CN106932262A - The test solution preparation method of iron content in a kind of pyrrolidones of measure N methyl 2 - Google Patents
The test solution preparation method of iron content in a kind of pyrrolidones of measure N methyl 2 Download PDFInfo
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- CN106932262A CN106932262A CN201710098217.4A CN201710098217A CN106932262A CN 106932262 A CN106932262 A CN 106932262A CN 201710098217 A CN201710098217 A CN 201710098217A CN 106932262 A CN106932262 A CN 106932262A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
- G01N2001/4027—Concentrating samples by thermal techniques; Phase changes evaporation leaving a concentrated sample
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Abstract
The invention discloses a kind of test solution preparation method of iron content in pyrrolidones of measure N methyl 2, the method comprises the following steps：1) weigh the pyrrolidones sample of N methyl to be measured 2 and be positioned on heater and just occur one layer of oily residue to container bottom in 300~380 DEG C of heating evaporations；2) to step 1) in sample after the evaporation that obtains add concentrated nitric acid, heated solution is to clarifying；3) by step 2) in solution cool down backward solution in add sulfuric acid solution；4) heating stepses 3) in the solution that obtains make solution there is sulfuric acid cigarette to emerge, untill there is white liquid in container bottom；5) by step 4) in gained white liquid cooled down, dilute with water, until solution become it is limpid, obtain the test solution to be prepared.Test solution preparation method of the invention substantially shortens preparation time, and the residue in solution is fully dissolved, while avoiding introducing the material of influence follow-up test.
Description
Technical field
The present invention relates to a kind of test solution preparation method for determining iron content in higher boiling Organic chemical products, specially determine
The test solution preparation method of iron content in METHYLPYRROLIDONE.
Background technology
METHYLPYRROLIDONE (hereinafter referred to as NMP) is a kind of strong and good stability the polar solvent of selectivity, in work
The absorbent of acetylene and senior alkynes is often used as in industry.In actual production, the iron being dissolved in NMP can produce shadow to catalyst
Ring, a small amount of iron also can inactivate catalyst, therefore it is required that the iron content in NMP is more low better.
The content of the invention
Regarding to the issue above, the present invention provides a kind of test solution preparation side for determining iron content in METHYLPYRROLIDONE
Method.
According to an aspect of the present invention, there is provided a kind of test solution preparation side for determining iron content in METHYLPYRROLIDONE
Method, the method comprises the following steps：
1) NMP samples to be measured are weighed to be put into container and be positioned on heater in 300~380 DEG C of heating evaporations to appearance
Just there is one layer of oily residue, the sample after being evaporated in device bottom；
2) to step 1) in sample after the evaporation that obtains add the concentrated nitric acid to dissolve residue, heated solution is to clarifying；
3) by step 2) in solution cooling, backward solution in addition sulfuric acid solution further dissolving residual residue；
4) heating stepses 3) in the solution that obtains make solution there is sulfuric acid cigarette to emerge, until white liquid occurs in container bottom being
Only；
5) by step 4) in gained white liquid cooled down, dilute with water, until solution become it is limpid, determined
The test solution of iron content in NMP.
According to one embodiment of present invention, step 1) in METHYLPYRROLIDONE sample to be measured be commercially available N- first
Base -2-Pyrrolidone.
According to one embodiment of present invention, step 1) in heater be electric boiling plate.
According to one embodiment of present invention, step 2) in the volume of concentrated nitric acid that is added and initial sample volume ratio
It is 1:4~6.
According to one embodiment of present invention, step 3) in volume and the N- methyl -2- pyrrolidines of sulfuric acid solution that add
The ratio between ketoboidies product 1:4~6.
Testing sample solution is heated to high temperature by test solution preparation method of the invention using heater, to ensure higher boiling
Nmp solvent can rapid evaporation, shorten evaporation step used by time.After being evaporated using the mixed-acid dissolution of nitric acid and sulfuric acid
Residue, to ensure that residue fully dissolves.By in solution by way of heated solution makes it emit sulfuric acid cigarette after residue dissolving
The nitric acid of residual organic matter and excess is removed, it is to avoid be further introduced into influenceing the material of follow-up test.
Specific embodiment
It should be appreciated that embodiments of the invention shown in the exemplary embodiment are merely illustrative.Although in this hair
Only a small number of embodiments have been described in detail in bright, but those skilled in the art to be readily appreciated that and depart from the present invention in not essence
In the case of the teaching of theme, various modifications are feasible.Correspondingly, all such modifications should all be included in of the invention
In the range of.Without departing from the spirit of the invention, can be to the design of following exemplary embodiment, operating condition and ginseng
Number etc. makes others and replaces, changes, changes and delete.
Test solution preparation method of the invention is described in detail with reference to embodiment.
In the examples below, to be commercially available analysis pure for agents useful for same.
Embodiment one
(1) evaporation sample will be dried to the beaker of the 300mL of constant weight and is placed on the electronic balance that maximum magnitude is 220g, clearly
Zero.It is accurate it is parallel pipette 40.0mL commercially available METHYLPYRROLIDONEs (being denoted as NMP-1) to be measured and be put into beaker, record is moved
The quality m of the sample for taking.The beaker that will be equipped with sample is placed on electric boiling plate in 300 DEG C of heating evaporations, to remove major part
NMP, be evaporated to glass bottom just occur one layer of oily residue when untill.
(2), to adding the concentrated nitric acid of 10mL (ρ=1.4g/mL) with dissolved residue in beaker, heated solution is extremely for sour molten residue
Clarification.Solution after heating is removed and cooled down, to 8mL (9.0mol/L) sulfuric acid solution is added in the solution, beaker is reheated
In solution to there is sulfuric acid cigarette to emerge, a small amount of white liquid occurs in cup bottom, solution is removed into cooling, dilute with water, directly
Become limpid to solution, obtain determining the test solution used by iron content in METHYLPYRROLIDONE.
5 examinations are carried out by above-described embodiment one and GB/T 3049-2006 6.3,6.4 analytical procedure to sample NMP-1
Test, line blank test is entered in company with sample, result of the test see the table below 1.
Table 1
Embodiment two
(1) evaporation sample will be dried to the beaker of the 300mL of constant weight and is placed on the electronic balance that maximum magnitude is 220g,
Reset.It is accurate it is parallel pipette 50.0mL commercially available METHYLPYRROLIDONEs (being denoted as NMP-2) to be measured and be put into beaker, record institute
The quality m of the sample for pipetting.The beaker that will be equipped with sample is placed on electric boiling plate in 350 DEG C of heating evaporations, to remove major part
NMP, be evaporated to glass bottom just occur one layer of oily residue when untill.
(2), to adding the concentrated nitric acid of 10mL (ρ=1.4g/mL) with dissolved residue in beaker, heated solution is extremely for sour molten residue
Clarification.Solution after heating is removed and cooled down, to 10mL (9.0mol/L) sulfuric acid solution is added in the solution, beaker is reheated
In solution to there is sulfuric acid cigarette to emerge, a small amount of white liquid occurs in cup bottom, solution is removed into cooling, dilute with water, directly
Become limpid to solution, obtain determining the test solution used by iron content in METHYLPYRROLIDONE.
5 examinations are carried out by above-described embodiment two and GB/T 3049-2006 6.3,6.4 analytical procedure to sample NMP-2
Test, line blank test is entered in company with sample, result of the test see the table below 2.
Table 2
Embodiment three
(1) evaporation sample will be dried to the beaker of the 300mL of constant weight and is placed on the electronic balance that maximum magnitude is 220g,
Reset.It is accurate it is parallel pipette 60.0mL commercially available METHYLPYRROLIDONEs (being denoted as NMP-3) to be measured and be put into beaker, record institute
The quality m of the sample for pipetting.The beaker that will be equipped with sample is placed on electric boiling plate in 380 DEG C of heating evaporations, to remove major part
NMP, be evaporated to glass bottom just occur one layer of oily residue when untill.
(2), to adding the concentrated nitric acid of 10mL (ρ=1.4g/mL) with dissolved residue in beaker, heated solution is extremely for sour molten residue
Clarification.Solution after heating is removed and cooled down, to 12mL (9.0mol/L) sulfuric acid solution is added in the solution, beaker is reheated
In solution to there is sulfuric acid cigarette to emerge, a small amount of white liquid occurs in cup bottom.Solution is removed into cooling, dilute with water, directly
Become limpid to solution, obtain determining the test solution used by iron content in METHYLPYRROLIDONE.
In the above-described embodiments, the amount of the sulfuric acid solution of addition is determined by the amount of residual residue.Add sulfuric acid solution
It is incomplete that amount can cause residual residue to dissolve very little, and excessive concentrated nitric acid is difficult to remove；Add the amount of sulfuric acid solution too many
Can make test solution that excessive ammoniacal liquor is consumed during subsequent measurements iron content.
The test solution prepared using the method for the present invention determines the detailed process of wherein iron content with reference in GB/T3049-2006
6.3 and 6.4, determine the iron content in gained test solution.Blank test simultaneously is carried out simultaneously with sample, is provided by with the present invention
The identical step of preparation method and equal amount prepare blank solution and enter line blank test, obtain blank value.According to formulaObtain the iron content in test solution, wherein m1、m0It is the test solution and blank examination checked in from standard curve
Iron content in testing.
5 examinations are carried out by above-described embodiment three and GB/T 3049-2006 6.3,6.4 analytical procedure to sample NMP-3
Test, line blank test is entered in company with sample, result of the test see the table below 3.
Table 3
Data draw from table 1~3, the favorable reproducibility of this test method, and relative standard deviation is 3.31%~6.99%
Between, meet test requirements document.
Presently preferred embodiments of the present invention is the foregoing is only, not for limiting practical range of the invention；If do not taken off
From the spirit and scope of the present invention, the present invention is modified or equivalent, all should covered in the claims in the present invention
In the middle of protection domain.
Claims (4)
1. it is a kind of determine METHYLPYRROLIDONE in test solution used by iron content preparation method, it is characterised in that including following
Step：
1) weigh METHYLPYRROLIDONE sample to be measured and be put into container and be positioned on heater and add in 300~380 DEG C
Thermal evaporation has just occurred one layer of oily residue, the sample after being evaporated to container bottom；
2) to step 1) in sample after the evaporation that obtains add the concentrated nitric acid to dissolve residue, heated solution is to clarifying；
3) by step 2) in solution cooling, backward solution in addition sulfuric acid solution further dissolving residual residue；
4) heating stepses 3) in the solution that obtains make solution there is sulfuric acid cigarette to emerge, untill there is white liquid in container bottom；
5) by step 4) in gained white liquid cooled down, dilute with water, until solution become it is limpid, obtain determine N- first
Test solution in base -2-Pyrrolidone used by iron content.
2. the preparation method for determining test solution used by iron content in METHYLPYRROLIDONE according to claim 1, it is special
Levy and be, step 1) in heater be electric boiling plate.
3. the preparation method for determining test solution used by iron content in METHYLPYRROLIDONE according to claim 1, it is special
Levy and be, step 2) in the volume of concentrated nitric acid that is added and the volume ratio of initial sample be 1:4~6.
4. the preparation method for determining test solution used by iron content in METHYLPYRROLIDONE according to claim 1, it is special
Levy and be, step 3) in the ratio between the volume of sulfuric acid solution that adds and METHYLPYRROLIDONE volume 1:4~6.
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| CN201710098217.4A CN106932262A (en) | 2017-02-23 | 2017-02-23 | The test solution preparation method of iron content in a kind of pyrrolidones of measure N methyl 2 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112986218A (en) * | 2021-02-07 | 2021-06-18 | 天津艾克凯胜石墨烯科技有限公司 | N-methyl pyrrolidone element content detection method |
Citations (2)
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| CN101373185A (en) * | 2007-08-23 | 2009-02-25 | 佳能株式会社 | Structure, target substance detection element and target substance detection kit |
| CN101498717A (en) * | 2005-04-30 | 2009-08-05 | 艾康生物技术(杭州)有限公司 | Sample collecting device used for collecting solid or semi-solid sample |
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2017
- 2017-02-23 CN CN201710098217.4A patent/CN106932262A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101498717A (en) * | 2005-04-30 | 2009-08-05 | 艾康生物技术(杭州)有限公司 | Sample collecting device used for collecting solid or semi-solid sample |
| CN101373185A (en) * | 2007-08-23 | 2009-02-25 | 佳能株式会社 | Structure, target substance detection element and target substance detection kit |
Non-Patent Citations (3)
| Title |
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| 中华人民共和国国家质量监督检验检疫总局等: "《中华人民共和国国家标准GB/T3049-2006》", 29 December 2006 * |
| 杨惠: "N-甲基吡咯烷酮纯度检测法之我见", 《化工技术与开发》 * |
| 连小彬等: "气相色谱串联质谱法检测纺织品中1-甲基-2-吡咯烷酮", 《上海纺织科技》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112986218A (en) * | 2021-02-07 | 2021-06-18 | 天津艾克凯胜石墨烯科技有限公司 | N-methyl pyrrolidone element content detection method |
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