CN108801954B - Method for measuring content of iron ions in organic silicon product - Google Patents
Method for measuring content of iron ions in organic silicon product Download PDFInfo
- Publication number
- CN108801954B CN108801954B CN201810688800.5A CN201810688800A CN108801954B CN 108801954 B CN108801954 B CN 108801954B CN 201810688800 A CN201810688800 A CN 201810688800A CN 108801954 B CN108801954 B CN 108801954B
- Authority
- CN
- China
- Prior art keywords
- sample
- organic silicon
- solution
- iron ions
- iron
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for measuring the content of iron ions in an organic silicon product, which comprises the steps of comparing an iron standard curve, pretreating an organic silicon sample, adding an o-phenanthroline solution, and calculating the concentration of the iron ions in the sample according to the absorption coefficient of a spectrophotometer. The invention utilizes the ultrasonic cleaning principle to ensure that a sample, deionized water, an acidic substance and an oxidant can be fully mixed and reacted without causing solution emulsification; in an acidic environment, hydrogen peroxide is used as an oxidant, so that the structure of the main organosilicon product is not affected, but impurities in the organosilicon product can be effectively oxidized to form ions which are dissolved in water, and the accuracy of a detection result is ensured; the method is simple and convenient, does not need a long-time organic substance digestion process, has high detection precision, and avoids expensive ICP detection.
Description
Technical Field
The invention belongs to the technical field of organic silicon production, and particularly relates to a method for measuring the total iron content in an organic silicon product.
Background
The organic silicon product has both inorganic material and organic performance, has the basic properties of low surface tension, small viscosity-temperature coefficient and the like, has the excellent characteristics of high and low temperature resistance, electrical insulation, oxidation resistance stability and the like, and is widely applied to the industries of aerospace, electronics, electricity, buildings and the like. The organic silicon products are various in types, more than ten thousand products are obtained according to incomplete statistics, and more than 90 percent of the products are synthesized by taking methylchlorosilane hydrolysate as a raw material. In the industrial production process, due to the corrosion of equipment, the quality of raw materials and auxiliary materials and the like, the content of impurities in the methyl chlorosilane hydrolysate is high, the product quality is greatly influenced, particularly, iron impurities directly influence the apparent color of the product, and further influence the application range of the product.
At present, no national standard or industrial standard for detecting iron substances in methylchlorosilane hydrolysate exists at home and abroad, and the common detection method cannot accurately detect the iron substances because the methylchlorosilane hydrolysate has the characteristics of low total iron content (generally lower than 2ppm), high organic matter content, stable physicochemical property, difficult biochemical degradation and the like.
In view of the above, the present invention provides a method for rapidly and effectively detecting the total iron content in methylchlorosilane hydrolysate.
Disclosure of Invention
The invention aims to provide a method for measuring the total iron content in methylchlorosilane hydrolysate.
The present invention achieves the above objects by the following methods.
A method for measuring the total iron content in methylchlorosilane hydrolysate comprises the following steps:
(1) sample pretreatment: placing a detection sample, water, acid and hydrogen peroxide in a high-pressure reaction kettle, releasing pressure after ultrasonic oscillation (the ultrasonic oscillation treatment temperature is 40-90 ℃ and the time is 30-90 min), standing for layering, and detecting the lower-layer liquid;
the silicone products tested were siloxane related liquid products including but not limited to a mixture of one or more of a hydrolysate, a hydroxy silicone oil, and DMC.
The volume ratio of the sample to the deionized water to the acid to the hydrogen peroxide is 1: 0.5-10: 0.01-0.1: 0.1-1.
Further preferably, the volume ratio of the sample, the deionized water, the acid and the hydrogen peroxide is 1: 0.7: 0.02: 0.28.
the acid includes but is not limited to nitric acid and hydrochloric acid.
(2) Determination of iron standard curve: taking Fe2+Adding a hydroxylamine hydrochloride solution, an o-phenanthroline solution and an acetic acid-sodium acetate buffer solution into a colorimetric tube, adding water to dilute to a scale, standing for 8-15min, measuring the absorbance at 510nm, and taking a reagent blank as a reference;
specifically, 0.001mg/ml of Fe is taken respectively2+0, 5, 10, 15, 20 and 25ml of standard solution is respectively and sequentially added into 6 colorimetric tubes of 50ml, 1ml of hydroxylamine hydrochloride solution with the mass fraction of 10%, 2ml of o-diazepine solution with the mass fraction of 0.15% and 5ml of acetic acid-sodium acetate buffer solution are added into the colorimetric tubes, water is added into the colorimetric tubes to be diluted to a scale, the colorimetric tubes are uniformly shaken and placed for 10min, a 1cm cuvette is used on a spectrophotometer, a reagent blank is used as a reference, the absorbance of each solution is measured at 510nm, the iron content is used as a horizontal coordinate, the absorbance is used as a vertical coordinate, and a standard curve is drawn.
(3) And (3) determination of a sample: putting the sample obtained in the step (1) into a colorimetric tube, adding a hydroxylamine hydrochloride solution, an o-phenanthroline solution and an acetic acid-sodium acetate buffer solution, adding water to dilute to a scale, fully shaking up, standing for 8-15min, measuring absorbance at 510nm, and calculating the iron ion content of the organic silicon product according to the following formula: x is nm/V; in the formula: x is the content of iron ions in the organic silicon product, mg/L; m is the mass of iron ions corresponding to the measured absorbance, found from the standard curve, in mg; v is the volume of the water sample, ml; and n is the dilution multiple.
Taking 10ml of the (1) treated water sample, putting the water sample into a 20ml colorimetric tube, respectively and sequentially adding 1ml of 10% hydroxylamine hydrochloride solution, 2ml of 0.15% o-phenanthroline solution and 5ml of acetic acid-sodium acetate buffer solution, adding water to dilute to a scale, and fully shaking up. After standing for 10min, absorbance was measured at 510nm on a spectrophotometer using a 1cm cuvette with a reagent blank as a reference.
The invention has the following beneficial effects:
(1) by utilizing the ultrasonic cleaning principle, the sample, the deionized water, the acidic substance and the oxidant can be fully mixed and reacted, the emulsification phenomenon can not be generated, and the subsequent standing and layering are facilitated.
(2) The acidic substance is adopted to react with the hydrogen peroxide, the structure of the main product of the organic silicon (a compound consisting of Si-O chain links and containing no iron element) is not influenced, but the oxidation performance of the hydrogen peroxide can be improved, other impurities (possibly containing iron substances) in the organic silicon product can be effectively oxidized, and ionic Fe is formed under the action of the acidic substance3+And the detection reagent is dissolved in deionized water to ensure the accuracy of the detection result.
(3) The method is simple, avoids long-time digestion process of organic substances, has high detection precision, and avoids expensive ICP detection.
Drawings
FIG. 1 is a graph of the standard iron ion in example 1.
FIG. 2 is a graph of the standard iron ion curve of example 2.
FIG. 3 is a graph of the standard iron ion curve of example 3.
Detailed Description
Example 1
(1) Sample pretreatment: weighing 100ml of hydrolysate (specificallyProducts of hydrolysis of dimethyldichlorosilane including HO- [ Si (CH)3)2]nLinear siloxanes such as-OH and [ -O-Si (CH)3)2-]nCyclic siloxane), 70ml deionized water, 2ml nitric acid and 28ml hydrogen peroxide are placed in a high-pressure storage tank made of steel lining tetrafluoro material, and then placed in an ultrasonic cleaning machine to be oscillated and mixed at 90 ℃ for 40 min; after pressure relief, placing the mixture into a separating funnel for standing and layering; and (3) transferring 50ml of lower-layer liquid into a 100ml volumetric flask, metering the volume by using deionized water, shaking up, standing, sucking 50ml of upper-layer clear liquid by using a pipette when the solution is clarified, and using the pipette for next detection while making a sample blank.
(2) Determination of iron standard curve: respectively taking 0.001mg/ml of Fe 2+0, 5, 10, 15, 20 and 25ml of standard solution is put into a colorimetric tube of 6 50ml, 1ml of 10 percent hydroxylamine hydrochloride solution, 2ml of 0.15 percent phenanthroline solution and 5ml of acetic acid-sodium acetate buffer solution are respectively added in turn, water is added for dilution to the scale, and the mixture is fully shaken up. After standing for 10min, on a spectrophotometer, a 1cm cuvette was used, a reagent blank was used as a reference, the absorbance of each solution was measured at 510nm, and a standard curve was drawn with the iron content as abscissa and the absorbance as ordinate.
(3) And (3) determination of a sample: taking 10ml of the water sample treated by the method (1) to a 20ml colorimetric tube, respectively and sequentially adding 1ml of 10% hydroxylamine hydrochloride solution, 2ml of 0.15% o-phenanthroline solution and 5ml of acetic acid-sodium acetate buffer solution, adding water to dilute to the scale, and fully shaking up. After standing for 10min, absorbance was measured at 510nm on a spectrophotometer using a 1cm cuvette with a reagent blank as a reference, and the measurement results were as follows:
the water sample is subjected to 6 times of standard adding experiments, the standard adding concentration is 0.1mg/L, and the detection result is as follows:
through calculation, the total iron content of the hydrolysate is 1.80mg/L, the standard adding recovery rate is 99.0%, the RSD is 1.41%, the standard adding recovery rate and the precision are good, and the detection requirement is met.
Example 2
(1) Sample pretreatment: weighing 100ml of hydroxyl silicone oil, 80ml of deionized water, 2ml of nitric acid and 18ml of hydrogen peroxide, placing the materials in a high-pressure storage tank made of a steel lining PTFE material, and then placing the materials in an ultrasonic cleaning machine to be oscillated and mixed for 80min at 40 ℃; after pressure relief, placing the mixture into a separating funnel for standing and layering; and (3) transferring 50ml of lower-layer liquid into a 100ml volumetric flask, metering the volume by using deionized water, shaking up, standing, sucking 50ml of upper-layer clear liquid by using a pipette when the solution is clarified, and using the pipette for next detection while making a sample blank.
(2) Determination of iron standard curve: respectively taking 0.001mg/ml of Fe 2+0, 5, 10, 15, 20 and 25ml of standard solution is put into a colorimetric tube of 6 50ml, 1ml of 10 percent hydroxylamine hydrochloride solution, 2ml of 0.15 percent phenanthroline solution and 5ml of acetic acid-sodium acetate buffer solution are respectively added in turn, water is added for dilution to the scale, and the mixture is fully shaken up. After standing for 10min, on a spectrophotometer, a 1cm cuvette was used, a reagent blank was used as a reference, the absorbance of each solution was measured at 510nm, and a standard curve was drawn with the iron content as abscissa and the absorbance as ordinate.
(3) And (3) determination of a sample: taking 10ml of the water sample treated by the method (1) to a 20ml colorimetric tube, respectively and sequentially adding 1ml of 10% hydroxylamine hydrochloride solution, 2ml of 0.15% o-phenanthroline solution and 5ml of acetic acid-sodium acetate buffer solution, adding water to dilute to the scale, and fully shaking up. After standing for 10min, absorbance was measured at 510nm on a spectrophotometer using a 1cm cuvette with a reagent blank as a reference, and the measurement results were as follows:
the water sample is subjected to 6 times of standard adding experiments, the standard adding concentration is 0.05mg/L, and the detection result is as follows:
through calculation, the total content of iron in the hydroxyl silicone oil is 0.96mg/L, the standard addition recovery rate is 99.3%, the RSD is 1.63%, the standard addition recovery rate and the precision are good, and the detection requirement is met.
Example 3
(1) Sample pretreatment: weighing 100ml of DMC, 70ml of deionized water, 3ml of nitric acid and 27ml of hydrogen peroxide, placing the DMC in a high-pressure storage tank made of a steel lining PTFE material, and then placing the high-pressure storage tank in an ultrasonic cleaning machine to perform oscillation mixing for 60min at 65 ℃; after pressure relief, placing the mixture into a separating funnel for standing and layering; and (3) transferring 50ml of lower-layer liquid into a 100ml volumetric flask, metering the volume by using deionized water, shaking up, standing, sucking 50ml of upper-layer clear liquid by using a pipette when the solution is clarified, and using the pipette for next detection while making a sample blank.
(2) Determination of iron standard curve: respectively taking 0.001mg/ml of Fe 2+0, 5, 10, 15, 20 and 25ml of standard solution is put into a colorimetric tube of 6 50ml, 1ml of 10 percent hydroxylamine hydrochloride solution, 2ml of 0.15 percent phenanthroline solution and 5ml of acetic acid-sodium acetate buffer solution are respectively added in turn, water is added for dilution to the scale, and the mixture is fully shaken up. After standing for 10min, on a spectrophotometer, a 1cm cuvette was used, a reagent blank was used as a reference, the absorbance of each solution was measured at 510nm, and a standard curve was drawn with the iron content as abscissa and the absorbance as ordinate.
(3) And (3) determination of a sample: taking 10ml of the water sample treated by the method (1) to a 20ml colorimetric tube, respectively and sequentially adding 1ml of 10% hydroxylamine hydrochloride solution, 2ml of 0.15% o-phenanthroline solution and 5ml of acetic acid-sodium acetate buffer solution, adding water to dilute to the scale, and fully shaking up. After standing for 10min, absorbance was measured at 510nm on a spectrophotometer using a 1cm cuvette with a reagent blank as a reference, and the measurement results were as follows:
the water sample is subjected to 6 times of standard adding experiments, the standard adding concentration is 0.04mg/L, and the detection result is as follows:
through calculation, the total amount of iron contained in DMC is 0.56mg/L, the standard recovery rate is 98.8%, the RSD is 2.62%, the standard recovery rate and the precision are good, and the detection requirement is met.
Claims (3)
1. A method for measuring the content of iron ions in an organic silicon product is characterized by comprising the following steps: the method comprises the following steps:
(1) sample pretreatment: placing a detection sample, deionized water, acid and hydrogen peroxide in a high-pressure reaction kettle, releasing pressure after ultrasonic oscillation, standing and layering, detecting lower-layer liquid, wherein the detected organic silicon product is a liquid product of siloxane and comprises one or more of hydrolysate, hydroxyl silicone oil and DMC, and the volume ratio of the sample, the deionized water, the acid and hydrogen peroxide is 1: 0.5-10: 0.01-0.1: 0.1-1, and treating by ultrasonic oscillation at 40-90 ℃ for 30-90 min;
(2) determination of iron standard curve: taking Fe2+Adding a hydroxylamine hydrochloride solution, an o-phenanthroline solution and an acetic acid-sodium acetate buffer solution into a colorimetric tube, adding water to dilute to a scale, standing for 8-15min, measuring the absorbance at 510nm, and taking a reagent blank as a reference;
(3) and (3) determination of a sample: putting the sample obtained in the step (1) into a colorimetric tube, adding a hydroxylamine hydrochloride solution, an o-phenanthroline solution and an acetic acid-sodium acetate buffer solution, adding water to dilute to a scale, fully shaking up, standing for 8-15min, measuring absorbance at 510nm, and calculating the iron ion content of the organic silicon product according to the following formula: x = nm/V; in the formula: x is the content of iron ions in the organic silicon product, mg/L; m is the mass of iron ions corresponding to the measured absorbance, found from the standard curve, in mg; v is the volume of the water sample, ml; and n is the dilution multiple.
2. The method for measuring the content of iron ions in an organosilicon product according to claim 1, wherein: in the step (1), the volume ratio of the sample, the deionized water, the acid and the hydrogen peroxide is 1: 0.7: 0.02: 0.28.
3. the method for measuring the content of iron ions in an organosilicon product according to claim 1, wherein: the acid comprises nitric acid or hydrochloric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810688800.5A CN108801954B (en) | 2018-06-28 | 2018-06-28 | Method for measuring content of iron ions in organic silicon product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810688800.5A CN108801954B (en) | 2018-06-28 | 2018-06-28 | Method for measuring content of iron ions in organic silicon product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108801954A CN108801954A (en) | 2018-11-13 |
| CN108801954B true CN108801954B (en) | 2021-05-14 |
Family
ID=64072230
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810688800.5A Active CN108801954B (en) | 2018-06-28 | 2018-06-28 | Method for measuring content of iron ions in organic silicon product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108801954B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110455732B (en) * | 2019-08-28 | 2021-09-28 | 吉林大学 | Biological sample treatment method, ferrous ion or total ferric ion determination method of biological sample and detection kit |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103555951A (en) * | 2013-10-23 | 2014-02-05 | 泸州北方化学工业有限公司 | Method for extracting copper from organic silicon scrap |
| CN107512809A (en) * | 2016-06-17 | 2017-12-26 | 上海善泽环保科技有限公司 | A kind of method of organic silicon wastewater processing |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3301662B2 (en) * | 1993-11-30 | 2002-07-15 | ホーヤ株式会社 | Coating layer removing agent, method of recovering substrate, and method of manufacturing article having coating layer |
| CN105061490B (en) * | 2015-08-19 | 2017-10-27 | 湖北兴瑞化工有限公司 | A kind of method for reducing impurity content in organosilicon DMC |
| CN105293807A (en) * | 2015-11-18 | 2016-02-03 | 武汉致衡环境安全工程技术有限公司 | Organosilicone waste water purifying processing system and method thereof |
| CN107118822A (en) * | 2016-05-10 | 2017-09-01 | 南京工业大学 | The method that organic-silicon-modified fatty acid ester prepares silicon substrate Biolubrication oil base oil |
-
2018
- 2018-06-28 CN CN201810688800.5A patent/CN108801954B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103555951A (en) * | 2013-10-23 | 2014-02-05 | 泸州北方化学工业有限公司 | Method for extracting copper from organic silicon scrap |
| CN107512809A (en) * | 2016-06-17 | 2017-12-26 | 上海善泽环保科技有限公司 | A kind of method of organic silicon wastewater processing |
Non-Patent Citations (2)
| Title |
|---|
| 有机硅废触体的综合利用;冯亮 等;《化工新型材料》;20141231;第42卷(第12期);第226-228，237页 * |
| 铁碳微电解-Fenton氧化联合预处理有机硅生产废水的试验研究;沈松;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20131215(第12期);第35-36页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108801954A (en) | 2018-11-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105606590A (en) | Method for simultaneously determining contents of various elements in soil or deposits | |
| CN108801954B (en) | Method for measuring content of iron ions in organic silicon product | |
| CN112730591B (en) | Sampling and testing method for measuring content of trace impurity elements in high-purity germanium tetrafluoride | |
| CN109187395A (en) | The measuring method of total phosphorus content in a kind of detergent | |
| CN101059442A (en) | Method for determining minim arsenic of aluminium ingot | |
| CN110836888A (en) | Method for determining metal impurities in organic silicon product | |
| CN111965180A (en) | Quantitative detection method for alkyl nitrate in diesel oil | |
| CN111551668A (en) | Method for measuring acid value content in perfluoropolyether | |
| CN105712393A (en) | Method for preparing zinc-oxide/simple-substance-carbon core-shell structure | |
| Cui et al. | γ-mercaptopropyltrimethoxysilane coated stir bar sorptive extraction combined with inductively coupled plasma mass spectrometry for the determination of copper, cadmium, and mercury in environmental water samples | |
| Ji‐Yan et al. | Headspace solid‐phase microextraction of butyltin species in sediments and their gas chromatographic determination | |
| CN109187384B (en) | Mercury enrichment material in water sample and headspace mercury enrichment and measurement method | |
| CN104764633B (en) | Chemical sample preparation method for testing heavy metal content in soil and sewage | |
| CN106596457B (en) | Method for simultaneously detecting content of vinyl and silicon-hydrogen functional groups in sample | |
| CN105668674A (en) | Device and method for lowering content of COD and ammonia nitrogen in wastewater through negative pressure blowoff | |
| CN110320196A (en) | A kind of highly sensitive method for detecting inorganic mercury and organic mercury | |
| Koh et al. | Spectrophotometric determination of copper (II) by formation of dicyanocuprate (I) and solvent extraction with methylene blue | |
| Fujimura et al. | Flow Injection Spectrophotometric Determination of Sub-mg dm− 3 Silver (I) in a Strongly Acidic Solution Containing Concentrated Copper (II) Using a Pyridylazo Reagent | |
| CN112730281B (en) | Method for detecting iron content in 1, 2-benzisothiazolin-3-one | |
| CN115684461A (en) | Method for determining COD (chemical oxygen demand) in water by rapid digestion-volumetric method | |
| Khoshnood et al. | Sensitive and Selective Potentiometric Sensor Based on Carbon Paste Electrode for Determining Cerium (III) Ions in Soil and Water Samples; Simplex Lattice Mixture Design Application | |
| Abdukayum et al. | A Highly Sensitive Optical Chemical Sensor Based on Organically Modified Silicate Film for Trace Amounts of Nitrite | |
| CN114199664A (en) | Digestion method of methyl silicone oil and determination method of content of impurity nitrogen in methyl silicone oil | |
| SU1680958A1 (en) | Compound for oil well water inflow stopping | |
| CN2840020Y (en) | Nickel colorimetric estimation cylinder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210623 Address after: 443711 Pingyikou Industrial Park, Xiakou Town, Xingshan County, Yichang City, Hubei Province Patentee after: YICHANG COLLIN SILICON MATERIAL Co.,Ltd. Address before: 443007 No. 66-2 Ting Ting Road, Ting Ting District, Yichang, Hubei Patentee before: HUBEI XINGRUI SILICON MATERIAL Co.,Ltd. |
|
| TR01 | Transfer of patent right |