CN109580824A - A kind of two hydrazine method for detecting purity of oxalyl - Google Patents
A kind of two hydrazine method for detecting purity of oxalyl Download PDFInfo
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- CN109580824A CN109580824A CN201811600474.4A CN201811600474A CN109580824A CN 109580824 A CN109580824 A CN 109580824A CN 201811600474 A CN201811600474 A CN 201811600474A CN 109580824 A CN109580824 A CN 109580824A
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- oxalyl
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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
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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
- G01N2030/042—Standards
- G01N2030/047—Standards external
Abstract
The present invention provides a kind of two hydrazine method for detecting purity of oxalyl, comprising: a certain amount of two hydrazine of oxalyl is dissolved in the water, testing sample solution is made；The testing sample solution is measured to obtain chromatogram using high performance liquid chromatography, wherein, chromatographic column is one of Hilic chromatographic column, phenyl column or chromatography in series column, the chromatography in series column is formed by C18 chromatographic column or C8 chromatographic column with Hilic Coupled columns, and mobile phase includes the acetonitrile and water that mass ratio is 90:5~5:95；The purity of two hydrazine of oxalyl is determined according to the chromatogram.The method for detecting purity of two hydrazine of oxalyl provided in an embodiment of the present invention improves the separating degree of impurity Yu two hydrazine of oxalyl by using specific chromatographic separation condition, avoids the interference of impurity, improves the accuracy and stability of two hydrazine purity test of oxalyl.
Description
Technical field
The present invention relates to chemical analysis technology fields, specifically provide a kind of two hydrazine method for detecting purity of oxalyl.
Background technique
Two hydrazine of oxalyl is not only the foaming agent and industrial chemicals of synthetic rubber, plastics, rubber blend, but also is a kind of
Important solid propellant function additive, purity are the important indicators of its quality control, it is therefore necessary to establish suitable test side
Method.
Its related method for detecting purity only sees Chinese periodical " Second metrology and measurement and space flight development forum " report text
" research of two hydrazine method for detecting purity of oxalyl " is offered, this document propose using N-bromo-succinimide as standard titration solution, is passed through
To the calibration mode of standard solution, sample dissolving method and sulfuric acid medium quantifier elimination, a kind of two hydrazine of measurement oxalyl is established
The capacity analysis method of purity, although method is simple, which is based on two hydrazine of oxalyl and hydrolyzes generation hydrazine in acid condition
And the redox reaction carried out, certain impurity therein are found in real work, can be reacted with titrant, and test is seriously affected
As a result accuracy.It yet there are no other open reports about two hydrazine method for detecting purity of oxalyl.
Summary of the invention
Aiming at the problems existing in the prior art, the embodiment of the invention provides a kind of two hydrazine method for detecting purity of oxalyl,
The separating degree of impurity Yu two hydrazine of oxalyl is improved by using specific chromatographic separation condition, avoids the interference of impurity, is improved
The accuracy and stability of two hydrazine purity test of oxalyl.
The technical solution of the invention is as follows:
A kind of two hydrazine method for detecting purity of oxalyl, comprising the following steps:
(1) a certain amount of two hydrazine of oxalyl is dissolved in the water, testing sample solution is made；
(2) testing sample solution is measured to obtain chromatogram using high performance liquid chromatography, wherein chromatographic column
For one of Hilic chromatographic column, phenyl column or chromatography in series column, the chromatography in series column is by C18 chromatographic column or C8 chromatographic column
It is formed with Hilic Coupled columns, mobile phase includes the acetonitrile and water that mass ratio is 90:5~5:95；
(3) purity of two hydrazine of oxalyl is determined according to the chromatogram.
In an alternative embodiment, testing sample solution described in step (1) before the assay via hole diameter be 0.22 μm or
0.45 μm of needle type filtration head filtering.
In an alternative embodiment, chromatographic column described in step (2) be C18 chromatographic column and Hilic Coupled columns and
At, the mobile phase is made of acetonitrile, first alcohol and water, wherein acetonitrile volume ratio be 40~60%, methanol volume ratio be 5~
10%.
In an alternative embodiment, chromatographic column described in step (2) be Hilic chromatographic column, the mobile phase by acetonitrile,
First alcohol and water composition, wherein acetonitrile volume ratio is 5~15%.
In an alternative embodiment, chromatographic column described in step (2) be Hilic chromatographic column, the mobile phase by acetonitrile,
First alcohol and water composition, and gradient elution is used, acetonitrile volume ratio is 5~15%, methanol volume ratio in the mobile phase when initial
It is 5~15%, the volume ratio of acetonitrile in the mobile phase is adjusted to the volume of 40~60%, methanol in 2.5~3.5min
Than being adjusted to 5~10%, each component content in the mobile phase is adjusted to initial content in 7.5~8.5min, and retain
1.5~2.5min.
In an alternative embodiment, chromatographic column described in step (2) is phenyl column, and the mobile phase is by acetonitrile, methanol
It is formed with ammonium acetate aqueous solution, acetonitrile volume ratio is 5~15% in the mobile phase, methanol volume ratio is 5~15%, and surplus is
The ammonium acetate aqueous solution, the concentration of the ammonium acetate aqueous solution are 1~20mmol/L.
In an alternative embodiment, the flow velocity of the mobile phase is 0.6~1mL/min.
In an alternative embodiment, when being measured using high performance liquid chromatography to the testing sample solution, detection
Device is evaporative light scattering detector, and temperature is 25 DEG C~50 DEG C, and gain value is 6-8.
In an alternative embodiment, the concentration of step (1) described testing sample solution is 10-5~10-3g/mL。
In an alternative embodiment, step (3) determines the purity of two hydrazine of oxalyl according to the chromatogram, comprising:
The purity that two hydrazine of oxalyl is primarily determined according to areas of peak normalization method will when the purity primarily determined >=97%
Purity of the purity as two hydrazine of oxalyl carries out external standard correction using standard sample as the purity < 97% primarily determined,
Obtain the purity of two hydrazine of oxalyl.
Compared with the prior art, the invention has the advantages that:
The method for detecting purity of two hydrazine of oxalyl provided in an embodiment of the present invention, mentions by using specific chromatographic separation condition
The separating degree for having risen impurity Yu two hydrazine of oxalyl, avoids the interference of impurity, improve two hydrazine purity test of oxalyl accuracy and
Stability.
Detailed description of the invention
Fig. 1 is the high-efficient liquid phase chromatogram that the embodiment of the present invention 1 provides；
Fig. 2 is the high-efficient liquid phase chromatogram that the embodiment of the present invention 2 provides
Fig. 3 is the high-efficient liquid phase chromatogram that the embodiment of the present invention 3 provides；
Fig. 4 is the high-efficient liquid phase chromatogram that the embodiment of the present invention 4 provides
Fig. 5 is the high-efficient liquid phase chromatogram that the embodiment of the present invention 5 provides.
Specific embodiment
A specific embodiment of the invention is described in further details below with reference to drawings and the specific embodiments.
The embodiment of the invention provides a kind of two hydrazine method for detecting purity of oxalyl, comprising the following steps:
(1) a certain amount of two hydrazine of oxalyl is dissolved in the water, testing sample solution is made；
Specifically, in the embodiment of the present invention, sample can be dissolved in the water by ultrasound, is preferably 42Khz in frequency
± 6%, power is to dissolve 30min or more under 100W；
(2) testing sample solution is measured to obtain chromatogram using high performance liquid chromatography, wherein chromatographic column
For one of Hilic chromatographic column, phenyl column or chromatography in series column, the chromatography in series column is by C18 chromatographic column and Hilic chromatography
Column be connected in series perhaps by C8 chromatographic column and Hilic Coupled columns form chromatographic column filler partial size can for 2.7 μm or
2.5 μm or 5 μm, mobile phase includes the acetonitrile and water that mass ratio is 90:5~5:95；When measurement, sample volume preferably 2 μ of μ l~50
L, detector can be diode array detector, UV detector, in Detection wavelength preferred 218nm, 254nm, 300nm extremely
Few one kind；In an alternative embodiment, the preferred evaporative light scattering detector of detector, temperature is 25 DEG C~50 DEG C, and gain value is
6-8；The flow velocity of mobile phase preferably 0.6~1mL/min；
(3) purity of two hydrazine of oxalyl is determined according to the chromatogram.
The method for detecting purity of two hydrazine of oxalyl provided in an embodiment of the present invention, mentions by using specific chromatographic separation condition
The separating degree for having risen impurity Yu two hydrazine of oxalyl, avoids the interference of impurity, improve two hydrazine purity test of oxalyl accuracy and
Stability.
In an alternative embodiment, testing sample solution described in step (1) before the assay via hole diameter be 0.22 μm or
0.45 μm of needle type filtration head filtering.
In an alternative embodiment, chromatographic column described in step (2) be C18 chromatographic column and Hilic Coupled columns and
At, the mobile phase is made of acetonitrile, first alcohol and water, wherein acetonitrile volume ratio be 40~60%, methanol volume ratio be 5~
10%.The advantages of two kinds of chromatography post separations of the chromatographic column set, so that two hydrazine of oxalyl and each impurity good separating effect.
In an alternative embodiment, chromatographic column described in step (2) be Hilic chromatographic column, the mobile phase by acetonitrile,
First alcohol and water composition, wherein acetonitrile volume ratio is 5~15%, methanol volume ratio is 2~10%.In an alternative embodiment, step
Suddenly chromatographic column described in (2) is Hilic chromatographic column, and the mobile phase is made of acetonitrile, first alcohol and water, and is drenched using gradient
It washes, acetonitrile volume ratio is 5~15% in the mobile phase when initial, methanol volume ratio is 5~15%, in 2.5~3.5min
The volume ratio that the volume ratio of acetonitrile in the mobile phase is adjusted to 40~60%, methanol is adjusted to 5~10%, 7.5~
Each component content in the mobile phase is adjusted to initial content when 8.5min, and retains 1.5~2.5min.Made by walking gradient
It obtains target components to be sufficiently separated with impurity, while detecting two hydrazine object of oxalyl, filtering by using evaporative light scattering detector
Fall to evaporation impurity jamming target object peak area of the light emission detector without response, to ensure that test effect.
In an alternative embodiment, chromatographic column described in step (2) is phenyl column, and the mobile phase is by acetonitrile, methanol
It is formed with ammonium acetate aqueous solution, acetonitrile volume ratio is 5~15% in the mobile phase, methanol volume ratio is 5~15%, and surplus is
The ammonium acetate aqueous solution, the concentration of the ammonium acetate aqueous solution are 1~20mmol/L.The preferred Diode Array Detector of detector
Device, the preferred 300nm of Detection wavelength；By the adjusting of ammonium acetate solution, chromatography peak type is improved, ensure that two hydrazine of object oxalyl
Peak type it is good, while by selection 300nm UV absorption wavelength, avoid impurity composition to two hydrazine chromatographic peak area of oxalyl
Interference, ensure that purity in the test accuracy of 97% test sample below.
In an alternative embodiment, the flow velocity of the mobile phase is 0.6~1mL/min.
In an alternative embodiment, when being measured using high performance liquid chromatography to the testing sample solution, gain
Value is 6~8.
In an alternative embodiment, the concentration of step (1) described testing sample solution is 10-5~10-3g/mL。
In an alternative embodiment, step (3) determines the purity of two hydrazine of oxalyl according to the chromatogram, comprising:
The purity that two hydrazine of oxalyl is primarily determined according to areas of peak normalization method will when the purity primarily determined >=97%
Purity of the purity as two hydrazine of oxalyl carries out external standard correction using standard sample as the purity < 97% primarily determined,
Obtain the purity of two hydrazine of oxalyl.Wherein, the standard sample can be commercially available standard items, and purity is to mark purity on specification,
When using single point correction, prepare certain density control sample using standard items, according to its peak area and to test sample peak area into
Row calculates, and with the peak area to test sample divided by the peak area of control sample, gained percentage is multiplied by standard sample purity and standard sample
The ratio of concentration and sample concentration is to test sample Reinheitszahl；When using external standard calibration curve method, one is prepared using standard sample
The standard solution of series of concentrations establishes standard curve with control sample concentration and peak area value, calculate to test sample purity meter.
The following are several specific embodiments of the invention, each embodiment material therefor is commercial product:
Embodiment 1
C18 chromatography short column used in the present embodiment is bought from U.S.'s phenomenex company, model ACE C-18, and column length is
50mm, internal diameter 4.6mm, packing material size is 2.5 μm, Hilic chromatographic column is bought from Agilent company, the U.S., model
120 Hillic column length of Agilent poroshell be 150mm, internal diameter 4.6mm, 2.7 μm of partial size；
Step 1 prepares test sample: weighing seven parts of two hydrazines of oxalyl, sample weighting amount be respectively 0.0208g, 0.0509g,
0.0401g, 0.0355g, 0.0907g, 0.01079g and 0.0080g dissolve ultrasound 30min with ultrapure water, complete to sample solution
After portion's clear, constant volume is stood.Solution to be measured is formed, concentration is respectively 4.16 × 10-4g/mL、1.08×10-4g/mL、
8.02×10-4g/mL、7.10×10-4g/mL、1.83×10-3g/mL、2.16×10-4G/mL and 1.6 × 10-4G/mL, respectively
It is filtered using 0.22 μm of aperture needle type filtration head.
Testing conditions: step 2 is measured sample solution with high performance liquid chromatography (HPLC), chromatographic separation condition
Are as follows: chromatographic column is C18 chromatography short column and Hilic Coupled columns, and chromatographic column filler partial size is respectively 2.5 μm and 2.7 μm；Flowing
It is mutually acetonitrile/methanol/water=55/5/40；Flow velocity is 0.6mL/min, and sample volume is 10 μ l；Detector is Diode Array Detector
Device, wavelength 218nm.Gained chromatogram is as shown in Figure 1.
Step 3 is quantified using areas of peak normalization method.
Step 4 forms detection data: experimental results.Its seven determination datas are respectively as follows: 98.60%,
98.52%, 98.63%, 98.72%, 98.97%, 98.85%, 98.74%；Average value is 98.72%；Method relative standard
Deviation is 0.17%.
Embodiment 2
C18 chromatographic column used in the present embodiment is bought from Agilent company, the U.S., model Agilent poroshell
120 EC C-18, column length 50mm, internal diameter 4.6mm, packing material size is 2.7 μm, Hilic chromatographic column is bought from the U.S.
Agilent company, 120 Hillic column length of model Agilent poroshell are 150mm, internal diameter 4.6mm, grain
Diameter is 2.7 μm.
Step 1 prepares test sample: weighing seven parts of two hydrazines of oxalyl, sample weighting amount be respectively 0.0208g, 0.0509g,
0.0401g, 0.0355g, 0.0907g, 0.01079g and 0.0080g dissolve ultrasound 30min with ultrapure water, complete to sample solution
After portion's clear, constant volume is stood.Solution to be measured is formed, concentration is respectively 4.16 × 10-4g/mL、1.08×10-4g/mL、
8.02×10-4g/mL、7.10×10-4g/mL、1.83×10-3g/mL、2.16×10-4G/mL and 1.6 × 10-4G/mL, respectively
It is filtered using 0.22 μm of aperture needle type filtration head.
Step 2 determines testing conditions: being measured with high performance liquid chromatography (HPLC) to sample solution, chromatographic isolation
Condition are as follows: C18 short column and Hilic Coupled columns, chromatographic column filler partial size is 2.7 μm；Flow velocity is 0.6mL/min；Flowing
It is mutually acetonitrile: methanol: water=55:5:40；Sample volume is 10 μ l；Detector is diode array detector, wavelength 254nm.
Step 3 is quantified using areas of peak normalization method.
Step 4 forms detection data: experimental results.Seven determination datas are respectively as follows: 98.34%, 98.40%,
98.43%, 98.32%, 98.53,98.47%, 98.41%；Average value is 98.41%；Method relative standard deviation is
0.09%.
Embodiment 3:
C18 chromatography short column used in the present embodiment is bought from U.S.'s phenomenex company, model ACE C-18, and column length is
50mm, internal diameter 4.6mm, packing material size are 2.7 μm；Hilic chromatographic column is bought from Agilent company, the U.S., model
120 Hillic column length of Agilent poroshell be 150mm, internal diameter 4.6mm, 2.7 μm of partial size；Two hydrazine mark of oxalyl
Sample is purchased from Sigma Co., USA, and mark purity is 97.36% on specification.
Step 1 prepares test sample: weighing two hydrazine of oxalyl, sample weighting amount 0.0220g dissolves ultrasound with ultrapure water
30min stands constant volume after sample solution whole clear.Solution to be measured is formed, concentration is 4.40g × 10-4/ mL is used
0.22 μm of aperture needle type filtration head filtering.
Testing conditions: step 2 is measured sample solution with high performance liquid chromatography (HPLC), chromatographic separation condition
Are as follows: chromatographic column is C18 chromatography short column and Hilic Coupled columns, and chromatographic column filler partial size is respectively 2.5 μm and 2.7 μm；Flowing
It is mutually acetonitrile/methanol/water=55/5/40；Flow velocity is 0.6mL/min, and sample volume is 10 μ l；Detector is Diode Array Detector
Device, wavelength 218nm.
Step 3 is quantified using areas of peak normalization method.
Step 4 forms detection data: experimental results.Its purity is 97.18%.
Embodiment 4:
Hilic chromatographic column used in the present embodiment is bought from Agilent company, the U.S., model Agilent poroshell
120 Hillic, column length 150mm, internal diameter 4.6mm, partial size are 2.7 μm.
Step 1 prepares test sample: weighing two hydrazine of oxalyl of 0.0217g first, dissolves ultrasound 30min with ultrapure water,
After sample solution whole clear, constant volume is stood.Solution to be measured is formed, concentration is 4.34 × 10-4G/mL, using aperture
It is filtered for 0.22 μm of needle type filtration head.
Step 2 determines testing conditions: being measured with high performance liquid chromatography (HPLC) to sample solution, using gradient
Elution, mobile phase are as follows: Hilic chromatographic column；Mobile phase is A water: B methanol: C acetonitrile=90:5:5, condition of gradient elution are as follows
Shown in table:
Flow velocity is 1mL/min, and sample volume is 2 μ l；Detector is evaporative light scattering detector.Evaporative light scattering detector temperature
Spending range is 32 DEG C, and gain value is 7.
Step 3 is quantified using external standard correction method.According to step 1, solution is prepared, control sample concentration is 4.30 ×
10-4g/mL.Two hydrazine standard specimen of oxalyl is purchased from Sigma Co., USA, and mark purity is 97.36% on specification.It is obtained according to step 2
To peak area be 21656.89 and the peak area to test sample is 18967.10.According to control sample purity be 97.36% calculate, with to
For the peak area of test sample divided by the peak area of control sample, gained percentage is Reinheitszahl.
Step 4 forms detection data: experimental results.Its Reinheitszahl is 84.48%.
Embodiment 5:
Step 1 prepares test sample: weighing two hydrazine of oxalyl of 0.0217g first, dissolves ultrasound 30min with ultrapure water,
After sample solution whole clear, constant volume is stood.Solution to be measured is formed, concentration is 4.34 × 10-4G/mL, using aperture
It is filtered for 0.45 μm of needle type filtration head.
Step 2 determines testing conditions: being measured with high performance liquid chromatography (HPLC) to sample solution, chromatographic isolation
Condition are as follows: chromatographic column is phenyl chromatographic column, and from U.S.'s phenomenex company, phenyl column type number is 5 μ C6- of Gemini for purchase
Phenyl C-18, column length 250mm, internal diameter 4.60mm, packing material size is 5 μ, control sample is that our unit is self-produced, this is right
It is in the same old way good for propellant service performance.Purity is in terms of 100%；Mobile phase is acetonitrile: methanol: 10mmol/L ammonium acetate aqueous solution
=5:5:90, sample volume are 2 μ l；Flow velocity is 0.8mL/min, and detector is diode array detector, wavelength 300nm.
Step 3 is quantified using external standard Single Point Correction Method.Two hydrazine standard specimen of oxalyl is purchased from Sigma Co., USA, explanation
It is 97.36% that purity is marked on book.According to step 1, preparing control sample solution concentration is 4.34 × 10-4g/mL.According to step 2
Obtain the peak area 21971.23 of control sample and the peak area 19196.24 to test sample.It is 97.36% calculating by control sample purity,
With the peak area to test sample divided by the peak area of control sample, gained percentage is Reinheitszahl.
Step 4 forms detection data: experimental results.Reinheitszahl is 87.28%
The sample of same purity is using volumetric analysis reported in the literature measurement, purity 126.51%, seriously with reality
Concentration is not inconsistent.
The above, a specific embodiment only of the invention, but scope of protection of the present invention is not limited thereto, appoints
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of, all by what those familiar with the art
It is covered by the protection scope of the present invention.
Unspecified part of the present invention belongs to common sense well known to those skilled in the art.
Claims (10)
1. a kind of two hydrazine method for detecting purity of oxalyl, which comprises the following steps:
(1) a certain amount of two hydrazine of oxalyl is dissolved in the water, testing sample solution is made；
(2) testing sample solution is measured to obtain chromatogram using high performance liquid chromatography, wherein chromatographic column is
One of Hilic chromatographic column, phenyl column or chromatography in series column, the chromatography in series column by C18 chromatographic column or C8 chromatographic column with
Hilic Coupled columns form, and mobile phase includes the acetonitrile and water that mass ratio is 90:5~5:95；
(3) purity of two hydrazine of oxalyl is determined according to the chromatogram.
2. two hydrazine method for detecting purity of a kind of oxalyl according to claim 1, which is characterized in that described in step (1) to
Via hole diameter is 0.22 μm or 0.45 μm of needle type filtration head filtering to sample solution before the assay.
3. two hydrazine method for detecting purity of a kind of oxalyl according to claim 1, which is characterized in that described in step (2)
Chromatographic column is that C18 chromatographic column is formed with Hilic Coupled columns, and the mobile phase is made of acetonitrile, first alcohol and water, wherein acetonitrile
Volume ratio is 40~60%, methanol volume ratio is 5~10%.
4. two hydrazine method for detecting purity of a kind of oxalyl according to claim 1, which is characterized in that described in step (2)
Chromatographic column is Hilic chromatographic column, and the mobile phase is made of acetonitrile, first alcohol and water, and wherein acetonitrile volume ratio is 5~15%.
5. two hydrazine method for detecting purity of a kind of oxalyl according to claim 1, which is characterized in that described in step (2)
Chromatographic column is Hilic chromatographic column, and the mobile phase is made of acetonitrile, first alcohol and water, and uses gradient elution, stream when initial
Acetonitrile volume ratio is 5~15% in dynamic phase, methanol volume ratio is 5~15%, in 2.5~3.5min by second in the mobile phase
The volume ratio that the volume ratio of nitrile is adjusted to 40~60%, methanol is adjusted to 5~10%, in 7.5~8.5min by the flowing
Each component content is adjusted to initial content in phase, and retains 1.5~2.5min.
6. two hydrazine method for detecting purity of a kind of oxalyl according to claim 1, which is characterized in that described in step (2)
Chromatographic column is phenyl column, and the mobile phase is made of acetonitrile, methanol and ammonium acetate aqueous solution, acetonitrile volume ratio in the mobile phase
It is 5~15% for 5~15%, methanol volume ratio, surplus is the ammonium acetate aqueous solution, and the concentration of the ammonium acetate aqueous solution is
1~20mmol/L.
7. described in any item two hydrazine method for detecting purity of a kind of oxalyl according to claim 1~6, which is characterized in that the stream
The flow velocity of dynamic phase is 0.6~1mL/min.
8. described in any item two hydrazine method for detecting purity of a kind of oxalyl according to claim 1~6, which is characterized in that using high
When effect liquid phase chromatogram method is measured the testing sample solution, detector is evaporative light scattering detector, and temperature is 25 DEG C
~50 DEG C, gain value is 6-8.
9. two hydrazine method for detecting purity of a kind of oxalyl according to claim 1, which is characterized in that step (1) is described to be measured
The concentration of sample solution is 10-5~10-3g/mL。
10. two hydrazine method for detecting purity of a kind of oxalyl according to claim 1, which is characterized in that step (3) is according to
Chromatogram determines the purity of two hydrazine of oxalyl, comprising:
The purity that two hydrazine of oxalyl is primarily determined according to areas of peak normalization method, it is when the purity primarily determined >=97%, this is pure
The purity as two hydrazine of oxalyl is spent, as the purity < 97% primarily determined, external standard correction is carried out using standard sample, is obtained
The purity of two hydrazine of oxalyl.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3839105A (en) * | 1972-03-10 | 1974-10-01 | Thiokol Chemical Corp | Oxalyl dihydrazide compositions and use as a coolant in gas generating process |
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2018
- 2018-12-26 CN CN201811600474.4A patent/CN109580824B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3839105A (en) * | 1972-03-10 | 1974-10-01 | Thiokol Chemical Corp | Oxalyl dihydrazide compositions and use as a coolant in gas generating process |
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| YOSHIHITO OHBA ET AL.: "Liquid chromatography of fatty acids with chemiluminescence detection", 《ANALYTICA CHIMICA ACTA》 * |
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