CN102520082A - Method for determining volatile components in polyvinyl alcohol in full-evaporation headspace gas chromatography - Google Patents
Method for determining volatile components in polyvinyl alcohol in full-evaporation headspace gas chromatography Download PDFInfo
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Abstract
The invention relates to a method for determining volatile components in substances like polyvinyl alcohol resin, which adopts a full-evaporation headspace gas chromatography for analyzing and includes the following steps: sealing 0.1g-0.5g polyvinyl alcohol resin in a 20ml headspace bottle, placing the bottle in a headspace sample injector, heating at temperature of 115 DEG C to 125 DEG C for 85min to 95min to lead the volatile components to be evaporated totally, adopting gas chromatography for analyzing, recording a spectrogram of the volatile components, and calculating content of the volatile components through a standard regression curve. The analysis condition is that: adopting a DB-1 type chromatographic column, adopting a flame ionization detector (FID) detector with the column temperature at 40 DEG C, the detector temperature at 200 DEG C and the sampler temperature at 150 DEG C. The method is good in data repeatability and accurate and reliable in data analysis and has the advantages of being easy and convenient to operate, fast in analysis and high in sensitivity, and the volatile components in samples are good in separation effect.
Description
Technical field
The invention belongs to the instrumental analysis field, relate to this method and measure volatile constituent Determination on content method in polyvinyl alcohol (PVA) (PVA) the resene material, specifically is the content of measuring the volatile constituent in the polyvinyl alcohol (PVA) (PVA).
Background technology
Polyvinyl alcohol (PVA) (Polyvinyl Alcohol) is a kind of macromolecular organic compound; Be to be solvent with methyl alcohol, polyvinyl acetate (PVA) got through alkali catalyzed alcoholysis, itself to human non-toxic, have no side effect; To the skin nonirritant; Have good water-solubility and biocompatibility, become the maximum water-soluble polymers of output in the world at present, be of wide application.Because solvent methanol is poisonous and hazardous material; Residual methyl alcohol influences its use in the polyvinyl alcohol (PVA), and particularly the product of outlet is strict to methanol content, sets up methanol content measuring method in the polyvinyl alcohol (PVA); Methyl alcohol is residual in the control polyvinyl alcohol (PVA), necessary concerning manufacturing enterprise.
Domestic the existing people of methanol content measuring in the polyvinyl alcohol (PVA) is carried out research, mainly contained oxidimetry, conventional vapor-phase chromatography and conventional static headspace gas chromatography three major types.Oxidimetry has higher accuracy to the methyl alcohol of high-load in the polyvinyl alcohol (PVA), but proving time is long, and energy consumption is high, and efficient is low; Conventional vapor-phase chromatography and conventional static headspace gas chromatography remolding sensitivity are higher, but need accurately to measure the partition factor of component to be measured, this often difficult realization.
Static headspace technique is to be used as headspace sample container (bottle) evaporator and to realize a kind of technology to volatile ingredient quantitative test in the sample.This technology is to be grown up by Markelov and Guzowski in 1993 at first; Be at a certain temperature sample and solvent (or object of reference) to be heated to certain degree; Original liquid in sample bottle (Gu) mutually in tested component can be counted as and almost all be transferred to gas phase; Its concentration of gas phase with its stoste (Gu) amount of tested composition in mutually becomes direct linear relationship, thereby quantitative test goes out conclusion.
But there is following defective in volatile constituent Determination on content in the polyvinyl alcohol (PVA) with static headspace gas chromatography:
1, each measurement all need add solvent or object of reference, complicated operation in sample.
2, because the adding of solvent causes certain interference to analysis, and stability is not high, repeatability is bad.
3, in the static headspace gas chromatography,, make that the work difficulty of the partition factor of component i to be measured in concentrating phase (L) and gas phase (G) is very big because the existence of solvent (perhaps object of reference) is arranged.
Summary of the invention
Deficiency to prior art; The assay method that the purpose of this invention is to provide volatile constituent in a kind of polyvinyl alcohol (PVA) (PVA) resene material; This method is passed through head-space sampler; With the mode of pervaporation, with the content of certain composition in the gas chromatography determination sample, the content of volatile constituent such as methyl alcohol in polyvinyl alcohol (PVA) (PVA) the resene material for example.
Technical scheme of the present invention is:
The invention provides the content with volatile constituent in the pervaporation Headspace Gas Chromatography polyvinyl alcohol resin class material, adopt the headspace gas chromatography instrument to analyze, concrete steps are:
Polyvinyl alcohol resin class material 0.1 gram～0.5 gram is sealed in 20 milliliters of head space bottles; Be put in the head-space sampler; Heating evaporated volatile constituent in 85 minutes～95 minutes fully under 115 ℃～125 ℃ condition; Adopt gc analysis then, write down the spectrogram of volatile constituent, calculate the content of volatile constituent again with the standard regression curve method.
According to embodiments of the invention, preferred said analytical conditions for gas chromatography is: adopt DB-1 type chromatographic column, adopt fid detector, stationary phase is the quartz capillary column of 100% dimethyl polysiloxane, and carrier gas is N
2, flow velocity 1.0mL/min, split ratio is 1: 100, H
2Flow velocity 30mL/min, air velocity 300mL/min; 40 ℃ of column temperatures, 200 ℃ of detector temperatures; 150 ℃ of injector temperature; Headspace sampling, 120 ℃ of equilibrium temperatures, equilibration time 90min, head space bottle sample size 1.0mL;
Said volatile constituent is other volatile constituents such as methyl alcohol, acetone, methyl acetate, and the appearance time of methyl alcohol is 1.771min, and the appearance time of acetone is 1.897min, and the appearance time of methyl acetate is 2.11lmin.
Do further explanation and explanation in the face of the present invention down:
The quantitative theoretical foundation of pervaporation head space chromatographic technique is following:
The gross mass m of component i to be measured in the primary sample in the system
iCan be expressed as through the mass balance of system:
m
i＝c
iG(K
iV
L+V
G)..........................................(1)
In the formula (1), V
LAnd V
GBe respectively liquid in the system (Gu) mutually or claim to concentrate the volume of phase (L) and gas phase (G); K
iBe the ratio of the concentration of component i to be measured in concentrating phase (L) and gas phase (G) in the system under the constant temperature equilibrium state, be called partition factor, K
i=c
IL/ c
IGc
ILAnd c
IGBe respectively the equilibrium concentration of component i to be measured in concentrating phase (L) and gas phase (G), be expressed as respectively: c
IL=m
IL/ V
LAnd c
IG=m
IG/ V
G, m
ILAnd m
IGBe respectively the quality of component i to be measured in concentrating phase (L) and gas phase (G) under the constant temperature equilibrium state.
Work as K
iV
L＜＜V
GThe time, formula (1) can be reduced to m
i≈ c
IGV
G=m
IG, promptly original concentrate mutually in component to be measured can be counted as and almost all be transferred to gas phase.According to chromatogram quantification ultimate principle, c
IG=f
iA
i, f
iBe the absolute correction factor of component i to be measured, A
iIt is the peak area of component i to be measured.Thereby have
m
i≈c
iGV
G＝f
iA
iV
G ..........................................(2)
Because the precision of most stratographic analysis only 5%, is therefore worked as K
iV
LDuring＜5%VG, just can application formula (2) carry out quantitatively.Because distribution constant K
iRising with temperature increases, so under the condition of very little in sample size of higher temperature, just can reach K
iV
L＜5%V
GRequirement, let volatile ingredient to be measured can fully or be similar to fully evaporation.
Take by weighing about 0.1 gram of sample～0.5 gram, be accurate to 0.1 milligram, place the head space bottle, under above-mentioned chromatographic condition, measure the record chromatogram.Methanol content in the polyvinyl alcohol (PVA) of representing with mass percent w is calculated as follows.
The characteristics of this method are to proofread and correct the influence that does not receive tested composition two phase distribution constants.Bearing calibration is simple, even the reagent of available standards is proofreaied and correct.
Compared with prior art, advantage of the present invention is:
Volatile constituent in a, the employing pervaporation Headspace Gas Chromatography polyvinyl alcohol resin; Need in sample, not add solvent and object of reference; Do not need to measure in advance component to be measured at two distribution constants in mutually, simple to operate, it is good to analyze data reappearance; Analyze data accurately and reliably, and volatile constituent good separating effect in the sample.
The sample injection method of b, this method once can heat 9 samples simultaneously, measures respectively then, can save time high efficiency.
C., the method for the volatile constituent in the employing pervaporation Headspace Gas Chromatography polyvinyl alcohol resin also extensively is suitable for the mensuration of volatile constituent in the hard resin class material.
Description of drawings
Fig. 1 is methyl alcohol concentration and peak area graph of a relation on FID among the embodiment 1;
Fig. 2 is the linear relationship chart of peak area inverse to comparing of methyl alcohol in the polyvinyl alcohol (PVA) among the embodiment 1;
Fig. 3 is an impurity pervaporation head space chromatogram in the polyvinyl alcohol (PVA) among the embodiment 1.
Embodiment
Embodiment 1:
The assay method of methyl alcohol in polyvinyl alcohol (PVA) of the present invention (PVA) the resene material
0.1 gram～0.5 gram polyvinyl alcohol (PVA) (PVA) resene material is put in the head-space sampler with 20 milliliters of head space bottle sealings; Under 120 ℃ condition, heating volatile constituents such as making methyl alcohol in 90 minutes evaporates fully; Analyze with vapor-phase chromatography; The spectrogram of volatile constituents such as record methyl alcohol is with the content of volatile constituents such as standard regression curve method calculating methyl alcohol.
1, the instrumentation condition is a gas chromatograph: Agilent 6890 gas chromatographs (Agilent Technologies); DB-1 chromatographic column (J&W Scientific, 30m * 0.45mm * 2.55 μ m, 100% dimethyl polysiloxane); DK-3001A type head-space sampler (in Beijing emerging analytical instrumentation techniques research institute); XSl05 double-range electronic analytical balance (METTLER TOLEDO); 20 milliliters of head space bottles (Agilent Technologies); Methyl alcohol, acetone, methyl acetate are chromatographically pure; Industrial-grade polyethylene alcohol (Xiangwei Co Ltd, Hunan Prov.'s product).
2, chromatographic condition
Stationary phase is the quartz capillary column (0.445mm * 30m, 2.25 μ m) of 100% dimethyl polysiloxane, and carrier gas is N
2, flow velocity 1.0mL/min, split ratio is 1: 100, H
2Flow velocity 30mL/min, air velocity 300mL/min.40 ℃ of column temperatures, 200 ℃ of detector temperatures; 150 ℃ of injector temperature; Headspace sampling, 120 ℃ of equilibrium temperatures, equilibration time 90min, head space bottle sample size 1.0mL.
3, the mensuration of linear relationship investigation and absolute correction factor
Accurately take by weighing 0 milligram of chromatographically pure methyl alcohol, 2.84 milligrams, 3.70 milligrams, 6.14 milligrams, 7.16 milligrams, 9.38 milligrams respectively, place 20mL head space bottle, by above-mentioned chromatographic condition, the sealing sample introduction, the record chromatogram, the result sees table 1.
The response measurement result of table 1 methyl alcohol on FID
| Methanol concentration, mg/ |
0 | 0.142 | 0.185 | 0.307 | 0.358 | 0.469 |
| Peak area, |
0 | 6248 | 8527 | 13373 | 17009 | 20757 |
With determinand methyl alcohol peak area is ordinate, and methanol concentration is a horizontal ordinate, carries out linear regression, sees Fig. 1.As can beappreciated from fig. 1, the related coefficient of methanol concentration and methyl alcohol peak area reaches 0.9979, explains that in given scope, methyl alcohol peak area and methanol concentration are good linear relationship, and obtains the absolute response value s of methyl alcohol on FID
iBe 44003 (pAmLs)/mg, therefore absolute correction factor f
i=2.2226 * 10
-5Mg/ (pAmLs) it should be noted that absolute correction factor answers regular calibration.Under given condition, methyl alcohol evaporates and gas heating fully, and the pressure of the head space bottle of 9.38mg methyl alcohol has reached about 1.8atm, for not causing that sample leaks or damage head space bottle, should not linear upper range be amplified again.When actual sample is analyzed, consider the evaporation fully of all volatile constituents that comprise methyl alcohol, the peak area sum that on FID, responds with all components is advisable near reaching the corresponding peak area value of methyl alcohol upper limit concentration in the table 1.The FID of this method instrument can respond little peak area to 0.5pAs, can realize low detection to 0.01 μ g/mL methyl alcohol in the head space bottle.Methyl alcohol is concentration and peak area graph of a relation on FID, and is as shown in Figure 1.
4, the mensuration of partition factor
K
iV
L＜＜V
GBe the prerequisite that can formula (2) be used, need K
iAnd V
LSimultaneously all smaller.V
LAnd V
GBe easy to obtain, can converse V by the quality of sample and the density of sample
L, polyvinyl alcohol (PVA) density is 1.19g/mL～1.31g/mL, and it is the polyvinyl alcohol (PVA) of 1.2g/mL that the present invention adopts density, and establishing sample quality is m, then V
L=m/1.2, V
G=20-V
LTherefore also need measure partition factor K
iCan value could judgement formula (2) be used.
The partition factor K here
i, be meant that the head space bottle reaches the constant temperature balance after, the concentration and the ratio that evaporate into the concentration of methyl alcohol in the head space bottle gas phase of still wrapping up or being adsorbed on methyl alcohol on the polyvinyl alcohol (PVA) solid.At a certain temperature, K
iValue should be relevant with the character of sample, like the surface of the chemical constitution of sample, crystallinity, sodium acetate content, sample and pore structure etc.; K
iValue does not have literature value to search, and measures but can adopt the change of researchs such as Wang Baohua to compare the method for measuring partition factor.To formula (1), establish c
I0Be the original concentration of component i in the primary sample in the system, i.e. m
i=c
I0V
L, substitution formula (1) has after the arrangement
c
i0＝c
iG(K
i+V
G/V
L)................................................(4)
Make V
G/ V
L=R is called gas-solid and compares, and substitution formula (4), and distortion have
1/c
iG＝(K
i+R)/c
i0................................................(5)
In constant temperature and closed system, K
iWith R be constant, c
IG=f
iA
i, substitution formula (5), and arrangement has
1/A
i＝f
iK
i/c
i0+f
iR/c
i0..........................................(6)
Can find out from formula (6),, promptly change gas-solid and compare R, carry out headspace gas chromatography and measure, the 1/A reciprocal of chromatographic peak area through taking by weighing different quality polyvinyl alcohol (PVA) sample
iTo comparing the R mapping, can obtain straight line y=ax+b, wherein a=f
i/ c
I0, b=f
iK
i/ c
I0, partition factor K then
i=b/a.
Test takes by weighing about 0.3 gram, 0.4 gram, 0.5 certain sample of gram, under the chromatographic condition of regulation, measures the peak area of methyl alcohol, and calculates corresponding gas-solid and compare, and sees Table 2.
Table 2 difference is compared down the peak area of methyl alcohol in the polyvinyl alcohol (PVA) of measuring
Use 1/A
iTo comparing the R mapping, see Fig. 2, thereby obtain K
i=(7.2755 * 10
-7)/(1.8296 * 10
-6) ≈ 0.4.
The similar method of a plurality of samples using is measured K
iValue is between 0.02～0.4.Here adopt bigger K
iValue 0.4, the sample for 0.5 gram has
V
L＝0.5/1.2≈0.42mL
K
iV
L＝0.4×0.42≈0.17mL
V
G＝20-V
L＝20-0.42≈19.6mL
K
iV
L/V
G≈0.9％
Be K
iV
L＜＜V
G, satisfy the condition of formula (2).When the methanol content of sample lower, and K
iValue hour increases sample size, the sensitivity that can improve mensuration.In the practical measurement, satisfying under the prerequisite of sensitivity, it is favourable to measuring to reduce sample size; Reduce sample size simultaneously, also help the pressure that reduces the head space bottle, prevent the leakage of volatile constituent or damage the head space bottle, also can reduce because of the excessive influence that headspace sample is extracted of head space bottle pressure.
Can also measure acetone with similar method, the partition factor of methyl acetate (both appearance times are seen Fig. 3, and concrete data are seen table 3).
Impurity pervaporation head space chromatographic data table in table 3 polyvinyl alcohol (PVA)
| Signal | Retention time, min | Peak width, min | Area, pAs | Area % | The component title |
| 1 | ?1.566 | 0.061 | 2.20275 | 0.01317 | |
| 1 | ?1.771 | 0.016 | 15278 | 91.32234 | Methyl alcohol |
| 1 | ?1.897 | 0.016 | 50.86407 | 0.30404 | Acetone |
| 1 | ?1.999 | 0.024 | 42.03497 | 0.25126 | |
| 1 | ?2.111 | 0.019 | 1223.44254 | 7.31313 | Methyl acetate |
| 1 | ?2.204 | 0.023 | 2.34672 | 0.01403 | |
| 1 | ?2.391 | 0.023 | 25.09287 | 0.14999 | |
| 1 | ?2.506 | 0.026 | 45.08338 | 0.26949 | |
| 1 | ?2.716 | 0.027 | 14.11443 | 0.08437 | |
| 1 | ?2.808 | 0.037 | 1.72815 | 0.01033 | |
| 1 | ?3.047 | 0.036 | 4.03483 | 0.02412 | |
| 1 | ?4.223 | 0.055 | 6.18491 | 0.03697 | |
| 1 | ?5.229 | 0.074 | 7.22754 | 0.04320 |
5, sample analysis
Take by weighing about 0.1 gram of sample～0.5 gram, be accurate to 0.1 milligram, place the head space bottle, under above-mentioned chromatographic condition, measure the record chromatogram.Methanol content in the polyvinyl alcohol (PVA) of representing with mass percent w.Calculate the methanol content in the polyvinyl alcohol resin by formula (3).
In the formula:
A
i---the peak area of methyl alcohol, pAs;
f
i---the absolute correction factor of methyl alcohol, mg/ (pAmLs); f
i=2.2226 * 10
-5Mg/ (pAmLs)
M---the quality of polyvinyl alcohol (PVA) sample, milligram;
V
G---head space bottle gaseous phase volume, milliliter, V
G=20-m/1.2.
Embodiment 2:
Take by weighing sample 0.2235 gram, be accurate to 0.1mg, place 20 milliliters of head space bottles to seal, heating is 85 minutes in 120 ℃ head-space sampler; DB-1 type chromatographic column, 30 meters of column lengths, 40 ℃ of column temperatures; Fid detector is measured under the above-mentioned chromatographic condition, and peak area is 56233.6 square measures.Formula with embodiment 1 calculates, and the methanol content in the polyvinyl alcohol (PVA) of representing with mass percent w is 1.2498%.
Embodiment 3:
Take by weighing sample 0.3936 gram, be accurate to 0.1mg, place 20 milliliters of head space bottles to seal, heating is 95 minutes in 115 ℃ head-space sampler; DB-1 type chromatographic column, 30 meters of column lengths, 40 ℃ of column temperatures; Fid detector is measured under the above-mentioned chromatographic condition, and peak area is 76263.9 square measures.Formula with embodiment 1 calculates, and the methanol content in the polyvinyl alcohol (PVA) of representing with mass percent w is 1.6743%.
Embodiment 4:
Take by weighing sample 0.3398 gram, be accurate to 0.1mg, place 20 milliliters of head space bottles to seal, heating is 90 minutes in 125 ℃ head-space sampler; DB-1 type chromatographic column, 30 meters of column lengths, 40 ℃ of column temperatures; Fid detector is measured under the above-mentioned chromatographic condition, and peak area is 32280 square measures.Formula with embodiment 1 calculates, and the methanol content in the polyvinyl alcohol (PVA) of representing with mass percent w is 0.7167%.
Embodiment 5:
Take by weighing sample 0.4103 gram, be accurate to 0.1mg, place 20 milliliters of head space bottles to seal, heating is 90 minutes in 120 ℃ head-space sampler; DB-1 type chromatographic column, 30 meters of column lengths, 40 ℃ of column temperatures; Fid detector is measured under the above-mentioned chromatographic condition, and peak area is 12933 square measures.Formula with embodiment 1 calculates, and the methanol content in the polyvinyl alcohol (PVA) of representing with mass percent w is 0.2868%.
Claims (2)
1. with the method for the volatile constituent in the pervaporation Headspace Gas Chromatography polyvinyl alcohol (PVA), adopt the headspace gas chromatography instrument to analyze, it is characterized in that concrete steps are:
Polyvinyl alcohol resin 0.1 gram～0.5 gram is sealed in 20 milliliters of head space bottles; Put into head-space sampler; Heating evaporated volatile constituent in 85 minutes～95 minutes fully under 115 ℃～125 ℃ condition; Adopt gc analysis then, write down the spectrogram of volatile constituent, calculate the content of volatile constituent again with the standard regression curve method.
2. according to the said method of claim 1 with the volatile constituent in the pervaporation Headspace Gas Chromatography polyvinyl alcohol (PVA); It is characterized in that; Said analytical conditions for gas chromatography is: adopt DB-1 type chromatographic column; Adopt fid detector, stationary phase is the quartz capillary column of 100% dimethyl polysiloxane, and carrier gas is N
2, flow velocity 1.0mL/min, split ratio is 1: 100, H
2Flow velocity 30mL/min, air velocity 300mL/min; 40 ℃ of column temperatures, 200 ℃ of detector temperatures; 150 ℃ of injector temperature; Headspace sampling, 120 ℃ of equilibrium temperatures, equilibration time 90min, head space bottle sample size 1.0mL;
Said volatile constituent is methyl alcohol, acetone or methyl acetate, and the appearance time of methyl alcohol is 1.771min, and the appearance time of acetone is 1.897min, and the appearance time of methyl acetate is 2.111min.
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