CN103954730B - The detection method of barium and zinc in liquid barium zinc compound stabilizer - Google Patents
The detection method of barium and zinc in liquid barium zinc compound stabilizer Download PDFInfo
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- CN103954730B CN103954730B CN201410220352.8A CN201410220352A CN103954730B CN 103954730 B CN103954730 B CN 103954730B CN 201410220352 A CN201410220352 A CN 201410220352A CN 103954730 B CN103954730 B CN 103954730B
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Abstract
The invention discloses the detection method of barium and zinc in a kind of liquid barium zinc compound stabilizer, (1) liquid barium zinc compound stabilizer sample No. 120 industrial napthas are dissolved, the ratio of sample quality and industrial naptha volume is 1:10 ~ 15 (g/ml), add absolute ethyl alcohol constant volume again, the volume of constant volume is V, shakes up; (2) solution that two parts of same volume steps (1) are obtained is pipetted, a copy of it adds ammonium fluoride and water, ammonium fluoride is dissolved, add the ammonia-ammonium chloride buffer solution of pH=10 again, add chromium black T indicator number to drip, utilize EDTA standard titration solution to carry out titration, becoming pure blue to solution is titration end-point, and record consumes the volume V of EDTA standard titration solution
1, calculate the content of zinc in sample; Another part does not add ammonium fluoride, and all the other processing procedures are identical, and record consumes the volume V of EDTA standard titration solution
2, calculate by formula 2, obtain the content of barium in sample.This method instrument is simple, and can measure the content of zinc and barium respectively, result accurately and reliably.
Description
Technical field
The present invention relates to a kind of detection method, specifically, relate to the detection method of barium and zinc in a kind of liquid barium zinc compound stabilizer.
Background technology
Liquid barium zinc compound stabilizer, because of its clean environment firendly, is convenient to metering, produces and application process no dust pollution, and is widely used in the fields such as adhesive tape, plastics, chemical industry.
At present, in liquid barium zinc compound stabilizer, the method for inspection of metal is: take (0.2 ~ 0.3) g (being accurate to 0.0001g) sample, be placed in 250ml Erlenmeyer flask, with after 5mlNY-200 solvent oil (A.1.5) dilution (can heating water bath be used if desired), add (30 ~ 50) ml ethanol (A.1.4) to shake up, accurately add 10mlEDTA standard titration solution (0.05mol/L) to shake up, then 10ml ammonia buffer (PH=10) is added, add a small amount of chromium black T indicator (0.5%) again with zinc chloride standard titration solution (0.05mol/L) titration, when solution is terminal mutually by the general purple of blueness.
Be calculated as follows:
In formula: C
2the concentration of-EDTA standard titration solution, mol/L;
V
2the volume that-EDTA the standard titration solution that adds consumes, ml;
The concentration of C-zinc chloride standard titration solution, mol/L;
The volume of the zinc chloride standard titration solution that V-titration consumes, ml;
0.137-suitable for 1.00mlEDTA standard solution [C (EDTA)=1.000mol/L] a gram quality for the metal represented;
The quality of m-sample, g.
This detection method exists following not enough:
(1) tenor that what the method recorded is barium and zinc is total, cannot determine barium and zinc content separately;
(2) coefficient 0.137 taken advantage of in computing formula, is suitable for 1.00mlEDTA standard solution [C (EDTA)=1.000mol/L] a gram quality for the barium represented, and have ignored the existence of zinc, therefore measurement result is greater than actual metal content;
(3) titration method is back titration, larger with direct titrimetric method phase ratio error.
And for liquid barium zinc compound stabilizer, its barium content should control at 5.1-6.0%, Zn content should control at 1.1-1.6%, so both content must all detect, generally atomic absorption spectrophotometry is adopted in prior art, but atomic absorption spectrophotometer (AAS) price general charged costly, be unfavorable for promoting the use of of the method for inspection.
Summary of the invention:
For the deficiencies in the prior art, the object of this invention is to provide the detection method of barium and zinc in a kind of liquid barium zinc compound stabilizer, this detection method adopts compleximetry, makes screening agent with ammonium fluoride, efficiently solves the interference of Ba when surveying Zn.The method testing instruments are simple, and cost is lower, and can measure the content of barium and zinc respectively, result accurately and reliably.
For achieving the above object, the present invention adopts following technical scheme:
A detection method for barium and zinc in liquid barium zinc compound stabilizer, comprises the following steps:
(1) fully dissolved by liquid barium zinc compound stabilizer sample No. 120 industrial napthas, the ratio of sample quality and industrial naptha volume is 1:10 ~ 15 (g/ml), then adds absolute ethyl alcohol constant volume, and the volume of constant volume is V, shakes up, for subsequent use;
(2) pipette two parts of volumes and be V
0the obtained solution of step (1), a copy of it adds the ammonium fluoride aqueous solution that mass concentration is 10%, add the ammonia-ammonium chloride buffer solution of pH=10 again, add chromium black T indicator number to drip, EDTA standard titration solution is utilized to carry out titration, becoming pure blue to solution is titration end-point, and record consumes the volume V of EDTA standard titration solution
1, calculate by formula 1, obtain the content of zinc in sample;
Formula 1: Zn content (%)=[(C × V
1× 0.0653)/(V
0/ V × m)] × 100%
In formula, C is the concentration of EDTA standard titration solution, mol/L;
V
1for the volume of the EDTA standard titration solution that titration zinc consumes, ml;
V is the volume of sample constant volume, ml;
V
0for pipetting the volume of sample solution after constant volume, ml;
0.0653-is suitable for 1.00mlEDTA standard solution [C (EDTA)=1.000mol/L] a gram quality for the zinc represented;
M is the quality of sample, g;
Another part does not add ammonium fluoride, and all the other processing procedures are identical, and record consumes the volume V of EDTA standard titration solution
2, calculate by formula 2, obtain the content of barium in sample;
Formula 2: barium content (%)=[(C × (V
2-V
1) × 0.137)/(V
0/ V × m)] × 100%
In formula, C is the concentration of EDTA standard titration solution, mol/L;
V is the volume of sample constant volume, ml;
V
0for pipetting the volume of sample solution after constant volume, ml;
V
1for the volume of the EDTA standard titration solution that titration zinc consumes, ml;
V
2for the volume of the EDTA standard titration solution that titration zinc and barium consume, ml;
0.137-is suitable for 1.00mlEDTA standard solution [C (EDTA)=1.000mol/L] a gram quality for the barium represented;
M-is the quality of sample, g.
In step (1), the ratio of sample quality and industrial naptha volume is preferably 1:10 (g/ml);
In step (2), addition and the ratio of the volume pipetting solution of ammonium fluoride are 1:25 ~ 30 (g/ml), are preferably 1:25; The addition of ammonia-ammonium chloride buffer solution is 1:5 ~ 8 with the volume ratio pipetting solution, is preferably 1:5.
The present invention has following beneficial effect relative to prior art:
(1) can measure the content of barium and zinc in liquid barium zinc compound stabilizer respectively, result accurately, reliably;
(2) testing instruments are simple, and cost is lower, is easy to carry out promotion and application.
Accompanying drawing explanation
Fig. 1 ammonium fluoride addition is on the impact of Zn content testing result.
Embodiment
The present invention is further illustrated in conjunction with the embodiments, should be noted that following explanation is only to explain the present invention, not limiting its content.
Embodiment 1
(1) take liquid barium zinc compound stabilizer sample 1.0000g, add 10ml120 industrial naptha and fully dissolve, be settled to 100ml with absolute ethyl alcohol, shake up, for subsequent use.
(2) solution that the step (1) of two parts of each 50ml is obtained is pipetted, a copy of it adds the ammonium fluoride aqueous solution of 20ml10%, add the ammonia-ammonium chloride buffer solution 10ml of pH=10 again, add chromium black T indicator 5, EDTA standard titration solution is utilized to carry out titration, becoming pure blue to solution is titration end-point, and record consumes the volume V of EDTA standard titration solution
1; Another part does not add ammonium fluoride, and all the other processing procedures are identical, and record consumes the volume V of EDTA standard titration solution
2; Calculate by formula 1 and formula 2, the results are shown in Table 1.
Table 1 barium, zinc-content determination result
Embodiment 2
Methodological study:
(1) specificity
Metal values in liquid barium zinc organic composite stabilizing agent of the present invention only has barium and zinc, using industrial naptha and absolute ethyl alcohol as solvent in experimental technique, so whole experimentation institute's solubilizer and medicine are without other obvious foreign ion interference.Take ammonium fluoride as screening agent, PH controls, 10, to shelter barium ion, thus can detect each component concentration of metal.By investigating the addition of ammonium fluoride, determine the suitable scope of ammonium fluoride addition.
The results are shown in Figure 1, as seen from the figure: when ammonium fluoride addition is on the low side, interfering ion is had to participate in reaction, Zn content testing result is higher, and the fluorine ion in this experiment ammonium fluoride mainly shelters barium, when to add massfraction in 50ml sample solution be 10% ammonium fluoride aqueous solution 17ml, Zn content testing result tends towards stability, illustrating that the object of sheltering reaches, in order to remove interference completely, preferably adding the ammonium fluoride aqueous solution of 10% of 20ml massfraction.
(2) precision
Get same liquid barium zinc compound stabilizer sample, sampled respectively by same analyst, replication 6 times, the results are shown in Table 3.
Table 3 precision measurement result
Embodiment 3
Contrast test:
Get with a collection of liquid barium zinc compound stabilizer sample, adopt atomic absorption spectrophotometry and method of the present invention to measure respectively, the results are shown in Table 2.
Table 2 different measuring methods results contrast
By relatively finding out, method of the present invention and atomic absorption spectroscopy determination result close, therefore, method of the present invention can be used for measuring the content of barium and zinc in liquid barium zinc compound stabilizer.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (4)
1. the detection method of barium and zinc in liquid barium zinc compound stabilizer, comprises the following steps:
(1) fully dissolved by liquid barium zinc compound stabilizer sample No. 120 industrial napthas, the ratio of sample quality and industrial naptha volume is 1:10 ~ 15, g/ml, then adds absolute ethyl alcohol constant volume, and the volume of constant volume is V, shakes up, for subsequent use;
(2) pipette two parts of volumes and be V
0the obtained solution of step (1), a copy of it adds the ammonium fluoride aqueous solution that mass concentration is 10%, add the ammonia-ammonium chloride buffer solution of pH=10 again, add chromium black T indicator number to drip, EDTA standard titration solution is utilized to carry out titration, becoming pure blue to solution is titration end-point, and record consumes the volume V of EDTA standard titration solution
1, calculate by formula 1, obtain the content of zinc in sample;
Formula 1: Zn content (%)=[(C × V
1× 0.0653)/(V
0/ V × m)] × 100%
In formula, C is the concentration of EDTA standard titration solution, mol/L;
V
1for the volume of the EDTA standard titration solution that titration zinc consumes, ml;
V is the volume of sample constant volume, ml;
V
0for the volume of the solution that the step (1) pipetted obtains, ml;
0.0653-be with 1.00ml concentration be the EDTA standard solution of 1.000mol/L suitable with a gram quality for the zinc represented;
M is the quality of sample, g;
Another part does not add ammonium fluoride, and all the other processing procedures are identical, and record consumes the volume V of EDTA standard titration solution
2, calculate by formula 2, obtain the content of barium in sample;
Formula 2: barium content (%)=[(C × (V
2-V
1) × 0.137)/(V
0/ V × m)] × 100%
In formula, C is the concentration of EDTA standard titration solution, mol/L;
V is the volume of sample constant volume, ml;
V
0for the volume of the solution that the step (1) pipetted obtains, ml;
V
1for the volume of the EDTA standard titration solution that titration zinc consumes, ml;
V
2for the volume of the EDTA standard titration solution that titration zinc and barium consume, ml;
0.137-be with 1.00ml concentration be the EDTA standard solution of 1.000mol/L suitable with a gram quality for the barium represented;
M-is the quality of sample, g;
In step (2), the addition of ammonium fluoride is 1g:25 ~ 30ml with the ratio of the volume pipetting solution, and the addition of ammonia-ammonium chloride buffer solution is 1g:5 ~ 8ml with the volume ratio pipetting solution.
2. the detection method of barium and zinc in a kind of liquid barium zinc compound stabilizer according to claim 1, it is characterized in that, in step (1), the ratio of sample quality and industrial naptha volume is 1g:10ml.
3. the detection method of barium and zinc in a kind of liquid barium zinc compound stabilizer as claimed in claim 1, it is characterized in that, in described step (2), the addition of ammonium fluoride is 1g:25ml with the ratio of the volume pipetting solution; The addition of ammonia-ammonium chloride buffer solution is 1g:5ml with the volume ratio pipetting solution.
4. the detection method of barium and zinc in a kind of liquid barium zinc compound stabilizer as claimed in claim 1, is characterized in that, comprise the following steps:
(1) take liquid barium zinc compound stabilizer sample 1.0000g, add 10ml No. 120 industrial napthas and fully dissolve, be settled to 100ml with absolute ethyl alcohol, shake up;
(2) solution that the step (1) of two parts of each 50ml is obtained is pipetted, a copy of it adds the ammonium fluoride aqueous solution of 20ml 10%, add the ammonia-ammonium chloride buffer solution 10ml of pH=10 again, add chromium black T indicator 5, EDTA standard titration solution is utilized to carry out titration, becoming pure blue to solution is titration end-point, and record consumes the volume V of EDTA standard titration solution
1; Another part does not add ammonium fluoride, and all the other processing procedures are identical, and record consumes the volume V of EDTA standard titration solution
2; By formula 1: Zn content (%)=[(C × V
1× 0.0653)/(V
0/ V × m)] × 100%, and formula 2: barium content (%)=[(C × (V
2-V
1) × 0.137)/(V
0/ V × m)] × 100% to calculate.
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| CN110988256A (en) * | 2019-12-30 | 2020-04-10 | 江苏艾兰得营养品有限公司 | EDTA titration method for rapidly determining Zn content in vitamin C + zinc sustained release tablets |
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| CN101344488A (en) * | 2008-05-31 | 2009-01-14 | 潍坊学院 | Analytical method and special reagent for zinc chloride content in acidic zincing solution |
| CN101696940A (en) * | 2009-10-10 | 2010-04-21 | 四川省畜科饲料有限公司 | Method for measuring zinc lactate content by measuring zinc content |
| CN102183518A (en) * | 2011-01-26 | 2011-09-14 | 中节能六合天融环保科技有限公司 | Method for quickly measuring sulfate radical content in magnesium method desulfurization process |
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| CN101344488A (en) * | 2008-05-31 | 2009-01-14 | 潍坊学院 | Analytical method and special reagent for zinc chloride content in acidic zincing solution |
| CN101696940A (en) * | 2009-10-10 | 2010-04-21 | 四川省畜科饲料有限公司 | Method for measuring zinc lactate content by measuring zinc content |
| CN102183518A (en) * | 2011-01-26 | 2011-09-14 | 中节能六合天融环保科技有限公司 | Method for quickly measuring sulfate radical content in magnesium method desulfurization process |
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