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A method for determining the concentration of aniline in aromatic amines in workplaces

An aromatic amine, workplace technology, applied in the field of chemical compound detection, can solve the problems of increased column damage, column damage, high price, etc., to achieve the effect of ensuring accuracy, reducing usage, and ensuring precision and accuracy

Active Publication Date: 2017-09-01
JIANGSU TAIJIE INSPECTION TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If you can’t find the right conditions, the peak will not come out or the peak will be incomplete, which will affect the accuracy of the detection data
[0003] For many items detected by gas chromatography, according to the standard requirements, different items require different chromatographic columns, so frequent replacement of chromatographic columns leads to increased risk of column damage
A chromatographic column is very expensive (a capillary is about 5,000 yuan a piece), and frequent replacement of the column can easily cause damage to the column, and it is time-consuming

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Adopt gas chromatography to measure the detection method of cyclohexylamine:

[0019] 1. Instrument

[0020] Silicone tube, solvent desorption type, filled with 200mg / 100mg silica gel.

[0021] Activated carbon tube, solvent desorption type, filled with 100mg / 50mg activated carbon.

[0022] Air sampler, flow rate 0~500ml / min.

[0023] Solvent analysis bottle, 5ml

[0024] Microsyringe, 10ml

[0025] Gas Chromatograph, Hydrogen Flame Ionization Detector

[0026] 2. Instrument testing conditions:

[0027] HP-INWWAX capillary column;

[0028] The column temperature is 180 degrees;

[0029] The vaporization chamber temperature is 220 degrees;

[0030] The temperature of the detection room is 240 degrees;

[0031] The carrier gas flow rate is 5ml / min.

[0032] 3. Reagents:

[0033] Desorption solution: absolute ethanol

[0034] 4. Sample collection:

[0035] Short-term sampling: At the sampling point, open both ends of the silicone tube and collect air samples f...

Embodiment 2

[0060] Precision measurement experiment of the present invention:

[0061] Draw four samples of 30 μl into four 1ml analysis bottles, respectively labeled 183, 184, 185 and 186, and carry out the determination of the sample concentration by the sample determination method of Example 1, the results are as follows:

[0062] Sample number A (absorbance) C (concentration μg / ml) Aniline 183 297.356 378.482 Aniline 184 297.391 378.528 Aniline 185 297.463 378.619 Aniline 186 297.427 378.573

[0063] After calculation, the average concentration of aniline is 378.551μg / ml, and the results of the sample show that the precision test meets the requirements of the standard.

[0064] After setting the appropriate measurement conditions in this example, the detection of other compounds in aromatic compounds can also be carried out at the same time, which solves the problem of frequent column replacement and easy damage to the column and time-consu...

Embodiment 3

[0066] Spike recovery experiment:

[0067] Pipette 30μl of 12.58mg / ml concentrated standard and 30μl of aniline sample into 1ml analysis bottle respectively, and the recoveries of each standard addition are shown in the table below:

[0068] Sample number A C Aniline 1 305.337 388.638 Aniline 2 308.180 392.292 Aniline 3 308.263 392.358 Aniline 4 305.295 388.582

[0069] Calculated: the recovery rate of the addition of sample 1 is 99.97%;

[0070] The standard recovery rate of sample 2 was 100.93%;

[0071] The standard recovery rate of sample 3 was 100.95%;

[0072] Spike recovery for sample 4 was 99.95%

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PUM

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Abstract

The invention discloses a method for measuring the concentration of aniline in aromatic amines in workplaces, which includes sample collection, sample processing, preparation and measurement of standard solutions, preparation and measurement of standard curves, and the gas phase conditions of the gas chromatograph in the determination steps are set as HP-INWWAX capillary column is used, the column temperature is 180 degrees, the vaporization chamber temperature is 220 degrees, the detection chamber temperature is 240 degrees, and the carrier gas flow rate is 5ml / min. In the method for measuring the concentration of aniline in aromatic amines in the workplace of the present invention, the column temperature is 180 degrees, the temperature of the vaporization chamber is 220 degrees, the temperature of the detection chamber is 240 degrees, and the flow rate of the carrier gas is 5ml / min to detect aromatic amines. The detection data of aniline compounds is accurate, in line with national requirements, time-saving and efficient. After choosing this HP‑INWWAX capillary and setting appropriate measurement conditions, it can also detect other compounds in aromatic compounds at the same time, which solves the problem of frequent Replacing the column is easy to cause damage to the column and time-consuming problems, which saves time and more importantly, ensures the accuracy of the data.

Description

technical field [0001] The invention relates to a method for measuring the concentration of aniline in aromatic amines in a workplace, belonging to the field of chemical detection of compounds. Background technique [0002] For the determination of air toxic substances in the workplace, the detection method of aromatic compounds is generally by gas chromatography. The national standard requires the determination of aromatic anilines to be 2m×4mm, FFAP`:KOH:chromosorb WAWDMCS=10:100 Chromatographic column, column temperature: 170 degrees; vaporization chamber temperature: 230 degrees; detection chamber temperature: 260 degrees; carrier gas (nitrogen) flow rate: 40ml / min. Similarly, gas chromatography can also be used in the determination of other aromatic air toxic substances. The core technology is to select and use a suitable chromatographic column and suitable column temperature, vaporization chamber temperature, detection chamber temperature and carrier gas flow. If no s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/60G01N30/06
Inventor 周树华袁亚丹
Owner JIANGSU TAIJIE INSPECTION TECH