CN104165848A - Method for measuring antimony content of polyester slice - Google Patents
Method for measuring antimony content of polyester slice Download PDFInfo
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- CN104165848A CN104165848A CN201410345606.9A CN201410345606A CN104165848A CN 104165848 A CN104165848 A CN 104165848A CN 201410345606 A CN201410345606 A CN 201410345606A CN 104165848 A CN104165848 A CN 104165848A
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Abstract
The invention relates to a method for measuring the antimony content of a polyester slice. The method is developed on the basis of a conventional malachite green photometric method and used to measure the antimony content of a polyester slice for preparing a membrane. Under an acidic condition, low-valent antimony is oxidized and converted into antimony (V); the antimony (V) carries out reactions with malachite green to generate a green complex; then the green complex is extracted by isoamyl acetate; the extract is placed in a cuvette (1cm), the absorbance of the extract is measured at 625 nm, and the Beer's law is correct, when the antimony concentration is in a range of 0.0 ug/mL to 10.0 ug/mL. In the method, a sample is burned to ash through a dry method, and then the ash is completely dissolved in sulfuric acid. The sodium citrate and isoamyl acetate are added at first, then a malachite green solution is added, so that the generated complex can immediately enter the isoamyl acetate layer so as to avoid the phenomenon that green complex is unstable in water. Moreover, a universal ultraviolet spectrophotometer is adopted in the method, and the analysis cost is reduced.
Description
Technical field
The present invention relates to the assay method of antimony content in a kind of polyester slice, be in particular the assay method of antimony content in a kind of polyester for film section.
Background technology
Polyester (PET) is to take the fine polymkeric substance that closes that pure terephthalic acid and ethylene glycol is main material production.Be one of most important synthetic fiber material, in fields such as packing, industrial yarn and engineering plastics, also have important use.At present to produce what adopt be to take the antimony-based catalyst that the compound of heavy metal antimony is principal ingredient to the PET in the whole world 90%, thereby residual a small amount of antimony in product inevitably, because antimony is the harmful element with the property accumulated, there is the human body of destruction metabolism, the harm such as contaminated environment are therefore very necessary for the check of antimony in PET.
The common analysis that detects at present antimony has peacock green spectrophotometric method, hydrogenation atomic fluorescence method, atomic absorption method, plasma emission spectroscopy method, x ray fluorescence spectrometry etc.These data, from different applications, have been introduced the assay method of antimony by different detection meanss.Owing to being subject to the restriction of fund and experiment condition, the instrument analytical methods such as Hydride generation atomic absorption spectrometry fluorescence method, atomic absorption method, plasma emission spectroscopy method, x ray fluorescence spectrometry are difficult to popularize, and although traditional peacock green spectrophotometric method is economical, fast, the method requirement that antimony content is measured in the many places such as sample preparation can not meet polyester slice.
At present, not yet find the report with antimony content in peacock green spectrophotometry polyester slice.
Summary of the invention
The object of the present invention is to provide the method for antimony content in a kind of peacock green spectrophotometry polyester slice.Traditional peacock green spectrophotometric method is: under acid condition, antimony is oxidized to quinquevalence antimony at a low price, more ashamed with generating green network platform thing with peacock green, with colorimetric assay after organic solvent extraction, because the green complex compound of antimony and peacock green generation is unstable in water.
In operation after optimization, first add organic extractant, then add malachite green solution, make the complex compound generating enter immediately organic layer, green complex compound unsettled phenomenon in water of having avoided antimony and peacock green to generate; Sample carries out, after dry process, with sulfuric acid, dissolving, and makes the antimony in sample be transformed into antimony ion, and then according to the operating conditions after optimizing, form green complex compound with peacock green, with after isoamyl acetate extract and separate, the cuvette of 1cm for organic phase, measures its absorbance in 625nm place.
Technical scheme of the present invention is as follows:
1) under acid medium, first the antimony ion in system is reduced into trivalent antimony ion, and then is oxidized to quinquevalence antimony, quinquevalence antimony and peacock green are ashamed with generating green complex compound; With after organic solvent extraction, place layering, aqueous phase discarded;
2) organic phase is dewatered by being added with in advance the little funnel of anhydrous sodium sulfate, and the cuvette of 1cm for the organic phase after dehydration, take blank reagent solution as reference, at 625nm place, measure corresponding absorbance, take antimony content as horizontal ordinate, and absorbance is ordinate, and drawing is bent; The antimony content curve of working within the scope of 0.0ug～10.0ug.
3) to sample, adopt dry ashing method to process, take sample 0.0002g, in quartz beaker, charing on electric furnace, is then placed in muffle furnace in 550 ℃ of calcinations to ashing completely, takes out and is cooled to room temperature, add wherein the concentrated sulphuric acid, sample is dissolved completely, be then transferred in the volumetric flask of 50mL, be diluted with water to scale, use transfer pipet sample thief, according to the assay method of working curve, at 625nm place, measure corresponding absorbance, from working curve, find corresponding antimony content.
Described polyester slice is polyester for film section, and polyester for film section is a kind of of polyester slice.
The analytical instrument of using is spectrophotometer.
Described acid medium is to control with watery hydrochloric acid, and its concentration is the volume ratio 5:1 of hydrochloric acid and water, and consumption is 4mL～6mL.
The concentration of described peacock green is 0.2g/mL, and consumption is 1mL～1.5mL.
Described organic solvent extract is for analyzing pure isoamyl acetate reagent, and its consumption is 5mL～10mL.
Under acid medium, first the antimony ion in system is reduced into trivalent antimony ion, and then be oxidized to quinquevalence antimony, quinquevalence antimony and peacock green are ashamed to be preferably by the method that generates green complex compound: first with reductive agent stannous chloride, the antimony ion in system is reduced into trivalent antimony ion, its concentration is 0.12g/mL, and consumption is to disappear and excessive 2 to solution is yellow; With oxygenant sodium nitrite, by trivalent antimony ionic oxide formation, be quinquevalence antimony ion again, its concentration is 0.2g/mL, and consumption is 1mL～1.5mL.
The assay method of antimony content in described a kind of polyester slice, first with the antimony standard solution curve of working, and then carries out sample analysis.
Basic fundamental thinking of the present invention is: the test condition in peacock green spectrophotometric method is optimized, because the green complex compound of antimony and peacock green generation is unstable in water, in operation, first add isoamyl acetate, add again malachite green solution, make the complex compound generating enter immediately isoamyl acetate layer; And adopt dry ashing method to process sample, sample is dissolved completely, by the detection of antimony in this technology application polyester for film section sample.
Advantage of the present invention is: solved in traditional peacock green spectrophotometric method that complex compound is unstable, measurement result poor reproducibility and existing sample treatment, can not make the consoluet shortcoming of sample; And because the analytical instrument of the method employing is general spectrophotometer, also reduced analysis cost.
The method of antimony content in a kind of peacock green spectrophotometry polyester slice is provided.Solved in traditional peacock green spectrophotometric method that complex compound is unstable, measurement result poor reproducibility and existing sample treatment, can not make the consoluet shortcoming of sample; And because the analytical instrument of the method employing is general spectrophotometer, also reduced analysis cost.
Accompanying drawing explanation
Fig. 1 antimony standard working curve.
Embodiment
The method with embodiment, the present invention being proposed is below further described:
The present invention, in real work, first with the antimony standard solution curve of working, and then carries out sample analysis.
Embodiment 1
The drafting of standard working curve:
Get antimony standard solution 0.00,0.10,0.30,0.50,0.70, the 1.00mL of 10ug/mL, be placed in respectively the 125mL separating funnel that is added with in advance 4mL water, 4mL volume ratio 5:1 watery hydrochloric acid, add the stannous chloride solution of 0.12g/mL to disappear and excessive 2 to yellow, mix, place 5 minutes, the sodium nitrite solution that adds 1mL0.2g/mL, mix, and blow with rubber bulb, catch up with the brown oxides of nitrogen gas in most separating funnel, then the urea liquid that adds 2.5mL volume ratio 1:1, fully vibration shakes up, and is placed in solution and overflows without bubble.The sodium citrate, 5mL isoamyl acetate, the 1mL0.2g/mL malachite green solution that add 10mL0.2g/mL, fully vibration, places layering, aqueous phase discarded, organic phase is dewatered by being added with in advance the little funnel of anhydrous sodium sulfate, the cuvette of 1cm for organic phase after dehydration, take blank reagent solution as reference, measures corresponding absorbance at 625nm place, take antimony amount as horizontal ordinate, absorbance is ordinate, and drawing curve, is shown in Fig. 1.Antimony concentration is from 0.0 to 10.0ug time, linear good.Its regression equation Y=0.0639x+0.0058, related coefficient is 0.9994.
The analysis of sample:
To a certain section sample, recommendation Sb 16.21ug/g, take 4.0g sample, accurately to 0.0002g, in quartz beaker, careful ashing on electric furnace, then be placed in muffle furnace in 550 ℃ of calcinations 2 hours, take out and be cooled to room temperature. add wherein 5mL concentrated sulfuric acid dissolution sample, after dissolving, solution should be clarified, then be transferred in the volumetric flask of 50mL, be diluted with water to scale.Get 1mL sample and be placed in the 125mL separating funnel that is added with in advance 4mL water, 4mL volume ratio 5:1 watery hydrochloric acid, according to the assay method of working curve, at 625nm place, measure corresponding absorbance, from working curve, find corresponding antimony content, according to sample weighting amount, calculate the actual antimony content in sample.Analytical sample has been carried out respectively to replication 5 times, and experimental result is in Table 1.
Table 1 sample experimental result
Comparative example 1
Same section sample to recommendation Sb 16.21ug/g, except measuring wavelength 620nm, other condition is with embodiment 1, and measurement result is in Table 2.
Table 2 sample experimental result
Comparative example 2
Same section sample to recommendation Sb 16.21ug/g, except measuring wavelength 630nm, other condition is with embodiment 1, and measurement result is in Table 3
Table 3 sample experimental result
Embodiment 2
Section sample to a certain unknown antimony content, measures according to the condition determination of embodiment 1, the results are shown in Table 4.
Table 4 sample experimental result
Embodiment 3
The investigation of method precision, according to the condition of embodiment 2, has carried out respectively replication to 5 analytical samples 5 times, and test findings is in Table 4.
Table 5 Precision Experiment result
Claims (7)
1. an assay method for antimony content in polyester slice, is characterized in that step is as follows:
1) the antimony concentration curve of working within the scope of 0.0ug/mL～10.0ug/mL is first reduced into trivalent antimony ion by the antimony ion in system, and then is oxidized to quinquevalence antimony under acid medium, and quinquevalence antimony and peacock green are ashamed with generating green complex compound; With after organic solvent extraction, place layering, aqueous phase discarded;
2) organic phase is dewatered by being added with in advance the little funnel of anhydrous sodium sulfate, and the cuvette of 1cm for the organic phase after dehydration, take blank reagent solution as reference, at 625nm place, measure corresponding absorbance, take antimony content as horizontal ordinate, and absorbance is ordinate, and drawing is bent;
3) to sample, adopt dry ashing method to process, take sample 0.0002g, in quartz beaker, charing on electric furnace, is then placed in muffle furnace in 550 ℃ of calcinations to ashing completely, takes out and is cooled to room temperature, add wherein the concentrated sulphuric acid, sample is dissolved completely, be then transferred in the volumetric flask of 50mL, be diluted with water to scale, use transfer pipet sample thief, according to the assay method of working curve, at 625nm place, measure corresponding absorbance, from working curve, find corresponding antimony content.
2. method according to claim 1, is characterized in that described polyester slice is polyester for film section.
3. method according to claim 1, is characterized in that used equipment is for spectrophotometer.
4. method according to claim 1, is characterized in that described acid medium is to control with watery hydrochloric acid, and its concentration is the volume ratio 5:1 of hydrochloric acid and water, and consumption is 4mL～6mL.
5. method according to claim 1, is characterized in that the concentration of described peacock green is 0.2g/mL, and consumption is 1mL～1.5mL.
6. method according to claim 1, is characterized in that described organic solvent is for analyzing pure isoamyl acetate reagent, and its consumption is 5mL～10mL.
7. method according to claim 1, is characterized in that first with stannous chloride, the antimony ion in system being reduced into trivalent antimony ion, and its concentration is 0.12g/mL, and consumption is 2～4; With sodium nitrite, by trivalent antimony ionic oxide formation, be quinquevalence antimony ion again, its concentration is 0.2g/mL, and consumption is 1mL～1.5mL.
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| CN201410345606.9A CN104165848A (en) | 2014-07-18 | 2014-07-18 | Method for measuring antimony content of polyester slice |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104390922A (en) * | 2014-12-10 | 2015-03-04 | 江苏盛虹科技股份有限公司 | Method for determining content of antimony in fiber-grade polyester chip |
| CN107589082A (en) * | 2017-07-31 | 2018-01-16 | 成都中建材光电材料有限公司 | The assay method of antimony in a kind of high purity cadmium |
| CN107703070A (en) * | 2017-08-28 | 2018-02-16 | 成都中建材光电材料有限公司 | The assay method of antimony element content in a kind of tin sample |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52150687A (en) * | 1976-06-09 | 1977-12-14 | Nippon Electric Glass Co | Method and apparatus for increasing measuring precision of atomic absorption spectrum |
| CN102608044A (en) * | 2012-02-23 | 2012-07-25 | 安徽皖仪科技股份有限公司 | Sample treatment method for measuring antimony in polyester chip with flame atomic absorption spectrometry |
-
2014
- 2014-07-18 CN CN201410345606.9A patent/CN104165848A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52150687A (en) * | 1976-06-09 | 1977-12-14 | Nippon Electric Glass Co | Method and apparatus for increasing measuring precision of atomic absorption spectrum |
| CN102608044A (en) * | 2012-02-23 | 2012-07-25 | 安徽皖仪科技股份有限公司 | Sample treatment method for measuring antimony in polyester chip with flame atomic absorption spectrometry |
Non-Patent Citations (1)
| Title |
|---|
| 中华人民共和国卫生部 等: "《GB/T 5009.101-2003 食品容器及包装材料用聚酯树脂及其成型品中锑的测定》", 1 January 2004 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104390922A (en) * | 2014-12-10 | 2015-03-04 | 江苏盛虹科技股份有限公司 | Method for determining content of antimony in fiber-grade polyester chip |
| CN107589082A (en) * | 2017-07-31 | 2018-01-16 | 成都中建材光电材料有限公司 | The assay method of antimony in a kind of high purity cadmium |
| CN107703070A (en) * | 2017-08-28 | 2018-02-16 | 成都中建材光电材料有限公司 | The assay method of antimony element content in a kind of tin sample |
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Application publication date: 20141126 |