CN105136542A - Method for measuring lead and cadmium in water by using chitosan enrichment - Google Patents
Method for measuring lead and cadmium in water by using chitosan enrichment Download PDFInfo
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Abstract
The invention discloses a method for measuring lead and cadmium in water by using chitosan enrichment, characterized by performing micro-column separation and enrichment on the lead and the cadmium by taking chitosan as an adsorbent and building a flame atomic absorption spectrometry detection method. In a concentration range of 1 to 25 mu. G/mL, absorbancy and the concentration of lead ions in sample liquid are in good linear relation: A=0.023C+0.013, wherein C represents concentration with the unit of mu. G/mL, and a linear correlation coefficient is that R2=0.9951; in a concentration range of 1 to 6 mu. G/mL, the absorbancy and the concentration of cadmium ions in the sample liquid are in good linear relation: A=0.11C+0.152, wherein C represents concentration with the unit of mu. G/mL, and a linear correlation coefficient is that R2=0.9995. The method improves detection sensitivity and selectivity, and automatic detection on the low-concentration lead and cadmium ions is easy.
Description
Technical field
The invention belongs to water body detection technique field, be specifically related to a kind of method utilizing lead, cadmium in shitosan gathering and measuring water.
Background technology
Along with the steady lifting of contemporary people's living standard and quality, the hypergrowth of scientific and technological level, people rise to the demand of various resource, and the utilization factor of natural resources also progressively rises.The heavy metal pollution in wastewater of industrial discharge is also got over serious, and a large amount of heavy metals enters our ecological circulation from waste water, and heavy metal not only directly can enter air, water body and soil, causes direct environmental pollution.Mutually can also move between three, cause each environmental element indirectly to pollute.After a large amount of lead ion enters human body, can by the immune system of human body self except the lead ion of minute quantity, by outside various discharge regime excretion, remaining major part lead dissolves in blood at short notice, hinders the synthesis of blood.Frequent headache, intestine gastric ulcer, weakness of limbs, sleepy, constipation and myalgia, the symptom such as artery sclerosis, intestine gastric ulcer also causes because lead ion pollutes.Cadmium is a kind of transitional heavy metal of atypia with metallic luster, is arranged in periodic table of elements period 5 II B-group.Cadmium element is that a kind of bioconcentration is strong, toxicity is lasting, have the hypertoxic element that " three cause " act on.Cadmium, by being combined or substitution effect with enzyme sulfydryl, displaces desmoenzyme type systematic, reduces the activity of body antioxidase, the ability of body scavenging free radicals is declined, causes oxidative damage; Cadmium can occupy calcium channel and enter in cell, makes intracellular calcium homeostasis unbalance, also can be combined in the outer zinc site of antigenic determinant born of the same parents before entering cell on the orphan receptor of cell surface, interference cell metabolism; The formation of cadmium energy inducing metal sulfoprotein, metallothionein take part in the absorption of cadmium in body, transhipment, excretion and accumulation; Cadmium can cause DNA single bond rupture, and damages DNA repair system, causes cell death.
Shitosan (chitasan, CTS) is chitin deacetylase based products, by aquatic products processing accessory substance---the preparations such as shrimp shell, crab shell.Research shows, the amino in CTS is the optimum activity site be combined with metallic ion, has stable coordination to metallic ion, and acetyl group increase the maximum binding capacity that can reduce CTS heavy metal.Meanwhile, because shitosan has biodegrability, biocompatibility, biologically active and unique performance such as nontoxic, Chitosan-phospholipid complex has obtained paying much attention to and extensively research in water treatment field in recent years.Application in environmental protection, shitosan can make the flocculating agent of water treatment.As the process of food industrial wastewater, purified tap water, drink the process of water purification, heavy metal wastewater thereby.Study for a long time according to scientist, chitosan molecule chain is a mass of a large amount of free oh groups and amino group, and shitosan in some dilute acid solns, its amino is easily protonated (such as dust technology), thus making shitosan proton turn to the polyelectrolyte of positively charged solubility, we can judge that shitosan has the effect of cationic flocculant.Therefore shitosan is the desirable flocculating agent purified waste water in waterworks, and it not only effectively except the suspension in anhydrating and particle, can also remove the organism that some are harmful.
Along with growth in the living standard, heavy metal ion discharge capacity in industrial waste water also change is all the more many, the heavy metal ion of the absorption of people is hard to guard against, various places heavy metal ion poisoning also change is all the more many, and thus everybody day by day pays close attention in food and the content of heavy metal ion in each large water source.Applicant determines the optimal extract process of the trace elements such as cadmium in shitosan enrichment-aas determination water is plumbous, for monitoring water quality provides technical support.
Summary of the invention
The invention reside in the flame atomic absorption spectrometry method that a kind of high selectivity separation and concentration-mensuration water sample medium trace element is provided.
The present invention realizes especially by following technical scheme:
Utilize a method that is plumbous in shitosan gathering and measuring water, cadmium, completed by following steps:
1) chitosan for separating and enriching lead, cadmium ion
Taking shitosan to add in post to 2/3rds places, adds lead or cadmium solution collects efflux, gets supernatant, load constant volume in volumetric flask after centrifugal; Xiang Zhuzhong adds parsing agent wash-out by the ion adsorbed, and supernatant got by centrifugal eluent, takes 1mL and adds constant volume in the volumetric flask of 10mL, and elute soln is used for follow-up Atomic Absorption Spectrometry;
2) detection method
Determining instrument: atomic absorption spectrophotometer (AAS); 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 lead, the concentration of cadmium ions in Flame Atomic Absorption Spectrometry Determination step (1) gained eluent;
3) drafting of standard working curve
The plumbous standard solution of 10.0mL or cadmium standard solution are carried out separation and concentration and Atomic Absorption Spectrometry according to step (1) and step (2); In 1-25 μ g/mL concentration range, in absorbance and sample liquid, plumbum ion concentration is good linear relationship: A=0.023C+0.013, C are concentration, and its unit is μ g/mL, linearly dependent coefficient R
2=0.9951; In 1-6 μ g/mL concentration range, in absorbance and sample liquid, concentration of cadmium ions is good linear relationship: A=0.11C+0.152, C are concentration, and its unit is μ g/mL, linearly dependent coefficient R
2=0.9995;
4) mensuration that is plumbous in test sample, cadmium content is treated
Lead ion sample solution or cadmium ion sample solution are carried out separation and concentration and Atomic Absorption Spectrometry according to step (1) and step (2), obtains absorbance A; Finally calculate plumbous in sample solution or concentration of cadmium ions according to calibration curve.
Further, the adsorption conditions in step (1) is described lead or cadmium solution pH value is 5, and temperature is 25 DEG C.
Further, in step (1), adsorption time is: lead ion solution 4h, cadmium-ion solution 6h.
Further, described parsing agent is the H of 1mol/L
2sO
4solution.
Further, described elution requirement is: shitosan is 1.2:20g/ml with the mass volume ratio of parsing agent, and elution time is 30min.
Beneficial effect of the present invention is: 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, detection that is plumbous for super low concentration, cadmium is easy to robotization.
Accompanying drawing explanation
Fig. 1 is the relation of Absorption of Heavy Metal ion with Chitosan lead and pH;
Fig. 2 is the relation of Absorption of Heavy Metal ion with Chitosan cadmium and pH;
Fig. 3 is the time that shitosan adsorpting lead ion arrives saturated extent of adsorption;
Fig. 4 is the time that shitosan Adsorption of Cadmium arrives saturated extent of adsorption;
Fig. 5 is the relation of Absorption of Heavy Metal ion with Chitosan lead and temperature;
Fig. 6 is the relation of Absorption of Heavy Metal ion with Chitosan cadmium and temperature;
Fig. 7 is that different parsing agent is on the impact of wash-out heavy metal ion lead;
Fig. 8 is that different parsing agent is on the impact of wash-out heavy metal ion cadmium;
Fig. 9 is that different agent consumption of resolving is to the effect of resolving heavy metal ion lead;
Figure 10 is that different agent consumption of resolving is to the effect of resolving heavy metal ion cadmium;
Figure 11 is the impact of parsing time on wash-out heavy metal ion lead;
Figure 12 is the impact of parsing time on wash-out heavy metal ion cadmium.
Embodiment
Below in conjunction with embodiment, the present invention is described further, the following stated, only to preferred embodiment of the present invention, not do other forms of restriction to the present invention, any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed to the Equivalent embodiments of equal change.Everyly do not depart from the present invention program's content, any simple modification done following examples according to technical spirit of the present invention or equivalent variations, all drop in protection scope of the present invention.
The present invention determines the optimal extract process of the trace elements such as cadmium in shitosan enrichment-aas determination water is plumbous by single-factor variable, orthogonal test, the technological process of the enrichment Adsorption of Heavy Metal Ions of shitosan is optimized, completes especially by following process.
1. the preparation of typical curve
Get the volumetric flask of 10 10mL, by label paper number consecutively 1,2,3,4,5,6,7,8,9,10,11,12.In 1 to No. 6 volumetric flasks, add the lead mark liquid of 1,5,10,15,20,25mL0.1 μ g/mL with transfer pipet successively, be then settled to scale with the salpeter solution of 0.5%, shake up.In 7 to No. 12 volumetric flasks, add the cadmium mark liquid of 1,2,3,4,5,6mL1 μ g/mL successively, be then settled to scale with the salpeter solution of 0.5%, shake up.Detect absorbance that is plumbous and cadmium respectively with Flame Atomic Absorption Spectrometry spectroscopic, testing result is as shown in table 1.
table 1 typical curve
Linear regression is tried to achieve typical curve that is plumbous and cadmium and is respectively
A=0.023C
1+0.013；
A=0.11C
2+0.152。
In formula, A-represents absorbance;
C
1-represent lead concentration, μ g/mL;
C
2-represent cadmium concentration, μ g/mL.
Show that the related coefficient of typical curve is respectively R by equation of linear regression
1 2=0.9951, R
2 2=0.9995.
2. the lead ion in shitosan enrichment planar water
Take shitosan → add in post and (be at least added to 2/3rds of post) → add plumbous storing solution → efflux centrifuging and taking supernatant → take 1mL to add in the volumetric flask of 10mL → dilute sulfuric acid wash-out → centrifugal eluent that constant volume → Xiang Zhuzhong adds 1mol/L gets supernatant → take 1mL and to add in the volumetric flask of 10mL → constant volume.
3. the cadmium ion in shitosan enrichment planar water
Take shitosan → add in post and (be at least added to 2/3rds of post) → add cadmium storing solution → efflux centrifuging and taking supernatant → take 1mL to add in the volumetric flask of 10mL → dilute sulfuric acid wash-out → centrifugal eluent that constant volume → Xiang Zhuzhong adds 1mol/L gets supernatant → take 1mL and to add in the volumetric flask of 10mL → constant volume.
4. detection method
Determining instrument: atomic absorption spectrophotometer (AAS); 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 lead in Flame Atomic Absorption Spectrometry Determination eluent, concentration of cadmium ions.
the impact of embodiment 1pH value team shitosan absorption
The beaker that 6 100mL put into by 6 parts of 1.2g shitosans is taken with electronic balance, the plumbous standard reserving solution accurately measuring the 1g/L of 6 parts of 1mL adds in the beaker of 100mL respectively, add 59mL ultrapure water again and be diluted to 60mL, regulate pH to 2,3,4,5,6,7 respectively with the watery hydrochloric acid of 1mol/L and the sodium hydroxide solution of 1mol/L.Put into difunctional digital display constant temperature oscillator and shake 4h, number centrifugal for 10mL solution numbers that takes out each from 6 beakers, the 1mL got in supernatant is settled in the volumetric flask of 10mL, and result is as Fig. 1,2 and table 2,3.
the relation of table 2 Absorption of Heavy Metal ion with Chitosan lead and pH
| pH | Adsorption rate (%) |
| 2 | 13.9 |
| 3 | 47.8 |
| 4 | 84.3 |
| 5 | 97.4 |
| 6 | 71.3 |
| 7 | 45.2 |
the relation of table 3 Absorption of Heavy Metal ion with Chitosan cadmium and pH
Can be found out by Fig. 1,2, along with pH raises, shitosan heavy metal is plumbous, and the adsorption rate of heavy metal cadmium raises, and after waiting until that pH is more than 5, shitosan adsorption rate starts again to reduce gradually.Therefore solution acid alkalinity is when being pH=5, shitosan heavy metal ion adsorption rate that is plumbous and heavy metal ion cadmium is maximum.
the impact that embodiment 2 time adsorbs shitosan
Take 30mL(1g/L respectively) plumbous standard reserving solution and cadmium standard reserving solution, be placed in the conical flask filling 0.3g shitosan, regulate pH=5 with watery hydrochloric acid and dilute sulfuric acid, be placed on oscillator and vibrate, every 1h sample thief once, getting 1mL at every turn and diluting is settled in 50mL volumetric flask, get 10 times altogether, get 1mL and dilution is settled in 50mL volumetric flask at every turn, measure the content of each ion in filtrate, calculate saturated extent of adsorption, result is as Fig. 3,4 and table 4,5.
table 4 Absorption of Heavy Metal ion with Chitosan lead and the relation of time
| Time (h) | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Adsorbance (mg) | 5.980 | 7.965 | 10.337 | 11.065 | 11.087 | 11.061 | 11.050 | 11.061 | 11.054 | 11.043 |
the relation of table 5 Absorption of Heavy Metal ion with Chitosan cadmium and time
| Time (h) | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Adsorbance (mg) | 12.85 | 16.454 | 18.313 | 19.478 | 21.099 | 21.193 | 20.933 | 21.437 | 20.996 | 21.043 |
Can be found out by Fig. 3,4, elongated along with adsorption time, the adsorbance of shitosan is saturated gradually, when adsorption time arrives 4h, lead ion reaches capacity, when adsorption time arrives 6h, cadmium ion reaches capacity, after along with the slowly propelling of time, absorption that is plumbous due to shitosan heavy metal ion, cadmium arrives saturated, and therefore adsorbance remains unchanged.Still to think that Absorption of Heavy Metal ion with Chitosan lead arrives time of saturated extent of adsorption be 4h, the time that Absorption of Heavy Metal ion with Chitosan cadmium arrives saturated extent of adsorption is 6h.
the impact that embodiment 3 temperature is adsorbed shitosan
With 1.2g shitosan dress post, measure 7 parts of cadmium solutions and each 1mL of lead solution 1g/L, be then diluted to 60mL, be placed in a series of conical flask respectively, regulate pH=5.0 with watery hydrochloric acid and dilute sulfuric acid, then regulate temperature to be 25,30,35,40,45,50,55,60 degrees Celsius.Take out 1mL and be settled in 10mL volumetric flask, with the content of each ion of flame atomic absorption spectrometry.Result is as figure, and result is as Fig. 5,6 and table 6,7.
the relation of table 6 Absorption of Heavy Metal ion with Chitosan lead and temperature
| Temperature | Adsorption rate (%) |
| 25 | 100.0 |
| 30 | 94.8 |
| 35 | 87.0 |
| 40 | 71.3 |
| 45 | 63.5 |
| 50 | 47.8 |
| 55 | 16.5 |
| 60 | 0.8 |
the relation of table 7 Absorption of Heavy Metal ion with Chitosan cadmium and temperature
| Temperature | Adsorption rate (%) |
| 25 | 103.1 |
| 30 | 97.1 |
| 35 | 94.4 |
| 40 | 81.8 |
| 45 | 79.1 |
| 50 | 56.7 |
| 55 | 46.9 |
| 60 | 33.3 |
Can be found out by Fig. 5,6, along with the rising of temperature, the adsorption rate of shitosan reduces gradually, and after temperature is more than 55 degrees Celsius, the adsorbance of shitosan is close to 0.Therefore we can show that adsorption process is a kind of exothermic process, and under normal temperature, the n in isothermal adsorption formula meets Q=KC close to 1, and the effective group of chitosan molecule of particle surface increases.
embodiment 4 shitosan analysis condition
1) with 1.2g shitosan dress post, measure 3 parts of cadmium solutions and each 1mL of lead solution 1g/L, be diluted to 60mL, be placed in a series of conical flask respectively, regulate pH=5.0, under the normal temperature of 25 degree with watery hydrochloric acid and dilute sulfuric acid.Use the 1mol/L dilute sulfuric acid of 20mL, the 1mol/L watery hydrochloric acid with 20ml, the 1mol/L dust technology with 20ml as eluant, eluent respectively, with the flow velocity wash-out of 1mL/min, eluent is settled in 10mL volumetric flask, with the content of each ion of flame atomic absorption spectrometry, result is as Fig. 7,8 and table 8,9.
the plumbous relation with resolving agent of heavy metal ion resolved by table 8 shitosan
| Resolve agent | Resolution factor (%) |
| Dust technology | 12.2 |
| Watery hydrochloric acid | 64.3 |
| Dilute sulfuric acid | 100.9 |
table 9 shitosan resolves heavy metal ion cadmium and the relation of resolving agent
| Resolve agent | Resolution factor (%) |
| Dust technology | 0.8 |
| Watery hydrochloric acid | 61.3 |
| Dilute sulfuric acid | 98.4 |
Can be found out by Fig. 7,8, dilute sulfuric acid as elute effect the best in these three eluant, eluents, under above-mentioned top condition, selects 1mol/LH respectively
2sO
4, HCl, HNO
3as eluant, eluent, result shows, 1mol/LHCl, HNO
3shitosan all can be made to become thickness because of protonated, experimental selection 1mol/LH
2sO
4as eluant, eluent.
2) consumption of agent is resolved
With 1.2g shitosan dress post, measure 3 parts of cadmium solutions and each 1ml of lead solution 1g/L, be diluted to 60ml, be placed in a series of conical flask respectively, regulate pH=5.0, under the normal temperature of 25 degree with watery hydrochloric acid and dilute sulfuric acid.Use the 1mol/L dilute sulfuric acid of 10ml, the 1mol/L dilute sulfuric acid with 20mL, the 1mol/L dilute sulfuric acid with 30mL as eluant, eluent respectively, with the flow velocity wash-out of 1mL/min, eluent is settled in 10mL volumetric flask, with the content of each ion of flame atomic absorption spectrometry, result is as Fig. 9,10 and table 10,11.
table 10 resolves the consumption of agent to the relation of wash-out heavy metal ion lead
| Resolve the consumption (mL) of agent | Resolution factor (%) |
| 10 | 56.1 |
| 20 | 99.1 |
| 30 | 99.1 |
table 11 resolves the consumption of agent to the relation of wash-out heavy metal ion cadmium
| Resolve the consumption of agent | Resolution factor (%) |
| 10 | 66.7 |
| 20 | 99.2 |
| 30 | 99.1 |
Can be found out by Fig. 9,10, along with the rising of resolving agent consumption, the amount of resolving heavy metal ion from the shitosan adsorbing heavy metal also raises gradually, and in time using 20mL to resolve agent parsing, the lead ion quality parsed is close to the heavy metal ion total amount equaled by adsorbing.In time using 30mL to resolve agent parsing, resolution factor is compared with slightly decline before (because error becomes greatly after dilution).This consumption showing to resolve agent is best analysis condition when 20mL.
3) selection of time is resolved
With 1.2g shitosan dress post, measure 3 parts of cadmium solutions and each 1mL of lead solution 1g/L, be diluted to 60mL, be placed in a series of conical flask respectively, regulate pH=5.0, under the normal temperature of 25 degree with watery hydrochloric acid and dilute sulfuric acid.With the dilute sulfuric acid of the 1mol/L of 20mL as eluant, eluent, with the flow velocity of 1mL/min wash-out 10min, 20min, 30min respectively, be settled to by eluent in 10mL volumetric flask, with the content of each ion of flame atomic absorption spectrometry, result is as Figure 11,12 and table 12,13.
the relation of time to wash-out heavy metal ion lead resolved by table 12
| The time (min) of resolving | Resolution factor (%) |
| 10 | 61.7 |
| 20 | 89.6 |
| 30 | 97.4 |
the relation of time to wash-out heavy metal ion cadmium resolved by table 13
| The time (min) of resolving | Resolution factor (%) |
| 10 | 49.3 |
| 20 | 96.2 |
| 30 | 99.9 |
Can be found out by Figure 11,12, along with the increase of the time of parsing, resolution factor increases gradually, and when the parsing time is 20 minutes, resolution factor peaks substantially, when the parsing time is 30 minutes, resolution factor peaks, and now resolution factor is 99%, after along with the increase of time, owing to almost being resolved by the heavy metal ion of adsorbing completely, therefore resolution factor was best analysis condition 30 minutes time.
the orthogonal experiment of embodiment 5 shitosan
The consumption of 4 single factor test, temperature, pH value, parsing time, parsing agent is chosen from the above variable of shitosan.With 1.2g shitosan dress post, measure 3 parts of cadmium solutions and each 1mL of lead solution 1g/L, be diluted to 60mL, be placed in a series of conical flask respectively, regulate pH with watery hydrochloric acid and dilute sulfuric acid, at different temperature, with the parsing agent of difference amount as eluant, eluent, with the flow velocity of 1mL/min wash-out different time respectively, take out 1mL eluent and be also settled in 10mL volumetric flask, with the content of each ion of flame atomic absorption spectrometry, result is as table 14.
table 14 factor level table
| Level | A environment temperature (DEG C) | B resolves agent consumption (mL) | C solution pH value | The time (min) that D resolves |
| 1 | 20 | 10 | 4 | 20 |
| 2 | 25 | 20 | 5 | 30 |
| 3 | 30 | 30 | 6 | 40 |
the orthogonal test of table 15 shitosan heavy metal ion lead
table 16 factor level table
| Level | A environment temperature (DEG C) | B resolves the consumption (mL) of agent | C solution pH value | The time (min) that D resolves |
| 1 | 20 | 10 | 4 | 20 |
| 2 | 25 | 20 | 5 | 30 |
| 3 | 30 | 30 | 6 | 40 |
the orthogonal test of table 17 shitosan heavy metal ion cadmium
Can be found out by table 16 and table 17, selected temperature be 25 degrees Celsius, solution ph is 5, resolve agent consumption is 20mL and under the parsing time is the condition of 30min, the resolution factor of the heavy metal ion lead of shitosan absorption is close to and reaches absolutely.Can be found out by table 16 and table 17, selected temperature be 25 degrees Celsius, solution ph is 5, resolve agent consumption is 20mL and under the parsing time is the condition of 20min, the resolution factor of the heavy metal ion lead of shitosan absorption is close to and reaches absolutely.So we can regard as the optimum experimental condition that these conditions are the trace element such as cadmium, lead in shitosan enrichment-aas determination water.
In sum:
1. the absorption of shitosan
At room temperature (25 DEG C), under the condition that pH value of solution is different, have studied the adsorption rate of Absorption of Heavy Metal ion with Chitosan lead, cadmium, solution acid alkalinity, on the impact of shitosan absorption affinity, determines Absorption of Heavy Metal ion with Chitosan lead according to single factor experiment, the potential of hydrogen condition of cadmium is that pH equals 5.
At room temperature (25 DEG C), under pH equals the condition of 5, have studied Absorption of Heavy Metal ion with Chitosan to reach capacity time of adsorbance, the time determining the plumbous adsorbance that reaches capacity of Absorption of Heavy Metal ion with Chitosan according to experiment of single factor is 4h, and the time that Absorption of Heavy Metal ion with Chitosan cadmium arrives saturated extent of adsorption is 6h.
Equal the condition of 5 at pH under, adsorb in constant temperature oven, adsorption time is above-mentioned Best Times, under different thermogrades, have studied shitosan optimal adsorption temperature conditions at different temperatures.The optimal adsorption temperature that investigated Absorption of Heavy Metal ion with Chitosan according to experiment of single factor is 25 DEG C
2. the parsing of shitosan
Be 20mL at parsing agent consumption, the parsing time is under the condition of 30min.The best eluant, eluent determining shitosan parsing according to experiment of single factor is dilute sulfuric acid, and watery hydrochloric acid can make shitosan dissolve, and dust technology can make shitosan protonated and impact parsing, therefore determines that dilute sulfuric acid is best eluant, eluent.
The identical parsing agent (dilute sulfuric acid) of use, the parsing time is under the condition of 30min, and determining the best parsing agent consumption of resolving agent parsing shitosan according to experiment of single factor is 20mL.
The identical parsing agent (dilute sulfuric acid) of use, the consumption of resolving agent is under the condition of 20mL, and determining the best parsing time of resolving agent parsing shitosan according to experiment of single factor is 30mL.
3. determining room temperature (25 DEG C), solution ph is 5, resolve under agent uses dilute sulfuric acid, resolves condition that the consumption of agent is 20mL.The resolution factor of shitosan under above-mentioned top condition is determined up to more than percent 95 by orthogonal test.
Claims (5)
1. utilize a method that is plumbous in shitosan gathering and measuring water, cadmium, it is characterized in that, comprise the following steps:
1) chitosan for separating and enriching lead, cadmium ion
Taking shitosan to add in post to 2/3rds places, adds lead or cadmium solution collects efflux, gets supernatant, load constant volume in volumetric flask after centrifugal; Xiang Zhuzhong adds parsing agent wash-out by the ion adsorbed, and supernatant got by centrifugal eluent, takes 1mL and adds constant volume in the volumetric flask of 10mL, and elute soln is used for follow-up Atomic Absorption Spectrometry;
2) detection method
Determining instrument: atomic absorption spectrophotometer (AAS); 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 lead, the concentration of cadmium ions in Flame Atomic Absorption Spectrometry Determination step (1) gained eluent;
3) drafting of standard working curve
The plumbous standard solution of 10.0mL or cadmium standard solution are carried out separation and concentration and Atomic Absorption Spectrometry according to step (1) and step (2); In 1-25 μ g/mL concentration range, in absorbance and sample liquid, plumbum ion concentration is good linear relationship: A=0.023C+0.013, C are concentration, and its unit is μ g/mL, linearly dependent coefficient R
2=0.9951; In 1-6 μ g/mL concentration range, in absorbance and sample liquid, concentration of cadmium ions is good linear relationship: A=0.11C+0.152, C are concentration, and its unit is μ g/mL, linearly dependent coefficient R
2=0.9995;
4) mensuration that is plumbous in test sample, cadmium content is treated
Lead ion sample solution or cadmium ion sample solution are carried out separation and concentration and Atomic Absorption Spectrometry according to step (1) and step (2), obtains absorbance A; Finally calculate plumbous in sample solution or concentration of cadmium ions according to calibration curve.
2. a kind of method utilizing lead, cadmium in shitosan gathering and measuring water according to claim 1, it is characterized in that, the adsorption conditions in step (1) is described lead or cadmium solution pH value is 5, and temperature is 25 DEG C.
3. a kind of method utilizing lead, cadmium in shitosan gathering and measuring water according to claim 1, it is characterized in that, in step (1), adsorption time is: lead ion solution 4h, cadmium-ion solution 6h.
4. a kind of method utilizing lead, cadmium in shitosan gathering and measuring water according to claim 1, it is characterized in that, described parsing agent is the H of 1mol/L
2sO
4solution.
5. a kind of method utilizing lead, cadmium in shitosan gathering and measuring water according to claim 1, it is characterized in that, described elution requirement is: shitosan is 1.2:20g/ml with the mass volume ratio of parsing agent, and elution time is 30min.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN114699802A (en) * | 2022-04-27 | 2022-07-05 | 华中科技大学 | Method for desorbing, enriching and recovering Cd/Pb step by step |
| CN114699802B (en) * | 2022-04-27 | 2022-11-22 | 华中科技大学 | Method for desorbing, enriching and recovering Cd/Pb step by step |
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