CN104165945A - Method for detecting phthalate - Google Patents
Method for detecting phthalate Download PDFInfo
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- CN104165945A CN104165945A CN201410403232.1A CN201410403232A CN104165945A CN 104165945 A CN104165945 A CN 104165945A CN 201410403232 A CN201410403232 A CN 201410403232A CN 104165945 A CN104165945 A CN 104165945A
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Abstract
The invention provides a method for detecting phthalate. The method comprises the following steps: (1) cutting a sample to be detected into pieces, and putting the pieces into a test tube with a cover on a screw cap; (2) adding tetrahydrofuran into the test tube, screwing on the cover, and putting the test tube into water-bath ultrasonic waves for ultrasonic extraction; (3) taking out the test tube, cooling to room temperature, adding 20mL of methyl alcohol into the test tube, screwing on the cover, shaking up, and standing for 15min; (4) after liquid in the test tube is layered, filtering upper clear liquid, and putting a filtered clear solution into a 2mL gas chromatogram bottle; and (5) putting 0.8mL of filtered clear solution into the gas chromatogram bottle, adding 0.2mL of 10mg/LBB inner standard solution, mixing uniformly, analyzing by a gas chromatograph, and calculating to obtain the result. The method can be used for extracting phthalate from the sample at the utmost, and methyl alcohol can precipitate macromolecular substances in extraction liquid so as to facilitate filtering and protect instruments. Compared with a standard method, the method has the advantage that methyl alcohol replaces normal hexane so as to obtain a better precipitation effect.
Description
Technical field
The present invention relates to a kind of detection method of phthalic ester, belong 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, GB/T22048, ultrasonic extraction method, as GB/T20388, EN14372, ISO/TS16181 etc.
Normative reference method of the present invention is: CPSC-CH-C1001-09.03 (2010) (Standard Operating Procedure for Determination of Phthalates April 1st, 2010), in this standard, sample sample weighting amount is very few, and the data result error causing due to sample inequality is very large; Whether select to jolt, ultrasonic, heating be not clear and definite especially, normal hexane sedimentation effect is not best.
Summary of the invention
The object of the present invention is to provide a kind of detection method of phthalic ester, the method, for the data result recording is accurate, specifies concrete pre-treatment operation.
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, comprises the following steps:
(1) get testing sample 5g, be cut into fragment, after stir, take 0.30g sample fragment in 50mL screw socket test tube with cover;
(2) in above-mentioned test tube, add 10mL tetrahydrofuran, tighten lid, be placed in water-bath ultrasound wave and extract;
(3) take out test tube and be cooled to room temperature; In test tube, add 20mL methyl alcohol, tighten lid, shake up rear standing 15min;
(4), after layering in test tube, get supernatant liquid and filter, to 2mL gas chromatography bottle;
(5) get 0.8mL and filtered settled solution in gas chromatography bottle, adding 0.2mL concentration is the BB(Ergol of 10mg/L) in mark mix after standard solution, upper gas chromatograph analysis, and result of calculation.
Further, in described step (1), sample chip size is 2mm × 2mm.
Further, in described step (2), extraction conditions is 40 DEG C of ultrasonic extraction 60min.
Further, described step (4) be filtered into the organic filtering with microporous membrane of 0.22um.
Further, described step (5) if in test result exceed the range of linearity, need dilution corresponding multiple go up again gas chromatograph analysis.
The beneficial effect that the present invention compared with prior art has is: the present invention can maximum possible extract the phthalic ester in sample, and methyl alcohol can precipitate the macromolecular substances in extract, convenient filtration, protection instrument; The present invention, compared with standard method, has changed normal hexane into methyl alcohol, can obtain better sedimentation effect.
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.
A detection method for phthalic ester, comprises the following steps:
(1) get testing sample 5g, be cut into the specification fragment of 2mmx2mm, stir, take 0.30g sample fragment in 50mL screw socket test tube with cover;
(2) in test tube, add 10mL tetrahydrofuran, tighten lid, be placed in water-bath ultrasound wave, 40 DEG C of ultrasonic extraction 60min;
(3) take out test tube and be cooled to room temperature; In test tube, add 20mL methyl alcohol, tighten lid, shake up rear standing 15min;
(4), after layering in test tube, get supernatant liquid and cross the organic filtering with microporous membrane of 0.22um, to 2mL gas chromatography bottle;
(5) get 0.8mL and filtered settled solution in gas chromatography bottle, add mark standard solution in 0.2mL 10mg/L Ergol to mix, upper gas chromatograph analysis, and result of calculation.
Step (5) if in test result exceed the range of linearity, need dilution corresponding multiple go up again gas chromatograph analysis.
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 amendment of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (5)
1. a detection method for phthalic ester, is characterized in that, comprises the following steps:
(1) get testing sample 5g, be cut into fragment, after stir, take 0.30g sample fragment in 50mL screw socket test tube with cover;
(2) in above-mentioned test tube, add 10mL tetrahydrofuran, tighten lid, be placed in water-bath ultrasound wave and extract;
(3) take out test tube and be cooled to room temperature; In test tube, add 20mL methyl alcohol, tighten lid, shake up rear standing 15min;
(4), after layering in test tube, get supernatant liquid and filter, to 2mL gas chromatography bottle;
(5) get 0.8mL and filtered settled solution in gas chromatography bottle, adding 0.2mL concentration is after mark standard solution, to mix in the Ergol of 10mg/L, upper gas chromatograph analysis, and result of calculation.
2. the detection method of phthalic ester according to claim 1, is characterized in that: in described step (1), sample chip size is 2mm × 2mm.
3. the detection method of phthalic ester according to claim 2, is characterized in that: in described step (2), extraction conditions is 40 DEG C of ultrasonic extraction 60min.
4. the detection method of phthalic ester according to claim 3, is characterized in that: described step (4) be filtered into the organic filtering with microporous membrane of 0.22um.
5. the detection method of phthalic ester according to claim 4, is characterized in that: described step (5) if in test result exceed the range of linearity, need dilution corresponding multiple go up again gas chromatograph analysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410403232.1A CN104165945A (en) | 2014-08-15 | 2014-08-15 | Method for detecting phthalate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410403232.1A CN104165945A (en) | 2014-08-15 | 2014-08-15 | Method for detecting phthalate |
Publications (1)
| Publication Number | Publication Date |
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| CN104165945A true CN104165945A (en) | 2014-11-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410403232.1A Pending CN104165945A (en) | 2014-08-15 | 2014-08-15 | Method for detecting phthalate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108613960A (en) * | 2018-03-27 | 2018-10-02 | 广西壮族自治区食品药品检验所 | The Raman spectra detection process of phthalic ester plasticizer |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000135435A (en) * | 1998-08-26 | 2000-05-16 | Mitsubishi Chemicals Corp | Separating agent, separation of estrogen compound and estrogenic substance, and screening, adsorbing and removing of estrogenic substance |
| CN101858897A (en) * | 2010-07-05 | 2010-10-13 | 深圳出入境检验检疫局玩具检测技术中心 | Detection method of phthalate plasticizer |
-
2014
- 2014-08-15 CN CN201410403232.1A patent/CN104165945A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000135435A (en) * | 1998-08-26 | 2000-05-16 | Mitsubishi Chemicals Corp | Separating agent, separation of estrogen compound and estrogenic substance, and screening, adsorbing and removing of estrogenic substance |
| CN101858897A (en) * | 2010-07-05 | 2010-10-13 | 深圳出入境检验检疫局玩具检测技术中心 | Detection method of phthalate plasticizer |
Non-Patent Citations (5)
| Title |
|---|
| DR.R.G.VISSER: "《Institute for Interlaboratory Studies》", 30 April 2010 * |
| HYUN JUNG KOO ET AL.: "ESTIMATED EXPOSURE TO PHTHALATES IN COSMETICS AND RISK ASSESSMENT", 《JOURNAL OF TOXICOLOGY AND ENVIRONMENTAL HEALTH》 * |
| 刘海文 等: "塑料玩具中7 种环境雌激素含量检测", 《中国公共卫生》 * |
| 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》 * |
| 李丹 等: "溶解-沉淀-GC/MS法测定聚氯乙烯塑料中的邻苯二甲酸酯类增塑剂", 《塑料科技》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108613960A (en) * | 2018-03-27 | 2018-10-02 | 广西壮族自治区食品药品检验所 | The Raman spectra detection process of phthalic ester plasticizer |
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Application publication date: 20141126 |