CN110567945A - Method for testing nitrogen and sulfur content in petroleum products - Google Patents

Method for testing nitrogen and sulfur content in petroleum products Download PDF

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Publication number
CN110567945A
CN110567945A CN201910706864.8A CN201910706864A CN110567945A CN 110567945 A CN110567945 A CN 110567945A CN 201910706864 A CN201910706864 A CN 201910706864A CN 110567945 A CN110567945 A CN 110567945A
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CN
China
Prior art keywords
sample
testing
nitrogen
sulfur content
steps
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Pending
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CN201910706864.8A
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Chinese (zh)
Inventor
徐娜
程瑞琴
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WUXI ZHONGTIAN SOLID WASTE DISPOSAL Co Ltd
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WUXI ZHONGTIAN SOLID WASTE DISPOSAL Co Ltd
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Priority to CN201910706864.8A priority Critical patent/CN110567945A/en
Publication of CN110567945A publication Critical patent/CN110567945A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/76Chemiluminescence; Bioluminescence

Abstract

The invention discloses a method for testing the nitrogen and sulfur content in petroleum products, which comprises the following steps: 1) selecting a sample, wherein the sample is a solid sample or a liquid sample; 2) carrying out pretreatment work on the sample, and carrying out primary treatment work on the sample selected in the step 1); 3) weighing the sample pretreated in the step 2); 4) carrying out test work on the sample weighed in the step 3); 5) and (4) carrying out corresponding data processing on the data tested in the step 4). The invention effectively solves the problems of long test time, limitation, low accuracy and the like in the prior art, and the test method of the invention can test hazardous wastes in a wide variety, wherein the solid includes: samples such as organic solid residues, activated carbon, sludge, coal slag and the like; the liquid samples comprise various organic waste liquids, petroleum and the like, the operation is simple, the convenience in testing is effectively improved, and the use of people is facilitated.

Description

Method for testing nitrogen and sulfur content in petroleum products
Technical Field
The invention relates to the field of nitrogen and sulfur testing, in particular to a method for testing the content of nitrogen and sulfur in petroleum products.
Background
the influence of nitrogen on the performance of petroleum products is complex, and the naturally-occurring nitrogen can become an effective component for resisting the wear of diesel oil and can also become a negative factor of the oxidation stability of lubricating oil; certain synthetic nitrogen-containing compounds are excellent additives for improving product properties.
the quality index of sulfur content in petroleum products not only affects the emission of automobile exhaust, but also is an important index related to the corrosion of engine equipment, because sulfur in fuel oil can generate sulfate in an exhaust system of an engine to form particulate matters and be emitted, and sulfur dioxide formed after the sulfur is combusted is also an important substance causing air pollution; meanwhile, the large amount of sulfur content also reduces the oxidation stability of the oil product, deepens the color of the oil product, generates sediments to reduce the quality of the oil product, and has more active chemical properties of sulfur element.
If partial hydrogen sulfide or sulfur dioxide exists in the exhaust gas of a petroleum device in a refinery, the exhaust gas reacts with moisture in the air to quickly form acid rain, so that the environment is polluted, the ecological balance is destroyed, a certain amount of sulfide is added into another petroleum product, the quality of the oil product can be improved, the activity and the service life of a catalyst are improved, and the quality of the oil product is improved.
Disclosure of Invention
The invention mainly aims to provide a method for testing the content of nitrogen and sulfur in petroleum products, which effectively solves the problems of long testing time, limitation, low accuracy and the like in the prior art, and the testing method can test a wide variety of hazardous wastes, wherein the solid substances comprise: samples such as organic solid residues, activated carbon, sludge, coal slag and the like; the liquid samples comprise various organic waste liquids, petroleum and the like, the operation is simple, the convenience in testing is effectively improved, and the use of people is facilitated.
In order to achieve the purpose, the invention adopts the technical scheme that:
The invention discloses a method for testing the nitrogen and sulfur content in petroleum products, which comprises the following steps:
1) selecting a sample, wherein the sample is a solid sample or a liquid sample;
2) Carrying out pretreatment work on the sample, and carrying out primary treatment work on the sample selected in the step 1);
3) Weighing the sample pretreated in the step 2);
4) Carrying out test work on the sample weighed in the step 3);
5) and (4) carrying out corresponding data processing on the data tested in the step 4).
Preferably, the solid sample in the step 1) adopts organic solid residue, activated carbon, sludge and coal cinder.
preferably, the liquid sample in step 1) is organic waste liquid or petroleum liquid sample.
preferably, in the step 2), the solid sample is pretreated by screening and crushing, and the liquid sample is pretreated by adding a diluent or solvent oil.
Preferably, heptane or isooctane is adopted as the diluent, and No. 6 solvent oil is selected as the solvent oil.
preferably, the total nitrogen standard solution of the solid sample or the hydraulic sample after 0, 100, 500 and 1000mg/L pretreatment in the step 2) is selected to draw a curve.
Preferably, after the curve linearly meets the test requirements, the test is performed using the solid sample or the liquid sample used in the curve.
preferably, the pretreated solid sample or liquid sample is weighed in the step 4) and transferred to a sample injection system for testing, wherein the sample injection system adopts a TNS-3000 chemiluminescence nitrogen measuring instrument detection system.
Compared with the prior art, the invention has the following beneficial effects:
The problems of long test time, limitation, low accuracy and the like in the prior art are effectively solved, the test method disclosed by the invention can test hazardous wastes in a wide variety, wherein the solid category comprises: samples such as organic solid residues, activated carbon, sludge, coal slag and the like; the liquid samples comprise various organic waste liquids, petroleum and the like, the operation is simple, the convenience in testing is effectively improved, and the use of people is facilitated.
Drawings
FIG. 1 is a flow chart of a method for testing the nitrogen and sulfur content in petroleum products according to the present invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
total nitrogen and total sulfur content test of fuel oil
Drawing a standard curve: respectively transferring 0 mg/TS (total nitrogen concentration)/10 uL (total nitrogen concentration)/TS (total nitrogen concentration) standard solutions of 0mg/L, 10 mg/TS, 50 mg/L and 100mg/L into a quartz support boat, introducing the quartz support boat into a TNS-3000 chemiluminescence nitrogen measuring instrument detection system under the action of high-purity oxygen and high-purity argon at 950 ℃, detecting, making three parallel samples, taking an average value, recording data, and drawing a standard curve or a low-concentration curve;
weighing 2-8uL of fuel oil, completing sample selection, sample wafer pretreatment and weighing of the pretreated sample in a quartz boat, entering a TSN-3000 chemiluminescence nitrogen measuring instrument detection system under the action of 950 ℃, high-purity oxygen and high-purity argon, performing detection work, simultaneously measuring the nitrogen and sulfur content, making three parallel samples, and taking an average value;
Thirdly, data processing and averaging are carried out, and detailed data are shown in the following table one:
Watch 1
example 2
Total nitrogen and total sulfur content test of waste activated carbon
Drawing a standard curve: respectively transferring 0 mg/TS (total nitrogen concentration)/10 uL (total nitrogen concentration)/TS (total nitrogen concentration) standard solutions of 0mg/L, 10 mg/TS, 50 mg/L and 100mg/L into a quartz support boat, introducing the quartz support boat into a TNS-3000 chemiluminescence nitrogen measuring instrument detection system under the action of high-purity oxygen and high-purity argon at 950 ℃, detecting, making three parallel samples, taking an average value, recording data and drawing a standard curve;
Secondly, crushing and polishing the active carbon, respectively weighing 2-8mg of samples after screening out uniform samples, recording the specific numerical value to be accurate to 0.00001, finishing the sample selection, sample pretreatment and the work of weighing the pretreated samples, entering a TNS-3000 chemiluminescence nitrogen detector detection system in a quartz support boat under the action of 950 ℃ high-purity oxygen and high-purity argon for detection, simultaneously measuring the nitrogen and sulfur content, making three parallel samples, and taking an average value;
thirdly, data processing and averaging are carried out, and detailed data are shown in the following table two:
Watch two
example 3
Organic waste liquid nitrogen and sulfur content test
Drawing a standard curve: respectively transferring 10uL of TN/TS standard solution of 0mg/L, 100mg/L, 500 mg/L and 1000mg/L into a quartz support boat, introducing into a TNS-3000 chemiluminescence nitrogen measuring instrument detection system under the action of high-purity oxygen and high-purity argon at 950 ℃, detecting, making three parallel samples, taking an average value, recording data and drawing a standard curve;
diluting an organic waste liquid sample by 10 times with No. 6 solvent oil, transferring a 2-8uL sample, completing sample selection, sample pretreatment and sample weighing after pretreatment, entering a TNS-3000 chemiluminescence nitrogen measuring instrument detection system in a quartz boat under the action of 950 ℃, high-purity oxygen and high-purity argon for detection, simultaneously measuring the nitrogen and sulfur content, making three parallel samples, and taking an average value;
thirdly, data processing and averaging are carried out, and detailed data are shown in the following table three:
Watch III
In the above embodiments 1-3, different organic solid and liquid samples are detected to obtain the nitrogen and sulfur content therein, the steps are simple, the operation is convenient, the data accuracy is high, and the problems of long test time, limitation, low accuracy and the like in the past are effectively solved. Samples such as organic solid residues, activated carbon, sludge, coal slag and the like; the liquid samples comprise various organic waste liquids, petroleum and the like, so that the convenience in testing is effectively improved, and the use by people is facilitated.
the foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (8)

1. A method for testing the content of nitrogen and sulfur in petroleum products is characterized by comprising the following steps: the method comprises the following steps:
1) Selecting a sample, wherein the sample is a solid sample or a liquid sample;
2) carrying out pretreatment work on the sample, and carrying out primary treatment work on the sample selected in the step 1);
3) Weighing the sample pretreated in the step 2);
4) Carrying out test work on the sample weighed in the step 3);
5) And (4) carrying out corresponding data processing on the data tested in the step 4).
2. The method for testing the nitrogen and sulfur content in the petroleum product according to claim 1, wherein the method comprises the following steps: the solid sample in the step 1) adopts organic solid residues, activated carbon, sludge and coal cinder.
3. The method for testing the nitrogen and sulfur content in the petroleum product according to claim 2, wherein the method comprises the following steps: the liquid sample in the step 1) adopts organic waste liquid and petroleum liquid samples.
4. the method for testing the nitrogen and sulfur content in the petroleum product according to claim 1, wherein the method comprises the following steps: in the step 2), screening and crushing are adopted to pretreat the solid sample, and diluent or solvent oil is selected to be added to pretreat the liquid sample.
5. The method for testing the nitrogen and sulfur content in the petroleum product according to claim 4, wherein the method comprises the following steps: the diluent adopts heptane or isooctane, and the solvent oil is No. 6 solvent oil.
6. the method for testing the nitrogen and sulfur content in the petroleum product according to claim 1, wherein the method comprises the following steps: and 2) selecting total nitrogen standard solution of the solid sample or the hydraulic sample after 0, 100, 500 and 1000mg/L pretreatment in the step 2) to draw a curve.
7. The method for testing the nitrogen and sulfur content in the petroleum product according to claim 6, wherein the method comprises the following steps: after the curve linearly meets the test requirements, the solid sample or the liquid sample adopted in the curve is used for testing.
8. The method for testing the nitrogen and sulfur content in the petroleum product according to claim 1, wherein the method comprises the following steps: and 4) weighing the pretreated solid sample or liquid sample in the step 4), transferring the solid sample or liquid sample to a sample introduction system for testing, wherein the sample introduction system adopts a TNS-3000 chemiluminescence nitrogen measuring instrument detection system.
CN201910706864.8A 2019-08-01 2019-08-01 Method for testing nitrogen and sulfur content in petroleum products Pending CN110567945A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN203732524U (en) * 2014-01-07 2014-07-23 南京信息工程大学 Wireless communication networked sulfur-nitrogen element analyzer
CN103969456A (en) * 2013-02-01 2014-08-06 姜堰市高科分析仪器有限公司 Automatic sulfur-nitrogen determination instrument
CN203870059U (en) * 2014-04-03 2014-10-08 南京信息工程大学 Portable sulfur and nitrogen elemental analyzer
CN204116235U (en) * 2014-10-29 2015-01-21 江苏新高科分析仪器有限公司 A kind of chemiluminescence azotometer
CN109342405A (en) * 2018-11-28 2019-02-15 东营联合石化有限责任公司 The detection method of wax oil nitrogen content

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103969456A (en) * 2013-02-01 2014-08-06 姜堰市高科分析仪器有限公司 Automatic sulfur-nitrogen determination instrument
CN203732524U (en) * 2014-01-07 2014-07-23 南京信息工程大学 Wireless communication networked sulfur-nitrogen element analyzer
CN203870059U (en) * 2014-04-03 2014-10-08 南京信息工程大学 Portable sulfur and nitrogen elemental analyzer
CN204116235U (en) * 2014-10-29 2015-01-21 江苏新高科分析仪器有限公司 A kind of chemiluminescence azotometer
CN109342405A (en) * 2018-11-28 2019-02-15 东营联合石化有限责任公司 The detection method of wax oil nitrogen content

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
吴国良: "发光法测定石油产品中的硫氮含量", 《第十届全固有机分析学术研讨会》 *

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