CN104977268B - The detection method of Residual acrylamide monomer in a kind of PAMC - Google Patents

The detection method of Residual acrylamide monomer in a kind of PAMC Download PDF

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CN104977268B
CN104977268B CN201510466292.2A CN201510466292A CN104977268B CN 104977268 B CN104977268 B CN 104977268B CN 201510466292 A CN201510466292 A CN 201510466292A CN 104977268 B CN104977268 B CN 104977268B
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acrylamide
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pamc
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CN104977268A (en
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杨青波
靳琳琳
马国林
金丰富
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Zhejiang Youlian Chemical Industry Co Ltd
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Abstract

The detection method of Residual acrylamide monomer in a kind of PAMC, the Laemmli sample that cationic degree is 5~70% is configured to the mixture that concentration is 0.01~0.15g/mL with extractant, utilize ultrasonic wave extraction Residual acrylamide monomer, by the supernatant liquid filtering of extract solution, dilution, in surveying its absorbance on ultraviolet specrophotometer, with reference to acrylamide standard curve, the content of Residual acrylamide in PAMC is calculated.The present invention being extracted and being detected to Residual acrylamide monomer in the water treatment agent polyacrylamide of different cationic degrees, the colloid of formation is flexible, extract solution is clarified, extraction to Residual acrylamide monomer is completely, quickly, content detection is accurate, required equipment is simple, energy-conservation, simple and convenient extraction, it is time-consuming it is short, recovery rate is high, meet the requirement that different mud and sewage industries detect to Residual acrylamide monomer in different cationic degree polyacrylamides.

Description

The detection method of Residual acrylamide monomer in a kind of PAMC
Technical field
The invention belongs to Residual acrylamide content of monomer detection field, and in particular in a kind of PAMC The detection method of Residual acrylamide monomer.
Background technology
Higher and higher want is proposed to water quality with the raising of human living standard, people with the development of science and technology Ask, this has naturally also just promoted the rapid development of water technology science.Utilize polyacrylamide (PAM) processing waste water existing six More than ten years history, water treatment flocculant polyacrylamide include PAMC, PAMA, nonionic Polyacrylamide and amphion polyacrylamide.In recent years because wastewater source becomes increasingly complex, intractability is increasing, and Cationic-type polyacrylamide has many advantages, such as high stability, good water solubility, therefore, its (fine oil that receives much concern Work, 2004,6:54~57), it has also become the main flow flocculant in modern water treatment applications.
In daily life, human body is more and extensive with cationic-type polyacrylamide route of exposure, and frequency is higher, cation Polyacrylamide itself is nontoxic, and the acrylamide monomer wherein remained has toxicity, due to acrylamide enter human body with Afterwards, human body can be caused to be poisoned, even result in gene mutation in human body cell (Biol Reprod, 2005,72:157~163), draw Play the most attention that countries in the world are detected to Residual acrylamide in water body.
Monomeric acrylamide mass fraction standard is in China's regulation acrylamide polymer:High-class product:0.02%~ 0.04%;Primes:0.05%~0.09%;Certified products:0.10%~0.20%.Some developed countries of foreign countries at present, it is such as beautiful The states such as state, Britain, France, Japan are respectively less than 0.05% to the regulation of acrylamide quality.
The height of PAMC (CPAM) ion degree determines its sewage disposal process adapted to.With people Growth in the living standard, the product of production is more and more diversified and the diversity of sewage composition make it that the difficulty of Treatment of Sludge is more next Higher, therefore, different according to the property of mud and sewage, quick detection goes out to best suit poly- the third of the different cationic degrees of practical application The analysis method of Residual acrylamide monomer is most important in acrylamide, increasingly attracts attention.
The polyacrylamide of low cationic degree is selected for the relatively single sanitary sewage of composition, for complicated component, turbid The higher industrial wastewater of degree and sludge are from the higher polyacrylamide of cationic degree.Due to the polyacrylamide of highly cationic Amine needs to introduce the quaternary ammonium salt cationic of high content, and this allows for conjunction of the polyacrylamide than low cationic degree of highly cationic It is also higher into complex process difficulty, price.
At present, more research is to be directed to Residual acrylamide in the polyacrylamide that cationic degree is 30~40%, and The not yet systematic analysis of measure to the polyacrylamide residual monomer of other different cationic degree scopes.
The pre-treatment of Chinese patent CN 102590121A cationic Laemmli samples is to soak 24h in a solvent Obtain, pretreatment time is longer;The volume ratio of extract is adjusted when being determined with ultraviolet specrophotometer repeatedly, step is more It is cumbersome;The method extraction Residual acrylamide monomer of Chinese patent CN 103439447A ultrasonic extractions, although the method shortens The time of sample pre-treatments, still, this method are the detections for anion or non-ionic polyacrylamide residual monomer, cloudy Ion or non-ionic polyacrylamide are dissolved in water, are formed by the extremely strong acrylamide of hydrophily and acrylates copolymerization, insoluble In organic solvent, therefore, the extraction of anion or non-ionic polyacrylamide residual monomer can select for a post what organic solvent and water Miscible to be extracted, and PAMC introduces cation quaternary ammonium salt hydrophobic grouping, being dissolved in it some has Solvent, the extraction process that this allows for PAMC are more much more complex than anion or nonionic polyacrylamide.
The content of the invention
It is right it is an object of the invention to provide a kind of detection method of Residual acrylamide monomer in PAMC For Residual acrylamide monomer (AM) in the polyacrylamide (CPAM) of the different cationic degrees of water treatment agent extract And detect, the colloid of formation is flexible, extract solution clarification, and the extraction to Residual acrylamide monomer completely, quickly, examine by content It is accurate to survey, and required equipment is simple, energy-conservation, simple and convenient extraction, it is time-consuming it is short, recovery rate is high, meet different mud and sewage industries The requirement detected to Residual acrylamide monomer in different cationic degree polyacrylamides.
To achieve these goals, technical scheme provided by the invention is as follows:
The detection method of Residual acrylamide content of monomer, comprises the following steps in a kind of PAMC:
1) PAMC mixture is prepared
It is 0.01~0.15g/mL that the Laemmli sample that cationic degree is 5~70% is configured into concentration with extractant Mixture;Described extractant is the mixed solvent of organic solvent and water, wherein, the volume ratio of organic solvent and water for 66~ 95:34~5;
2) the Residual acrylamide monomer in PAMC is extracted
The power for adjusting ultrasonic cleaner is 50~200W, and extraction time is 20~60min, obtains extract solution;
3) acrylamide standard liquid is prepared
Prepare the acrylamide standard liquid of 2~20mg/L series concentrations;
4) acrylamide standard curve is drawn
By the acrylamide standard liquid described in step 3) in surveying its absorbance on ultraviolet specrophotometer, with acrylamide Concentration is abscissa, and absorbance is ordinate, draws acrylamide standard curve;
5) Residual acrylamide content of monomer in extract solution is determined
Take the supernatant of the extract solution of step 2), filtering, dilution, in surveying its absorbance on ultraviolet specrophotometer, according to The acrylamide standard curve of step 4) reads the concentration of acrylamide, is calculated according still further to formula I in PAMC The content of Residual acrylamide;
In formula:
c:The concentration of acrylamide in extract solution, unit mg/L;
m:PAMC sample quality, unit g;
V:Extracting liquid volume, unit mL;
n:Extension rate.
Further, it is described when the mixture for the PAMC that cationic degree is 5~70% is prepared in step 1) Organic solvent is selected from ethanol, acetonitrile, isopropanol, ethylene glycol, diethylene glycol, propane diols, glycerine, tetrahydrofuran and dioxane At least one of.
Preferably, it is organic when the mixture for the PAMC that cationic degree is 5~10% is prepared in step 1) The volume ratio of solvent and water is 66~70:34~30;The cation polypropylene that cationic degree is 10~20% is prepared in step 1) During the mixture of acid amides, the volume ratio of the organic solvent and water is 71~80:29~20;It is 20~40% to prepare cationic degree Polyacrylamide mixture when, the volume ratio of organic solvent and water is 81~90:19~10;Prepare cationic degree be 40~ During the mixture of 70% polyacrylamide, the volume ratio of organic solvent and water is 91~95:9~5.
Preferably, it is residual using ultrasonic cleaner extraction in step 2) when the cationic degree of polyacrylamide is 5~10% The extraction time for staying acrylamide monomer is 50~60min;When the cationic degree of polyacrylamide is 10~20%, in step 2) Extraction time using ultrasonic cleaner extraction Residual acrylamide monomer is 40~50min;The cation of polyacrylamide Spend for 20~40% when, in step 2) using the extraction time of ultrasonic cleaner extraction Residual acrylamide monomer for 30~ 40min;When the cationic degree of polyacrylamide is 40~70%, ultrasonic cleaner extraction residual propylene acyl is utilized in step 2) The extraction time of amine monomers is 20~30min.
In the present invention, by Laemmli sample and the organic solvent and the mixed solvent of water that cationic degree is 5~70% Be configured to concentration be 0.01~0.15g/mL mixture, make the solution absorbance in this concentration range in standard curve and its Concentration is linear, is easy to calculate.
Because acrylamide monomer is dissolved in water, insoluble in most of organic solvents, and PAMC can not only Be dissolved in water, can also be dissolved in the segment polarity organic solvent such as methanol, ether, acetone, the present invention according to PAMC with The deliquescent difference of acrylamide, extractant is made with the mixed solvent of organic solvent and water, is dissolved in PAMC Water, swelling disperse wherein undissolved Residual acrylamide, Residual acrylamide is dissolved in organic solvent, recycle ultrasonic wave Cavitation effect increase polyacrylamide and extractant contact area, improve acrylamide be transferred to from polyacrylamide it is organic Mass transfer rate in solvent, extracts acrylamide.
PAMC dissolves in the segment polarity organic solvent such as methanol, ether, acetone, during extraction, causes glue Body is sticky, and extraction is difficult, and acetone has absorbance to interfere measure in selected survey given wavelength, PAMC Though insoluble in the non-polar solven such as benzene,toluene,xylene, it has ultraviolet interference, therefore, the present invention using ethanol, acetonitrile, Isopropanol, ethylene glycol, diethylene glycol, propane diols, glycerine, tetrahydrofuran or dioxane gather as organic solvent to cation Acrylamide is extracted, and these solvents can be miscible with water, and is neither dissolved again without ultraviolet by PAMC Interference, extraction effect are preferable.
PAMC is dissolved in water, because its intramolecular contains quaternary ammonium salt hydrophobic grouping, it is dissolved in part Organic solvent, although the solubility of the polyacrylamide of different cationic degrees in organic solvent slightly has difference, with cation The increase of degree, the content of hydrophobic grouping base ammonium salt also gradually increase, the solubility of PAMC in organic solvent Also increase therewith, still, solubility of the PAMC in water is still far longer than solubility in organic solvent, So with the increase of cationic degree, it is swelled polymer, the ratio of extractant reclaimed water diminishes, the ratio of organic solvent Example increase.
Present invention selection ethanol, acetonitrile, isopropanol, ethylene glycol, diethylene glycol, propane diols, glycerine, tetrahydrofuran and two At least one of ring of oxygen six be used as extractant as organic solvent is miscible with water, is 5 to cationic degree using ultrasonic extraction Residual acrylamide monomer in~70% polyacrylamide is extracted, and solubility is moderate, and colloid is flexible, extract solution Clarification, Residual acrylamide monomer are fully extracted out, and extraction effect is preferable, recycle spectrophotometric determination content, should Assay method is without ultraviolet interference.
Meanwhile present system analyze the choosing of optimal extraction time to the polyacrylamide of different cationic degrees Select, because ultrasonic radiation power is too small, caused mechanical effect, cavitation effect and fuel factor are all insufficient to allow acrylamide molecules The quick inside for reaching extractant, rapid extraction can not be carried out, the present invention is for the polyacrylamide of different cationic degrees, contrast Analyze the difference of ultrasonic extraction power and time, there is provided the optimal extractant of different cationic degree polyacrylamides and extraction Time, there is certain reference value to sewage treatment industry, compensate for both at home and abroad to the polyacrylamide of different cationic degrees The blank of residual monomer extraction and determination.
Compared with prior art, beneficial effects of the present invention:
1) present invention have found according to PAMC and the deliquescent difference of acrylamide and best suit actual answer Extractant and its solvent when Residual acrylamide monomer determines in the polyacrylamide that cationic degree is 5~70% are matched somebody with somebody Than making the volume ratio of the organic solvent in extractant and water control 66~95:When 34~5, polyacrylamide and residual propylene The solubility of amide monomer is moderate, and colloid is flexible, and extract solution clarification, Residual acrylamide monomer is fully extracted out.
2) present invention is systematically divided using the acrylamide monomer in ultrasonic extraction technology extraction PAMC The optimum extracting method of different cationic degree polyacrylamides is analysed, the power for controlling ultrasonic cleaner is 50~200W, is carried It is 20~60min to take the time, has different extraction processes for different cationic degrees, required equipment is simple, energy-conservation, extraction side The advantages of method is easy, time-consuming short, recovery rate is high, and the extracting method with convention stir is incomparable, has to sewage treatment industry There is certain reference value.
Brief description of the drawings
Fig. 1 is the acrylamide standard curve of the embodiment of the present invention.
Fig. 2 is Residual acrylamide monomer in the PAMC of different cationic degrees in the embodiment of the present invention 2 The curve that changes with ultrasonic time of absorbance.
Embodiment
The invention will be further described with reference to embodiments.
The drafting of acrylamide standard curve
Acrylamide 0.1g is weighed in beaker, is accurate to 0.1mg, is dissolved with ethanol and uses ethanol constant volume to hold in 100mL In measuring bottle, the solution is 1000mg/L acrylamide standard liquid, and the standard of 6 series concentrations is configured to this standard liquid Solution, concentration are respectively:20mg/L, 10mg/L, 8mg/L, 6mg/L, 4mg/L, 2mg/L, filtering, are surveyed with ultraviolet specrophotometer Filtrate absorbance at 220nm, blank control is done with ethanol, parallel determination takes its absorbance values three times, and draws propylene Acid amides standard curve, as shown in figure 1, linear equation is y=0.0228x+0.07046, linearly dependent coefficient (R2) be 0.99985。
Embodiment 1
Take the PAMC sample that cationic degree is respectively 5%, 10%, 15%, 20%, 30%, 40%, 70% Each 5g of product or so, be dissolved in 50mL different volumes than ethanol and the in the mixed solvent of water extracted, as a result as shown in table 1:
Table 1
It can be seen from Table 1 that in the CPAM of 5~10% cationic degrees extractant, ethanol and water volume ratio be 0~ 65:When 100~35, because the large percentage of water makes polyacrylamide dissolubility increase in extract solution cause colloid sticky, carry Take more difficult;When ethanol and water volume ratio are 71~100:When 29~0, because the large percentage of ethanol is carrying polyacrylamide Taking in liquid dissolubility to reduce causes soft in hard outside colloid, and sample does not have a complete swelling, and Residual acrylamide monomer is not complete Extract, extraction loss is big, only when ethanol and water volume ratio are 66~70:When 34~30,5~10% cationic degrees CPAM solubility is moderate so that colloid is flexible, and extract solution clarification, Residual acrylamide monomer is fully extracted out, extracts Effect is preferable.Similarly, the ethanol in the extractant of the cationic degree of other scopes and water also have optimal ratio.
To sum up, the CPAM of the cationic degree of the present embodiment 5%~10% optimum extraction agent is ethanol and water volume ratio is 66 ~70:34~30, the CPAM of 10%~20% cationic degree optimum extraction agent are ethanol and water volume ratio is 71~80:29~ 20, the CPAM of 20%~40% cationic degree optimum extraction agent are ethanol and water volume ratio is 81~90:19~10,40%~ The CPAM of 70% cationic degree optimum extraction agent is ethanol and water volume ratio is 91~95:9~5.
By the above-mentioned sample solution ultrasonic cleaner ultrasonic extraction prepared with optimum extraction agent, regulation power is After 150W, ultrasonic 60min, take supernatant, filtering, 10 times of dilution, after standing 30min, surveyed at ultraviolet specrophotometer 220nm Absorbance, blank control is done with ethanol, parallel determination takes its absorbance values three times, is calculated according to following equation residual in sample Stay acrylamide content.
The mass fraction of Residual acrylamide monomer is ω, and numerical value is represented with %, is calculated as follows:
In formula:
c:The concentration of acrylamide in sample solution, unit mg/L;
m:PAMC sample quality, unit g;
V:Extracting liquid volume, unit mL;
n:Extension rate.
The content of residual monomer is as shown in table 2 in the sample measured:
Table 2
The data of table 2 illustrate that, when regulation ultrasonic cleaner ultrasonic extraction power is 150W, ultrasonic 60min, the present invention is implemented Example is extracted with optimum extraction liquid and proportioning, and the polyacrylamide of different cationic degrees can be measured with reference to ultraviolet spectrophotometry The content of residual monomer in amine.
Comparative example 1
Make extractant by organic solvent of methanol in comparative example, the above-mentioned solvent ratios with optimum extraction agent are prepared mixed Close liquid ultrasonic cleaner ultrasonic extraction, step with described in embodiment 1, with reference to the different sun of determined by ultraviolet spectrophotometry from The content of residual monomer is as shown in table 3 in the polyacrylamide of sub- degree:
Table 3
As shown in Table 3, the organic solvent that the methanol that contrast does not have UV absorption in survey given wavelength is selected as extraction, is surveyed Absorbance in the optimum extraction liquid that the absorbance of residual monomer is selected in the embodiment of the present invention 1 much smaller than it in sample, And with the increase of cationic degree, pasty state is presented in polyacrylamide in methanol is as the extract solution of organic solvent, and extraction is difficult, Therefore the content of residual monomer also can not effectively be measured.
Embodiment 2
It is respectively 5%, 10%, 15%, 20%, 30%, 40%, 70% CPAM samples 2g or so to weigh cationic degree, Corresponded to embodiment 1 cationic degree optimum extraction agent 20mL (second alcohol and water) prepare polyacrylamide Mixture, and by this 7 Individual mixture adjusts 0~50W of ultrasonic power, taken respectively after ultrasonic 60min, 90min, 120min in ultrasonic cleaner Clear liquid filtering, 10 times of dilution, after placing 30min at room temperature, its absorbance is surveyed at ultraviolet specrophotometer 220nm, is surveyed As a result it is as shown in table 4:
Table 4
Also, weigh the CPAM samples 2g left sides that cationic degree is respectively 5%, 10%, 15%, 20%, 30%, 40%, 70% The right side, the optimum extraction agent 20mL (second alcohol and water) that cationic degree is corresponded to embodiment 1 prepare polyacrylamide Mixture, and will 7 mixture ultrasonic extractions in ultrasonic cleaner, regulation 50~200W of ultrasonic power, the ultrasonic 10min, 20min of difference, Supernatant liquid filtering, 10 times of dilution are taken after 30min, 40min, 50min, 60min, 90min, after placing 30min at room temperature, in purple Its absorbance is surveyed at outer spectrophotometer 220nm, measured result is as shown in Figure 2.
The CPAM samples of different cationic degrees are can be seen that from table 4 and Fig. 1, when 0~50W of ultrasonic power is arrived in regulation, i.e., Making ultrasonic time, its residual AM absorbance is increase as time went on but increasesd slowly more than 60min, illustrates to work as ultrasonic work( Rate is smaller i.e. in 0~50W, and increase ultrasonic time is to residual AM complete extraction and unobvious in CPAM samples.
It follows that AM absorbances are remained in the CPAM samples of different cationic degrees under different ultrasonic powers with ultrasound The change of time is as shown in table 5:
Table 5
In table 5, when 50~200W of ultrasonic power is arrived in regulation, AM suctions are remained in the CPAM of 5%~10% cationic degree Luminosity constantly increases in 0~50min, and residual AM is not fully extracted out, but its absorbance is in 50~60min and above base This no longer changes, and now remains AM and is fully extracted out.Similarly, AM is remained in the CPAM of 10%~20% cationic degree to inhale Luminosity constantly increases in 0~40min, and residual AM is not fully extracted out, but its absorbance is in 40~50min and above base This no longer changes, and now remains AM and is fully extracted out;AM absorbances are remained in the CPAM of 20%~40% cationic degree Constantly increase in 0~30min, residual AM is not fully extracted out, but its absorbance in 30~40min and the above substantially not Change again, now remain AM and be fully extracted out;Remained in the CPAM of 40%~70% cationic degree AM absorbances 0~ 20min constantly increases, and residual AM is not fully extracted out, but its absorbance no longer becomes substantially in 20~30min and the above Change, now remain AM and be fully extracted out.
The present invention improves determination efficiency, selectes and remain AM's in the CPAM samples of different cationic degrees to save the time Extracting method is as follows:50~200W of ultrasonic power is adjusted, the CPAM ultrasonic times of 5~10% cationic degrees are 50~60min, The CPAM of 10~20% cationic degrees ultrasonic time is 40~50min, and the CPAM ultrasonic times of 20~40% cationic degrees are 30~40min, the CPAM ultrasonic times of 40~70% cationic degrees are 20~30min.
By the supernatant liquid filtering of the present embodiment extract solution, 10 times are diluted, after standing 30min, in ultraviolet specrophotometer Absorbance to be surveyed at 220nm, blank control is done with corresponding organic solvent, parallel determination takes its absorbance values three times, according to Following equation calculates Residual acrylamide content in sample.
The mass fraction of Residual acrylamide monomer is ω, and numerical value is represented with %, is calculated as follows:
In formula:
c:The concentration of acrylamide in extract solution, unit mg/L;
m:PAMC sample quality, unit g;
V:Extracting liquid volume, unit mL;
n:Extension rate.
The content of residual monomer is as shown in table 6 in the sample measured:
Table 6
CPAM cationic degrees Ultrasonic time (min) Sample quality (g) Absorbance Single residual content/%
5% 55 2.005 0.346 0.1206
10% 50 2.012 0.336 0.1158
15% 45 2.001 0.307 0.1037
20% 40 2.026 0.289 0.0942
30% 35 2.034 0.255 0.0809
40% 30 2.015 0.205 0.0586
70% 20 2.018 0.192 0.0528
The data of table 6 illustrate that the present embodiment is to the optimum extraction liquid and proportioning, optimal ultrasonic power and time that filter out to sun Ion degree is that the residual monomer in 5-70% polyacrylamide is determined, 2 ultrasonic 60min of contrast table data, both The absolute error of residual monomer content measure is no more than 0.03%, illustrates shortening the corresponding of different cationic degree polyacrylamides On ultrasonic time, both measurement results are equivalent.

Claims (6)

1. the detection method of Residual acrylamide monomer, comprises the following steps in a kind of PAMC:
1) PAMC mixture is prepared
It is the mixed of 0.01~0.15g/mL that the Laemmli sample that cationic degree is 5~70% is configured into concentration with extractant Compound;Described extractant is the mixed solvent of organic solvent and water, wherein, the volume ratio of organic solvent and water is 66~95: 34~5;
Wherein, when the cationic degree of polyacrylamide is 5~10%, the volume ratio of organic solvent and water is 66~70:34~30; When the cationic degree of polyacrylamide is 10~20%, the volume ratio of organic solvent and water is 71~80:29~20;Polyacrylamide When the cationic degree of amine is 20~40%, the volume ratio of organic solvent and water is 81~90:19~10;Polyacrylamide sun from When sub- degree is 40~70%, the volume ratio of organic solvent and water is 91~95:9~5;
2) the Residual acrylamide monomer in PAMC is extracted
The power for adjusting ultrasonic cleaner is 50~200W, and extraction time is 20~60min, obtains extract solution;
3) acrylamide standard liquid is prepared
Prepare the acrylamide standard liquid of 2~20mg/L series concentrations;
4) acrylamide standard curve is drawn
By the acrylamide standard liquid described in step 3) in surveying its absorbance on ultraviolet specrophotometer, with acrylamide concentration For abscissa, absorbance is ordinate, draws acrylamide standard curve;
5) Residual acrylamide content of monomer in extract solution is determined
The supernatant of the extract solution of step 2) is taken, filtering, is diluted, in surveying its absorbance on ultraviolet specrophotometer, according to step 4) acrylamide standard curve reads the concentration of acrylamide, calculates in PAMC and remains according still further to formula I The content of acrylamide;
<mrow> <mi>&amp;omega;</mi> <mo>=</mo> <mfrac> <mrow> <mi>c</mi> <mo>*</mo> <mi>V</mi> <mo>*</mo> <mi>n</mi> <mo>*</mo> <msup> <mn>10</mn> <mrow> <mo>-</mo> <mn>6</mn> </mrow> </msup> </mrow> <mi>m</mi> </mfrac> <mo>&amp;times;</mo> <mn>100</mn> <mi>%</mi> <mo>-</mo> <mo>-</mo> <mo>-</mo> <mrow> <mo>(</mo> <mi>I</mi> <mo>)</mo> </mrow> </mrow>
In formula:
c:The concentration of acrylamide in extract solution, unit mg/L;
m:PAMC sample quality, unit g;
V:Extracting liquid volume, unit mL;
n:Extension rate.
2. the detection method of Residual acrylamide monomer in PAMC according to claim 1, its feature It is, the organic solvent in the extractant is selected from ethanol, acetonitrile, isopropanol, ethylene glycol, diethylene glycol, propane diols, the third three At least one of alcohol, tetrahydrofuran and dioxane.
3. the detection method of Residual acrylamide monomer in PAMC according to claim 1 or 2, it is special Sign is, when the cationic degree of polyacrylamide is 5~10%, ultrasonic cleaner extraction residual propylene acyl is utilized in step 2) The extraction time of amine monomers is 50~60min.
4. the detection method of Residual acrylamide monomer in PAMC according to claim 1, its feature It is, when the cationic degree of polyacrylamide is 10~20%, ultrasonic cleaner extraction residual propylene acyl is utilized in step 2) The extraction time of amine monomers is 40~50min.
5. the detection method of Residual acrylamide monomer in PAMC according to claim 1, its feature It is, when the cationic degree of polyacrylamide is 20~40%, ultrasonic cleaner extraction residual propylene acyl is utilized in step 2) The extraction time of amine monomers is 30~40min.
6. the detection method of Residual acrylamide monomer in PAMC according to claim 1, its feature It is, when the cationic degree of polyacrylamide is 40~70%, ultrasonic cleaner extraction residual propylene acyl is utilized in step 2) The extraction time of amine monomers is 20~30min.
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CN110320170B (en) * 2019-07-01 2021-10-15 浙江华正新材料股份有限公司 Method for measuring content of residual MAH monomer in PP-g-MAH material
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102590121A (en) * 2011-05-05 2012-07-18 重庆大学 Method for measuring content of residue acrylamide monomer in water treatment agent cationic polyacrylamide
CN103439447A (en) * 2013-08-13 2013-12-11 安徽天润化学工业股份有限公司 Detection method for residual quantity of acrylamide in anion/non-ionic type PAM

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7399428B2 (en) * 2004-02-18 2008-07-15 Intematix Corporation Compositions comprising high light-output yellow phosphors and their methods of preparation
KR100808130B1 (en) * 2006-11-02 2008-02-29 부경대학교 산학협력단 A composition for preventing and treating acetaminophen inducing liver injury comprising the protein extracts from porphyra yezoensis

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102590121A (en) * 2011-05-05 2012-07-18 重庆大学 Method for measuring content of residue acrylamide monomer in water treatment agent cationic polyacrylamide
CN103439447A (en) * 2013-08-13 2013-12-11 安徽天润化学工业股份有限公司 Detection method for residual quantity of acrylamide in anion/non-ionic type PAM

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
聚丙烯酰胺水凝胶中丙烯酰胺单体的提取及高效液相色谱测定;李杨;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;20080315;第27页 *

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