CN102841066A - Method for detecting hydrazine content of substances of very high concern (SVHC) by registration, evaluation, authorization and restriction of chemicals (REACH) - Google Patents
Method for detecting hydrazine content of substances of very high concern (SVHC) by registration, evaluation, authorization and restriction of chemicals (REACH) Download PDFInfo
- Publication number
- CN102841066A CN102841066A CN2012103029271A CN201210302927A CN102841066A CN 102841066 A CN102841066 A CN 102841066A CN 2012103029271 A CN2012103029271 A CN 2012103029271A CN 201210302927 A CN201210302927 A CN 201210302927A CN 102841066 A CN102841066 A CN 102841066A
- Authority
- CN
- China
- Prior art keywords
- hydrazine
- sample
- reach
- svhc
- substances
- 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.)
- Pending
Links
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for detecting hydrazine content of substances of very high concern (SVHC) by registration, evaluation, authorization and restriction of chemicals (REACH). When a sample to be detected is frozen and ground, hydrazine in the sample is extracted out in soxhlet extraction method through carbinol,extracting solution is dissolved by water after being concentrated, and dimethylaminobenzaldehyde is added to react with the hydrazine. An ultraviolet spectrophotometer detects the hydrazine content of generated yellow materials at a position of 458 nanometers. The method for detecting hydrazine content of substances of SVHC by the REACH is quick, reliable and convenient to implement.
Description
Technical field
The present invention relates to hydrazine Determination on content method, specifically, the present invention relates to a kind of REACH and show great attention to material hydrazine Determination on content method.
Background technology
Hydrazine (NH
2NH
2), claim hydrazine again, a kind of strong polar compound.Colourless, oily liquids can mix in water-soluble, the pure isopolarity solvent well.Hydrazine is a kind of good rocket fuel, cooperate with suitable oxygenant, but ratio of components dashes the highest liquid propellant stored.Hydrazine also can be used as monopropellant, generally is used in the attitude control of satellite and guided missile.The hydrate of hydrazine is called hydrazine hydrate (N
2H
4H
2O), the oxygen scavenger of making boiler water commonly used is the raw material of plastics, rubber pange agent, is the raw material of medicine such as isoniazid, also is used for the aspects such as manufacturing of polyamide and epoxy resin.On June 20th, 2011, European chemicals management board (ECHA) will increase the material hydrazine newly and formally include showing great attention in material (SVHC) inventory that the 5th batch of need of REACH (chemicals registration, assessment, permission and restriction) license in.National standard only about the assay method of hydrazine in water and the surrounding air, does not have the assay method about hydrazine in the solid sample yet in the document at present.Therefore, be necessary to set up fast and effectively a kind of, the high method of paying close attention to material hydrazine content of the detection REACH being convenient to implement helps monitoring showing great attention to material hydrazine content, guarantees the human body health and safety.
Summary of the invention
Technical matters to be solved by this invention is, selects for use suitable solvent and method to extract the hydrazine in the sample, and extract carries out quantitative test with ultraviolet spectrophotometer after treatment.
Technical matters to be solved by this invention can be able to solve through following technical scheme:
(1) take by weighing solid sample 0.5-2g to be measured after the freezing pulverizing, carry out cable-styled extraction after adding 10-50mL methyl alcohol, extract 70 ℃-90 ℃ of temperature, extraction time is 4-6h;
(2) extract rotary evaporation in 40 ℃ of water-baths is done near, and nitrogen blows to doing then, washes in the 25mL color comparison tube with 10mL;
(3) in color comparison tube, add 10mL paradime thylaminobenzaldehyde solution, to the 25mL scale, mixing behind the placement 20min, is poured in the 1cm cuvette, measures absorbance in the 458nm wavelength with distilled water diluting.
Technique effect of the present invention is to use hydrazine fine solubility in methyl alcohol, with cable-styled extraction method the hydrazine in the sample is extracted and separates, and hydrazine and paradime thylaminobenzaldehyde effect generate yellow complex, utilize the ultraviolet spectrophotometer quantitative test.The method that the present invention provides a kind of rapid and reliable, has been convenient to implement for hydrazine Determination on content in the solid sample.
Embodiment
The present invention will be described below in conjunction with specific embodiment, but the scope of the invention is not limited to this.
Embodiment 1:
Hydrazine standard stock solution (100mg/L): accurately take by weighing 0.3280g hydrazine hydrochloride (N
2H
42HCl), after the HCl solution dissolving with 1mol/L, quantitatively move in the 1000mL volumetric flask, and be diluted with water to scale mark.
Hydrazine standard solution (1.00 μ g/mL): draw 100mg/L hydrazine standard stock solution 1.00mL, move in the 100mL volumetric flask, be diluted with water to scale mark.
Paradime thylaminobenzaldehyde solution: take by weighing the 4g paradime thylaminobenzaldehyde and be dissolved in 200mL95% ethanol and the dense HCl solution of 20mL.
The drafting of typical curve: get 6 25mL color-comparison tubes, add 1.00ug/mL hydrazine standard solution 0,0.5,1.00,2.00,5.00,10.00mL respectively, add distilled water respectively to 10mL; Add 10mL paradime thylaminobenzaldehyde solution; To the 25mL scale, mixing is placed 20min with distilled water diluting; Pour cuvette into, measure absorbance in the 458nm wavelength.With the hydrazine concentration of standard solution is horizontal ordinate, and absorbance is an ordinate, and gained typical curve linear equation is Y=1.5391X+0.0002, its linearly dependent coefficient R
2=0.9996.
Show great attention to the analytical procedure of material hydrazine in the plastic sample: get an amount of sample and place freezing crusher to pulverize, mixing.Take by weighing and pulverize sample 1.0g, carry out cable-styled extraction behind the adding 25mL methyl alcohol, extracting temperature is 90 ℃, and extraction time is 6h.After extracting completion, extract is transferred to revolve and steams in the bottle, and near dried, nitrogen blows to doing then in 40 ℃ of water-bath rotary evaporations.With 10mL water extract is washed in the 25mL color comparison tube, adds 10mL paradime thylaminobenzaldehyde solution, with distilled water diluting to 25mL scale, mixing.After placing 20min, pour in the 1cm cuvette, measure absorbance in the 458nm wavelength.Find on typical curve that compound hydrazine content does not detect in corresponding this plastic sample.
Adopt the hydrazine standard substance of two variable concentrations of this plastic sample interpolation, 5 parallel sample of each concentration analysis, interpolation level, average recovery rate and coefficient of variation result of calculation are seen table 1.
Table 1 mark-on reclaims experimental result
| Mark-on concentration (μ g/mL) | Average recovery rate (%) | RSD(％) |
| 0.02 | 86.8 | 2.0 |
| 0.2 | 91.8 | 1.4 |
The recovery of method is at 85.0%-93.5%, and relative standard deviation is 1.4%-2.0%, satisfies and detects requirement.
Embodiment 2:
Present embodiment is measured showing great attention to material hydrazine content in the wood sample.
Get an amount of sample and place freezing crusher to pulverize, mixing.Take by weighing and pulverize sample 2.0g, carry out cable-styled extraction behind the adding 50mL methyl alcohol, extracting temperature is 80 ℃, and extraction time is 4h.After extract accomplishing, method of operating finds on typical curve with embodiment 1. that compound hydrazine content does not detect in corresponding this wood sample.
Obviously, those of ordinary skill in the art can measure the content that REACH shows great attention to the material hydrazine with the present invention.
The foregoing description only supplies to explain the present invention's usefulness; And be not to be limitation of the present invention; The those of ordinary skill in relevant technologies field without departing from the present invention, can also be made various variations and modification; Therefore all technical schemes that are equal to also should belong to category of the present invention, and scope of patent protection of the present invention should be limited each claim.
Claims (5)
1. a REACH shows great attention to material hydrazine Determination on content method; Comprise the steps: to pass through pretreated solid sample to be measured through organic solvent extraction; After extract concentrates; Sample after the water dissolving concentrates adds paradime thylaminobenzaldehyde and component hydrazine reaction to be measured then, carries out quantitative test with ultraviolet spectrophotometer at the 458nm place.
2. assay method according to claim 1 is characterized in that, the pretreatnlent of sample mode is freezing pulverizing, and extracting mode is cable-styled extraction.
3. cable-styled extracting mode according to claim 2 is characterized in that, described cable-styled extraction temperature is 70 ℃-90 ℃, and extraction time is 4-6h.
4. assay method according to claim 1 is characterized in that, selected organic solvent is a methyl alcohol.
5. solid sample according to claim 1 is characterized in that: said solid sample is plastics and plastic products, Rubber & Rubber Products, timber and timber-work thereof, textile and leather and fur products.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103029271A CN102841066A (en) | 2012-08-24 | 2012-08-24 | Method for detecting hydrazine content of substances of very high concern (SVHC) by registration, evaluation, authorization and restriction of chemicals (REACH) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103029271A CN102841066A (en) | 2012-08-24 | 2012-08-24 | Method for detecting hydrazine content of substances of very high concern (SVHC) by registration, evaluation, authorization and restriction of chemicals (REACH) |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102841066A true CN102841066A (en) | 2012-12-26 |
Family
ID=47368626
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012103029271A Pending CN102841066A (en) | 2012-08-24 | 2012-08-24 | Method for detecting hydrazine content of substances of very high concern (SVHC) by registration, evaluation, authorization and restriction of chemicals (REACH) |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102841066A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105784452A (en) * | 2014-12-18 | 2016-07-20 | 北京橡胶工业研究设计院 | Method for extracting and separating carbon black from vulcanized rubber |
| CN109540884A (en) * | 2018-12-29 | 2019-03-29 | 四川大学 | A method of detection hydrazine hydrate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4775633A (en) * | 1984-04-26 | 1988-10-04 | Thermedics Inc. | Detection of hydrazine compounds in gaseous samples by their conversion to nitric oxide-yielding derivatives |
| US6143890A (en) * | 1999-01-04 | 2000-11-07 | Ciba Specialty Chemicals Corporation | Naphthalenehydrazamimides and perylenehydrazamimides |
| CN102478521A (en) * | 2010-11-25 | 2012-05-30 | 北京瑞康医药技术有限公司 | Method for determining free hydrazine in medicine |
-
2012
- 2012-08-24 CN CN2012103029271A patent/CN102841066A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4775633A (en) * | 1984-04-26 | 1988-10-04 | Thermedics Inc. | Detection of hydrazine compounds in gaseous samples by their conversion to nitric oxide-yielding derivatives |
| US6143890A (en) * | 1999-01-04 | 2000-11-07 | Ciba Specialty Chemicals Corporation | Naphthalenehydrazamimides and perylenehydrazamimides |
| CN102478521A (en) * | 2010-11-25 | 2012-05-30 | 北京瑞康医药技术有限公司 | Method for determining free hydrazine in medicine |
Non-Patent Citations (1)
| Title |
|---|
| 孙宏等: "对二甲氨基苯甲醛分光光度法测定水中肼", 《环境科学》, vol. 16, no. 1, 28 February 1995 (1995-02-28), pages 74 - 77 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105784452A (en) * | 2014-12-18 | 2016-07-20 | 北京橡胶工业研究设计院 | Method for extracting and separating carbon black from vulcanized rubber |
| CN109540884A (en) * | 2018-12-29 | 2019-03-29 | 四川大学 | A method of detection hydrazine hydrate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Bi et al. | A novel naphthalimide-based probe for ultrafast, highly selective and sensitive detection of formaldehyde | |
| Ye et al. | Determination of phenols in environmental water samples by ionic liquid‐based headspace liquid‐phase microextraction coupled with high‐performance liquid chromatography | |
| CN101995400A (en) | Surface enhanced Raman spectroscopy detection method of bisphenol A | |
| Huang et al. | Cucurbit [7, 8] urils binding to gefitinib and the effect of complex formation on the solubility and dissolution rate of the drug | |
| Bai et al. | Alkyl substituted cucurbit [6] uril assisted competitive fluorescence recognition of lysine and methionine in aqueous solution | |
| CN102841066A (en) | Method for detecting hydrazine content of substances of very high concern (SVHC) by registration, evaluation, authorization and restriction of chemicals (REACH) | |
| Chen et al. | Miniaturized array gas membrane separation strategy for rapid analysis of complex samples by surface-enhanced Raman scattering | |
| CN102830194A (en) | Method for rapidly detecting residual amount of benzene-based pollutants in plastic particles | |
| CN109115898A (en) | Based on the remaining method of pesticide in eutectic solvent-inorganic salts double-aqueous phase system analysis water-like | |
| CN103191581B (en) | Method for separating/gathering trace ciprofloxacin in food | |
| CN104122218A (en) | Method for detecting heavy metals in plastics | |
| Dadfarnia et al. | Dispersive liquid-liquid microextraction-solidified floating organic drop combined with spectrophotometry for the speciation and determination of ultratrace amounts of selenium | |
| CN102323342B (en) | Detecting method of aromatic amine compound in water sample | |
| Yu et al. | Color responses of novel receptors for AcO− and a test paper for AcO− in pure aqueous solution | |
| CN103115972A (en) | Method for determining content of REACH substance of very high concern C16-18-fatty acid lead | |
| CN103472176B (en) | Detect the method for DMF residual quantity in PU leather | |
| Larsen et al. | Comparison of pressurized solvent and reflux extraction methods for the determination of perfluorooctanoic acid in polytetrafluoroethylene polymers using LC-MS-MS | |
| CN102830100A (en) | Determination method for inorganic selenium and organic selenium in food | |
| Rao et al. | Speciation of binary complexes of Pb (II) and Cd (II) with L-asparagine in dimethyl sulfoxide-water mixtures | |
| CN105806788A (en) | Rapid analysis method for concentration of cyanide in cyanide leaching solution of gold ore | |
| CN104844758A (en) | Mercury ion imprinting polymer and preparation method thereof | |
| CN105548430A (en) | Method for detecting aniline in soil | |
| Faraji et al. | Deprotonation of salicylic acid and 5-nitrosalicylic acid in aqueous solutions of ethanol | |
| CN107505316A (en) | The detection method of total formaldehyde is can extract in a kind of leather or fur | |
| CN104458967B (en) | The assay method of DBD contents in a kind of rubber chemistry peptizer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20121226 |