CN102608047A - Method for measuring trace content of iron in 1, 4-butanediol - Google Patents
Method for measuring trace content of iron in 1, 4-butanediol Download PDFInfo
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- CN102608047A CN102608047A CN2012100820849A CN201210082084A CN102608047A CN 102608047 A CN102608047 A CN 102608047A CN 2012100820849 A CN2012100820849 A CN 2012100820849A CN 201210082084 A CN201210082084 A CN 201210082084A CN 102608047 A CN102608047 A CN 102608047A
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Abstract
The invention discloses a method for measuring trace content of iron in 1, 4-butanediol, which comprises the following steps of: preparing iron standard solution, drawing a standard curve, measuring a sample and labeling a recovery test. In measuring the sample, a 1, 4-butanediol sample is firstly processed, i.e. a certain quantity of samples to be dried are evaporated to be dry, and dissolved through a small amount of hydrochloric acid solution, and then are transferred to a volumetric flask, and the pH (Potential Of Hydrogen) value is adjusted. The pH value is adjusted to be 2, the interference of Ca2+, Mg2+, Al3+, Zn2+ and other ions can be eliminated, and the interference of heavy metal ion can be eliminated. Through the analytical method, the trace content of the iron in the 1, 4-butanediol can be detected, an instrument used by the analytical method is simple, an analysis result is reliable, and the analytical method is more economical.
Description
Technical field
The present invention relates to a kind of determination of trace element method field, particularly, relate to a kind of 1, trace iron content assaying method in the 4-butylene glycol.
Background technology
1, the 4-butylene glycol is a kind of important organic and fine chemical material, is widely used in fields such as medicine, chemical industry, weaving, papermaking, automobile and daily-use chemical industry; 1, the downstream product that the 4-butylene glycol can be used for making has tetrahydrofuran, polybutylene terephthalate, γ-butyrolactone; Fields such as polyurethane slurry, and 1, the trace iron in the 4-butylene glycol might impact making downstream product; Domestic present analysis 1, the bibliographical information of trace iron has seldom set up 1 in the case in the 4-butylene glycol; Trace iron analysis on Content method in the 4-butylene glycol, downstream are produced the user has certain reference value.
Summary of the invention
The objective of the invention is to, propose a kind of 1, trace iron content assaying method in the 4-butylene glycol; With the basis that is determined as of 4.5 iron contents among the GB9009-1998, sample is carried out early stage handle, with 1; 10-phenanthroline spectrophotometry 1, trace iron content in the 4-butylene glycol.
Be to realize above-mentioned purpose, the technical scheme that the present invention adopts is: a kind of 1, trace iron content assaying method in the 4-butylene glycol comprises:
1, the principle of method
With ascorbic acid ferric iron in the test solution is reduced into ferrous iron, in pH 2～9 o'clock, ferrous ion can generate orange red complex compound with phenanthroline, measures its absorbance in spectrophotometer maximum absorption wavelength 510nm place.
2, instrument
2.1 common laboratory instrument;
2.2 spectrophotometer.
3, reagent and solution
3.1 hydrochloric acid: 6mol/L or 3mol/L;
3.2 hydrochloric acid: 1+10;
3.3 ammoniacal liquor: 10% or 2.5%;
3.4 sulfuric acid;
3.5 acetate-sodium acetate buffer solution: pH=4.5;
Take by weighing anhydrous sodium acetate 16.4g, water-soluble, add the 8.4mL glacial acetic acid, be diluted with water to 100mL;
3.6 ascorbic acid: 20g/L solution, this solution term of life is 10 days;
3.7 phenanthroline: 2g/L solution, this solution should keep in Dark Place, and only can use colourless solution.
4, preliminary work
4.1 iron standard solution:
With the basis that is determined as of 4.5 iron contents among the GB9009-1998, the preparation iron-holder is 0.200g/L iron standard solution and 0.010g/L iron standard solution;
4.1.1 1mL contains 0.200mg iron
Take by weighing 0.863g ammonium ferric sulfate (NH
4Fe (SO
4)
212H
2O), be accurate to 0.001g, place the 200mL beaker, add 100mL water, 10mL sulfuric acid is all transferred in the 500mL volumetric flask after the dissolving, is diluted with water to scale, shakes up;
4.1.2 1mL contains 0.020mg iron
Pipette the iron standard solution of 50.0mL step 4.1.1 preparation, place the 500mL volumetric flask, be diluted to scale, shake up;
4.2 the drafting of typical curve:
With 1,10-phenanthroline AAS drawing standard curve;
Draw 0,0.5,1.0,2.0,3.0,4.0 respectively, the iron standard solution of 5.0mL step 4.1.2 preparation is in the 100mL volumetric flask; Add water to about 60mL; Use the hydrochloric acid solution adjustment pH of step 3.1 preparation to be 1.8-2.2, check pH, add the ascorbic acid solution of 2.5mL step 3.6 preparation, the acetate-sodium acetate buffer solution of 10mL step 3.5 preparation, the phenanthroline solution of 5mL step 3.7 preparation with accurate pH test paper; Be diluted with water to scale, shake up;
In spectrophotometer 510nm wavelength, use the 5cm cuvette, be that reference is measured its absorbance with the blank reagent solution.With the absorbance is ordinate, and iron ion content is a horizontal ordinate, drawing standard curve, A=-0.0091+1.0250*C, correlation coefficient r=0.9998.Fe
2+Concentration range is 0～1.0, mgL
-1Meet Beer law in the scope, detect and be limited to 0.01mgL
-1
5, measure
With 1,4-butylene glycol sample heats, is evaporated to dried, and cooling adds dissolve with hydrochloric acid solution and carries out constant volume; Adjustment pH is 1.8-2.2; Be settled to scale after adding buffer solution, reductive agent and developer mixing, shake up;
Directly with hydrochloric acid solution, adjustment pH is 1.8-2.2, adds to be settled to scale after buffer solution, reductive agent and developer mix, and shakes up, as blank reagent solution;
Measure the absorbance of sample, calculate the massfraction of iron content.
6, the result calculates
C:1, the mass concentration of the iron content in the 4-butylene glycol sample, unit is mg/L;
M:1, the quality of 4-butylene glycol sample, unit is g.
The row of making even is measured the iron ion content of two results' arithmetic mean as sample.
7, mark-on recovery test
Add a certain amount of iron standard solution in the sample after processing and measure, it is measured the recovery that measured value that the result deducts sample obtains adding the iron standard solution.
Beneficial effect of the present invention is following:
Provided by the invention a kind of 1, trace iron content assaying method in the 4-butylene glycol is directly drawn the 50mL sample and is measured among the GB9009-1998, sample is not carried out any processing.And 1, the 4-butylene glycol is a kind of colourless oil liquid, the direct sample dilute with water is measured it; 1,4-butylene glycol meeting interference measurement therefore at first will be to 1; 4-butylene glycol sample is handled; Specifically be through quantity of sample is evaporated to do after, with a spot of dissolve with hydrochloric acid solution and be transferred to volumetric flask, adjusting pH value.The pH value is adjusted to 2, can eliminates Ca
2+, Mg
2+, Al
3+, Zn
2+Isoionic interference can be got rid of the interference of heavy metal ion.Add then and be settled to scale after buffer solution, reductive agent and developer mix.Reference solution does not add sample as blank solution to add the reagent of same quantity.On spectrophotometer, survey its absorbance with cuvette with certain wavelength, thus the trace iron content in the calculation sample.Can detect 1 through this analytical approach, trace iron content in the 4-butylene glycol, the used instrument of this analytical approach is simple, and analysis result is reliable, is a kind of comparatively economic analytical approach.
Through accompanying drawing and embodiment, technical scheme of the present invention is done further detailed description below.
Description of drawings
Fig. 1 is 1, in the 4-butylene glycol in the trace iron content assaying method with 1,10-phenanthroline AAS drawing standard curve synoptic diagram.
Embodiment
Below in conjunction with accompanying drawing the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein only is used for explanation and explains the present invention, and be not used in qualification the present invention.
According to the embodiment of the invention, provide a kind of 1, trace iron content assaying method in the 4-butylene glycol.Present embodiment comprises:
1, the principle of method
With ascorbic acid ferric iron in the test solution is reduced into ferrous iron, in pH 2～9 o'clock, ferrous ion can generate orange red complex compound with phenanthroline, measures its absorbance in spectrophotometer maximum absorption wavelength 510nm place.
2, instrument
2.1 common laboratory instrument;
2.2 spectrophotometer.
3, reagent and solution
3.1 hydrochloric acid: 6mol/L;
3.2 hydrochloric acid: 1+10;
3.3 ammoniacal liquor: 10%;
3.4 sulfuric acid;
3.5 acetate-sodium acetate buffer solution: pH=4.5;
Take by weighing anhydrous sodium acetate 16.4g, water-soluble, add the 8.4mL glacial acetic acid, be diluted with water to 100mL;
3.6 ascorbic acid: 20g/L solution, this solution term of life is 10 days;
3.7 phenanthroline: 2g/L solution, this solution should keep in Dark Place, and only can use colourless solution.
4, preliminary work
4.1 iron standard solution:
4.1.1 1mL contains 0.200mg iron
Take by weighing 0.863g ammonium ferric sulfate (NH
4Fe (SO
4)
212H
2O), be accurate to 0.001g, place the 200mL beaker, add 100mL water, 10mL sulfuric acid is all transferred in the 500mL volumetric flask after the dissolving, is diluted with water to scale, shakes up;
4.1.2 1mL contains 0.020mg iron
Pipette the iron standard solution of 50.0mL step 4.1.1 preparation, place the 500mL volumetric flask, be diluted to scale, shake up;
4.2 the drafting of typical curve:
Draw 0,0.5,1.0,2.0,3.0,4.0 respectively, the iron standard solution of 5.0mL step 4.1.2 preparation is in the 100mL volumetric flask; Add water to about 60mL; Using the hydrochloric acid solution adjustment pH of step 3.1 preparation is 2, checks pH with accurate pH test paper, adds the ascorbic acid solution of 2.5mL step 3.6 preparation, the acetate-sodium acetate buffer solution of 10mL step 3.5 preparation, the phenanthroline solution of 5mL step 3.7 preparation; Be diluted with water to scale, shake up;
In spectrophotometer 510nm wavelength, use the 5cm cuvette, be that reference is measured its absorbance with the blank reagent solution.With the absorbance is ordinate, and iron ion content is a horizontal ordinate, drawing standard curve, A=-0.0091+1.0250*C, correlation coefficient r=0.9998.Fe
2+Concentration range is 0～1.0, mgL
-1Meet Beer law in the scope, detect and be limited to 0.01mgL
-1, like Fig. 1.
5, measure
Take by weighing 10g1; 4-butylene glycol sample places the 100mL beaker, on electric boiling plate, slowly be evaporated to dried, the cooling; Add the dissolve with hydrochloric acid solution of 2.5mL step 3.2 preparation and be transferred in the 100mL volumetric flask, dissolve with the gradation of 60mL distilled water afterwards and be transferred in the volumetric flask.Using the hydrochloric acid solution of step 3.1 preparation or the ammoniacal liquor adjustment pH of step 3.3 preparation is 2, checks pH with accurate pH test paper.Add the ascorbic acid solution of 2.5mL step 3.6 preparation, the acetate-sodium acetate buffer solution of 10mL step 3.5 preparation, the phenanthroline solution of 5mL step 3.7 preparation, be diluted with water to scale, shake up;
Same step, the reagent of same quantity does not add sample as blank reagent solution;
In spectrophotometer 510nm wavelength, use the 5cm cuvette, with the blank reagent solution reference, measure the absorbance of sample.
6, the result calculates:
C:1, the mass concentration of the iron content in the 4-butylene glycol sample, unit is mg/L;
M:1, the quality of 4-butylene glycol sample, unit is g.
The row of making even is measured the iron ion content of two results' arithmetic mean as sample.
7,1, the mensuration of iron content in the 4-butylene glycol sample:
8, mark-on recovery test
Directly draw the 50mL sample among the GB9009-1998 and measure, sample is not carried out any processing.And 1, the 4-butylene glycol is a kind of colourless oil liquid, the direct sample dilute with water is measured it; 1,4-butylene glycol meeting interference measurement, so the present invention at first will be to 1; 4-butylene glycol sample is handled; Specifically be through quantity of sample is evaporated to do after, with a spot of dissolve with hydrochloric acid solution and be transferred to volumetric flask, adjusting pH value.The pH value is adjusted to 2, can eliminates Ca
2+, Mg
2+, Al
3+, Zn
2+Isoionic interference can be got rid of the interference of heavy metal ion.Add then and be settled to scale after buffer solution, reductive agent and developer mix.Reference solution does not add sample as blank solution to add the reagent of same quantity.On spectrophotometer, survey its absorbance with cuvette with certain wavelength, thus the trace iron content in the calculation sample.Can detect 1 through this analytical approach, trace iron content in the 4-butylene glycol, the used instrument of this analytical approach is simple, and analysis result is reliable, is a kind of comparatively economic analytical approach.
What should explain at last is: the above is merely the preferred embodiments of the present invention; Be not limited to the present invention; Although the present invention has been carried out detailed explanation with reference to previous embodiment; For a person skilled in the art, it still can be made amendment to the technical scheme that aforementioned each embodiment put down in writing, and perhaps part technical characterictic wherein is equal to replacement.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. one kind 1, the trace iron content assaying method is characterized in that in the 4-butylene glycol, comprising:
A iron standard solution preparation;
The drafting of B typical curve;
C measures sample
With 1,4-butylene glycol sample heats, is evaporated to dried, and cooling adds dissolve with hydrochloric acid solution and carries out constant volume; Adjustment pH is 1.8-2.2; Be settled to scale after adding buffer solution, reductive agent and developer mixing, shake up;
Directly with hydrochloric acid solution, adjustment pH is 1.8-2.2, adds to be settled to scale after buffer solution, reductive agent and developer mix, and shakes up, as blank reagent solution;
Measure the absorbance of sample, calculate the massfraction of iron content.
2. one kind 1, the trace iron content assaying method is characterized in that in the 4-butylene glycol, and the computing formula of the massfraction of described iron content is:
c-1, the mass concentration of the iron content in the 4-butylene glycol sample, the mg/L of unit;
The row of making even is measured the iron ion content of two results' arithmetic mean as sample.
3. one kind 1, the trace iron content assaying method is characterized in that in the 4-butylene glycol, described acetate-sodium acetate buffer solution: take by weighing anhydrous sodium acetate 16.4g, and water-soluble, add the 8.4mL glacial acetic acid, be diluted with water to 100mL, pH is 4.5.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102866124A (en) * | 2012-09-14 | 2013-01-09 | 天津力神电池股份有限公司 | Method for testing Fe<3+> content of lithium iron phosphate |
| CN105891129A (en) * | 2014-12-08 | 2016-08-24 | 江南大学 | Method for testing total amount of carotenoid in shell nacre layer |
| CN111007027A (en) * | 2019-12-31 | 2020-04-14 | 濮阳宏业环保新材料股份有限公司 | Method for measuring iron content in thiourea dioxide |
| CN112782261A (en) * | 2020-12-28 | 2021-05-11 | 新疆美克化工股份有限公司 | 1, 4-butanediol base number analysis method |
| CN113418930A (en) * | 2021-06-04 | 2021-09-21 | 西北工业大学 | Method for rapidly detecting whether surface coating of iron plate is complete |
Citations (2)
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| US4238197A (en) * | 1979-04-12 | 1980-12-09 | The United States Of America As Represented By The Secretary Of The Air Force | Analysis of lubricating oils for iron content |
| CN101233405A (en) * | 2005-05-24 | 2008-07-30 | 德士古发展公司 | Method and test kit for the determination or iron content of in-use lubricants |
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2012
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4238197A (en) * | 1979-04-12 | 1980-12-09 | The United States Of America As Represented By The Secretary Of The Air Force | Analysis of lubricating oils for iron content |
| CN101233405A (en) * | 2005-05-24 | 2008-07-30 | 德士古发展公司 | Method and test kit for the determination or iron content of in-use lubricants |
Non-Patent Citations (2)
| Title |
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| 化学工业部天津化工研究院: "《中华人民共和国国家标准 GB3049-86》", 18 April 1986, article "GB3049-86 化工产品中铁含量测定的通用方法邻菲啰啉分光光度法", pages: 3-6 * |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102866124A (en) * | 2012-09-14 | 2013-01-09 | 天津力神电池股份有限公司 | Method for testing Fe<3+> content of lithium iron phosphate |
| CN105891129A (en) * | 2014-12-08 | 2016-08-24 | 江南大学 | Method for testing total amount of carotenoid in shell nacre layer |
| CN105891129B (en) * | 2014-12-08 | 2018-11-30 | 江南大学 | The measuring method of carotenoid total amount in a kind of shell pearl layer |
| CN111007027A (en) * | 2019-12-31 | 2020-04-14 | 濮阳宏业环保新材料股份有限公司 | Method for measuring iron content in thiourea dioxide |
| CN112782261A (en) * | 2020-12-28 | 2021-05-11 | 新疆美克化工股份有限公司 | 1, 4-butanediol base number analysis method |
| CN113418930A (en) * | 2021-06-04 | 2021-09-21 | 西北工业大学 | Method for rapidly detecting whether surface coating of iron plate is complete |
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Application publication date: 20120725 |