CN102539340A - Method for determining oil content and organic matter content in synthetic ammonia - Google Patents
Method for determining oil content and organic matter content in synthetic ammonia Download PDFInfo
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- CN102539340A CN102539340A CN2010105882931A CN201010588293A CN102539340A CN 102539340 A CN102539340 A CN 102539340A CN 2010105882931 A CN2010105882931 A CN 2010105882931A CN 201010588293 A CN201010588293 A CN 201010588293A CN 102539340 A CN102539340 A CN 102539340A
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- synthetic ammonia
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Abstract
The invention provides a method for determining an oil content and an organic matter content in synthetic ammonia. The method is characterized in that a synthetic ammonia sampler with volume of 50-100 ml is adopted to accurately sample, and an infrared spectrum method is adopted to determine the oil content and the organic matter content in the synthetic ammonia. The method of the present invention has the following advantages that: the method has high sensitivity and high accuracy, the sampling amount of the used synthetic ammonia sampling container is small, the operation is convenient, rapid and accurate, and the method is applicable for synthetic ammonia production and production control analysis adopting the synthetic ammonia as the raw material.
Description
Technical field
The present invention relates to a kind of method of measuring in the synthetic ammonia oil and organic content, be applicable to that it is the analysis of production control of raw material that Ammonia Production reaches with synthetic ammonia.
Background technology
Oil has three kinds with organic method in the domestic and international existing analysis synthetic ammonia, i.e. three-wavelength infrared spectrophotometer, ultraviolet spectrophotometry and gravimetric method, and the common ground of three kinds of methods is all to need ammonia sample to be synthesized to volatilize afterwards with solvent extraction oil content wherein.But the three-wavelength infrared spectrophotometer needs the analytical instrument of more valuable precision and special cell for infrared absorption, and operation easier is big, and sensitivity is very low, and required sampling amount is bigger, has also limited its analysis speed.And the maximum drawback of gravimetric method is that analysis operation is loaded down with trivial details, and length consuming time can't satisfy the actual needs of production.And ultraviolet spectrophotometry receives the influence of oil ingredient kind bigger, and the sensitivity of different oil content uv absorption differs bigger, so this method is not suitable for analyzing the oil content content in the various different samples.
Summary of the invention
The object of the present invention is to provide a kind of method of measuring in the synthetic ammonia oil and organic content.
The present invention is achieved in that and uses volume accurately to take a sample as the synthetic ammonia ST of 50ml-100ml; Adopt oil and organism in the not beam split infrared spectroscopic determination synthetic ammonia; With carbon tetrachloride solution after purifying and standard solution calibration oil content concentration meter: will dissolve in the sample carbon tetrachloride solution of oily substance and measure with calibrated oil content concentration analyzer, the instrument displayed value is the total amount of oily substance in the sample.
Concrete steps are following:
1. the processing of phenixin
Phenixin (analyzing pure) is used the active carbon adsorption of activation, remove organic impurities wherein.
2. standard oil preparation
By 2,2,4-trimethylpentane (isooctane) (analyzing pure), n-hexadecane (analyzing pure) and benzene (analyzing pure) mix.
3. the preparation of standard oil calibration solutions
Take by weighing standard oil, with the phenixin dissolving and the constant volume that have purified.
Instrument, reagent that the present invention is used:
OCMA-220 type oil content concentration analyzer
Activated charcoal: 40-60 order, 350 ℃ of-400 ℃ of activation 2 hours.
Phenixin: use preceding through activated carbon chromatography post adsorption treatment.
2,2,4-trimethylpentane (isooctane):
N-hexadecane
Benzene
4. sample analysis: take sample with the synthetic ammonia ST, the ammonia to be synthesized oily substance of clean back after with the phenixin dissolving volatilization of equal-volume purified treatment that volatilize naturally shakes up.Carbon tetrachloride solution is transferred in the calibrated OCMA-220 type oil content concentration analyzer measuring cell, measures, instrument is the oily substance total amount in the show sample.
Good effect of the present invention is to adopt not beam split infra-red sepectrometry to analyze oil and organism in the synthetic ammonia; Measure C-H base total amount; Method detectability 0.1mg/L, the coefficient of variation is high less than 1.0% sensitivity, accuracy, the synthetic ammonia ST of employing; Sampling amount is few, and is easy to operate, quick, accurate.
Embodiment
Embodiment 1: oil and organism analytical approach in the raw material synthetic ammonia
Instrument reagent is prepared:
OCMA-220 type oil content concentration analyzer activated charcoal: 40-60 order, 350 ℃ of-400 ℃ of activation 2 hours.
Phenixin: with preceding through activated carbon chromatography post adsorption treatment.
2,2,4-trimethylpentane (isooctane)
N-hexadecane
Benzene
The processing of phenixin
Get one of 150mI base buret, the lower end insert absorbent cotton a little, it is high to refill the about 90cm of the activated charcoal of inserting activation, existing activated carbon chromatography post.With the phenixin chromatographic column of flowing through, adsorbing and removing organic impurities wherein.This chromatographic column is once stared at and is purified about 6000ml phenixin.
The standard oil preparation:
By 37.5% 2,2,4-trimethylpentane (isooctane), 37.5% n-hexadecane and 25% benzene mix to be formed.
The preparation of standard oil calibration solutions
Accurately take by weighing about 0.3g standard oil (being accurate to 0.0001g) in the 150mI volumetric flask with analytical balance; With dissolving of the phenixin that purified and constant volume, draw constant volume again after concentration be solution 6.00ml to the 300ml volumetric flask of 120mg/L and shake up with the phenixin constant volume.
Instrument calibration: carbon tetrachloride solution is added sample cell, measure and return to zero with the zero-bit adjusting knob: then above-mentioned standard solution is added sample cell, measurement, and regulated quantity to make instrument readings apart from knob be to mark the liquid actual concentrations.Repeat soil and state step 3 time, note must fully cleaning the sample measurement pond when changing test fluid at every turn, stable until instrument readings.
Sample analysis: take certain producer's synthetic ammonia sample with the synthetic ammonia sampling jar, in vent cabinet, ammonia to be synthesized volatilizees totally naturally.The phenixin of having handled with equal-volume dissolves the oily substance after volatilizing, and shakes up.Carbon tetrachloride solution is transferred in the calibrated QCMA-220 type oil content concentration analyzer measuring cell, measures, instrument is the oily substance total amount in the show sample.Learn in this synthetic ammonia that oil and organic content are 36mg/L.
When measuring the result is unit when quoting with mg/Kg, oil and organic content=36/1.914, i.e. 56.4mg/Kg.
Embodiment 2: this example is the analysis whether leakage of oil is carried out oil and organism in the synthetic ammonia product of inspection synthetic ammonia compressor for Ammonia Production unit.1. to oil content analysis in the compressor inlet synthetic ammonia; Operation steps is with embodiment 1; Record the result for 15mg/L 2. to oil content analysis in the compressor outlet synthetic ammonia, operation steps is with embodiment 1, oil-containing has increased 30mg/L to this compressor in the synthetic ammonia because of seepage causes for 45mg/L dies to record the result.
Claims (2)
1. the present invention relates to a kind of method of measuring in the synthetic ammonia oil and organic content, it is characterized in that with the volume being that the liquefied ammonia ST of 50ml-100ml is accurately taken a sample oil and organism in the employing infrared spectroscopic determination liquefied ammonia.
2. according to the described a kind of method of measuring oil and organic content in the synthetic ammonia of claims 1; It is characterized in that: with carbon tetrachloride solution after purifying and standard solution calibration oil content concentration meter: will dissolve in the sample carbon tetrachloride solution of oily substance and measure with calibrated oil content concentration analyzer, the instrument displayed value is the total amount of oily substance in the sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105882931A CN102539340A (en) | 2010-12-15 | 2010-12-15 | Method for determining oil content and organic matter content in synthetic ammonia |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105882931A CN102539340A (en) | 2010-12-15 | 2010-12-15 | Method for determining oil content and organic matter content in synthetic ammonia |
Publications (1)
| Publication Number | Publication Date |
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| CN102539340A true CN102539340A (en) | 2012-07-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2010105882931A Pending CN102539340A (en) | 2010-12-15 | 2010-12-15 | Method for determining oil content and organic matter content in synthetic ammonia |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103558116A (en) * | 2013-11-21 | 2014-02-05 | 李耀文 | Method for determining concentration of ammonium chloride liquid ammonia solution |
| CN104807715A (en) * | 2015-04-21 | 2015-07-29 | 国家电网公司 | Method for quantifying mineral oil content in sulfur hexafluoride gas |
| CN111366551A (en) * | 2018-12-26 | 2020-07-03 | 中核北方核燃料元件有限公司 | Method for determining carbon content in uranium zirconium alloy |
-
2010
- 2010-12-15 CN CN2010105882931A patent/CN102539340A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103558116A (en) * | 2013-11-21 | 2014-02-05 | 李耀文 | Method for determining concentration of ammonium chloride liquid ammonia solution |
| CN104807715A (en) * | 2015-04-21 | 2015-07-29 | 国家电网公司 | Method for quantifying mineral oil content in sulfur hexafluoride gas |
| CN111366551A (en) * | 2018-12-26 | 2020-07-03 | 中核北方核燃料元件有限公司 | Method for determining carbon content in uranium zirconium alloy |
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Application publication date: 20120704 |