CN103776925A - Detection method for content of target substances of industrial potassium chloride - Google Patents
Detection method for content of target substances of industrial potassium chloride Download PDFInfo
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- CN103776925A CN103776925A CN201410008279.8A CN201410008279A CN103776925A CN 103776925 A CN103776925 A CN 103776925A CN 201410008279 A CN201410008279 A CN 201410008279A CN 103776925 A CN103776925 A CN 103776925A
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Abstract
The invention discloses a detection method for the content of target substances of industrial potassium chloride. The content of the target substances is used for determining the quality grade of the industrial potassium chloride. The method comprises the following steps: dissolving a potassium chloride sample into water to prepare a potassium chloride sample solution with the concentration of mmg/mL and recording the concentration m; detecting the concentration C of target ions in the sample solution by an ion chromatograph; and calculating the content of the target substances corresponding to the target ions in the potassium chloride sample. The method disclosed by the invention is easy to operate and high in accuracy and can be used for detecting the content of sodium chloride, which cannot be directly detected in the prior art; the detection on the content of the plurality of target substances can be finished by one time of sample feeding.
Description
Technical field
The present invention relates to the content of material detection field of industrial chemistry articles for use, particularly the detection method of industrial potassium chloride content of material.
Background technology
The quality grade of industrial potassium chloride is the important parameter often using in producing.According to the requirement of State Standard of the People's Republic of China GB/T7118-2008, in the quality grade of industrial potassium chloride detects, except need to detecting the content of potassium chloride, also want the content of sodium chloride in testing product, calcium ion, magnesium ion and sulfate radical.The principle that prior art detects the content of above-mentioned these materials is first potassium chloride sample to be made into certain density solution, recycle the analytical approachs such as classical gravimetric method, volumetric method or photometry and respectively the various ion concentrations in solution are detected, then by calculating the content of various materials.These method operation stepss tediously long time-consuming, sensitivity is low, be easily disturbed, and cannot directly measure the content of sodium chloride, can only draw by calculating indirectly, error is larger.
Summary of the invention
The invention provides a kind of target substance detection method of content of industrial potassium chloride, with solve the detection method of prior art tediously long time-consuming, sensitivity is low, be easily disturbed and cannot directly measure the problem of the content of sodium chloride.
For achieving the above object, technical scheme of the present invention is achieved in that
The invention provides a kind of target substance detection method of content of industrial potassium chloride, described target substance content is for determining the quality grade of described industrial potassium chloride, and described method comprises,
In above formula:
W---the massfraction of the target substance corresponding with described object ion in described potassium chloride sample, %;
The concentration of the described object ion recording in C---step 102, mg/L;
The concentration of sample in the described sample solution recording in m---step 101, mg/mL;
Conversion coefficient between the quality of the mass of ion of K---described object ion and corresponding target substance.
Alternatively, to screen and record the object ion of concentration be potassium ion to step 102;
Answer in contrast, the target substance of step 103 is potassium chloride; And,
Answer in contrast, in the formula of step 103, K value is 1.9068.
Alternatively, the sensing range of described potassium concentration is 50mg/L～1000mg/L.
Alternatively, to screen and record the object ion of concentration be sodion to step 102;
Answer in contrast, the target substance of step 103 is sodium chloride; And,
Answer in contrast, in the formula of step 103, K value is 2.5421.
Alternatively, the sensing range of described Na ion concentration is 0.1mg/L～50mg/L.
Alternatively, to screen and record the object ion of concentration be calcium ion and magnesium ion to step 102;
Answer in contrast, the target substance of step 103 is calcium ion and magnesium ion; And,
Answer in contrast, in the formula of step 103, K value is 1.
Alternatively, the sensing range of described calcium ion concentration is 0.1mg/L～20mg/L;
The sensing range of described magnesium ion concentration is 0.1mg/L～20mg/L.
Alternatively, to screen and record the object ion of concentration be sulfate ion to step 102;
Answer in contrast, the target substance of step 103 is sulfate ion; And,
Answer in contrast, in the formula of step 103, K value is 1.
Alternatively, the sensing range of described sulfate ion concentration is 0.1mg/L～50mg/L.
Alternatively, in above-mentioned detection, 1 gram of potassium chloride sample dissolution is mixed with to the sample solution that 1 liter of concentration is 1mg/mL in water.
From above-mentioned, of the present invention comprising: " potassium chloride sample dissolution is mixed with to the potassium chloride sample solution that concentration is mmg/mL in water, and records this concentration m; Detect the concentration C of the object ion in described sample solution by ion chromatograph; Calculate the target substance corresponding with the described object ion content in potassium chloride sample with algorithm " method proposed a kind of detect industrial potassium chloride by ion chromatograph in the method for target substance content; the method is simple to operate, accuracy is high, can detect the content of the sodium chloride that prior art can not direct-detection, and can complete the detection of multiple target substance content by single injected sampling.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the inventive method.
Embodiment
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing, embodiment of the present invention is described further in detail.
Core concept of the present invention is, utilize ion chromatograph to detect the concentration of specific ion in potassium chloride sample solution, then the concentration in potassium chloride sample solution according to the concentration of these ions and potassium chloride sample, calculates the content of potassium chloride, sodium chloride, calcium ions and magnesium ions and sulfate radical in potassium chloride sample accurately by algorithm of the present invention.Based on this, can realize the assay that completes fast and accurately potassium chloride, sodium chloride, calcium ions and magnesium ions and sulfate radical, and can avoid disturbing by ion chromatographic method, and then determine fast and accurately the quality grade of potassium chloride.
Chromatography of ions (being called for short IC) is wherein the high performance liquid chromatography one of (being called for short HPLC), and the chromatography of ions is a kind of liquid-phase chromatography method for separating of ion, and the method is prior art.Compare with analytical approachs such as classical gravimetric method, volumetric method and photometries, it is good, highly sensitive, quick, easy that the chromatography of ions has selectivity, can measure multi-component advantage simultaneously.Since 1975 come out, the important analysis means of yin, yang ion in aqueous solution are become very soon.
The basic procedure of the detection method of industrial potassium chloride target substance content of the present invention is referring to Fig. 1, and in the present invention, the target substance of detection is different and different with testing goal.One of content purposes that detects target substance in industrial potassium chloride is that industrial potassium chloride is carried out to quality grade evaluation.According to the requirement of State Standard of the People's Republic of China GB/T7118-2008, the chemical index of industrial potassium chloride quality testing comprises the content of potassium chloride, sodium chloride, calcium ion, magnesium ion and sulfate radical.As completed by single injected sampling the detection of all target substances in the quality grade evaluation of industrial potassium chloride, the target substance that carries out content detection comprises: potassium chloride, sodium chloride, calcium ions and magnesium ions and sulfate radical.As completed the detection of all target substances in the quality grade evaluation of industrial potassium chloride by sample introduction repeatedly, the target substance that carries out content detection comprises: one or more in potassium chloride, sodium chloride, calcium ions and magnesium ions and sulfate radical.Certainly, content of material detection method of the present invention also can be for the purposes outside the quality grade evaluation of industrial potassium chloride, the target substance that now carries out content detection can comprise one or several in potassium chloride, sodium chloride, calcium ions and magnesium ions and sulfate radical, also can comprise as required other target substances.The embodiment of the present invention describes as an example of the detection that completes all target substances in the quality grade evaluation of industrial potassium chloride by single injected sampling example.
Fig. 1 is the process flow diagram of the inventive method, and as shown in Figure 1, the detection method of industrial potassium chloride target substance content of the present invention comprises:
Method for optimizing is, weighs potassium chloride sample 1g, is accurate to 0.001g, be placed in 250mL beaker, the 100mL that adds water is transferred in 1000mL volumetric flask after it is fully dissolved, and is diluted with water to scale mark and shakes up, and can obtain like this concentration is the potassium chloride sample solution of 1g/L.Certainly, also can adopt additive method preparation sample solution, and sample solution can be mixed with to other concentration.Because the quality of potassium chloride sample and the volume of potassium chloride sample solution are known, so the concentration m of potassium chloride sample is also known in potassium chloride sample solution, recorded the value of concentration m simultaneously.
In the present invention, the object ion of detection is different and different with the desired substance detecting.Carry out in quality grade evaluation at industrial potassium chloride, as completed by single injected sampling the detection of all target substances in the quality grade evaluation of industrial potassium chloride, the target substance that carries out content detection comprises: potassium chloride, sodium chloride, calcium ions and magnesium ions and sulfate radical.Accordingly, object ion comprises: potassium ion, sodion, calcium ion, magnesium ion and sulfate ion.As completed the detection of all target substances in the quality grade evaluation of industrial potassium chloride by sample introduction repeatedly, object ion is the ion corresponding with the target substance of this mensuration content, the object ion that carries out concentration detection comprises: one or more in potassium ion, sodion, calcium ion, magnesium ion and sulfate ion, when method of the present invention is during for object outside the quality grade evaluation of industrial potassium chloride, object ion changes according to the variation of target substance, can comprise the ion outside above-mentioned ion.The embodiment of the present invention describes as an example of the detection that completes all target substances in the quality grade evaluation of industrial potassium chloride by single injected sampling example.
Utilizing before ion chromatograph detects the concentration of the object ion in described sample solution, should first detect a series of standard solution that comprise certain object ion with ion chromatograph, to obtain the calibration curve of various ions.
First prepare a series of standard solution that comprise certain object ion, the water of obtain solution is the secondary deionized water that resistivity is 18.2M Ω .cm, and in these standard solution, the concentration of this kind of object ion is known.Can be specifically:
Preparation Na ion concentration is the each portion of standard solution of 0.1mg/L, 0.5mg/L, 2mg/L, 10mg/L, 50mg/L;
Preparation potassium concentration is the each portion of standard solution of 50mg/L, 100mg/L, 200mg/L, 500mg/L, 1000mg/L;
Preparation calcium ion concentration is the each portion of standard solution of 0.1mg/L, 0.2mg/L, 1mg/L, 5mg/L, 20mg/L;
Preparation magnesium ion concentration is the each portion of standard solution of 0.1mg/L, 0.2mg/L, 1mg/L, 5mg/L, 20mg/L;
Preparation sulfate concentration is the each portion of standard solution of 0.1mg/L, 0.5mg/L, 2mg/L, 10mg/L, 50mg/L.
Then detect above-mentioned standard solution with ion chromatograph, obtain the relation between concentration and the ion chromatograph response of certain object ion.
In the time detecting, can adopt the aqueous sodium carbonate of 5mmol/L as the mobile phase of negative ion, adopt the nitric acid of 1.7mmol/L and pyridine-2 of 0.7mmol/L, the mixed liquor of 6-dicarboxylic acid aqueous solution is as cationic mobile phase.Prepare the mobile phase container that is imported ion chromatograph after mobile phase, while detection, import the sample presentation device of ion chromatograph using the portion in above-mentioned standard solution as testing sample, until detected all above-mentioned standard solution at every turn.Obtain after testing the ion chromatograph response corresponding with standard solution ion concentration to be measured.
The ion concentration of standard solution to be measured and corresponding ion chromatograph response thereof are processed the calibration curve that generates various ions through workstation.In process of the test of the present invention, concentration range and the related coefficient of various ions being carried out to actual detection are as shown in table 1.
Concentration sensing range and the correlation coefficient charts of table 1 ion
In the linear equation of table 1, Q is ion concentration, and A is ion chromatograph response.
As can be seen from Table 1, within the scope of the ion concentration shown in table 1, the calibration curve linearly dependent coefficient of various ions is all greater than 0.999, and linear relationship is good, illustrates within the scope of the ion concentration shown in table 1 and to have good accuracy by the concentration that ion chromatograph detects these several ions.Because the ion concentration scope shown in table 1 can meet the needs of the target substance content detection of industrial potassium chloride, therefore for exceed shown in table 1 ion concentration scope time, whether the concentration that detects these several ions with ion chromatograph has good accuracy, and the present invention verifies.Therefore, do not advise detecting outward in the ion concentration scope shown in table 1.
Detect after the scope of application in the linear equation and the concentration that obtain each object ion, detect the potassium chloride sample solution of preparation in step 101 of the present invention with this ion chromatograph, for saving operation, can complete by single injected sampling the content detection of all target substances in the quality grade evaluation of industrial potassium chloride, object ion now comprises potassium ion, sodion, calcium ion, magnesium ion and sulfate ion (during for purposes outside the quality grade evaluation of industrial potassium chloride, object ion is determined according to actual needs in method of the present invention).
Like this, detect by ion chromatograph the potassium concentration just obtaining in potassium chloride sample solution
na ion concentration
calcium ion concentration
magnesium ion concentration
and sulfate ion concentration
The algorithm that calculates the content of the target substance corresponding with described object ion in potassium chloride sample is:
In above formula:
W---the massfraction of the target substance corresponding with described object ion in described potassium chloride sample, %;
The concentration of the described object ion recording in C---step 102, mg/L;
The concentration of sample in the described sample solution recording in m---step 101, mg/mL;
Conversion coefficient between the quality of the mass of ion of K---described object ion and corresponding target substance.
The concentration of the object ion recording according to the concentration value m in step 101 and step 102 is calculated the content of potassium chloride, sodium chloride, calcium ions and magnesium ions total amount and sulfate radical in potassium chloride sample.
Specifically:
Calculate respectively the content of potassium chloride, sodium chloride, calcium ions and magnesium ions total amount and sulfate radical in potassium chloride sample with following algorithm:
In above formula:
W
1---the massfraction of potassium chloride in potassium chloride sample, %;
W
2---the massfraction of sodium chloride in potassium chloride sample, %;
W
3---the massfraction of potassium chloride calcium in sample magnesium ion total amount (being the number percent that the quality sum of calcium ion and magnesium ion accounts for potassium chloride sample gross mass), %;
W
4---the massfraction of sulfate radical in potassium chloride sample, %;
The concentration of sample in the described sample solution recording in m---step 101, mg/mL, that is: the concentration of potassium chloride sample in the potassium chloride sample solution that in step 101 of the present invention, preparation obtains;
1.9068---the conversion coefficient between the potassium chloride quality of potassium ion quality and same number;
2.5421---the conversion coefficient between the sodium chloride quality of sodion quality and same number.
Adopt step 101 of the present invention respectively randomly draw 4 industrial potassium chloride samples to be detected to method and the art methods of step 103, testing result is in table 2.
Table 2 potassium chloride sample detection result data table
As can be seen from Table 2, adopt step 101 of the present invention to the method for step 103 can obtain easily evaluating in State Standard of the People's Republic of China GB/T7118-2008 four chemical index of industrial potassium chloride quality grade requirement.It is more approaching that the KCE content result that simultaneously adopts step 101 of the present invention to the method for step 103 to detect to obtain and the method that adopts defined in State Standard of the People's Republic of China GB/T7118-2008 detect the KCE content result obtaining, and the rationality of step 101 of the present invention to the method for step 103 has been described.
Obtaining after the content of potassium chloride in industrial potassium chloride sample, sodium chloride, calcium ions and magnesium ions total amount and sulfate radical, record again the content of water-insoluble and moisture in industrial potassium chloride sample according to prior art, can evaluate the quality grade of industrial potassium chloride sample.
The foregoing is only preferred embodiment of the present invention, be not intended to limit protection scope of the present invention.All any modifications of doing within the spirit and principles in the present invention, be equal to replacement, improvement etc., be all included in protection scope of the present invention.
Claims (10)
1. a target substance detection method of content for industrial potassium chloride, described target substance content, for determining the quality grade of described industrial potassium chloride, is characterized in that, described method comprises,
Step 101, preparation sample solution: in water, being mixed with concentration is the potassium chloride sample solution of mmg/mL by potassium chloride sample dissolution, and records this concentration m;
Step 102, detects the concentration C of the object ion in described sample solution by ion chromatograph;
Step 103, calculate the content of the target substance corresponding with described object ion in potassium chloride sample by following algorithm:
In above formula:
W---the massfraction of the target substance corresponding with described object ion in described potassium chloride sample, %;
The concentration of the described object ion recording in C---step 102, mg/L;
The concentration of sample in the described sample solution recording in m---step 101, mg/mL;
Conversion coefficient between the quality of the mass of ion of K---described object ion and corresponding target substance.
2. detection method according to claim 1, is characterized in that,
The object ion that concentration was screened and recorded to step 102 is potassium ion;
Answer in contrast, the target substance of step 103 is potassium chloride; And,
Answer in contrast, in the formula of step 103, K value is 1.9068.
3. detection method according to claim 2, is characterized in that,
The sensing range of described potassium concentration is 50mg/L～1000mg/L.
4. detection method according to claim 1, is characterized in that,
The object ion that concentration was screened and recorded to step 102 is sodion;
Answer in contrast, the target substance of step 103 is sodium chloride; And,
Answer in contrast, in the formula of step 103, K value is 2.5421.
5. detection method according to claim 4, is characterized in that,
The sensing range of described Na ion concentration is 0.1mg/L～50mg/L.
6. detection method according to claim 1, is characterized in that,
The object ion that concentration was screened and recorded to step 102 is calcium ion and magnesium ion;
Answer in contrast, the target substance of step 103 is calcium ion and magnesium ion; And,
Answer in contrast, in the formula of step 103, K value is 1.
7. detection method according to claim 6, is characterized in that,
The sensing range of described calcium ion concentration is 0.1mg/L～20mg/L;
The sensing range of described magnesium ion concentration is 0.1mg/L～20mg/L.
8. detection method according to claim 1, is characterized in that,
The object ion that concentration was screened and recorded to step 102 is sulfate ion;
Answer in contrast, the target substance of step 103 is sulfate ion; And,
Answer in contrast, in the formula of step 103, K value is 1.
9. detection method according to claim 8, is characterized in that,
The sensing range of described sulfate ion concentration is 0.1mg/L～50mg/L.
10. according to the detection method described in any one in claim 1 to 9, it is characterized in that, 1 gram of potassium chloride sample dissolution is mixed with to the sample solution that 1 liter of concentration is 1mg/mL in water.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106706767A (en) * | 2015-11-12 | 2017-05-24 | 中石化石油工程技术服务有限公司 | Detection method of content of carbonates in carbonate rock reservoir |
| CN110261442A (en) * | 2019-07-24 | 2019-09-20 | 武汉轻工大学 | A kind of method that Fast synchronization detects sodium chloride and potassium chloride in food |
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| CN101936962A (en) * | 2010-05-02 | 2011-01-05 | 陈建文 | Method for determining weight percent of sodium chloride in common salt |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106706767A (en) * | 2015-11-12 | 2017-05-24 | 中石化石油工程技术服务有限公司 | Detection method of content of carbonates in carbonate rock reservoir |
| CN110261442A (en) * | 2019-07-24 | 2019-09-20 | 武汉轻工大学 | A kind of method that Fast synchronization detects sodium chloride and potassium chloride in food |
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