CN106226454A - A kind of measure the ion chromatographic method of trace chloro ion in trimethyl gallium - Google Patents
A kind of measure the ion chromatographic method of trace chloro ion in trimethyl gallium Download PDFInfo
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Abstract
The invention discloses and a kind of measure the ion chromatographic method of trace chloro ion in trimethyl gallium, belong to chemical analysis technology field.In mensuration trimethyl gallium of the present invention, the ion chromatographic method of trace chloro ion includes: testing sample is carried out pre-treatment by (1): after the pH value of trimethyl gallium sample solution to be detected is adjusted to 7.0 8.0, upper pre-treatment post carried out post process；(2) use standard addition method or standard curve method to carry out ion chromatography, finally determine the content of trace chloro ion in trimethyl gallium.The inventive method is simple to operate, reproducible, highly sensitive, can effectively measure chloride ion content in trimethyl gallium, solve simultaneously and measure the problem that chromatographic column and suppressor are polluted damage by heavy metals in process gallium.
Description
Technical field
The present invention relates to measure the ion chromatographic method of trace chloro ion, particularly relate to measure in trimethyl gallium trace amounts of chlorine from
The ion chromatographic method of son, belongs to chemical analysis technology field.
Background technology
Trimethyl gallium (TMG) is the important source metal in MO source material, and it applies to effectively reduce in LED industry photograph
The power consumption effect in a series of fields such as bright, has huge economic benefit.Owing to preparing of TMG uses halo in synthesis technique
Compound chlorinated compound, the content of the chloride ion of residual can have a strong impact on the performance of TMG.For guaranteeing the performance of product, need
Set up a kind of method the trace chloro ion in TMG product and production process is measured.
Have no relevant report about the report of trace chloro ion in TMG, hence set up that a kind of pre-treating method is simple, Yi Chong
Multiple, and method is highly sensitive, solves simultaneously and measures the problem that chromatographic column and suppressor are polluted damage by heavy metals in process gallium
Mensuration TMG in the ion chromatographic method of trace chloro ion have very important significance.
Summary of the invention
It is an object of the invention to provide the pre-treating method of trace chloro ion, the method in a kind of ion chromatography TMG
Simple to operate, reproducible and highly sensitive.
The present invention reaches above-mentioned purpose and is achieved through the following technical solutions:
First the present invention discloses and a kind of measures the ion chromatographic method of trace chloro ion in trimethyl gallium, including following step
Rapid:
(1) testing sample is carried out pre-treatment: after the pH value of trimethyl gallium sample solution to be detected is adjusted to 7.0-8.0
Upper pre-treatment post carried out post and processed；
(2) configuration working curve solution, carries out ion chromatography, obtains Cl under variable concentrations-Peak area, with chlorine from
The concentration of son is abscissa, with its peak area for vertical coordinate drawing curve；
(3) by the trimethyl gallium sample solution row ion chromatography after pre-treatment, Cl is obtained-Peak area；
(4) according to working curve and Cl-Peak area, obtain Cl in trimethyl gallium-Content.
Invention further provides and a kind of measure the ion chromatographic method of trace chloro ion in trimethyl gallium, including following
Step:
(1) testing sample is carried out pre-treatment: after the pH value of trimethyl gallium sample solution to be detected is adjusted to 7.0-8.0
Upper pre-treatment post carried out post and processed；
(2) configuration standard curve solution；
(3) the trimethyl gallium sample solution after standard curve solution and pre-treatment is carried out ion under identical chromatographic conditions
Chromatography, respectively obtains Cl-Peak area, compare, to obtain final product.
Wherein, described pH value is 7.0.
Owing to sample is acidity through the solution that 5% dilute sulfuric acid dissolves；If sample introduction has found that free in this condition
H+Content is the highest, result in background conductance the highest, so that baseline drift is relatively big, affects the quantitative of chloride ion；In addition sample
The retention time of Chlorine in Solution ion is than retention time phase retardation 2min of chloride ion standard solution.In order to ensure in sample solution
The accuracy of determination of chloride ion result so that the retention time of chloride ion and the reservation of chloride ion in standard solution in sample solution
The concordance of time, the pH value of sample solution is regulated by the present invention, and final result shows when the pH value of sample solution is adjusted
To close to neutral (pH=7), chloride ion conductor result is not affected by baseline drift, and the reservation of chloride ion in sample solution
Time and the retention time of chloride ion in standard solution are closest to (differing 0.09min).
The type of described sample pre-treatments post is H post, and its capacity is 2.5cc；
Chromatographic column and suppressor can be caused damage, hence into ion color by the substantial amounts of gallium owing to containing in TMG sample
Before spectra system, need sample solution is crossed H type pre-treatment post.Eliminate the principle of heavy metal gallium: due to filling out in H type pre-treatment post
For sulfonic acid ion exchange resin, (i.e. there is substantial amounts of H on surface to material+), H+Displacement reaction is carried out with the gallium ion in sample solution,
Gallium ion in sample solution is incorporated on H type pre-treatment post, thus has reached to remove the mesh of heavy metal gallium in sample solution
's.
Leacheate used in described ion chromatography is sodium carbonate and sodium bicarbonate mixed solution；Preferably, described
The sodium carbonate liquor that leacheate is concentration 1.8mmol/L and concentration be the sodium bicarbonate solution of 1.7-1.6mmol/L；More preferably
, described leacheate is the sodium carbonate of concentration 1.8mmol/L and concentration is the sodium bicarbonate solution of 1.7mmol/L.
For guaranteeing determination of chloride ion accuracy, it is necessary to assure chloride ion chromatographic peak is not disturbed by other peaks, i.e. with adjacent
Separating degree between chromatographic peak reaches more than 1.5；In this experiment, the interference of chloride ion is mainly derived from the hydrogen-oxygen in sample solution
Radical ion, therefore can change retention time hydroxy by adjusting the concentration of bicarbonate radical in leacheate.
On the premise of selected chromatographic column, the present invention is respectively to 1.8/1.0,1.9/1.7,1.8/1.8,1.8/1.7,1.8/
The chromatographic condition of 1.6 and 1.8/2.5 (sodium carbonate/bicarbonate) is tested, obtain under six kinds of chromatographic conditions chloride ion with
Separating degree between adjacent chromatographic peak and analysis deadline.Result of the test shows, 1.8/1.0 and 1.8/1.7 (sodium carbonate/carbon
Acid hydrogen sodium) meet the requirement measuring separating degree, and from the point of view of the whole process analysis time, select the chromatographic condition of 1.8/1.7, its
Analysis efficiency is obviously improved than other condition, and therefore the final sodium carbonate that leacheate is concentration 1.8mmol/L selected is molten
Liquid and the solution that concentration is 1.7mmol/L sodium bicarbonate.
Technical solution of the present invention compared with prior art has the advantages that
In ion chromatography TMG of the present invention, the pre-treating method of trace chloro ion is simple to operate, reproducible and sensitive
Degree height, can effectively measure chloride ion content in TMG, solves mensuration heavy metals in process gallium dirty to chromatographic column and suppressor simultaneously
The problem that dye is damaged.
Accompanying drawing explanation
Fig. 1 Standard entertion 10 μ g/L Chloride Solution chromatogram；
Fig. 2 standard addition method working curve；
Fig. 3 chloride ion standard solution chromatogram；
Fig. 4 sample solution chromatogram.
Detailed description of the invention
Below in conjunction with specific embodiment further describe the present invention, advantages of the present invention and feature will be with describe and
Apparent.It should be understood that described embodiment is only exemplary, the scope of the present invention is not constituted any restriction.This area
Skilled artisans appreciated that, lower without departing from the spirit and scope of the present invention can to the details of technical solution of the present invention and
Form is modified or replaces, but these amendments or replacement each fall within protection scope of the present invention.
1.1 instruments and reagent
WY-IC6200 type ion chromatograph；Anion suppressor；Electric conductivity detector；(Qingdao Ai Li analyses H type pre-treatment post
Experiment science and technology)；
TMG sample (client's offer)；Sodium carbonate (standard reagent)；Sodium bicarbonate (top grade is pure)；Sodium hydroxide (top grade is pure).
1.2 chromatographic condition
Chloride ion quasi-stock solution 1000mg/L；Flow velocity: 1.0mL/min；Electric conductivity detector temperature: 40 DEG C；Column temperature: 50
℃；Suppression electric current: 30mA；Sample size: 20 μ L.
The configuration of 1.3 solution
(1) preparation of leacheate
Accurate weighing 0.1918g sodium carbonate standard reagent and 0.1428g sodium bicarbonate, be placed in 1000mL volumetric flask, uses
Secondary deionized water is dissolved and is settled to scale, and the mixing obtaining the sodium carbonate of 1.8mmol/L and 1.7mmol/L sodium bicarbonate is molten
Liquid, in this, as leacheate.
(2) preparation of standard working solution
Accurately pipette 50 μ L Cl-In Standard Stock solutions 50mL volumetric flask, it is settled to scale by secondary deionized water,
To Cl-Concentration is 1.0mg/L.
(3) preparation of blank solution
Accurately pipette the sulfuric acid solution of 1.0mL5%, be diluted to 10mL with the sodium hydroxide solution of 0.125mol/L.
(4) preparation of standard addition method working curve solution
Accurately pipette 0,10,20,50,100 and 200 μ L 1.0 μ g/mL Cl-Standard solution in 6 2mL sample bottles,
And it is separately added into the blank solution of 1000,990,980,950,900 and 800 μ L, and mixing, obtain the Cl of standard addition method-Dense
Degree is respectively 0,10,20,50,100 and 200 μ g/L.
(5) preparation of standard curve solution
Accurately pipette the standard working solution of 100 μ L 1.0 μ g/mL chloride ion, add 900 μ L secondary deionized water, mixed
Even, obtaining its concentration is 100 μ g/L.
(6) preparation of repeatability solution
Accurately pipette 10.0 μ L standard working solution, add 990 μ L blank solutions, mixing, obtain the Cl of mark-on 10 μ g/L-
Solution.
The determination of the sodium carbonate/bicarbonate ratio of experimental example 1 leacheate
For guaranteeing determination of chloride ion accuracy, it is necessary to assure chloride ion chromatographic peak is not disturbed by other peaks, i.e. with adjacent
Separating degree between chromatographic peak reaches more than 1.5；In this experiment, the interference of chloride ion is mainly derived from the hydrogen-oxygen in sample solution
Radical ion, therefore can change retention time hydroxy by adjusting the concentration of bicarbonate radical in leacheate.
On the premise of selected chromatographic column, this method is respectively to 1.8/1.0,1.9/1.7,1.8/1.8,1.8/1.7,1.8/
The chromatographic condition of 1.6 and 1.8/2.5 (sodium carbonate/bicarbonate) is tested, obtain under six kinds of chromatographic conditions chloride ion with
Separating degree between adjacent chromatographic peak and analysis deadline, it is shown in Table 1.
1.8/1.0,1.8/1.8,1.8/1.6 and 1.8/1.7 (sodium carbonate/bicarbonate) are basic as can be seen from Table 1
Meet the requirement measuring separating degree, and from the point of view of the whole process analysis time, 1.8/1.7 and 1.8/1.8 is shorter for analysis time, knot
Close separating degree data, finally select the chromatographic condition of 1.8/1.7, chloride ion is disturbed to be affected by adjacent chromatographic peak dropping to very
Low, its analysis efficiency will improve a lot simultaneously, therefore the solution of the final sodium carbonate that eluent concentration is 1.8mmol/L selected
Solution with the sodium bicarbonate that concentration is 1.7mmol/L.
The impact on chromatography of table 1 leacheate
The determination of experimental example 2 sodium hydroxide volume
Sample is acidity through the solution that 5% dilute sulfuric acid dissolves；If sample introduction has found that free H in this condition+
Content is the highest, result in background conductance the highest, so that baseline drift is relatively big, affects the quantitative of chloride ion；In addition sample solution
The retention time of middle chloride ion is than retention time phase retardation 2min of chloride ion standard solution.In order to ensure in sample solution chlorine from
The accuracy of sub-measurement result, and the retention time of chloride ion and the retention time of chloride ion in standard solution in sample solution
Concordance, utilizes the pH value of sodium hydroxide solution regulation sample solution.
Take 4 parts of identical sample solutions respectively with 1:6,1:8,1:10,1:12 (sample solution: sodium hydroxide solution, V/V)
Thinner ratio carry out testing the difference of chloride ion retention time and standard solution retention time in the sample solution of different volumes ratio,
It is shown in Table 2.
1:10 thinner ratio (i.e. the addition of sodium hydroxide solution be 10mL) is found through experiments, is adjusted to close to neutral (pH
=7) time, chloride ion conductor result is not affected by baseline drift, and the retention time of chloride ion and standard in sample solution
The retention time of Chlorine in Solution ion is closest to (difference 0.09min).
The impact on chromatography of the table 2 sodium hydroxide solution addition
In experimental example 3TMG, trace chloro ion measures
1, the pre-treatment of sample solution
(1) under the conditions of lucifuge, the quality accurately weighing TMG sample is 0.2000g, is placed in 100mL volumetric flask；
(2) it is rapidly added the sulfuric acid solution of 5% with burette to be dissolved, and is settled to scale with the sulfuric acid solution of 5%,
Obtain the sample solution of TMG；
(3) accurately pipette the sample solution in 1.0mL (2), be placed in 10mL volumetric flask, by the hydroxide of 0.125mol/L
Sodium solution dilutes and is settled to scale, obtains the need testing solution of TMG；
(4) take entrance ion chromatography system after the need testing solution in (3) crosses sample H type pre-treatment post to be analyzed, its
The front 3mL sample solution of middle sample to discard.
Wherein chromatographic column and suppressor can be caused damage by the substantial amounts of gallium owing to containing in TMG sample, hence into from
Before sub-chromatographic system, need sample solution is crossed H type pre-treatment post, it may be assumed that H type pre-treatment post must use 15mL to go for bis-times before using
Ionized water activates, and activation method is: using 5mL syringe to be rinsed with the speed of 2.0mL/min, the volume of flushing is
15mL, and the secondary deionized water finally developed is measured, if measuring containing Cl-, then need to proceed to rinse,
Until Cl in the secondary deionized water developed-It is not detected.
Eliminate the principle of heavy metal gallium: owing to the filler in H type pre-treatment post is sulfonic acid ion exchange resin (i.e. table
There is substantial amounts of H in face+), H+Carrying out displacement reaction with the gallium ion in sample solution, the gallium ion in sample solution is incorporated into H type
On pre-treatment post, thus reach to remove the purpose of heavy metal gallium in sample solution.
2, the analysis of standard addition method solution
(1) repeatability
To repeatability solution continuous sample introduction 6 times, obtain Cl-The chromatogram (see Fig. 1) of Standard entertion liquor analysis, and obtain
The retention time of chloride ion chromatographic peak and the relative standard deviation of peak area are respectively 0.27% and 0.70%.
(2) linear relationship
Linear solvent to the standard addition method of preparation, carries out sample introduction according to the Loading sequence from low concentration to high concentration and divides
Analysis, obtains Cl under variable concentrations-Peak area, with the concentration (mg/L) of chloride ion as abscissa, with its peak area as vertical coordinate
Drawing curve, is shown in Fig. 2.
3, the analysis of standard curve solution
Cl to 100 μ g/L of preparation-Standard solution sample introduction is analyzed, and obtains Cl-Chromatogram, see Fig. 3.
4, the mensuration of chloride ion content and recovery of standard addition in TMG sample
Under selected chromatographic condition, the TMG sample solution handled well is detected, obtain the color of actual sample detection
Spectrogram, is shown in Fig. 4, the most respectively according to standard addition method and single-point external standard method to the Cl in actual sample-Carry out quantitatively, and obtain
Use Cl in the sample solution of two kinds of computational methods-Concentration, records and the results are shown in Table 3, as can be seen from the table, according to Standard entertion
Method and standard curve method be calculated the relative standard deviation of the concentration of chloride ion between 1.2～7.99%, it was demonstrated that these are two years old
Kind of method in for TMG in chloride ion conductor result concordance preferable.
Actual sample carries out recovery of standard addition test, and the sample recording mark-on 10.0,20.0 and 100 μ g/L respectively reclaims
Rate, records and the results are shown in Table 4, and the rate that can be recycled from table is between 84.2～106.6%, and demonstrate this experimental technique can
By property.
Cl in table 3 sample solution-The measurement result of concentration
Table 4 carries out recovery of standard addition test specimen determination of recovery rates result to sample
Claims (7)
1. one kind measures the ion chromatographic method of trace chloro ion in trimethyl gallium, it is characterised in that comprise the following steps:
(1) testing sample carries out pre-treatment: go forward after the pH value of trimethyl gallium sample solution to be detected is adjusted to 7.0-8.0 place
Reason post carried out post and processed；
(2) configuration working curve solution, carries out ion chromatography, obtains Cl under variable concentrations-Peak area, with chloride ion
Concentration is abscissa, with its peak area for vertical coordinate drawing curve；
(3) by the trimethyl gallium sample solution row ion chromatography after pre-treatment, Cl is obtained-Peak area；
(4) according to working curve and Cl-Peak area, determine Cl in trimethyl gallium sample solution-Content.
2. one kind measures the ion chromatographic method of trace chloro ion in trimethyl gallium, it is characterised in that comprise the following steps:
(1) testing sample is carried out pre-treatment: go forward after the pH value of trimethyl gallium sample solution to be detected is adjusted to 7.0-8.0
Process post and carry out post process；
(2) configuration standard curve solution；
(3) the trimethyl gallium sample solution after standard curve solution and pre-treatment is carried out chromatography of ions under identical chromatographic conditions
Analyze, respectively obtain Cl-Peak area, compare, obtain Cl in testing sample-Content.
3. according to the ion chromatographic method described in claim 1 or 2, it is characterised in that: by molten for trimethyl gallium sample to be detected
The pH value of liquid is gone up pre-treatment post and was carried out post process after being adjusted to 7.0.
4. according to the ion chromatographic method described in claim 1 or 2, it is characterised in that: the type of described pre-treatment post is H post,
Its capacity is 2.5cc.
5. according to the ion chromatographic method described in claim 1 or 2, it is characterised in that: used by described ion chromatography
Leacheate is sodium carbonate and sodium bicarbonate mixed solution.
6. according to the ion chromatographic method described in claim 1 or 2, it is characterised in that: described leacheate is that concentration is
The sodium carbonate liquor of 1.8mmol/L and concentration are the sodium bicarbonate solution of 1.7-1.6mmol/L.
7. according to the ion chromatographic method described in claim 6, it is characterised in that: described leacheate be concentration be 1.8mmol/L
Sodium carbonate liquor and concentration be the sodium bicarbonate solution of 1.7mmol/L.
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Cited By (3)
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| CN109060976A (en) * | 2018-07-09 | 2018-12-21 | 德山化工（浙江）有限公司 | Chlorine ion concentration measuring method in silica |
| CN110568102A (en) * | 2019-09-11 | 2019-12-13 | 苏州普耀光电材料有限公司 | method for determining MO source purity by gas chromatograph |
| CN115166075A (en) * | 2022-06-24 | 2022-10-11 | 南大光电半导体材料有限公司 | Method for detecting content of chloride ions in MO source |
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| CN115166075B (en) * | 2022-06-24 | 2024-02-27 | 南大光电半导体材料有限公司 | Method for detecting chloride ion content in MO source |
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