CN104458394A - Method of improving detection sensitivity of formaldehyde with diacetone spectrophotometry - Google Patents
Method of improving detection sensitivity of formaldehyde with diacetone spectrophotometry Download PDFInfo
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- CN104458394A CN104458394A CN201410841257.XA CN201410841257A CN104458394A CN 104458394 A CN104458394 A CN 104458394A CN 201410841257 A CN201410841257 A CN 201410841257A CN 104458394 A CN104458394 A CN 104458394A
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- formaldehyde
- diacetone
- alcohol
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Abstract
The invention relates to a method of improving detection sensitivity of formaldehyde with diacetone spectrophotometry. The sensitivity of the classic diacetone spectrophotometry is improved by more than one time by utilizing n-butyl alcohol as an extraction agent. The method can be used for detecting formaldehyde in partial rice and noodle products; the adding standard recovery rate of samples ranges from 85% to 92% and the variable coefficient of the parallel determinations for five times is less than 5%.
Description
Technical field
The present invention relates to a kind of method improving the sensitivity of diacetone Photometric Determination of Formaldehyde, belong to detection field.
Background technology
Diacetone spectrophotometric method measures the ideal analytical approach of formaldehyde, all adopted, GB/T 15516, SN/T 2183 and NY/T 1283 etc. in many industry standards or national standard.Method is in the buffer system of acetic acid-ammonium acetate, and formaldehyde and diacetone, under the condition of boiling water bath, form stable 2,6-dimethyl-3,5-diacetyls-Isosorbide-5-Nitrae-dihydropyridine yellow compound, then wavelength be 413nm place measure.Little due to the whole extinction area of adopted color development system (chromophore and conjugated system thereof), belong to muting sensitivity method; Color-developing compounds is neither chelate or associated matter, and organism that neither be general, cannot adopt the extractant that this three classes system is conventional.When this method is applied to content of formaldehyde lower detected object, relative sensitivity is lower.
Summary of the invention
In order to reach the sensitivity improving diacetone Photometric Determination of Formaldehyde, the present invention, by a large amount of tests, have selected suitable alcohol organic solvent as extractant, the sensitivity of formaldehyde diacetone spectrphotometric method for measuring is doubled.
The feature of the alcohol organic solvent that method is used is, be slightly soluble in water and be insoluble in the normal butyl alcohol of water, isobutyl alcohol, sec-butyl alcohol, the tert-butyl alcohol, 1-amylalcohol, 2-amylalcohol, 3-amylalcohol, 2-methyl-1-butene alcohol, 2-methyl-2-butanols, 3-methyl-2-butanols, 3-methyl-1-butanol, 2,2-dimethyl-1-propyl alcohol, hexanol are preferably normal butyl alcohol.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, the unrestricted content of the present invention to help understanding.
The mensuration of content of formaldehyde in rice product:
1. main solution and preparation thereof
Formaldehyde standard solution: get 38% ~ 40% formalin 10mL, adds people 0.5mL sulfuric acid (1+35), is diluted to 500mL.Its concentration is demarcated by iodimetric titration.Be diluted to the standard operation liquid of 10 μ g/mL before use.
Diacetone solution (now with the current): add ammonium acetate 25g, glacial acetic acid 3mL, diacetone 0.40mL in 100mL deionized water, be stored in brown bottle after dissolving.
2. test method
The formaldehyde standard operation liquid of accurate absorption certain volume is in 25mL color-comparison tube.Add deionized water 10.00mL, diacetone 1.00mL successively, shake up.Then be placed in boiling water bath and heat 3min, take out and place cooling, add normal butyl alcohol 5mL, oscillation extraction leaves standstill completely afterwards.Draw organic layer, using 1cm cuvette, take reagent blank as reference, measures absorbance in wavelength 413nm place.
3. sample preparation
Accurately take drying, pulverizing rice product 5.0g in 250mL triangular flask, add deionized water 100mL, vibrate 30min in 80 DEG C of water bath with thermostatic control oscillators, take out and at room temperature cool rapidly with flowing water, add 40g/L NaOH 6mL, 100g/L zinc sulfate 10mL, abundant mixing, leave standstill 10min, pour into concentrator bowl, in triangular flask, supplement the distilled water of 34mL more fully vibrates with the formaldehyde more than absorption of residual, merge sample solution, to get supernatant liquor after the centrifugal 10min of 3000r/min, do blank assay simultaneously
4. the drafting of typical curve
Draw formaldehyde standard operation liquid 0.00,0.25,0.50,1.00,1.50,2.50mL is placed in 25mL color-comparison tube respectively, surveys its absorbance respectively by test method.Content of formaldehyde is within the scope of 0 ~ 5.0 μ g/mL, and absorbance and concentration of formaldehyde present good linear relationship; Extract and not extraction phase ratio, the absorbance with gained under concentration levels increases and is twice.
5. sample determination
Accurate absorption 10mL sample treatment liquid measures, and each sample determination 5 times, acquired results is in table 1.
Table 1 sample determination and parallel experiment result
6. mark-on recovery test
Each sample takes two parts (each heavy 5.0g) respectively, and a copy of it adds a certain amount of formaldehyde standard and carries out recovery test, the results are shown in Table 2.
Table 2 formaldehyde recovery test
Result shows: with this understanding, and recovery of standard addition is 85% ~ 92%.
Claims (2)
1. improve a method for diacetone Photometric Determination of Formaldehyde sensitivity, it is characterized in that, by the extraction of alcohol organic solvent, the sensitivity of method can be made to double.
2. alcohol organic solvent according to claim 1, it is characterized in that, be slightly soluble in water and be insoluble in the normal butyl alcohol of water, isobutyl alcohol, sec-butyl alcohol, the tert-butyl alcohol, 1-amylalcohol, 2-amylalcohol, 3-amylalcohol, 2-methyl-1-butene alcohol, 2-methyl-2-butanols, 3-methyl-2-butanols, 3-methyl-1-butanol, 2,2-dimethyl-1-propyl alcohol, hexanol are preferably normal butyl alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410841257.XA CN104458394A (en) | 2014-12-30 | 2014-12-30 | Method of improving detection sensitivity of formaldehyde with diacetone spectrophotometry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410841257.XA CN104458394A (en) | 2014-12-30 | 2014-12-30 | Method of improving detection sensitivity of formaldehyde with diacetone spectrophotometry |
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| CN104458394A true CN104458394A (en) | 2015-03-25 |
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| CN201410841257.XA Pending CN104458394A (en) | 2014-12-30 | 2014-12-30 | Method of improving detection sensitivity of formaldehyde with diacetone spectrophotometry |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1731156A (en) * | 2005-08-19 | 2006-02-08 | 中国检验检疫科学研究院 | Method for quick detection of formaldehyde in food |
| CN102706819A (en) * | 2012-06-11 | 2012-10-03 | 江南大学 | Acetylacetone extraction spectrophotometry method for measuring formaldehyde in food |
| CN103760123A (en) * | 2014-01-08 | 2014-04-30 | 广东省石油化工研究院 | Analytical measurement method for didecyl dimethyl ammonium chloride in seawater |
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2014
- 2014-12-30 CN CN201410841257.XA patent/CN104458394A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1731156A (en) * | 2005-08-19 | 2006-02-08 | 中国检验检疫科学研究院 | Method for quick detection of formaldehyde in food |
| CN102706819A (en) * | 2012-06-11 | 2012-10-03 | 江南大学 | Acetylacetone extraction spectrophotometry method for measuring formaldehyde in food |
| CN103760123A (en) * | 2014-01-08 | 2014-04-30 | 广东省石油化工研究院 | Analytical measurement method for didecyl dimethyl ammonium chloride in seawater |
Non-Patent Citations (1)
| Title |
|---|
| 李春建 等: "乙酰基丙酮荧光法测定水发产品浸泡液中甲醛的研究", 《现代预防医学》 * |
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Application publication date: 20150325 |