Method for measuring chloride ions in polycarboxylate superplasticizer

A measurement method and technology of water reducer, applied in chemical method analysis, chemical analysis by titration method, measuring device, etc., can solve the problems of ineffective separation of chloride ion and thiocyanate, error of test results, etc., and achieve large-scale equipment Cost advantage, high precision, and the effect of improving accuracy

Active Publication Date: 2016-12-21
安徽海螺材料科技股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] This method is used to process the water reducer sample. If the water reducer has a single formula and no other impurities, the accuracy of the test can be guaranteed. However, when there is thiocyanate in t

Method used

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  • Method for measuring chloride ions in polycarboxylate superplasticizer
  • Method for measuring chloride ions in polycarboxylate superplasticizer
  • Method for measuring chloride ions in polycarboxylate superplasticizer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Take the batch numbers J160412-1, J160610-1, J160713-1, and J160718-1 of the batch numbers of the theoretical values ​​of the formulas produced by our company respectively 0.013%, 0.015%, 0.020%, and 0.015%, and test them according to the following steps Chloride content.

[0047] First, determine the endpoint potential E corresponding to the titration endpoint ep

[0048] Weigh 0.1000g of sodium chloride, put it in a 400mL beaker, add 4mL of nitric acid solution (1+1), add water to 200mL, add 10mL of starch solution with a concentration of 10g / L, put in a magnetic stirrer, and place the beaker under a magnetic force On the stirrer, insert the silver electrode and reference electrode connected to the potentiometric titrator, turn on the magnetic stirrer, then add dropwise the silver nitrate standard solution with a concentration of 0.1000mol / L, record the burette reading V and the corresponding silver electrode potential E ;

[0049] When the titration is close to th...

Embodiment 2

[0080] For the four batches of water reducer samples whose batch numbers are J160412-1, J160610-1, J160713-1, and J160718-1 in Example 1 of the present invention, the chloride ion content was measured by the method of GB / T 8077-2012 respectively, and the obtained Results of Table 2:

[0081] Table 2:

[0082] Sample lot number

[0083] As can be seen from Table 2, the chloride ion content measured by the method of the present invention is closer to the theoretical value, and therefore has higher accuracy than the method of GB / T8077-2012.

Embodiment 3

[0085] Take the water reducer sample with the batch number J160713-1, weigh 40.0000g in six parts each, add a certain amount of chloride ion standard sample, and use the improved method to carry out the recovery rate test. The test results are shown in Table 3:

[0086] table 3:

[0087] serial number

Water reducer, g

The amount of chloride ion added, mg

Measured value, mg

Recovery amount, mg

Recovery rate,%

1

40.0000

0.00

7.2

/

/

2

40.0000

5.00

12.1

4.9

98.00

3

40.0000

10.00

17.3

10.1

101.00

4

40.0000

15.00

22.1

14.9

99.33

5

40.0000

20.00

27.3

20.1

100.50

6

40.0000

25.00

32.2

25.0

100.00

[0088] Wherein, the preparation of chloride ion standard sample is as follows: Accurately weigh 1.6485g of sodium chloride burned to constant weight in a high-temperature furnace at 500°C to 600°C, dissolve it in a 1000ml volumetric f...

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Abstract

The invention provides a method for measuring chloride ions in a polycarboxylate superplasticizer. The method comprises the following steps: decomposing thiocyanate radicals by using hydrogen peroxide under alkaline conditions, acidifying a test solution, and then measuring the chloride ions by using potentiometric titration, wherein the main reaction equation is as follows: SCN<->+4H2O2+2OH<->=SO4<2->+OCN<->+5H2O; AgCl<+>+AgCl<->=AgCl. By adoption of the method, the interference of the thiocyanate radicals is effectively eliminated, the accuracy of the method is improved, and thus the method has the advantages of small errors and high precision; and compared with the ion chromatography in the GB/T8077-2012, the method has a great advantage of equipment cost, thereby being easier to promote and use.

Description

technical field [0001] The invention relates to the technical field of potentiometric titration, in particular to a method for determining chloride ions in polycarboxylate water reducers. Background technique [0002] The current national standard GB / T 8077-2012 includes potentiometric titration and ion chromatography for the determination of chloride ions in water reducers. Among them, the investment in finished products of ion chromatography is too high, and the commonly used potentiometric titration method is not suitable for water reducers with a single formula. The measurement accuracy is high, but with the diversification and complexity of the formula of the water reducing agent, it is no longer possible to accurately measure the content of chloride ions in the water reducing agent. [0003] GB / T 8077-2012 "Test Method for Homogeneity of Concrete Admixtures" adopts potentiometric titration method to measure chloride ion as follows: silver electrode or chloride ion elec...

Claims

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Application Information

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IPC IPC(8): G01N30/96G01N31/16
CPCG01N30/96G01N31/164
Inventor 张大康明金龙王书华谭静进江元华
Owner 安徽海螺材料科技股份有限公司
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