CN108469472A - The assay method of concentration of formaldehyde in solid waste - Google Patents
The assay method of concentration of formaldehyde in solid waste Download PDFInfo
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- CN108469472A CN108469472A CN201711379050.5A CN201711379050A CN108469472A CN 108469472 A CN108469472 A CN 108469472A CN 201711379050 A CN201711379050 A CN 201711379050A CN 108469472 A CN108469472 A CN 108469472A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
Abstract
The present invention relates to the assay methods of concentration of formaldehyde in the solid waste of offer, respectively low concentration standard working curve is drawn according to the formaldehyde derivatives standard solution that mass concentration is 5ug/L 100ug/L, high standard working curve is drawn according to the formaldehyde derivatives standard solution that mass concentration is 0.5mg/L 10mg/L, and the low concentration standard working curve drawn out and high standard working curve is linear good, the limit of detection, preci-sion and accuracy meet method requirement, are conducive to the sample test for carrying out multiregion；Reduce derivatization reagent 2, a concentration of 0.6mg/mL of 4 dinitrobenzene hydrazine solutions (DNPH), 2,4 dinitrobenzene hydrazine solutions (DNPH) belong to moderately toxic dangerous material, the usage amount of DNPH reagents is reduced, experimental cost is reduced and reduces and pollute；Derivative reaction temperature is improved to 60 DEG C, the raising of reaction temperature makes reaction rate be improved, and keeps derivative reaction more complete, and will not be had an impact to derivatization process.
Description
Technical field
The present invention relates to the technical field of the measurement of pernicious gas content in waste more particularly to a kind of solid wastes
The assay method of concentration of formaldehyde in object.
Background technology
Formaldehyde is magma poisonous substance, after people sucks high-concentration formaldehyde, it may appear that the serious stimulation of respiratory tract and oedema, eye pierce
Bitterly, it has a headache, bronchial asthma can also occur.Direct skin contact formaldehyde can cause dermatitis, color spot, necrosis, and often sucking is few
Formaldehyde is measured, the symptoms such as headache, weak, insomnia and vegetative nervous disorder is had, slow poisoning can be caused, mucous membrane hyperemia, skin occur
Skin stimulates disease, allergic dermatitis etc..Formaldehyde positions carcinogenic and causes deformed material by the World Health Organization, is generally acknowledged change
One of state reaction source, and potential strong mutagen.
The test range of linearity is not known in the existing high performance liquid chromatography for measuring solid waste content of formaldehyde, only refers to
Prepare the working curve standard items of 100ug/L；From the aspect of specification continuous mode and raising measurement accuracy, it is necessary to existing
There is method to propose to improve.
Invention content
The purpose of the present invention is to provide a kind of assay methods of concentration of formaldehyde in solid waste, to solve to be found
It is existing measurement solid waste content of formaldehyde high performance liquid chromatography in be clearly test the range of linearity the technical issues of.
First aspect of the present invention provides：The assay method of concentration of formaldehyde in a kind of solid waste, the method includes：
Sample to be tested extraction step：It weighs 25g solid samples or measures 25mL fluid samples, it is molten that 500mL extractions are added
Liquid extracts sample to be tested with the rotating speed of 30rpm rotation sample bottle 18h on shaking table, glass funnel and fiber filter paper is used in combination to filter
Extract obtains sample to be tested；
Liquid-liquid derivative reaction step：In sample to be tested, the buffer solution of 5mL PH=5 is added, then add 5.0mL matter
The 2,4-dinitrophenylhydrazine solution of a concentration of 0.6g/L is measured, mixing is capped, 1h is reacted in 60 DEG C of shaking bath devices, is taken out cold
But to room temperature, sample to be tested derivative solution is obtained；
Purifying step：Sample to be tested derivative solution is continuously extracted in separatory funnel twice, every time with dichloromethane
10mL obtains extract to be measured；Merge in extract to be measured to the bottle equipped with 5.0g anhydrous sodium sulfates, completes to wait for by shaking
Survey the drying process of extract；The concentrate of sample to be tested is obtained by distillation technique again, solvent acetonitrile is added, is settled to
5mL, as sample to be tested test fluid；
Detecting step：The detection chromatographic condition of high performance liquid chromatograph is set, and testing result is subtracted sky by sample detection
White experiment value, and compare low concentration standard working curve or high standard working curve obtains first in sample to be tested test fluid
The residual quantity concentration of aldehyde；
Calculate step：The residual quantity concentration of formaldehyde in sample is calculated according to following formula,
In formula：
CiIndicate that the residual quantity concentration of sample formaldehyde, unit are ug/kg or ug/L；
C indicates the corresponding formaldehyde of sample liquid obtained by standard working curve, unit ug/L；
ViIndicate the volume of sample to be tested test fluid, unit mL；
M (V) indicates that the quality or volume of sample, unit are g or mL；
The low concentration standard working curve is molten according to the formaldehyde derivatives standard that mass concentration is 5ug/L-100ug/L
Liquid is drawn；The high standard working curve is according to the formaldehyde derivatives mark that mass concentration is 0.5mg/L-10mg/L
Quasi- solution is drawn.
Second aspect of the present invention is further provided on the basis of first scheme：The detection chromatographic condition set as：
Chromatographic column：Diamonsil 5um C18；Mobile phase：Acetonitrile/water=70/30；Column temperature：35℃；Flow velocity：1.0mL/min；Detection
Device：UV detector, 360nm；Sampling volume：10ul.
Third aspect of the present invention is further provided on the basis of alternative plan：The low concentration standard working curve
Method for drafting with the high standard working curve is：It is vertical with peak area according to the detection chromatographic condition of setting
Coordinate, low concentration formaldehyde derivative standard solution or or the corresponding concentration of formaldehyde of high-concentration formaldehyde derivative standard solution be cross
Coordinate draws standard working curve.
Fourth aspect of the present invention is further provided on the basis of third program：The low concentration formaldehyde derivative mark
The preparation method of quasi- solution is：It is 5ug/L, 10ug/L, 20ug/L, 40ug/L, 100ug/L formaldehyde to prepare mass concentration respectively
Standard solution, and pipette respectively in the tool plug graded tube for being 10mL to capacity, the acetate buffer solution of 4mL PH=5 is added,
It adds the 2,4-dinitrophenylhydrazine solution that mass concentration is 0.6g/L and is settled to 10.0mL, be capped mixing, water is vibrated at 60 DEG C
1h is reacted in bath, taking-up is cooled to room temperature；
The preparation method of the high-concentration formaldehyde derivative standard solution is：It is 0.5mg/L to prepare mass concentration respectively,
1.0mg/L, 2.0mg/L, 4.0mg/L, 10.0mg/L formaldehyde standard solution, and pipetted respectively to the tool plug that capacity is 10mL and carved
It spends in pipe, the acetate buffer solution of 4mL PH=5 is added, add the 2,4-dinitrophenylhydrazine that mass concentration is 0.6g/L
Solution is settled to 10.0mL, is capped mixing, 1h is reacted in 60 DEG C of shaking bath devices, taking-up is cooled to room temperature.
Fifth aspect of the present invention is further provided on the basis of first scheme：The preparation method of the extraction solution
For：The sodium hydroxide solution and 5.7mL glacial acetic acid for being 4g/100mL with 64.3mL mass concentrations mix, and are settled to 1L with water and obtain
It arrives.
Sixth aspect of the present invention is further provided on the basis of first scheme：The acetate buffer solution is matched
Method processed is：1.32g sodium acetates are weighed, water dissolution is added, 0.5mL glacial acetic acids are added, 250mL are settled to water, using hydrogen-oxygen
Change sodium solution or hydrochloric acid solution adjusts PH to 5.0.
Above-mentioned technical proposal provided by the invention can reach following expected advantageous effect：
The assay method of concentration of formaldehyde in solid waste provided by the invention is respectively 5ug/L- according to mass concentration
The formaldehyde derivatives standard solution of 100ug/L draws low concentration standard working curve, is 0.5mg/L- according to mass concentration
The formaldehyde derivatives standard solution of 10mg/L draws high standard working curve, and the low concentration standard work drawn out
Curve and high standard working curve it is linear good, the limit of detection, preci-sion and accuracy meet method requirement, have
Conducive to the sample test of development multiregion；Reduce a concentration of of derivatization reagent 2,4 dinitrophenyl hydrazine solution (DNPH)
0.6mg/mL, according to the mechanism of derivative reaction, formaldehyde and DNPH reagents generate formaldehyde derivatives, derivative reaction need into
Row depend entirely on DNPH amount of reagent number, by derivatization experiment and efficient liquid phase chromatographic analysis 2,4- dinitros are determined
A concentration of 0.6mg/mL of base phenylhydrazine solution (DNPH)；2,4 dinitrophenyl hydrazine solution (DNPH) belongs to moderately toxic danger
Product reduce the usage amount of DNPH reagents, reduce experimental cost and reduce and pollute；Improve derivative reaction temperature to 60 DEG C, instead
The raising for answering temperature, makes reaction rate be improved, and keeps derivative reaction more complete, and will not be to derivatization mistake
Journey has an impact.
Description of the drawings
Fig. 1 shows low concentration standard working curve figure；
Fig. 2 shows high standard working curve diagrams.
Specific implementation mode
In the following detailed description, it is proposed that many details, in order to complete understanding of the present invention.But
It will be apparent to those skilled in the art that some details that can be in not needing these details of the invention
In the case of implement.Below the description of embodiment is used for the purpose of providing to the present invention by showing the example of the present invention
More fully understand.
Exemplary embodiments of the present invention will be described below.
This illustrative embodiment discloses a kind of assay method of concentration of formaldehyde in solid waste, and the method for reference is former
Reason is：After the extracted liquid extraction of sample, under the buffer condition of the acetate buffer solution of pH=5,2,4-dinitrophenylhydrazine is used
(DNPH) it performs the derivatization, generates formaldehyde derivatives, through solid phase extractions or solvent extraction, detached and detected with HPLC, detect institute
Wavelength is 360nm.
The instrument and equipment used required for this illustrative embodiment has：Capacity is that the tool plug graded tube of 10mL is several,
Capacity is that the beaker of 250mL is several, and capacity is respectively that the volumetric flask of 100mL, 250mL, 1000mL are several, and capacity is respectively
The micro syringe of 10ul, 20ul, 50ul, capacity are respectively 100ul, the liquid-transfering gun of 1000ul, 5mL, water bath chader and height
Effect liquid phase chromatogram instrument.
The reagent used required for this illustrative embodiment has：The formaldehyde standard solution of a concentration of 1000mg/L or
The sodium hydroxide solution of the formalin of 37%-40%, dichloromethane, acetonitrile, anhydrous sodium sulfate, 1mol/L and 5mol/L,
The hydrochloric acid solution of 1mol/L, the 2,4-dinitrophenylhydrazine solution of 0.6g/L, acetate buffer solution and extraction solution.
Wherein, specifically, the preparation method of acetate buffer solution is：1.32g sodium acetates are weighed, water dissolution is added, adds
Enter 0.5mL glacial acetic acids, 250mL is settled to water, PH to 5.0 is adjusted using sodium hydroxide solution or hydrochloric acid solution.
Extraction solution preparation method be：The sodium hydroxide solution and 5.7mL for being 4g/100mL with 64.3mL mass concentrations
Glacial acetic acid mixes, and is settled to 1L with water and obtains.
After instrument, equipment and reagent are ready, that is, implement this illustrative embodiment, including
Sample to be tested extraction step：It weighs 25g solid samples or measures 25mL fluid samples, it is molten that 500mL extractions are added
Liquid extracts sample to be tested with the rotating speed of 30rpm rotation sample bottle 18h on shaking table, glass funnel and fiber filter paper is used in combination to filter
Extract obtains sample to be tested；
Liquid-liquid derivative reaction step：In sample to be tested, the buffer solution of 5mL PH=5 is added, then add 5.0mL matter
The 2,4-dinitrophenylhydrazine solution of a concentration of 0.6g/L is measured, mixing is capped, 1h is reacted in 60 DEG C of shaking bath devices, is taken out cold
But to room temperature, sample to be tested derivative solution is obtained；
Purifying step：Sample to be tested derivative solution is continuously extracted in separatory funnel twice, every time with dichloromethane
10mL obtains extract to be measured；Merge in extract to be measured to the bottle equipped with 5.0g anhydrous sodium sulfates, completes to wait for by shaking
Survey the drying process of extract；The concentrate of sample to be tested is obtained by distillation technique again, solvent acetonitrile is added, is settled to
5mL, as sample to be tested test fluid；
Detecting step：The detection chromatographic condition of high performance liquid chromatograph is set, and testing result is subtracted sky by sample detection
White experiment value, and compare low concentration standard working curve or high standard working curve obtains first in sample to be tested test fluid
The residual quantity concentration of aldehyde；
Calculate step：The residual quantity concentration of formaldehyde in sample is calculated according to following formula,
In formula：
CiIndicate that the residual quantity concentration of sample formaldehyde, unit are ug/kg or ug/L；
C indicates the corresponding formaldehyde of sample liquid obtained by standard working curve, unit ug/L；
ViIndicate the volume of sample to be tested test fluid, unit mL；
M (V) indicates that the quality or volume of sample, unit are g or mL；
The low concentration standard working curve is molten according to the formaldehyde derivatives standard that mass concentration is 5ug/L-100ug/L
Liquid is drawn；The high standard working curve is according to the formaldehyde derivatives mark that mass concentration is 0.5mg/L-10mg/L
Quasi- solution is drawn.
Wherein, the detection chromatographic condition set in this illustrative embodiment as：Chromatographic column：Diamonsil 5um C18；
Mobile phase：Acetonitrile/water=70/30；Column temperature：35℃；Flow velocity：1.0mL/min；Detector：UV detector, 360nm；Sample introduction
Volume：10ul.
Specifically, the method for drafting of low concentration standard working curve and the high standard working curve is：According to setting
The detection chromatographic condition set, using peak area as ordinate, low concentration formaldehyde derivative standard solution or or high-concentration formaldehyde
The corresponding concentration of formaldehyde of derivative standard solution is abscissa, draws standard working curve.
Wherein, the preparation method of low concentration formaldehyde derivative standard solution is：It is 5ug/L to prepare mass concentration respectively,
10ug/L, 20ug/L, 40ug/L, 100ug/L formaldehyde standard solution, and pipetted respectively to the tool plug graded tube that capacity is 10mL
In, the acetate buffer solution of 4mL PH=5 is added, adds the 2,4-dinitrophenylhydrazine solution that mass concentration is 0.6g/L
It is settled to 10.0mL, mixing is capped, 1h is reacted in 60 DEG C of shaking bath devices, taking-up is cooled to room temperature；
The preparation method of high-concentration formaldehyde derivative standard solution is：It is 0.5mg/L to prepare mass concentration respectively,
1.0mg/L, 2.0mg/L, 4.0mg/L, 10.0mg/L formaldehyde standard solution, and pipetted respectively to the tool plug that capacity is 10mL and carved
It spends in pipe, the acetate buffer solution of 4mL PH=5 is added, add the 2,4-dinitrophenylhydrazine that mass concentration is 0.6g/L
Solution is settled to 10.0mL, is capped mixing, 1h is reacted in 60 DEG C of shaking bath devices, taking-up is cooled to room temperature.
Fig. 1 and Fig. 2 respectively illustrates the low concentration standard working curve figure and high concentration of this illustrative embodiment drafting
Standard working curve figure.
Implement example embodiment of the present invention, reaches following expected advantageous effect：
The assay method of concentration of formaldehyde in solid waste provided by the invention is respectively 5ug/L- according to mass concentration
The formaldehyde derivatives standard solution of 100ug/L draws low concentration standard working curve, is 0.5mg/L- according to mass concentration
The formaldehyde derivatives standard solution of 10mg/L draws high standard working curve, and the low concentration standard work drawn out
Curve and high standard working curve it is linear good, the limit of detection, preci-sion and accuracy meet method requirement, have
Conducive to the sample test of development multiregion；Reduce a concentration of of derivatization reagent 2,4 dinitrophenyl hydrazine solution (DNPH)
0.6mg/mL, according to the mechanism of derivative reaction, formaldehyde and DNPH reagents generate formaldehyde derivatives, derivative reaction need into
Row depend entirely on DNPH amount of reagent number, by derivatization experiment and efficient liquid phase chromatographic analysis 2,4- dinitros are determined
A concentration of 0.6mg/mL of base phenylhydrazine solution (DNPH)；2,4 dinitrophenyl hydrazine solution (DNPH) belongs to moderately toxic danger
Product reduce the usage amount of DNPH reagents, reduce experimental cost and reduce and pollute；Improve derivative reaction temperature to 60 DEG C, instead
The raising for answering temperature, makes reaction rate be improved, and keeps derivative reaction more complete, and will not be to derivatization mistake
Journey has an impact.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than limits the protection domain of invention.It is aobvious
So, described embodiment is only section Example of the present invention, rather than whole embodiments.Based on these embodiments, ability
The every other embodiment that domain those of ordinary skill is obtained without creative efforts, belongs to the present invention
Scope of the claimed.Although with reference to above-described embodiment, invention is explained in detail, those of ordinary skill in the art
Still can creative work not be made to the according to circumstances phase of the feature in various embodiments of the present invention in the absence of conflict
Other adjustment are made in mutual combination, additions and deletions, to obtain other technologies scheme of the different, essence without departing from the design of the present invention,
These technical solutions similarly belong to invention which is intended to be protected.
Claims (6)
1. the assay method of concentration of formaldehyde in a kind of solid waste, characterized in that the method includes：
Sample to be tested extraction step：It weighs 25g solid samples or measures 25mL fluid samples, 500mL is added and extracts solution, is shaking
Sample to be tested is extracted with the rotating speed of 30rpm rotation sample bottle 18h on bed, glass funnel and fiber filter paper filtrated extract is used in combination,
Obtain sample to be tested；
Liquid-liquid derivative reaction step：In sample to be tested, the buffer solution of 5mL PH=5 is added, then add 5.0mL mass dense
Degree is the 2,4-dinitrophenylhydrazine solution of 0.6g/L, is capped mixing, and 1h is reacted in 60 DEG C of shaking bath devices, and taking-up is cooled to room
Temperature obtains sample to be tested derivative solution；
Purifying step：Sample to be tested derivative solution is continuously extracted in separatory funnel twice, each 10mL is obtained with dichloromethane
To extract to be measured；Merge in extract to be measured to the bottle equipped with 5.0g anhydrous sodium sulfates, extract to be measured is completed by shaking
Drying process；The concentrate of sample to be tested is obtained by distillation technique again, solvent acetonitrile is added, 5mL is settled to, as to be measured
Sample test liquid；
Detecting step：The detection chromatographic condition of high performance liquid chromatograph is set, and testing result is subtracted blank assay by sample detection
Value, and compare low concentration standard working curve or high standard working curve obtains the residual of formaldehyde in sample to be tested test fluid
Measure concentration；
Calculate step：The residual quantity concentration of formaldehyde in sample is calculated according to following formula,
In formula：
CiIndicate that the residual quantity concentration of sample formaldehyde, unit are ug/kg or ug/L；
C indicates the corresponding formaldehyde of sample liquid obtained by standard working curve, unit ug/L；
ViIndicate the volume of sample to be tested test fluid, unit mL；
M (V) indicates that the quality or volume of sample, unit are g or mL；
The low concentration standard working curve is drawn according to the formaldehyde derivatives standard solution that mass concentration is 5ug/L-100ug/L
It forms；The high standard working curve is painted according to the formaldehyde derivatives standard solution that mass concentration is 0.5mg/L-10mg/L
It makes.
2. the assay method of concentration of formaldehyde in solid waste as described in claim 1, characterized in that the detection of setting
Chromatographic condition is：Chromatographic column：Diamonsil 5um C18；Mobile phase：Acetonitrile/water=70/30；Column temperature：35℃；Flow velocity：
1.0mL/min；Detector：UV detector, 360nm；Sampling volume：10ul.
3. the assay method of concentration of formaldehyde in solid waste as claimed in claim 2, characterized in that the low concentration standard
The method for drafting of working curve and the high standard working curve is：According to the detection chromatographic condition of setting, with peak
Area is ordinate, low concentration formaldehyde derivative standard solution or or the corresponding formaldehyde of high-concentration formaldehyde derivative standard solution it is dense
Degree is abscissa, draws standard working curve.
4. the assay method of concentration of formaldehyde in solid waste as claimed in claim 3, characterized in that the low concentration formaldehyde
The preparation method of derivative standard solution is：Respectively prepare mass concentration be 5ug/L, 10ug/L, 20ug/L, 40ug/L,
100ug/L formaldehyde standard solution, and pipette respectively in the tool plug graded tube for being 10mL to capacity, the acetic acid of 4mL PH=5 is added
Salt buffer solution adds the 2,4-dinitrophenylhydrazine solution that mass concentration is 0.6g/L and is settled to 10.0mL, is capped mixing,
1h is reacted in 60 DEG C of shaking bath devices, taking-up is cooled to room temperature；
The preparation method of the high-concentration formaldehyde derivative standard solution is：It is 0.5mg/L, 1.0mg/ to prepare mass concentration respectively
L, 2.0mg/L, 4.0mg/L, 10.0mg/L formaldehyde standard solution, and pipette respectively in the tool plug graded tube for being 10mL to capacity,
The acetate buffer solution of 4mL PH=5 is added, adds the 2,4-dinitrophenylhydrazine solution constant volume that mass concentration is 0.6g/L
To 10.0mL, it is capped mixing, 1h is reacted in 60 DEG C of shaking bath devices, taking-up is cooled to room temperature.
5. the assay method of concentration of formaldehyde in solid waste as described in claim 1, characterized in that the extraction solution
Preparation method is：The sodium hydroxide solution and 5.7mL glacial acetic acid for being 4g/100mL with 64.3mL mass concentrations mix, with water constant volume
It is obtained to 1L.
6. the assay method of concentration of formaldehyde in solid waste as described in claim 1, characterized in that the acetate salt buffer
The preparation method of solution is：1.32g sodium acetates are weighed, water dissolution is added, 0.5mL glacial acetic acids are added, 250mL is settled to water,
PH to 5.0 is adjusted using sodium hydroxide solution or hydrochloric acid solution.
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| CN111693632A (en) * | 2020-07-24 | 2020-09-22 | 上海市食品药品检验所 | Method for extracting total formaldehyde in cosmetics and rapid detection method |
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