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A method for the determination of elemental sulfur content in environmental samples

A measurement method and environmental sample technology, applied in measuring devices, instruments, chemical analysis by combustion, etc., can solve problems such as low accuracy of measurement results, impact on the environment and human health, complex pretreatment of samples, etc., and achieve low cost , reliable data and simple steps

Active Publication Date: 2021-05-11
GUANGZHOU HKUST FOK YING TUNG RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods have their own drawbacks
Ion chromatography needs to be carried out under strong alkaline conditions (pH>12) and the measurement time is longer (more than 12 hours). In addition, the instability of the final determination product thiosulfate leads to low accuracy of the determination results
In spectrophotometry, highly toxic substances such as cyanide are used in order to convert elemental sulfur into thiocyanate as the final measurement, which has a great impact on the environment and human health.
In high performance liquid chromatography and inductively coupled plasma emission spectrometry, the instrumentation is expensive and the sample requires complex pretreatment (such as extraction or digestion)

Method used

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  • A method for the determination of elemental sulfur content in environmental samples
  • A method for the determination of elemental sulfur content in environmental samples
  • A method for the determination of elemental sulfur content in environmental samples

Examples

Experimental program
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Effect test

Embodiment 1

[0032] (1) Sample preparation:

[0033] ①Preparation of sodium bicarbonate solution (pH=9): Take 42g of sodium bicarbonate, dissolve it in 500mL of water, dilute to 1000mL, add sodium hydroxide solution to make the pH=9, mix well to get ready.

[0034] ② Weigh elemental sulfur samples of different weights (5, 10, 25, 50, 75, 100, 150, 200mg), mix them with 0.5g of combustion aid carbon powder and place them in a crucible.

[0035] (2) Preheat the calorimeter (6200 from Parr Company) to make the water temperature of the outer cylinder reach 30° C., seal the oxygen bomb and fill it with oxygen so that the pressure of the calorimeter reaches 2 MPa, and run the calorimeter. The running time for one sample is 6-7 minutes.

[0036] (3) After the calorimeter runs, take out the oxygen bomb, connect it to the two-stage absorption bottle containing sodium bicarbonate solution, slowly turn on the switch of the oxygen bomb, slowly release the gas in the oxygen bomb into the absorption bot...

Embodiment 2

[0043] Using the method of Example 1, take different weights of sodium sulfate (by the weight of sulfur) and measure to determine the interference of sodium sulfate on the determination of elemental sulfur content by this method. The measurement results are shown in table 2.

[0044] Table 2 Sodium sulfate sample determination result

[0045] Sodium sulfate content (mg S) Measured value ± SD (mg S) RSD (%, n=3) Recovery rate(%) 100 2.95±0.10 3.30 2.95 50 2.77±0.01 0.40 5.54 25 2.34±0.06 2.56 9.35

[0046] As can be seen from Table 2, the rate of recovery of sodium sulfate containing 100,50,25mg sulfur is only 2.95%, 5.54% and 9.35%, so when the mass ratio of elemental sulfur and sodium sulfate in the sample to be measured (by the weight of sulfur When greater than 2, the interference of sodium sulfate on the determination of elemental sulfur is less than 5%, which can be ignored.

[0047] When the mass ratio of elemental sulfur to sodi...

Embodiment 3

[0049] Using the method of Example 1, calcium sulfate (by weight of sulfur) of different weights was weighed and measured to determine the interference of calcium sulfate to the determination of elemental sulfur content by this method, and the measurement results are shown in Table 3.

[0050] Table 3 Calcium Sulfate Sample Determination Results

[0051] Calcium sulfate content (mg S) Measured value±SD(mgS) RSD (%, n=3) Recovery rate(%) 100 11.65±0.01 0.07 11.65 50 6.52±0.01 0.16 13.03 25 4.45±0.02 0.34 17.82

[0052] Find out from table 3, the rate of recovery containing the calcium sulfate of 100,50,25mg sulfur is only 11.65%, 13.03% and 17.82%, therefore when the mass ratio of elemental sulfur and calcium sulfate in the sample to be tested (by the weight of sulfur ) is greater than 4, the interference of calcium sulfate on the determination of elemental sulfur is less than 5%, which can be ignored.

[0053] When the mass ratio of el...

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Abstract

The application discloses a method for measuring elemental sulfur content in environmental samples, comprising the following steps: collecting samples; fully burning the samples under a pressure of 2 MPa; contacting the generated gas with sodium bicarbonate solution to react to generate sulfate ions; Determine the sulfate content; calculate the content of elemental sulfur in the sample based on the measured sulfate content. The method for measuring elemental sulfur content of the present invention is simple to operate, does not require complex pretreatment, and has simple steps; the medicament used in the method is safe and environmentally friendly; the measured results have high accuracy and reliable data; the cost is low and can be widely used.

Description

technical field [0001] The invention relates to a method for determining the content of elemental sulfur, in particular to a method for determining the content of elemental sulfur in environmental samples. Background technique [0002] Elemental sulfur, as an effective and inexpensive electron donor or acceptor, has been increasingly used in biological water treatment processes in recent years. For example, elemental sulfur can be used as an electron donor in the process of autotrophic denitrification process to treat drinking water and sewage; in the treatment of acid mine wastewater, sulfide generated by elemental sulfur as an electron acceptor can combine with metals in water to form precipitation, thereby removing it from the wastewater. In some cases, however, the presence of elemental sulfur can have some negative effects. For example, elemental sulfur deposited in pipes or biofilms can form sulfides, which can cause severe corrosion. In developed countries, the ann...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/96G01N30/06G01N30/14G01N31/12
Inventor 郝天伟昝飞翔陈光浩王宇
Owner GUANGZHOU HKUST FOK YING TUNG RES INST
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