CN103884795B - The chromatography of ions concurrently separates the method for zwitterion in salt lake bittern that measures - Google Patents
The chromatography of ions concurrently separates the method for zwitterion in salt lake bittern that measures Download PDFInfo
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Abstract
The invention discloses a kind of chromatography of ions and concurrently separate the method for zwitterion in salt lake bittern that measures, it comprises the steps: through 0.45 μm membrane filtration, the sample of salt lake bittern is obtained liquid to be measured, and dilutes 1000 times；Choose list mark solution C l of 1000 μ g/L respectively‑2mL、Br‑1mL、CO3 2‑1mL、SO4 2‑1mL、I‑1mL is mixed to get anion standard liquid in 250mL volumetric flask；The list mark solution Li of selection standard solution 1000 μ g/L respectively+0.5mL、Na+1mL、K+1mL、Rb+0.1mL、Mg2+2mL is mixed to get cation standard liquid in 250mL volumetric flask；Detect liquid to be measured and anions and canons standard liquid by the chromatography of ions respectively, record chromatogram, carry Software Integration through chromatographic apparatus and obtain peak area, calculate and respectively obtain the content of each zwitterion in liquid to be measured.Compared with prior art, the present invention can be to the Cl in salt lake bittern‑、Br‑、CO3 2‑、SO4 2‑、I‑、Li+、Na+、K+、Rb+、Mg2+Carry out concurrently separating mensuration, and measure simple and quick, and there is higher accuracy of measurement.
Description
Technical field
The present invention relates to a kind of assay method in chemical field, particularly a kind of chromatography of ions concurrently separates mensuration salt
The method of zwitterion in lake bittern water.
Background technology
Salt lake bittern aboundresources, is broadly divided into chloride type, sulfate type and carbonate-type both at home and abroad.The most
Famous chloride type salt lake is to be positioned at Israel, Jordan and the Dead Sea of Palestine's intersection and Qinghai Province of China Cha Er Han salt
Lake, the Sears lake of the U.S. and Great Salt lake are typical carbonate-type and sulfate type salt lake respectively.In salt lake bittern rich in potassium,
The Multifarious minerals resources such as sodium, magnesium, lithium, boron, bromine, along with people are increasing to the demand of resource and constantly the carrying of scientific and technological level
Height, the exploitation of salt lake resources are increasingly subject to the concern in the world.
Abroad having more than 100 year for Comprehensive Utilization of Bittern Resources history, one or both is simply provided by its initial stage of development
The exploitation in source, recently as scientific and technological progress and combine salt lake multicomponent system phasor analysis synchronize achieve potassium, sodium, magnesium,
The comprehensive development and utilization of the salt lake resources such as boron, lithium and bromine, achieves Circular Economy production model substantially.Wherein Cha Er Han Salt Lake
Being divided into Bie Letan, Da Buxun, Cha Er Han and 4 lake regions of Huo Buxun from West to East, the gross area is about 5856Km2, it is Largest In China
Salt lake, be also one of the most foremost inland brine lake.It has the salt ore resources that Qinghai is maximum, and total resources is 600
Many hundred million tons.Cha Er Han Salt Lake is owing to being affected by High aititude geographical position and plateau climate, and then forms the multiple of uniqueness
The phenomenon that anions and canons coexists, its cationic mainly includes K+、Na+、Mg2+、B3+、Li+、Rb+、Cs+Deng, anion includes
Cl-、SO4 2-、CO3 2-、Br-、I-Deng several, be wherein mainly based on sylvite, and simultaneously with the multiple ore deposit such as sodium, magnesium, lithium, boron, iodine
Produce the comprehensive salt lake, large-scale inland that resource coexists.It is confined to single ionic mensuration owing to measuring for bittern intermediate ion at present,
Thus separation determination is a problem demanding prompt solution while these ions, in order to carry for the exploitation of Cha Er Han Salt Lake Brine resources
For gross data support, promote the comprehensive utilization of salt lake salt ore resources.
Summary of the invention
The invention aims to provide a kind of chromatography of ions to concurrently separate and measure the side of zwitterion in salt lake bittern
Method.
For reaching above-mentioned purpose, the present invention implements according to techniques below scheme:
A kind of chromatography of ions concurrently separates the method for zwitterion in salt lake bittern that measures, and it comprises the steps:
1) sample of salt lake bittern is obtained liquid to be measured through 0.45 μm membrane filtration, and dilute 1000 times, standby；
2) list mark solution C l of 1000 μ g/L is chosen respectively-2mL、Br-1mL、CO3 2-1mL、SO4 2-1mL、I-1mL is in 250mL
Being mixed to get anion standard liquid in volumetric flask, the most each ion concentration is respectively as follows: Cl-(8mg/l)、Br-(4mg/l)、CO3 2-
(4mg/l)、SO4 2-(4mg/l)、I-(4mg/l), standby；
3) the list mark solution Li of 1000 μ g/L is chosen respectively+0.5mL、Na+1mL、K+1mL、Rb+0.1mL、Mg2+2mL in
Being mixed to get cation standard liquid in 250mL volumetric flask, the most each ion concentration is respectively as follows: Li+(2mg/l)、Na+(4mg/
l)、K+(4mg/l)、Rb+(0.4mg/l)、Mg2+(8mg/l), standby；
4) detect liquid to be measured and anion standard liquid respectively by the chromatography of ions, record chromatogram, through chromatographic apparatus
Carry Software Integration and obtain peak area, calculate and respectively obtain Cl in liquid to be measured-、Br-、CO3 2-、SO4 2-、I-Content, this chromatostrip
Part is as follows:
Use the ion chromatograph of DIONEX company ICS-1100Ion Chromatography System, use chromatogram
Post: anion-exchange column is DIONEX company, analytical column: Ionpac AS194 × 250mm, guard column: AG194 × 50mm, presses down
Device processed is DIONEX company ASRS 3004mm, and injection annulus is 25 μ L, experimental water resistivity: 18.25M Ω cm；
The KOH solution of flowing phase: 15mM-25mM；
Flow velocity: 0.8ml/min-1.2ml/min；
Column temperature: 32 DEG C；
As preferably, the concentration of described KOH solution is 22mM, and flow velocity is 1.0ml/min.
5) detect liquid to be measured and cation standard liquid respectively by the chromatography of ions, record chromatogram, through chromatographic apparatus
Carry Software Integration and obtain peak area, calculate and respectively obtain Li in liquid to be measured+、Na+、K+、Rb+、Mg2+Content, this chromatographic condition
As follows:
Use the ion chromatograph of DIONEX company ICS-90Ion Chromatography System.Employing chromatographic column:
Cation exchange column is DIONEX company, analytical column: Ionpac CS12A 4 × 250mm, and guard column: CG12A 4 × 50mm presses down
Device processed is DIONEX company CSRS 3004mm, and injection annulus is 25 μ L, experimental water resistivity: 18.25M Ω cm；
The MSA solution of flowing phase: 18mM-25mM；
Flow velocity: 0.8ml/min-1.0ml/min；
Column temperature: 32 DEG C；
Being 20mM as preferably selecting MSA concentration, flow velocity is 1.0ml/min
Compared with prior art, beneficial effects of the present invention: can be to the Cl in salt lake bittern-、Br-、CO3 2-、SO4 2-、
I-、Li+、Na+、K+、Rb+、Mg2+Carry out concurrently separating mensuration, and measure simple and quick, and there is higher mensuration
The degree of accuracy.
Accompanying drawing explanation
Fig. 1 is embodiment anion standard liquid standard colour chart spectrogram in the present invention；
Fig. 2 is the chromatogram of anion in embodiment liquid to be measured in the present invention；
Fig. 3 is embodiment cation standard liquid standard colour chart spectrogram in the present invention；
The chromatogram of embodiment liquid to be measured cation in Fig. 4 present invention；
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described, the illustrative examples invented at this and explanation
It is used for explaining the present invention, but not as a limitation of the invention.
In the present invention, each standard items are all purchased from Chinese Industrial Standards (CIS) material product, are national standard sample, Li+,Na+,K+,Rb+,
Mg2+, standard liquid: 1000ug/ml, country's non-ferrous metal and electronic material Institute of Analysis；
Each standard items are all purchased from Chinese Industrial Standards (CIS) material product, are national standard sample.Cl-,Br-,SO4 2-,I-Standard liquid:
1000ug/ml, country's non-ferrous metal and electronic material Institute of Analysis；Natrium carbonicum calcinatum: China National Measuring Science Research Inst..
A kind of chromatography of ions concurrently separates the method for zwitterion in salt lake bittern that measures, and it comprises the steps:
1) sample of salt lake bittern is obtained liquid to be measured through 0.45 μm membrane filtration, and dilute 1000 times, standby；
2) 1000 μ g/L Cl are chosen respectively-2mL、Br-1mL、CO3 2-1mL、SO4 2-1mL、I-1mL is in 250mL volumetric flask
Being mixed to get anion standard liquid, the most each ion concentration is respectively as follows: Cl-(8mg/l)、Br-(4mg/l)、CO3 2-(4mg/l)、
SO4 2-(4mg/l)、I-(4mg/l), standby；
3) the list mark solution Li of 1000 μ g/L is chosen respectively+0.5mL、Na+1mL、K+1mL、Rb+0.1mL、Mg2+2mL in
Being mixed to get cation standard liquid in 250mL volumetric flask, the most each ion concentration is respectively as follows: Li+(2mg/l)、Na+(4mg/
l)、K+(4mg/l)、Rb+(0.4mg/l)、Mg2+(8mg/l), standby；
4) detect liquid to be measured and anion standard liquid respectively by the chromatography of ions, record chromatogram, through chromatographic apparatus
Carry Software Integration and obtain peak area, calculate and respectively obtain Cl in liquid to be measured-、Br-、CO3 2-、SO4 2-、I-Content, this chromatostrip
Part is as follows:
Use the ion chromatograph of DIONEX company ICS-1100Ion Chromatography System, use chromatogram
Post: anion-exchange column is DIONEX company, analytical column: Ionpac AS194 × 250mm, guard column: AG194 × 50mm, presses down
Device processed is DIONEX company ASRS 3004mm, and injection annulus is 25 μ L, experimental water resistivity: 18.25M Ω cm；
The KOH solution of flowing phase: 22mM；
Flow velocity: 1.0ml/min；
Column temperature: 32 DEG C；
Now, Cl in liquid to be measured is obtained-、Br-、CO3 2-、SO4 2-、I-Content as shown in the table:
5) detect liquid to be measured and cation standard liquid respectively by the chromatography of ions, record chromatogram, through chromatographic apparatus
Carry Software Integration and obtain peak area, calculate and respectively obtain Li in liquid to be measured+、Na+、K+、Rb+、Mg2+Content, this chromatographic condition
As follows:
Use the ion chromatograph of DIONEX company ICS-90Ion Chromatography System.Employing chromatographic column:
Cation exchange column is DIONEX company, analytical column: Ionpac CS12A 4 × 250mm, and guard column: CG12A 4 × 50mm presses down
Device processed is DIONEX company CSRS 3004mm, and injection annulus is 25 μ L, experimental water resistivity: 18.25M Ω cm；
The MSA solution of flowing phase: 20mM；
Flow velocity: 1.0ml/min；
Column temperature: 32 DEG C；
Now, Li in liquid to be measured is obtained+、Na+、K+、Rb+、Mg2+Content as shown in the table:
Technical scheme is not limited to the restriction of above-mentioned specific embodiment, every does according to technical scheme
The technology deformation gone out, within each falling within protection scope of the present invention.
Claims (3)
1. a chromatography of ions concurrently separates the method for zwitterion in salt lake bittern that measures, it is characterised in that: under it includes
State step:
1) sample of salt lake bittern is obtained liquid to be measured through 0.45 μm membrane filtration, and dilute 1000 times, standby；
2) list mark solution C l of 1000 μ g/L is chosen respectively-2mL、Br-1mL、CO3 2-1mL、SO4 2-1mL、I-1mL is in 250mL capacity
Being mixed to get anion standard liquid in Ping, the most each ion concentration is respectively as follows: Cl-8mg/l、Br-4mg/l、CO3 2-4mg/l、
SO4 2-4mg/l、I-4mg/l, standby；
3) the list mark solution Li of 1000 μ g/L is chosen respectively+0.5mL、Na+1mL、K+1mL、Rb+0.1mL、Mg2+2mL holds in 250mL
Being mixed to get cation standard liquid in measuring bottle, the most each ion concentration is respectively as follows: Li+2mg/l、Na+4mg/l、K+4mg/l、Rb+0.4mg/l、Mg2+8mg/l, standby；
4) detect liquid to be measured and anion standard liquid respectively by the chromatography of ions, record chromatogram, carry through chromatographic apparatus
Software Integration obtains peak area, calculates and respectively obtains Cl in liquid to be measured-、Br-、CO3 2-、SO4 2-、I-Content, this chromatographic condition is such as
Under:
Use the ion chromatograph of DIONEX company ICS-1100Ion Chromatography System, use chromatographic column: be cloudy
Ion exchange column is DIONEX company, analytical column: Ionpac AS19 4 × 250mm, guard column: AG19 4 × 50mm, suppressor
For DIONEX company ASRS 3004mm, injection annulus is 25 μ l, experimental water resistivity: 18.25M Ω CM；
The KOH solution of flowing phase: 15mM-25mM；
Flow velocity: 0.8ml/min-1.2ml/min；
Column temperature: 32 DEG C；
5) detect liquid to be measured and cation standard liquid respectively by the chromatography of ions, record chromatogram, carry through chromatographic apparatus
Software Integration obtains peak area, calculates and respectively obtains Li in liquid to be measured+、Na+、K+、Rb+、Mg2+Content, this chromatographic condition is such as
Under:
Use DIONEX company ICS-90Ion Chromatography System ion chromatograph, use chromatographic column: sun from
Sub-exchange column is DIONEX company, analytical column: Ionpac CS12A 4 × 250mm, guard column: CG12A 4 × 50mm, suppressor
For DIONEX company CSRS 300 4mm, injection annulus is 25 μ l, experimental water resistivity: 18.25M Ω CM；
The MSA solution of flowing phase: 18mM-25mM；
Flow velocity: 1.0ml/min；
Column temperature: 32 DEG C.
The chromatography of ions the most according to claim 1 concurrently separates the method for zwitterion in salt lake bittern that measures, and it is special
Levying and be: the concentration of described KOH solution is 22mM, the concentration of described MSA solution is 20mM.
The chromatography of ions the most according to claim 1 concurrently separates the method for zwitterion in salt lake bittern that measures, and it is special
Levy and be: the flow velocity of described KOH solution and MSA solution is 1.0ml/min.
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| CN104090039B (en) * | 2014-07-08 | 2016-10-19 | 青海大学 | Measure inorganic anion and the method for organic acid anions in salt lake bittern simultaneously |
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