CN104111309B - The method for rapidly testing of iodide ion content in nylon polymer - Google Patents
The method for rapidly testing of iodide ion content in nylon polymer Download PDFInfo
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Abstract
The invention discloses the method for rapidly testing of iodide ion content in a kind of nylon polymer.First thread nylon polymer is shredded, take the nylon polymer after shredding and put into container, then add potassium nitrate solution, and supplementary high purity water stirs evenly, and obtains solution; Gained solution is put into household microwave oven together with container extract, take out after extraction, and supplementary high purity water stirs evenly, second time obtains solution, is cooled by gained solution, to be measured after cooling; Iodide ion concentration meter after correction is inserted in solution to be measured and measures, read after pending data is stable, thus measure the content of iodide ion in nylon polymer.Adopt household microwave oven to extract in technical solution of the present invention, extraction time is short, extraction efficiency is higher.Utilize the present invention to detect iodide ion content in nylon polymer, the test duration is short, test result is accurate, and reduces cost.
Description
Technical field
The present invention relates to inorganic detection technical field, particularly relate to the method for rapidly testing of iodide ion content in a kind of nylon polymer.
Background technology
At present, in polymkeric substance, the extraction method of testing of iodide ion content all adopts traditional type of heating electric hot plate heating, and this process is the process of in layer heat trnasfer, and electric hot plate transfers heat to container, container transmits feedwater again, and the iodide ion in polymkeric substance brings out by water.
And microwave abstracting utilizes the effect of electromagnetic field to make some organic components in solid or semi-solid material effectively be separated with matrix, and a kind of separation method of the script compound state of analytic target can be kept, microwave heating be directly by energy transferring to base matter, so its extraction efficiency is higher.Microwave abstracting has applied to the fields such as food analysis, drugs analysis, environmental analysis, biochemical analysis and mineral process.But, so far, and have no the application about detecting inorganic ions in nylon polymer by microwave-assisted extraction technique, more not about the bibliographical information detected by iodide ion content in microwave abstracting nylon polymer.Other technical field is carried out in microwave abstracting process, the microwave extracting apparatus that most application is special, expensive, causes production cost to improve, complex operation.And the rarer report of the application of household microwave oven in abstraction technique.
Micro-wave frequency is between 300 megahertz to 300 kilo-mega cycles per seconds, and the frequency of normal domestic use micro-wave oven is 2450 megahertzes, and in nylon polymer, effective vibration frequency of the extraction solvent water of iodide ion is also 2450 megahertzes.Therefore, household microwave oven to be effectively applied in nylon polymer in iodide ion test process by the present invention, household microwave oven effectively can act on hydrone, thus accelerate the motion of hydrone, iodide ion in polymkeric substance is brought out by hydrone, thus measures the content of iodide ion in nylon polymer.
Summary of the invention
The technical problem to be solved in the present invention is: the method for rapidly testing providing iodide ion content in a kind of nylon polymer.Adopt household microwave oven to extract in technical solution of the present invention, extraction time is short, extraction efficiency is higher.Utilize technical solution of the present invention to detect iodide ion content in nylon polymer, the test duration is short, test result is accurate.
In order to solve the problem, the technical solution used in the present invention is:
The invention provides the method for rapidly testing of iodide ion content in a kind of nylon polymer, described method of testing comprises the following steps:
A, first thread nylon polymer to be shredded, then the nylon polymer taken after shredding puts into container, then the potassium nitrate solution that mass percentage concentration is 10% is added, the proportionate relationship of nylon polymer and potassium nitrate solution addition is therebetween 1g:8 ~ 12mL, add high purity water afterwards to stir, after stirring, the quality of gained solution is 100 times of nylon polymer quality;
B, step a is stirred after solution put into micro-wave oven together with container and extract, extraction time is 15min;
C, by step b extract after the container with solution takes out, and supplement high purity water stir, after stirring, the quality of gained solution is 100 times of nylon polymer quality, then the container filling solution is carried out stirring cool, be cooled to 25 ± 3 DEG C to be measured;
D, iodide ion concentration meter to be corrected with the iodine standard solution of 10ppm and 100ppm successively, measure in solution to be measured for the iodide ion concentration meter inserting step c after correcting, read after pending data is stable, measure the content of iodide ion in nylon polymer.
According to the method for rapidly testing of iodide ion content in above-mentioned nylon polymer, in step a, nylon polymer shreds the length of rear silk is 2
~3cm.
According to the method for rapidly testing of iodide ion content in above-mentioned nylon polymer, the proportionate relationship of nylon polymer described in step a and potassium nitrate solution addition is therebetween 1g:10mL.
According to the method for rapidly testing of iodide ion content in above-mentioned nylon polymer, mass percentage concentration described in step a is the compound method of the potassium nitrate solution of 10%: take 10g and analyze pure potassium nitrate solid, dissolve with 90g high purity water, stir and obtain potassium nitrate solution, putting into reagent bottle stand-by.
According to the method for rapidly testing of iodide ion content in above-mentioned nylon polymer, micro-wave oven described in step b is family expenses Glanz MC-83105FB800W microwave oven with light wave, selects 70% firepower during micro-wave oven extraction.
According to the method for rapidly testing of iodide ion content in above-mentioned nylon polymer, the model of the meter of iodide ion concentration described in steps d is IM-20E.
According to the method for rapidly testing of iodide ion content in above-mentioned nylon polymer, the compound method of the iodine standard solution of 10ppm described in steps d is: take the commercially available iodide ion standard solution 10mL of 100ppm in the brown volumetric flask of 100mL, add 1.0g potassium nitrate solid or 10mL, mass percentage concentration is 10% potassium nitrate solution, be settled to scale mark with high purity water, shake up and get final product.
According to the method for rapidly testing of iodide ion content in above-mentioned nylon polymer, the compound method of the iodine standard solution of 100ppm described in steps d is: in the brown volumetric flask of 100mL, add 1.0g potassium nitrate solid, after dissolving with the iodide ion standard solution that a small amount of 100ppm is commercially available, the iodide ion standard solution commercially available with 100ppm is settled to scale mark, shakes up and get final product.
According to the method for rapidly testing of iodide ion content in above-mentioned nylon polymer, in nylon polymer described in steps d, the content of iodide ion is data × 100ppm that pending data stablizes rear reading.
positive beneficial effect of the present invention:
1, adopt household microwave oven to extract in technical solution of the present invention, extraction time is short, extraction efficiency is higher.Utilize technical solution of the present invention to detect iodide ion content in nylon polymer, the test duration is short, test result is accurate.
2, the present invention is by adopting the application of iodide ion in household microwave oven extraction nylon polymer, and by the 150min that extraction time is extracted by original electrical heating, foreshorten to 15min, extraction efficiency improves 90%; And by Optimum Operation step, the detection time of whole iodide ion foreshortens to 65min by original 300min, and single detection efficiency improves 78%.The detection method of the iodide ion in household microwave oven extraction nylon polymer is adopted to substantially increase detection efficiency.
3, microwave extraction method is applied in the detection of iodide ion content in nylon polymer by the present invention, substantially increases extraction efficiency, and extraction time foreshortens to 15min by original 150min, can using electricity wisely more than 3000 spend every year.
4, labour cost is saved every year:
Annual normal detection 365 times, adds survey 96 times for 2013.After shortening detection time, save labour cost 103604 yuan.Cost saving is analyzed and is referred to table 1.
.
5, current, the every platform of professional microwave abstracting equipment that microwave abstracting adopts needs about 70,000 yuan, and the every platform of household microwave oven that the present invention adopts only needs 700 yuan, the research and development of technical solution of the present invention are saved Meteorological altogether for this enterprise four laboratories and are: 4 × (70000-700)=277200 yuan.
6, " examination service in production ", when testing iodide ion content in nylon polymer owing to utilizing technical solution of the present invention, its test duration shortens greatly, can handshake result rapidly, and factory is more promptly made a response to problem.
Existing electric hot plate extraction and household microwave oven extraction of the present invention are contrasted below, thus prove to utilize the inventive method to test iodide ion content in nylon polymer, it detects accurately.Detailed process is as follows:
1), take 2 iodine standard specimens (nylon66 fiber polymkeric substance) respectively in 2 Erlenmeyer flasks, add 10mL respectively, mass percentage concentration is the potassium nitrate solution of 10%, and supplementary high purity water is 100g to gained solution total amount, obtains two parts of 100g solution, shakes up; Two Erlenmeyer flasks filling 100g solution obtained are drained into (micro-wave oven is family expenses Glanz MC-83105FB800W microwave oven with light wave) in household microwave oven, regulates firepower 70%, extraction 15min; Take out two Erlenmeyer flasks after extraction, and add high purity water respectively and stir, obtain two parts of 100g solution; Its two parts of 100g solution are poured in 150ml beaker respectively, and add stirrer put into water bath with thermostatic control stir cooling, until constant temperature is to 25 DEG C; Iodide ion concentration meter is corrected with the iodine standard solution of 10ppm and 100ppm successively, iodide ion concentration score after correcting is not inserted two parts to cool in the solution after constant temperature and detect, result is respectively 1450ppm and 1440ppm, and testing result meets standard specimen requirement (1440 ± 30) ppm.
2) same nylon66 fiber polymkeric substance is divided into 2 parts, takes 1.000g respectively in 2 Erlenmeyer flasks, and add 10mL, mass percentage concentration is the potassium nitrate solution of 10%, and supplement high purity water be 100g to gained solution total amount, obtain 100g solution, shake up; Extract by domestic microwave extraction of the present invention and traditional electrical heating plate mode respectively, surveyed continuously one month, detect data and refer to table 2.
。
Paired t-test method verification test result average is adopted to have indifference.
after testing, t < t
0
, test result average there was no significant difference is described, namely the testing result of two kinds of methods is consistent.
four, embodiment:
Set forth the present invention further below in conjunction with embodiment, but do not limit content of the present invention.
The mass percentage concentration adopted in following examples is the compound method of the potassium nitrate solution of 10%: take 10g and analyze pure potassium nitrate solid, dissolves, stir and obtain potassium nitrate solution, putting into reagent bottle stand-by with 90g high purity water.
The micro-wave oven adopted is family expenses Glanz MC-83105FB800W microwave oven with light wave, selects 70% firepower during micro-wave oven extraction.The model of iodide ion concentration meter is IM-20E.
The compound method of 10ppm iodine standard solution is: take the commercially available iodide ion standard solution 10mL of 100ppm in the brown volumetric flask of 100mL, add 1.0g potassium nitrate solid or 10mL, mass percentage concentration is 10% potassium nitrate solution, be settled to scale mark with high purity water, shake up and get final product.
The compound method of 100ppm iodine standard solution is: in the brown volumetric flask of 100mL, adds 1.0g potassium nitrate solid, and after dissolving with the iodide ion standard solution that a small amount of 100ppm is commercially available, the iodide ion standard solution commercially available with 100ppm is settled to scale mark, shakes up and get final product.
Embodiment 1:
The method for rapidly testing of iodide ion content in nylon polymer of the present invention, the detailed step of this method of testing is as follows:
A, first thread nylon66 fiber polymkeric substance is shredded that (length shredding rear silk is 2-3cm, the relative viscosity of nylon66 fiber polymkeric substance is 30), then take two parts shred after nylon66 fiber polymkeric substance 1.000g put into two Erlenmeyer flasks, then add 10mL respectively, mass percentage concentration is the potassium nitrate solution of 10%, supplement respectively afterwards and add high purity water and stir, obtain two parts of 100g solution, shake up;
B, step a is shaken up after two parts of solution put into micro-wave oven together with Erlenmeyer flask, regulate firepower 70% extract, extraction time is 15min;
C, step b is extracted after two Erlenmeyer flasks with solution takes out, and supplementary high purity water stirs, and obtains two parts of 100g solution after stirring; Its two parts of 100g solution are poured in 150mL beaker respectively, and add stirrer put into water bath with thermostatic control carry out stirring cooling, be cooled to constant temperature 25 DEG C to be measured;
D, iodide ion concentration meter to be corrected with the iodine standard solution of 10ppm and 100ppm successively, measure in two parts of solution that the other inserting step c that scored by iodide ion concentration after correction is to be measured, read after pending data is stable, the data × 100ppm of reading obtains testing result; The testing result of two parts of solution is respectively 1430ppm and 1437ppm, Parallel errors 7ppm, meet testing result ± 30ppm.
Embodiment 2:
The method for rapidly testing of iodide ion content in nylon polymer of the present invention, the detailed step of this method of testing is as follows:
A, first thread nylon66 fiber polymkeric substance is shredded that (length shredding rear silk is 2-3cm, the relative viscosity of nylon66 fiber polymkeric substance is 62), then take two parts shred after nylon66 fiber polymkeric substance 1.000g put into two Erlenmeyer flasks, then add 10mL respectively, mass percentage concentration is the potassium nitrate solution of 10%, supplement respectively afterwards and add high purity water and stir, obtain two parts of 100g solution, shake up;
B, step a is shaken up after two parts of solution put into micro-wave oven together with Erlenmeyer flask, regulate firepower 70% extract, extraction time is 15min;
C, step b is extracted after two Erlenmeyer flasks with solution takes out, and supplementary high purity water stirs, and obtains two parts of 100g solution after stirring; Its two parts of 100g solution are poured in 150mL beaker respectively, and add stirrer put into water bath with thermostatic control carry out stirring cooling, be cooled to constant temperature 25 DEG C to be measured;
D, iodide ion concentration meter to be corrected with the iodine standard solution of 10ppm and 100ppm successively, measure in two parts of solution that the other inserting step c that scored by iodide ion concentration after correction is to be measured, read after pending data is stable, the data × 100ppm of reading obtains testing result; The testing result of two parts of solution is respectively 1380ppm and 1370ppm, Parallel errors 10ppm, meet testing result ± 30ppm.
Embodiment 3:
The method for rapidly testing of iodide ion content in nylon polymer of the present invention, the detailed step of this method of testing is as follows:
A, first thread nylon66 fiber polymkeric substance is shredded that (length shredding rear silk is 2-3cm, the relative viscosity of nylon66 fiber polymkeric substance is 70), then take two parts shred after nylon66 fiber polymkeric substance 1.000g put into two Erlenmeyer flasks, then add 10mL respectively, mass percentage concentration is the potassium nitrate solution of 10%, add high purity water afterwards respectively to stir, obtain two parts of 100g solution, shake up;
B, step a is shaken up after two parts of solution put into micro-wave oven together with Erlenmeyer flask, regulate firepower 70% extract, extraction time is 15min;
C, step b is extracted after two Erlenmeyer flasks with solution takes out, and supplementary high purity water stirs, and obtains two parts of 100g solution after stirring; Its two parts of 100g solution are poured in 150mL beaker respectively, and add stirrer put into water bath with thermostatic control carry out stirring cooling, be cooled to constant temperature 25 DEG C to be measured;
D, iodide ion concentration meter to be corrected with the iodine standard solution of 10ppm and 100ppm successively, measure in two parts of solution that the other inserting step c that scored by iodide ion concentration after correction is to be measured, read after pending data is stable, the data × 100ppm of reading obtains testing result; The testing result of two parts of solution is respectively 1420ppm and 1430ppm, Parallel errors 10ppm, meet testing result ± 30ppm.
Claims (6)
1. the method for rapidly testing of iodide ion content in nylon polymer, it is characterized in that, described method of testing comprises the following steps:
A, first nylon polymer to be shredded, then the nylon polymer taken after shredding puts into container, then the potassium nitrate solution that mass percentage concentration is 10% is added, the proportionate relationship of nylon polymer and potassium nitrate solution addition is therebetween 1g:8 ~ 12mL, add high purity water afterwards to stir, after stirring, the quality of gained solution is 100 times of nylon polymer quality;
B, step a is stirred after solution put into micro-wave oven together with container and extract, extraction time is 15min;
C, by step b extract after the container with solution takes out, and supplement high purity water stir, after stirring, the quality of gained solution is 100 times of nylon polymer quality, then the container filling solution is carried out stirring cool, be cooled to 25 ± 3 DEG C to be measured;
D, iodide ion concentration meter to be corrected with the iodine standard solution of 10ppm and 100ppm successively, measure in solution to be measured for the iodide ion concentration meter inserting step c after correcting, read after pending data is stable, measure the content of iodide ion in nylon polymer, in nylon polymer, the content of iodide ion is data × 100ppm that pending data stablizes rear reading;
The compound method of described 10ppm iodine standard solution is: take the commercially available iodide ion standard solution 10mL of 100ppm in the brown volumetric flask of 100mL, add 1.0g potassium nitrate solid or 10mL, mass percentage concentration is 10% potassium nitrate solution, be settled to scale mark with high purity water, shake up and get final product;
The compound method of described 100ppm iodine standard solution is: in the brown volumetric flask of 100mL, add 1.0g potassium nitrate solid, after dissolving with the iodide ion standard solution that a small amount of 100ppm is commercially available, the iodide ion standard solution commercially available with 100ppm is settled to scale mark, shakes up and get final product.
2. the method for rapidly testing of iodide ion content in nylon polymer according to claim 1, is characterized in that: in step a, nylon polymer shreds the length of rear silk is 2 ~ 3cm.
3. the method for rapidly testing of iodide ion content in nylon polymer according to claim 1, is characterized in that: the proportionate relationship of nylon polymer described in step a and potassium nitrate solution addition is therebetween 1g:10mL.
4. the method for rapidly testing of iodide ion content in nylon polymer according to claim 1, it is characterized in that: to be the compound method of the potassium nitrate solution of 10% be mass percentage concentration described in step a: take 10g and analyze pure potassium nitrate solid, dissolve with 90g high purity water, stir and obtain potassium nitrate solution, putting into reagent bottle stand-by.
5. the method for rapidly testing of iodide ion content in nylon polymer according to claim 1, is characterized in that: micro-wave oven described in step b is family expenses Glanz MC-83105FB800W microwave oven with light wave, selects 70% firepower during micro-wave oven extraction.
6. the method for rapidly testing of iodide ion content in nylon polymer according to claim 1, is characterized in that: the model of the meter of iodide ion concentration described in steps d is IM-20E.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19507685B4 (en) * | 1995-03-04 | 2005-05-25 | Merck Patent Gmbh | Method and means for the determination of iodide |
| CN102565218A (en) * | 2011-12-22 | 2012-07-11 | 暨南大学 | Microwave test method for determining content of harmful substances in plastic package material |
| CN103018238A (en) * | 2012-12-06 | 2013-04-03 | 江南大学 | Method for measuring iodide ions quickly and efficiently |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002243717A (en) * | 2001-02-20 | 2002-08-28 | Sumitomo Metal Mining Co Ltd | Method of determining iodine in solution containing organic iodide |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19507685B4 (en) * | 1995-03-04 | 2005-05-25 | Merck Patent Gmbh | Method and means for the determination of iodide |
| CN102565218A (en) * | 2011-12-22 | 2012-07-11 | 暨南大学 | Microwave test method for determining content of harmful substances in plastic package material |
| CN103018238A (en) * | 2012-12-06 | 2013-04-03 | 江南大学 | Method for measuring iodide ions quickly and efficiently |
Non-Patent Citations (1)
| Title |
|---|
| 尼龙6高聚碘的制备及表征;王渊等;《工程塑料应用》;20140131;第42卷(第1期);第8页1.4性能测试(1)含碘量测定 * |
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