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A kind of method for measuring sodium carbonate or sodium bicarbonate content in solid sample

A technology of sodium bicarbonate and sodium carbonate, which is applied in the preparation of test samples, measuring devices, sampling, etc., can solve the problems of large result error, large end point error, time-consuming, etc., and achieves high sensitivity, small error, and easy operation. easy effect

Active Publication Date: 2019-04-26
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] For the analysis of components in mixed bases of sodium carbonate and sodium bicarbonate, the double indicator method is almost always used, however, due to the insufficient Kb1 / Kb2 of sodium carbonate, CO is formed at the end point 3 2- / HCO 3 - Buffer system, resulting in a gentle jump in the pH value of the first metering point, the color change of the indicator is not sharp at the end of the titration, and the result error is large. At the second end of the titration, due to the buffer system HCO in the solution 3 - / CO 2 Formation, methyl orange turns orange is also very slow, and the end point error is also large; use mixed indicator method, separation method using different solubility of sodium carbonate and sodium bicarbonate in sodium chloride aqueous solution, barium carbonate precipitation separation method, potential Titration etc., but these methods are all time-consuming, and the operator is difficult to grasp; Have the inductively coupled plasma atomic emission spectrometry (ICP-AES) method of gaseous carbon dioxide generation technology, measure the method for solid sodium carbonate and sodium bicarbonate, By continuously mixing dilute hydrochloric acid and a sample solution containing inorganic carbon on-line, the inorganic carbon in the sample solution is determined to form gaseous carbon dioxide, and the sample pretreatment is very complicated; when using infrared spectroscopy to quantify, complex methods need to be used. Constant ratio and absorbance correction method, the relative average error is only less than 7%

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  • A kind of method for measuring sodium carbonate or sodium bicarbonate content in solid sample
  • A kind of method for measuring sodium carbonate or sodium bicarbonate content in solid sample
  • A kind of method for measuring sodium carbonate or sodium bicarbonate content in solid sample

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Embodiment 1

[0030] Weigh 1 g each of the pure substances sodium carbonate, sodium bicarbonate, and sodium sulfate, grind and tablet, and use for Raman measurement to obtain the following standard mass spectrum. The spectrum of sodium carbonate is at 1080cm -1 and 700cm -1 Shows characteristic peaks at 1460, 1435, 1266, 1047 and 685cm in the spectrum of sodium bicarbonate -1 The characteristic peaks are shown at 1152, 1130, 1100, 994, 648, 633, 620, 465 and 450cm -1 , 1080cm of sodium carbonate -1 , 1047cm of sodium bicarbonate -1 994cm with sodium sulfate -1 The intensity of these three characteristic peaks is higher than that of other characteristic peaks. In order to reduce the experimental error, these three characteristic peaks were selected for quantitative calculation.

Embodiment 2

[0032] Weigh 1g each of the pure substances sodium carbonate, sodium bicarbonate, and sodium nitrate, grind and tablet, and use for Raman measurement to obtain figure 2 The Raman spectrum of the standard substance is shown. The spectrum of sodium carbonate is at 1080cm -1 and 700cm -1 Shows characteristic peaks at 1460, 1435, 1266, 1047 and 685cm in the spectrum of sodium bicarbonate -1 Shows characteristic peaks at 1384, 1067, 723cm for sodium nitrate -1 The characteristic peak is shown at 1080cm of sodium carbonate -1 , 1047cm of sodium bicarbonate -1 1067cm with sodium nitrate -1 They are stronger than other characteristic peaks. In order to reduce experimental errors, these three characteristic peaks can be selected for quantitative calculation.

Embodiment 3

[0034] Weigh 1g each of the pure substances sodium carbonate, sodium bicarbonate, and sodium acetate, grind and tablet, and use for Raman measurement to obtain image 3 The Raman spectrum of the standard substance is shown. The spectrum of sodium carbonate is at 1080cm -1 and 700cm -1 Shows characteristic peaks at 1460, 1435, 1266, 1047 and 685cm in the spectrum of sodium bicarbonate -1 Shows characteristic peaks at 2928, 1450, 1415, 1339, 924, 653, 623cm for sodium acetate -1 A characteristic peak is shown at 1080cm of sodium carbonate -1 , 1047cm of sodium bicarbonate -1 924cm with sodium acetate -1 They are stronger than other characteristic peaks. In order to reduce experimental errors, these three characteristic peaks can be selected for quantitative calculation.

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Abstract

The invention discloses a method for detecting the content of sodium carbonate or sodium bicarbonate in a solid sample. The method comprises the following steps: using fingerprint information provided by Raman spectroscopy to identify sodium carbonate and sodium bicarbonate; selecting a certain mass fraction of an internal standard substance, dividing the characteristic peak intensity of the sodium carbonate in 1047 cm<-1> or sodium bicarbonate in 1080 cm<-1> by the characteristic peak intensity of the internal standard substance, and making a standard curve by using the above obtained peak intensity ratio and respective mass fractions; and fully mixing and uniformly grinding a sample to be detected and the internal standard substance with the same mass fraction, detecting the intensity ratio of the characteristic peak of the sodium carbonate or sodium bicarbonate to the characteristic peak of the internal standard substance by Raman spectroscopy, and comparing the obtained intensity ratio with the standard curve to determine the content of sodium carbonate or sodium bicarbonate in the sample to be detected.

Description

technical field [0001] The invention relates to a method for determining the content of sodium carbonate or sodium bicarbonate in a solid sample, in particular to a method for determining the content of sodium carbonate or sodium bicarbonate in a solid sample by using Raman spectroscopy. Background technique [0002] Mixed alkali mainly refers to the mixture of sodium carbonate and sodium bicarbonate, sodium carbonate and sodium hydroxide, the latter is rarely encountered in actual production, but the former is often encountered. It is mainly used in soda ash industry, food and beverage, chemical and feed production industries. In these industries, the content of sodium carbonate and sodium bicarbonate in the mixed alkali should be analyzed frequently to determine the quality of raw materials and products, whether the process equipment is running normally and other technical indicators. [0003] At present, reports at home and abroad mainly contain the following several kin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/65G01N1/28
CPCG01N1/286G01N21/65G01N2001/2866
Inventor 沈爱国梁伟伟麦家铭
Owner WUHAN UNIV