroxyl multi-walled carbon nano-tube solid phase extraction column eluted, the wash-out solution of test sample or hybrid standard sample must be treated.
The method that flame atomic absorption spectrophotometer is measured includes：
（1）Determining instrument：Atomic absorption spectrophotometer;Determine the instrument condition of copper：Wavelength 324.8nm, slit 0.5nm, lamp current 3.0mA, acetylene flow 2.0L/min, air mass flow 10L/min;Determine the instrument condition of cadmium element：Wavelength 228.8nm, slit 0.5nm, lamp current 4.0mA, acetylene flow 2.0L/min, air mass flow 11.0L/min;Determine lead element Instrument condition：Wavelength 283.3nm, slit 0.5nm, lamp current 5.0mA, acetylene flow 2.0L/min, air mass flow 10.0L/ min;The wash-out solution of test sample or hybrid standard sample is treated using Flame Atomic Absorption Spectrometry Determination；
（2）The drafting of standard working curve：In 0.5 ~ 4.0 μ g/mL concentration ranges, Cu in absorbance and hybrid standard sample2+It is dense Degree is in good linear relationship：Abs=0.13820*C+0.01048, C are concentration, and its unit is μ g/mL, linearly dependent coefficient r= 0.9996；In 0.05 ~ 0.5 μ g/mL concentration ranges, Cd in absorbance and hybrid standard sample2+Concentration is in good linear relationship： Abs=0.31387*C+0.00263, C are concentration, and its unit is μ g/mL, linearly dependent coefficient r=0.9998, in 0.5 ~ 4.0 μ g/ In mL concentration ranges, Pb in absorbance and hybrid standard sample2+Concentration is in good linear relationship：Abs=0.02833*C+ 0.00166, C is concentration, and its unit is μ g/mL, linearly dependent coefficient r=0.9999；
（3）Treat Cu in test sample2+、Cd2+And Pb2+The measure of content：Absorbance A bs is obtained by flame atomic absorption spectrophotometer；Most Cu in sample solution is calculated according to standard working curve afterwards2+、Cd2+And Pb2+Concentration.

Claims (6)

1. it is a kind of detect tea oil in copper, cadmium, the method for lead, it is characterised in that comprise the following steps：
(1) weigh tea oil to obtain treating test sample after pretreatment, prepare hydroxyl multi-walled carbon nano-tube solid phase extraction column, and to hydroxyl Base multi-walled carbon nano-tube solid phase extraction column is cleaned and activated, while doing reagent blank；
(2) test sample or hybrid standard sample are treated using hydroxyl multi-walled carbon nano-tube solid phase extraction column separation and concentration, uses eluent Wash-out hydroxyl multi-walled carbon nano-tube solid phase extraction column obtains treating the wash-out solution of test sample or hybrid standard sample；
(3) wash-out solution is measured through flame atomic absorption spectrophotometer.
2. it is according to claim 1 it is a kind of detect tea oil in copper, cadmium, the method for lead, it is characterised in that：Tea oil is through pre- place The mode of reason is dry ashing method or Wet.
3. it is according to claim 1 and 2 it is a kind of detect tea oil in copper, cadmium, the method for lead, it is characterised in that：Prepare hydroxyl Base multi-walled carbon nano-tube solid phase extraction column step includes：
(1) through nitric acid dousing and solid phase extraction column is rinsed well；
(2) lower sieve plate, hydroxyl multi-walled carbon nano-tube filler are sequentially placed into, upper sieve plate is fixed and pressed by upper sieve plate, lower sieve plate Tight hydroxyl multi-walled carbon nano-tube packing layer.
4. copper, cadmium, the method for lead in a kind of detection tea oil according to claim 1 or 2 or 3, it is characterised in that：Hydroxyl Multi-walled carbon nano-tube solid phase extraction column carries out cleaning and activation step to be included：
(1) rinsed except residual in de-hydroxylated multi-walled carbon nano-tubes solid phase extraction column using absolute ethyl alcohol, salpeter solution successively Metal ion and other impurities；
(2) continue drip washing hydroxyl multi-walled carbon nano-tube solid phase extraction column with 10 ~ 15mL ultra-pure waters, complete many wall carbon of hydroxylating The cleaning and activation of nanotube solid phase extraction column.
5. copper, cadmium, the method for lead in a kind of detection tea oil according to claim 1 or 2 or 3 or 4, it is characterised in that： Test sample or hybrid standard sample are treated using hydroxyl multi-walled carbon nano-tube solid phase extraction column separation and concentration, elution hydroxyl is used Multi-walled carbon nano-tube solid phase extraction column obtains treating the wash-out solution of test sample or hybrid standard sample, comprises the following steps：
(1) 50.0 ~ 150mL is taken to treat test sample or contain Cu2+、Cd2+And Pb2+Hybrid standard sample（Cu2+、Cd2+And Pb2+Concentration point Other 0.2mg/L, 0.04mg/L, 0.2mg/L）, solution ph to 6.0- is adjusted with PBS or sodium hydroxide solution 8.0, it is solid by hydroxyl multi-walled carbon nano-tube with the flow velocity of 1.0-4.0mL/min under the control of solid-phase extraction device peristaltic pump Mutually extract pillar；
(2) use 5-10mL concentration be 1-3mol/L hydrochloric acid solution with the flow velocity of 1.0-2.0mL/min to being enriched Cu2+、Cd2+ And Pb2+Hydroxyl multi-walled carbon nano-tube solid phase extraction column eluted, the wash-out solution of test sample or hybrid standard sample must be treated.
6. copper, cadmium, the method for lead in a kind of detection tea oil according to claim 1 or 2 or 3 or 4 or 5, its feature exists In：The method that flame atomic absorption spectrophotometer is measured includes：
(1) determining instrument：Atomic absorption spectrophotometer;Determine the instrument condition of copper：Wavelength 324.8nm, slit 0.5nm, lamp current 3.0mA, acetylene flow 2.0L/min, air mass flow 10L/min;Determine the instrument condition of cadmium element：Wavelength 228.8nm, slit 0.5nm, lamp current 4.0mA, acetylene flow 2.0L/min, air mass flow 11.0L/min;Determine lead element Instrument condition：Wavelength 283.3nm, slit 0.5nm, lamp current 5.0mA, acetylene flow 2.0L/min, air mass flow 10.0L/ min;The wash-out solution of test sample or hybrid standard sample is treated using Flame Atomic Absorption Spectrometry Determination；
(2) drafting of standard working curve：In 0.5 ~ 4.0 μ g/mL concentration ranges, Cu in absorbance and hybrid standard sample2+It is dense Degree is in good linear relationship：Abs=0.13820*C+0.01048, C are concentration, and its unit is μ g/mL, linearly dependent coefficient r= 0.9996；In 0.05 ~ 0.5 μ g/mL concentration ranges, Cd in absorbance and hybrid standard sample2+Concentration is in good linear relationship： Abs=0.31387*C+0.00263, C are concentration, and its unit is μ g/mL, linearly dependent coefficient r=0.9998, in 0.5 ~ 4.0 μ g/ In mL concentration ranges, Pb in absorbance and hybrid standard sample2+Concentration is in good linear relationship：Abs=0.02833*C+ 0.00166, C is concentration, and its unit is μ g/mL, linearly dependent coefficient r=0.9999；
(3) Cu in test sample is treated2+、Cd2+And Pb2+The measure of content：Absorbance A bs is obtained by flame atomic absorption spectrophotometer；Most Cu in sample solution is calculated according to standard working curve afterwards2+、Cd2+And Pb2+Concentration.
CN201611083050.6A 2016-11-30 2016-11-30 Copper, cadmium in a kind of detection tea oil, the method for lead Pending CN106769926A (en)

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