CN104155392A - Detection method for phthalate in shoes and shoe materials - Google Patents
Detection method for phthalate in shoes and shoe materials Download PDFInfo
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- CN104155392A CN104155392A CN201410403274.5A CN201410403274A CN104155392A CN 104155392 A CN104155392 A CN 104155392A CN 201410403274 A CN201410403274 A CN 201410403274A CN 104155392 A CN104155392 A CN 104155392A
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- footwear
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- phthalic ester
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Abstract
The invention provides a detection method for phthalate in shoes and shoe materials. The detection method comprises the following steps: taking 5 g of a sample from a representative part of a shoe, shearing the sample, carrying out uniform mixing, weighing a part of sample fragments and putting the weighed sample fragments in a screwed tube which has a volume of 50 mL and has a cover for subsequent usage; adding an internal standard extraction reagent into the tube, screwing the lid of the tube down and putting the tube in water-bath ultrasonic waves for extraction; and filtering obtained extract with a filtering membrane into a gas chromatographic bottle with a volume of 2 mL, carrying out detection by using gas chromatography and calculating results. According to the invention, a small amount of the sample is taken, workload can be reduced, and efficiency is improved; phthalate in the sample can be totally extracted, the usage amount of a solvent can be reduced, and cost is saved; the extraction reagent is a directly prepared internal standard solution, so errors are reduced.
Description
Technical field
The detection method that the present invention relates to phthalic ester in a kind of footwear and footwear material, belongs to chemical detection technique field.
Background technology
In the standard of test phthalic ester, its pre-treating method is generally now: soxhlet extraction, and as EN15777, EN14372, GB/T22048, ultrasonic extraction method, as GB/T20388.
Normative reference method of the present invention is: ISO/TS16181 (Footwear-Critical substances potentially present in footwear and footwear components--Determination of phthalates in footwear materials)
In this standard, sample sample weighting amount is too much, and cost is high, and needs long time and a large amount of reagent.
Summary of the invention
The object of the present invention is to provide the detection method of phthalic ester in a kind of footwear and footwear material, the method can be optimized pre-treatment operation, saves reagent, reduces costs.
For solving the problems of the technologies described above, technology of the present invention by the following technical solutions:
A detection method for phthalic ester in footwear and footwear material, comprises the following steps:
(1) representative position sample thief 5g on footwear, and mix after sample is shredded, take 0.50g stand-by in 50mL screw socket test tube with cover;
(2) to adding in above-mentioned test tube to the 2mg/L dicyclohexyl phthalate inner mark solution that adds n-hexane/acetone preparation for 10mL in above-mentioned test tube, tighten test tube lid, be placed in water-bath ultrasound wave and extract;
(3) get extract filtering membrane obtained above and filter, detect to the promoting the circulation of qi phase chromatography of going forward side by side in 2mL gas chromatography bottle, and result of calculation.
Further, also comprise step (4): if test result exceeds the range of linearity, need the corresponding multiple of dilution to go up again machine analysis, then result of calculation.
Further, in described step (1) sample to shred rear size be 2mm * 2mm.
Further, normal hexane: acetone=4:1 in the middle n-hexane/acetone mixed solvent of described step (2).
Further, in described step (2), extraction conditions is 50 ℃ of ultrasonic extraction 60min, and temperature 50 C ultrasonic extraction 60min can maximum extracted.
Further, in described step (3), filter membrane is organic miillpore filter of 0.22 μ m or 0.45 μ m.
Further, in described step (3), filter membrane is organic miillpore filter of 0.22 μ m, and in the filter membrane of 0.45 μ m or two kinds of specifications of 0.22 μ m, the filter effect of 0.22 μ m is better.
The beneficial effect that the present invention compared with prior art has is:
1) sample that the present invention gets is few, can reduce workload, raises the efficiency; 2) in extracting sample completely, in phthalic ester, can also reduce solvent use amount, cost-saving; 3) extraction agent is the inner mark solution directly configuring, and can reduce error.
Embodiment
For allowing the more clear and intuitive understanding the present invention of those skilled in the art, below the present invention is further illustrated.
Embodiment 1
A detection method for phthalic ester in footwear and footwear material, comprises the following steps:
(1) representative position sample thief 5g on footwear, and mix after sample is shredded into 2mm * 2mm size, take 0.50g stand-by in 50mL screw socket test tube with cover;
(2) to adding in above-mentioned test tube to the 2mg/L dicyclohexyl phthalate inner mark solution that adds n-hexane/acetone preparation for 10mL in above-mentioned test tube, tighten test tube lid, be placed in water-bath ultrasound wave and extract;
(3) get organic filtering with microporous membrane that extract obtained above is crossed 0.22um, to going forward side by side in 2mL gas chromatography bottle, promoting the circulation of qi phase chromatography detects;
(4), if test result exceeds the range of linearity, need to go up again machine analysis after dilution, then result of calculation.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (7)
1. a detection method for phthalic ester in footwear and footwear material, is characterized in that comprising the following steps:
Representative position sample thief 5g on footwear, and mix after sample is shredded, take 0.50g stand-by in 50mL screw socket test tube with cover;
In above-mentioned test tube, add the 2mg/L dicyclohexyl phthalate inner mark solution of n-hexane/acetone preparation for 10mL, tighten test tube lid, be placed in water-bath ultrasound wave and extract;
Get extract filtering membrane obtained above and filter, detect to the promoting the circulation of qi phase chromatography of going forward side by side in 2mL gas chromatography bottle, and result of calculation.
2. the detection method of phthalic ester in footwear according to claim 1 and footwear material, characterized by further comprising step (4): if test result exceeds the range of linearity, need the corresponding multiple of dilution to go up machine analysis, then result of calculation again.
3. the detection method of phthalic ester in footwear according to claim 2 and footwear material, is characterized in that: it is 2mm * 2mm that the middle sample of described step (1) shreds rear size.
4. the detection method of phthalic ester in footwear according to claim 3 and footwear material, is characterized in that: normal hexane: acetone=4:1 in n-hexane/acetone mixed solvent in described step (2).
5. the detection method of phthalic ester in footwear according to claim 4 and footwear material, is characterized in that: in described step (2), extraction conditions is 50 ℃ of ultrasonic extraction 60min.
6. the detection method of phthalic ester in footwear according to claim 5 and footwear material, is characterized in that: in described step (3), filter membrane is organic miillpore filter of 0.22 μ m or 0.45 μ m.
7. the detection method of phthalic ester in footwear according to claim 6 and footwear material, is characterized in that: organic miillpore filter that in described step (3), filter membrane is 0.22um.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410403274.5A CN104155392A (en) | 2014-08-15 | 2014-08-15 | Detection method for phthalate in shoes and shoe materials |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410403274.5A CN104155392A (en) | 2014-08-15 | 2014-08-15 | Detection method for phthalate in shoes and shoe materials |
Publications (1)
| Publication Number | Publication Date |
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| CN104155392A true CN104155392A (en) | 2014-11-19 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410403274.5A Pending CN104155392A (en) | 2014-08-15 | 2014-08-15 | Detection method for phthalate in shoes and shoe materials |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106979986A (en) * | 2017-05-04 | 2017-07-25 | 南京大学 | It is a kind of to analyze the method that micro- plastics carrying phthalate compound is enriched with content in vivo |
| CN107702974A (en) * | 2017-11-28 | 2018-02-16 | 福建省国鼎检测技术有限公司 | PH detection method in a kind of artificial leather |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005011836A1 (en) * | 2003-07-29 | 2005-02-10 | University Of York | A separation process |
| CN103389348A (en) * | 2013-08-01 | 2013-11-13 | 陕西出入境检验检疫局检验检疫技术中心 | Method for detecting polyaromatic hydrocarbons (PAHs) and phthalic acid esters (PAEs) in plant extract |
-
2014
- 2014-08-15 CN CN201410403274.5A patent/CN104155392A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005011836A1 (en) * | 2003-07-29 | 2005-02-10 | University Of York | A separation process |
| CN103389348A (en) * | 2013-08-01 | 2013-11-13 | 陕西出入境检验检疫局检验检疫技术中心 | Method for detecting polyaromatic hydrocarbons (PAHs) and phthalic acid esters (PAEs) in plant extract |
Non-Patent Citations (5)
| Title |
|---|
| THE AUTHORITY OF THE STANDARDS POLICY AND STRATEGY: "《British Standard BS EN 15777:2009》", 30 November 2009, article "Textiles-Test method for phthalates" * |
| YING GUO ET AL.: "Occurrence and Profiles of Phthalates in Foodstuffs from China and Their Implications for Human Exposure", 《JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY》, vol. 60, 15 June 2012 (2012-06-15) * |
| 周宏斌 等: "人造革中六种邻苯二甲酸酯含量测定方法的研究", 《塑料科技》, vol. 42, no. 4, 30 April 2013 (2013-04-30) * |
| 李庆 等: "人造革中邻苯二甲酸酯类增塑剂的提取及检测研究", 《中国皮革》, vol. 42, no. 21, 30 November 2013 (2013-11-30) * |
| 顾虎 等: "一步萃取法检测纺织品中邻苯二甲酸酯", 《棉纺织技术》, vol. 41, no. 12, 31 December 2013 (2013-12-31) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106979986A (en) * | 2017-05-04 | 2017-07-25 | 南京大学 | It is a kind of to analyze the method that micro- plastics carrying phthalate compound is enriched with content in vivo |
| CN107702974A (en) * | 2017-11-28 | 2018-02-16 | 福建省国鼎检测技术有限公司 | PH detection method in a kind of artificial leather |
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Application publication date: 20141119 |