CN107179377A - The assay method of micro-moisture in organic solvent sample - Google Patents
The assay method of micro-moisture in organic solvent sample Download PDFInfo
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- CN107179377A CN107179377A CN201710372168.9A CN201710372168A CN107179377A CN 107179377 A CN107179377 A CN 107179377A CN 201710372168 A CN201710372168 A CN 201710372168A CN 107179377 A CN107179377 A CN 107179377A
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- 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
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Abstract
The invention discloses a kind of assay method of minim moisture from organic solvent, including：GC MS analytical parameters are set；Series concentration H is prepared with solvent2O standard liquid；Series concentration H is gathered by GC MS2The chromatography of ions figure of O standard liquids；The chromatography of ions peak integration of collection is quadratured using GC MS softwares, with H2O content is abscissa, using response as ordinate, draws H2O standard working curve；Correct H2O standard working curve；The chromatography of ions figure of organic solvent sample is gathered with GC MS, the chromatography of ions peak integration of the organic sample of collection is quadratured using GC MS softwares, the H after correction is utilized2H of the O standard working curve to organic solvent sample2O content carries out quantitative analysis；To the H of organic sample2O content is corrected.Suitable for the measure of all minim moisture from organic solvent contents, including aldehyde, ketone etc. have the organic solvent of reproducibility, test limit is low, the range of linearity is wide, amount of samples is few, environmentally friendly, easy to operate and fast analyze speed the features such as.
Description
Technical field
The present invention relates to a kind of assay method of micro-moisture in organic solvent sample.
Background technology
Organic solvent plays very important effect in modern industry, the continuous extension applied along with organic solvent,
Higher requirement is proposed to trace impurity in organic solvent, water is difficult to the impurity removed as a kind of widely distributed, to production
Quality has important influence, determines and control the content of minim moisture from organic solvent to modern industries such as product purifications
Development is significant.
At present, karl-Fischer method is used the assay method of minim moisture from organic solvent, however, karl-Fischer method has more
It uses upper limitation, can not such as detect that aldehyde, ketone have the moisture of the organic solvent of reproducibility, can not determine pyridine
In moisture, and it is poor to there is the feature of environmental protection（Use the organic solvents such as pyridine）, test limit is higher, cumbersome and analyze speed
Slow the shortcomings of.
The content of the invention
The present invention, should in order to solve the above technical problems, provide a kind of assay method of micro-moisture in organic solvent sample
Method, which is applied to the measure of all minim moisture from organic solvent contents, including aldehyde, ketone etc., has the organic solvent of reproducibility, its
Test limit is low, the range of linearity is wide, amount of samples is few, environmentally friendly, easy to operate and fast analyze speed the features such as.
In order to solve the above technical problems, the present invention provides a kind of assay method of micro-moisture in organic solvent sample, bag
Include following steps：Suitable GC-MS analytical parameters are set；Series concentration H is prepared with acetonitrile as solvents2O standard liquid；With institute
State GC-MS analytical parameters and gather the series concentration H2The chromatography of ions figure of O standard liquid；Using GC-MS softwares to collection
Chromatography of ions peak integration quadrature, with H2O（%）Content is abscissa, using response as ordinate, draws H2O standard work
Curve；To the H of drafting2O standard working curve is corrected；Organic solvent sample is gathered with the GC-MS analytical parameters
Chromatography of ions figure, and the chromatography of ions peak integration of the organic solvent sample of collection is quadratured using GC-MS softwares, recycle institute
State the H after correction2O standard working curve carries out quantitative analysis to the organic solvent sample and draws the organic solvent sample
H2O content；To the H of the organic solvent sample2O content is corrected.
Further, among the step of suitable GC-MS analytical parameters are set, including：By GC automatic sampler sample introduction bodies
Product is set to 1 μ L；GC injector temperatures are set to 250 DEG C；GC sample introduction patterns are set to：Shunt mode, split ratio is 10:
1；GC column flows are set to 1mL/min, constant current mode；GC temperature programming setting requirements：Initial temperature sets 80 DEG C, keeps 2min,
250 DEG C are warming up to 20 DEG C/min speed again, 1min is kept；MS mass scan ranges are set to 10~300amu;MS is molten
Agent delay is set to：“0”min；MS measurement patterns are set to ion selection, detection ion is set to m/z=18 and m/z=17,
Residence time is disposed as 60ms.
Further, series concentration H is prepared with acetonitrile as solvents2Among the step of O standard liquid, including：The first step：
Prepare 1.0%H2O standard reserving solutions：10mL volumetric flasks are put and removed the peel on the assay balance that sensibility reciprocal precision is 0.1mg, are moved with micro
Liquid device accurately pipettes 100 μ LH2O claims to be settled to volume with the acetonitrile solvent after quality 0.1g and claims total matter in the volumetric flask
Amount, is mixed, and stands more than 15min with standby；Second step：Prepare series concentration H2O standard liquids：Will with the acetonitrile as solvents
The 1.0%H2O standard reserving solutions be diluted to successively concentration be respectively 0.00%, 0.01%, 0.05%, 0.10%, 0.25%, 0.50%,
1.00% series H2O standard liquids.
Further, the acetonitrile is chromatographic grade, the H2O is ultra-pure water, before the volumetric flask, micropipettor use
Must clean dried.
Further, the series concentration H is gathered with the GC-MS analytical parameters2The chromatography of ions of O standard liquid
Figure, is quadratured using GC-MS softwares to the chromatography of ions peak integration of collection, with H2O（%）Content is abscissa, using response as
Ordinate, draws H2O standard working curve.
Further, formula is passed through：Response=Yi- Y0To the H of the drafting2O standard working curve is corrected,
Wherein, YiFor containing H2O amounts are i（I=0.00%, 0.01%, 0.05%, 0.10%, 0.25%, 0.50%, 1.00%）H2O standard liquids
Response, Y0For the response of acetonitrile solvent blank.
Further, in the H to the organic solvent sample2Among the step of O content is corrected, including：Pass through public affairs
Formula：H2OSample（%）=X×ρAcetonitrile/ ρSampleTo the H of the organic solvent sample2O content is corrected, wherein：H2OSample（%）For correction
Sample H afterwards2O content；X is to utilize the H after correction2O standard working curves carry out what quantitative analysis was drawn to organic solvent sample
H2O content（%）；ρAcetonitrileFor acetonitrile solvent density；ρSampleFor organic sample density.
The assay method of micro-moisture, has the advantages that in the organic solvent sample of the present invention：
The measure of micro-moisture suitable for all organic solvent samples, including can have the organic of reproducibility to aldehyde, ketone etc.
The measure of micro-moisture in solvent；
Test limit is low（0.0005%）, the range of linearity it is wide（0~10%）, amount of samples it is few（＜ 0.5mL）, it is environmentally friendly, easy to operate and point
Analyse speed fast.
Brief description of the drawings
Fig. 1 is the analytical equipment structural representation of determination of trace water in organic solvent sample of the present invention.
Fig. 2 is the flow chart of determination of trace water in organic solvent sample of the present invention.
Fig. 3 is that step S3 shown in Fig. 2 gathers H with GC-MS analytical parameters2The chromatography of ions figure of O standard liquid.
Fig. 4 is the H that step S4 shown in Fig. 2 is drawn2O standard working curve.
Fig. 5 is the H after the correction of step S5 shown in Fig. 22O standard working curve.
Fig. 6 is the H of the institute of step S6 shown in Fig. 2 test sample product normal hexane2O content examining report.
Embodiment
The present invention is described in detail with embodiment below in conjunction with the accompanying drawings.
Referred to incorporated by reference to Fig. 1 and Fig. 2, the present invention provides a kind of measure side of micro-moisture in organic solvent sample
Method, comprises the following steps：
Step S1, sets suitable GC-MS analytical parameters.It is specifically divided into following steps：
（1）GC automatic sampler sampling volumes are set to 1 μ L；
（2）GC injector temperatures are set to 250 DEG C；
（3）GC sample introduction patterns are set to：Shunt mode, split ratio is 10:1；
（4）GC column flows are set to 1mL/min, constant current mode；
（5）GC temperature programming setting requirements：Initial temperature sets 80 DEG C, keeps 2min, then is warming up to 250 DEG C with 20 DEG C/min speed,
Keep 1min；（Note：GC temperature programmings, which are set, to be changed according to the organic solvent sample difference of detection）；
（6）MS mass scan ranges are set to 10~300amu;
（7）MS solvent delays are set to：“0”min（Solvent-free delay）；
（8）MS measurement patterns are set to SIM（Ion is selected）, detect that ion is set to m/z=18（Object ion）With m/z=17
（Quota ion）, residence time is disposed as 60ms.
Step S2, series concentration H is prepared with acetonitrile as solvents2O standard liquid.It is specifically divided into following steps：
（1）Prepare 1.0%H2O standard reserving solutions：10mL volumetric flasks are put and removed the peel on the assay balance that sensibility reciprocal precision is 0.1mg, are used
Micropipettor accurately pipettes 100 μ LH2O claims quality in volumetric flask（About 0.1g）Volume is settled to acetonitrile solvent afterwards and is claimed total
Quality, is mixed, and stands more than 15min, standby.
（2）Prepare series concentration H2O standard liquids：With acetonitrile as solvents by above-mentioned 1.0%H2O standard reserving solutions dilute successively
Into containing H2O amounts are respectively 0.00%, 0.01%, 0.05%, 0.10%, 0.25%, 0.50%, 1.00% series H2O standard liquids（Note：
Acetonitrile solvent contain H2O amounts are not counted）.
Further, acetonitrile is chromatographic grade, H2O is ultra-pure water, volumetric flask, micropipettor and other need to use
Volumetric apparatus uses preceding palpus clean dried.
Step S3, series concentration H is gathered with GC-MS analytical parameters2The chromatography of ions figure of O standard liquid.
Step S4, is quadratured using GC-MS softwares to the chromatography of ions peak integration of collection, with H2O（%）Content is sat to be horizontal
Mark, with response（Peak area）For ordinate, H is drawn2O standard working curve（Because acetonitrile solvent contains H2O, the H of drafting2O's
Standard working curve is without origin）.
Step S5, to the H of drafting2O standard working curve is corrected.
Specifically, formula can be passed through in step s 5：Response=Yi- Y0The H drawn to step S42O standard
Working curve is corrected, wherein, YiFor containing H2O amounts are i（I=0.00%, 0.01%, 0.05%, 0.10%, 0.25%, 0.50%,
1.00%）H2The response of O standard liquids, Y0For the response of acetonitrile solvent blank.H after correction2O standard working curve
By origin.
Step S6, the chromatography of ions figure of organic solvent sample is gathered with GC-MS analytical parameters, and utilize GC-MS softwares pair
The chromatography of ions peak integration of the organic sample of collection is quadratured, the H after recycle step S5 corrections2O standard working curve pair
Organic solvent sample carries out quantitative analysis and then draws the H of the organic solvent sample2O content.
Step S7, to the H of organic solvent sample2O content is corrected.
Specifically, among step S7, formula can be passed through：
H2OSample（%）=X×ρAcetonitrile/ ρSampleThe water content of the organic solvent sample drawn to step S6 is corrected, wherein：H2OSample
（%）For the sample water content after correction；X is to utilize H2O standard working curves carry out quantitative analysis to organic solvent sample and drawn
Water content（%）；ρAcetonitrileFor acetonitrile solvent density；ρSampleFor organic sample density.
Embodiment>
The organic solvent sample that this example is provided is normal hexane, its H2The measure operating procedure of O content is as follows：
Step 1, the suitable GC-MS analytical parameters of setting, concrete operations are as follows：
GC analytical parameter setups：Chromatographic column DB-5MS（30m×0.25μm×0.32mmi.d.）；Carrier gas：Helium（He）, purity >=
99.999%；Automatic sampler sampling volume is set to 1 μ L；Injector temperature is set to 250 DEG C；Sample introduction pattern is set to：Point
Stream mode, split ratio is 10:1；Column flow is set to 1mL/min, constant current mode；Heating schedule：Initial temperature sets 80 DEG C, kept
2min, then 250 DEG C are warming up to 20 DEG C/min speed, keep 1min；Constant current flow：1mL/min.
MS detector analytical parameter setups：GC-MS interface temperatures are 280 DEG C, EI sources bombardment energy：70eV, ion source temperature
230 DEG C, 150 DEG C of quadrupole rod temperature；Solvent delay is set to：“0”min；Mass scan range is set to 10~300amu；Signal
Drainage pattern：SIM, detection ion is set to m/z=18（Object ion）With m/z=17（Quota ion）, residence time is respectively provided with
For 60ms.
Step 2, with acetonitrile as solvents prepare series concentration H2O standard liquid, concrete operation step is as follows：
1. 1.0%H is prepared2O standard reserving solutions：10mL volumetric flasks are put and removed the peel on the assay balance that sensibility reciprocal precision is 0.1mg, are used
Micropipettor pipettes 100 μ LH2O weighs quality for 0.10701g in volumetric flask, then is settled to acetonitrile volume and claims total matter
Measure as 7.7669g, mix, stand more than 15min, it is standby.H2O standard reserving solutions actual concentration is 1.3776%（m/m）.
2. series concentration H is prepared2O standard liquids：With acetonitrile as solvents by above-mentioned 1.3776%H2O standard reserving solutions are successively
It is diluted to containing H2O amounts are respectively
Arrange H2O standard liquids（Note：Acetonitrile solvent contain H2O amounts are not counted）.
Further, acetonitrile is chromatographic grade, H2O is ultra-pure water, and the volumetric apparatus such as volumetric flask, micropipettor uses preceding palpus
Clean dried.
The series concentration H 2. prepared in step 3, the GC-MS analytical parameters acquisition step 2 set with step 12O standard
The chromatography of ions figure of solution, as shown in Figure 3.
Step 4, using GC-MS softwares the chromatography of ions peak of collection integration is quadratured, with H2O（%）Content is abscissa,
Using response as ordinate, H is drawn2O standard working curve.As shown in Figure 4.
Step 5, pass through formula：Response（Peak area）=Yi- Y0The H drawn to step 42O standard working curve enters
Row correction, wherein, YiFor containing H2O amounts are i（i=0.0000%、0.0138%、0.0689%、0.1378%、0.3444%、0.6888%、
1.3776%）H2The response of O standard liquids, Y0For acetonitrile solvent（Blank）Response.H after correction2O standard work
Curve is as shown in Figure 5.
Step 6, the GC-MS analytical parameters set with step 1 gather the chromatography of ions figure of organic solvent sample, and utilized
GC-MS softwares are quadratured to the chromatography of ions peak integration of the organic sample of collection, the H after the correction that recycle step 5 is drawn2O
Standard working curve carries out quantitative analysis to organic solvent sample, as a result as shown in Figure 6.
Step 7, pass through formula：H2OSample（%）=X×ρAcetonitrile/ ρSampleThe water content of organic solvent sample is corrected：
According to examining report, in formula：X=0.02（%）、ρAcetonitrile=0.79、ρNormal hexane=0.692
Moisture is in sample normal hexane：H2ONormal hexane（%）=0.02 × 0.79/0.692=0.023.
The assay method of micro-moisture, has the advantages that in the organic solvent sample of the present invention：
（1）The measure of micro-moisture suitable for all organic solvent samples；
（2）This method test limit is low（0.0005%）, the range of linearity it is wide（0~10%）, amount of samples it is few（＜ 0.5mL）, environmental protection, behaviour
Make easy and analyze speed fast.
Embodiments of the present invention are these are only, are not intended to limit the scope of the invention, it is every to utilize the present invention
Equivalent structure or equivalent flow conversion that specification and accompanying drawing content are made, or directly or indirectly it is used in other related technologies
Field, is included within the scope of the present invention.
Claims (7)
1. the assay method of micro-moisture in a kind of organic solvent sample, it is characterised in that comprise the following steps：
Suitable GC-MS analytical parameters are set；
Series concentration H is prepared with acetonitrile as solvents2O standard liquid；
The series concentration H is gathered with the GC-MS analytical parameters2The chromatography of ions figure of O standard liquid；
The chromatography of ions peak integration of collection is quadratured using GC-MS softwares, with H2O（%）Content is abscissa, using response as
Ordinate, draws H2O standard working curve；
To the H of the drafting2O standard working curve is corrected；
The chromatography of ions figure of organic solvent sample is gathered with the GC-MS analytical parameters, and is had using GC-MS softwares to collection
The chromatography of ions peak integration of press proof product is quadratured, and recycles the H after the correction2O standard working curve is to described organic molten
Agent sample carries out the H that quantitative analysis draws the organic solvent sample2O content；
To the H of the organic solvent sample2O content is corrected.
2. assay method according to claim 1, it is characterised in that：
Among the step of suitable GC-MS analytical parameters are set, including：
GC automatic sampler sampling volumes are set to 1 μ L；
GC injector temperatures are set to 250 DEG C；
GC sample introduction patterns are set to：Shunt mode, split ratio is 10:1；
GC column flows are set to 1mL/min, constant current mode；
GC temperature programming setting requirements：Initial temperature sets 80 DEG C, keeps 2min, then is warming up to 250 DEG C, holding with 20 DEG C/min speed
1min；
MS mass scan ranges are set to 10~300amu;
MS solvent delays are set to：“0”min；
MS measurement patterns are set to ion selection, detection ion is set to m/z=18 and m/z=17, and residence time is disposed as
60ms。
3. assay method according to claim 1, it is characterised in that：
Series concentration H is prepared with acetonitrile as solvents2Among the step of O standard liquid, including：
The first step：Prepare 1.0%H2O standard reserving solutions：By 10mL volumetric flasks put sensibility reciprocal precision be 0.1mg assay balance up
Skin, 100 μ LH are accurately pipetted with micropipettor2O is settled in the volumetric flask after claiming quality 0.1g with the acetonitrile solvent
Volume simultaneously claims gross mass, mixes, and stands more than 15min with standby；
Second step：Prepare series concentration H2O standard liquids：With the acetonitrile as solvents by the 1.0%H2O standard reserving solutions are successively
It is respectively 0.00%, 0.01%, 0.05%, 0.10%, 0.25%, 0.50%, 1.00% series H to be diluted to concentration2O standard liquids.
4. assay method according to claim 3, it is characterised in that：
The acetonitrile is chromatographic grade, the H2O is ultra-pure water, and the volumetric flask, micropipettor use preceding palpus clean dried.
5. assay method according to claim 1, it is characterised in that：
The series concentration H is gathered with the GC-MS analytical parameters2The chromatography of ions figure of O standard liquid, utilizes GC-MS softwares
The chromatography of ions peak integration of collection is quadratured, with H2O（%）Content is abscissa, using response as ordinate, draws H2O mark
Quasi- working curve.
6. assay method according to claim 1, it is characterised in that：
To the H of the drafting2O standard working curve passes through formula：Response=Yi- Y0It is corrected, wherein, YiFor containing H2O
Measure as i（I=0.00%, 0.01%, 0.05%, 0.10%, 0.25%, 0.50%, 1.00%）H2The response of O standard liquids, Y0For second
The response of nitrile solvent blank.
7. assay method according to claim 1, it is characterised in that：
In the H to the organic solvent sample2Among the step of O content is corrected, including：Pass through formula：H2OSample（%）=X×
ρAcetonitrile/ ρSampleTo the H of the organic solvent sample2O content is corrected, wherein：H2OSample（%）For the sample H after correction2O content；
X is to utilize the H after correction2O standard working curves carry out the H that quantitative analysis is drawn to organic solvent sample2O content（%）；ρAcetonitrileFor
Acetonitrile solvent density；ρSampleFor organic sample density.
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Application publication date: 20170919 |