CN108802083B - Method for measuring sulfur and chlorine content in triphenylphosphine - Google Patents

Method for measuring sulfur and chlorine content in triphenylphosphine Download PDF

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CN108802083B
CN108802083B CN201810423351.1A CN201810423351A CN108802083B CN 108802083 B CN108802083 B CN 108802083B CN 201810423351 A CN201810423351 A CN 201810423351A CN 108802083 B CN108802083 B CN 108802083B
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sulfur
chlorine
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triphenylphosphine
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庞玉娜
冯庆霞
尹萌萌
冯立娟
宫斌
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Liaocheng Luxi Polyol New Material Technology Co ltd
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Abstract

The invention relates to a method for measuring the contents of sulfur and chlorine in triphenylphosphine, which mainly comprises the following steps: (1) preparation of sample solution: toluene is used as a solvent, and a toluene solution of triphenylphosphine is prepared as a solution to be detected and a blank is made after a triphenylphosphine sample is dissolved. (2) Preparing a sulfur and chlorine standard solution; (3) drawing a standard curve; (4) and (4) measuring the contents of sulfur and chlorine. The method has the advantages of high accuracy, good repeatability, simplicity in operation, rapidness and the like, and is suitable for measuring the contents of sulfur and chlorine in the same substances.

Description

Method for measuring sulfur and chlorine content in triphenylphosphine
Technical Field
The invention relates to a method for measuring the contents of sulfur and chlorine in triphenylphosphine, in particular to a method for measuring the contents of sulfur and chlorine in triphenylphosphine by using a single-wavelength X-ray fluorescence method.
Background
Triphenylphosphine is widely used as an important auxiliary material for the production process of butanol and isooctanol, and the poisoning activity of the catalyst is easily reduced when the sulfur and chlorine content is high. At present, a coulometry method is generally adopted in a method for measuring the contents of sulfur and chlorine in triphenylphosphine, but the method has larger error of a detection result and poorer repeatability because a sample is not completely combusted. Other detection methods for measuring sulfur and chlorine in triphenylphosphine have not been reported in the prior art.
Disclosure of Invention
In order to overcome the defects in the background art and overcome the defects of the background art, the invention provides the method for measuring the sulfur and chlorine content in the triphenylphosphine, which has the advantages of high accuracy, simple operation and high speed.
A method for measuring the contents of sulfur and chlorine in triphenylphosphine comprises the following steps:
(1) preparation of sample solution: toluene is used as a solvent, and a toluene solution of triphenylphosphine is prepared as a solution to be detected and a blank is made after a triphenylphosphine sample is dissolved.
(2) Preparation of sulfur and chlorine standard solutions: the standard solution of sulfur and chlorine with the concentration of 100 mug/mL is diluted by toluene to prepare the series standard solution of sulfur and chlorine with the concentration of 0.0, 1.0, 2.5, 5.0, 8.0 and 10.0 mug/mL.
(3) Drawing a standard curve: the counting rates of sulfur and chlorine elements in the standard solution of sulfur and chlorine are respectively measured by using a single-wavelength X-ray fluorescence spectrometer, and a curve is drawn by taking the contents of sulfur and chlorine in the standard solution as abscissa and the counting rates as ordinate.
(4) And (3) measuring the contents of sulfur and chlorine:
firstly, measuring a blank solution to obtain the counting rate of sulfur and chlorine elements in the blank solution, and obtaining concentration values C of the sulfur and chlorine elements in the blank solution according to a concentration-counting rate standard curve0；
Measuring the sample solution to obtain the counting rates of sulfur and chlorine in the sample solution, and obtaining the concentration values C of sulfur and chlorine in the sample solution according to the standard curves of sulfur and chlorine concentration-counting rateiAccording to the formula ω ═ Ci-C0) Calculating to obtain the contents of sulfur and chlorine in the triphenylphosphine, wherein omega represents the contents of sulfur and chlorine in the triphenylphosphine sample to be detected; ciExpressing the concentration of sulfur and chlorine in the sample solution to be detected; c0The concentration of sulfur and chlorine in the blank solution is shown; v represents the volume of the sample solution to be measured; m represents the mass of the triphenylphosphine sample to be tested.
Preferably, in the step (1), the sample weighing amount of triphenylphosphine is 1.0 g-2.0 g, and the adding amount of toluene is 10-20 mL.
Preferably, in both steps (1) and (2), the content of sulfur and chlorine in the toluene solvent is controlled to be 0.5. mu.g/mL or less.
The above formula ω ═ Ci-C0) In x V/m, the unit of each parameter is preferably selected for the convenience of calculation, wherein the unit of omega is mu g/g; ciAnd C0The unit of (a) is mu g/mL; the unit of V is mL; the unit of m is g.
The invention has the beneficial effects that: the invention provides a method for measuring the contents of sulfur and chlorine in triphenylphosphine by using a single-wavelength X-ray fluorescence method. The method has the advantages of high accuracy, good repeatability, simplicity in operation, rapidness and the like, and is suitable for measuring the contents of sulfur and chlorine in the same substances.
1. According to the invention, after the triphenylphosphine sample is completely dissolved by using the toluene solvent, the detection is directly carried out by using the single-wavelength X-ray fluorescence method, the combustion treatment process is avoided, and the accuracy of the detection result is improved.
2. The invention adopts single-wavelength X-ray fluorescence method to measure the sulfur and chlorine content in triphenylphosphine, and no report of the same type exists in China at present.
3. The method has the advantages of simple and rapid operation, good repeatability, high accuracy and the like, and is suitable for measuring sulfur and chlorine elements in the same substance.
Drawings
FIG. 1 is a chlorine content standard curve diagram, and FIG. 2 is a sulfur content standard curve diagram.
Detailed Description
In order to make the technical solution of the present invention better understood and make the above objects, features and advantages of the present invention more comprehensible, the present invention is described in further detail with reference to examples.
Example 1
(1) Preparation of sample solution: 1.0240g, 1.0203g, 1.1236g, 1.0574g and 1.0432g of triphenylphosphine samples are weighed in sequence and respectively put into a 50mL iodine measuring flask with a plug, 10mL of toluene solvent is added respectively to completely dissolve the triphenylphosphine samples to obtain 5 parts of a parallel solution to be tested, and meanwhile, blank is made.
(2) Preparation of sulfur and chlorine standard solutions: the standard solution of sulfur and chlorine with the concentration of 100 mug/mL is diluted by toluene to prepare the series standard solution of sulfur and chlorine with the concentration of 0.0, 1.0, 2.5, 5.0, 8.0 and 10.0 mug/mL.
(3) Drawing a standard curve: the counting rates of sulfur and chlorine elements in the standard solution of sulfur and chlorine are respectively measured by a single-wavelength X-ray fluorescence spectrometer, and the instrument automatically processes data and displays curves.
The linear fitting equation obtained by the sulfur element is that Y is 0.2446X +0.9006, and the correlation coefficient is that r is 0.9995; the linear fitting equation of chlorine element is 0.2532X +0.851, and the correlation coefficient is 0.9998, wherein Y represents the counting rate and X represents the concentration.
(4) And (3) measuring the contents of sulfur and chlorine: respectively measuring the counting rates of sulfur and chlorine elements in the blank solution and the sample solution by using a single-wavelength X-ray fluorescence spectrometer, respectively calculating the contents of the sulfur and chlorine elements in 5 parts of the sample solution according to a linear fitting equation, and then respectively calculating the contents of the sulfur and chlorine elements according to a formula omega ═ Ci-C0) Calculating the contents of sulfur and chlorine elements in the sample by multiplying by V/m, and taking an average value. The values obtained are shown in tables 1 and 2.
TABLE 1
Figure GDA0003034067260000031
TABLE 2
Figure GDA0003034067260000032
Example 2
(1) Preparation of sample solution: 1.5690g, 1.6231g, 1.5423g, 1.4986g and 1.6521g of triphenylphosphine samples are weighed in sequence and respectively put into a 50mL iodine measuring flask with a plug, 15mL of toluene solvent is added respectively to completely dissolve the triphenylphosphine samples to obtain 5 parts of a parallel solution to be tested, and meanwhile, blanks are made.
(2) Preparation of sulfur and chlorine standard solutions: the standard solution of sulfur and chlorine with the concentration of 100 mug/mL is diluted by toluene to prepare the series standard solution of sulfur and chlorine with the concentration of 0.0, 1.0, 2.5, 5.0, 8.0 and 10.0 mug/mL.
(3) Drawing a standard curve: the counting rates of sulfur and chlorine elements in the standard solution of sulfur and chlorine are respectively measured by a single-wavelength X-ray fluorescence spectrometer, and the instrument automatically processes data and displays curves.
The linear fitting equation obtained by the sulfur element is that Y is 0.2923X +0.3274, and the correlation coefficient is that r is 0.9998; the linear fitting equation of chlorine element is 0.2887X +0.3947, and the correlation coefficient is 0.9999, wherein Y represents the counting rate and X represents the concentration.
(4) And (3) measuring the contents of sulfur and chlorine: using single wavelength X-ray fluorescence spectroscopyMeasuring the counting rates of sulfur and chlorine in the blank solution and the sample solution, respectively calculating the contents of sulfur and chlorine in 5 parts of sample solution according to a linear fitting equation, and then according to a formula omega (C)i-C0) Calculating the contents of sulfur and chlorine elements in the sample by multiplying by V/m, and taking an average value. The values obtained are shown in tables 3 and 4.
TABLE 3
Figure GDA0003034067260000041
TABLE 4
Figure GDA0003034067260000042
Although the present invention has been described with reference to the specific embodiments, it should be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.

Claims (1)

1. A method for measuring the contents of sulfur and chlorine in triphenylphosphine comprises the following steps:
(1) preparation of sample solution: dissolving a triphenylphosphine sample by using toluene as a solvent to prepare a toluene solution of triphenylphosphine as a solution to be detected, and meanwhile, making a blank;
(2) preparation of sulfur and chlorine standard solutions: diluting a sulfur and chlorine standard solution with the concentration of 100 mug/mL by using methylbenzene to prepare a series of sulfur and chlorine standard solutions;
(3) drawing a standard curve: measuring the counting rates of sulfur and chlorine elements in the sulfur and chlorine standard solutions respectively by using a single-wavelength X-ray fluorescence spectrometer, and drawing a concentration-counting rate standard curve;
(4) and (3) measuring the contents of sulfur and chlorine: measuring the blank solution by using a single-wavelength X-ray fluorescence spectrometer to respectively obtain the counting rates of sulfur and chlorine elements in the blank solution according to the concentration-counting rate standardThe concentration values C of sulfur and chlorine in the blank solution are obtained by the curve0(ii) a Measuring the sample solution by using a single-wavelength X-ray fluorescence spectrometer, respectively obtaining the counting rates of sulfur and chlorine elements in the sample solution, and respectively obtaining the concentration values C of the sulfur and chlorine elements in the sample solution according to the standard curves of the concentration of sulfur and chlorine-counting ratei；
The method is characterized in that:
in the step (1), the sample weighing amount of triphenylphosphine is 1.0-2.0 g, and the adding amount of toluene is 10-20 mL; the sulfur and chlorine contents of the toluene solvent are controlled below 0.5 mu g/mL;
in the step (2), the concentrations of the series of sulfur and chlorine standard solutions are respectively 0.0, 1.0, 2.5, 5.0, 8.0 and 10.0 mu g/mL;
in the step (3), according to the concentration-count rate standard curve, a sulfur element linear fitting equation is obtained, wherein Y is 0.2923X +0.3274, and the correlation coefficient is 0.9998; the linear fitting equation obtained by the chlorine element is that Y is 0.2887X +0.3947, and the correlation coefficient is that r is 0.9999; wherein Y represents the counting rate and X represents the concentration;
in the step (4), the concentration values C of sulfur and chlorine elements in the blank solution0And obtaining the concentration values C of the sulfur and chlorine elements of the sample solution by the standard curveiThe conversion formula is as follows: ω ═ Ci-C0) The content of sulfur and chlorine in the triphenylphosphine is respectively calculated, wherein omega represents the content of sulfur and chlorine in the triphenylphosphine sample to be detected; ciExpressing the concentration of sulfur and chlorine in the sample solution to be detected; c0The concentration of sulfur and chlorine in the blank solution is shown; v represents the volume of the sample solution to be measured; m represents the mass of the triphenylphosphine sample to be detected;
the above formula ω ═ Ci-C0) In x V/m, the unit of ω is μ g/g; c0And CiThe unit of (a) is mu g/mL; the unit of V is mL; the unit of m is g.
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