CN104237424A - Method for separating and measuring trace chlorine in tar - Google Patents
Method for separating and measuring trace chlorine in tar Download PDFInfo
- Publication number
- CN104237424A CN104237424A CN201310245102.5A CN201310245102A CN104237424A CN 104237424 A CN104237424 A CN 104237424A CN 201310245102 A CN201310245102 A CN 201310245102A CN 104237424 A CN104237424 A CN 104237424A
- Authority
- CN
- China
- Prior art keywords
- tar
- chlorine
- separating
- sample
- sodium carbonate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses a method for separating and measuring trace chlorine in tar. The method comprises the following steps: a. heating a tar sample, and laying a layer of sodium carbonate on the surface of the tar after the tar is heated to be dissolved, wherein the mass ratio of sodium carbonate and the tar is 1 to (8-15); b. further burning the tar at the temperature of over 500 DEG C for ashing the tar, and eliminating organic matters; and c. cooling the sample to the room temperature after the tar sample is completely ashed, washing residual ash components by utilizing chlorine-free distilled water or deionized water, making up to volume after filtration, and measuring the content of chlorine in the solution by utilizing an ion chromatography. By adopting the burning separation technology, trace chlorine in the tar can be effectively separated and accurately measured, and a testing means is provided for accurate measurement of the content of chlorine in the tar.
Description
Technical field
The present invention relates to purification technique field, be specifically related to a kind of method of separating and assaying being separated Micro Amounts of Chlorine from tar.
Background technology
To dissociate in process of production chlorion containing a small amount of inorganic or organochlorine in tar, time in these chlorion dissolved waters of shelves, corrosion can be produced to production equipment and pipeline.Need to carry out Accurate Determining to the chlorinty in tar, assess the impact on production equipment and pipeline, to take corresponding measure further.
In prior art, in tar, the separation of Micro Amounts of Chlorine adopts extract and separate usually, namely mix with the tar after heating with without chlorine distilled water, the chlorine will adopted after water extraction in volumetric determination solution after stirring, the major defect of this technology is: 1. water can only dissolve inorganic chloride; 2. mix because water and tar are more difficult, and all chlorides all can not be extracted.Therefore, in prior art, the measurement result that the chlorine in tar is chloride is inaccurate, the chlorinity level in tar can not be reflected completely.
Summary of the invention
Therefore, the present invention to solve be difficult in the analysis of tar Micro Amounts of Chlorine accurate quantification problem, provide a kind of and can measure the method that in tar, Micro Amounts of Chlorine is chloride, be transferred in aqueous solution with ensureing the tested measured portions in tar.
Technical scheme of the present invention is, the method for separating and assaying of Micro Amounts of Chlorine in a kind of tar, and the method comprises:
A. heat tar sample, after tar heating dissolves, at tar surface paving one deck sodium carbonate, the mass ratio of described sodium carbonate and tar is 1:8-15;
B. further calcination tar, by tar ashing, organics removal, described calcination temperature is more than 500 DEG C;
C. sample is ashed completely, is cooled to room temperature, and with the ash without chlorine distilled water or deionized water wash residual, fixed rear constant volume, adopts the chlorinity in ion chromatography solution after filtration.
Sodium carbonate adopts guaranteed reagent, to grain size no requirement (NR).
In a preferred embodiment, described in described sodium carbonate, the mass ratio of sodium carbonate and tar is 1:9-12..
According to the method for separating and assaying of Micro Amounts of Chlorine in tar of the present invention, preferably, described calcination time is 1-10 hour.
Further, described calcination time is 2-5 hour.
Calcination time determines according to the size of the amount of tar sample, and sample size is large, then need the time of calcination longer; Sample size is few, then the time needed is shorter.Calcination simultaneously also ashing time and determining per sample, make the abundant ashing of tar.
According to the method for separating and assaying of Micro Amounts of Chlorine in tar of the present invention, preferably, described calcination temperature is 550 DEG C-700 DEG C.
According to the method for separating and assaying of Micro Amounts of Chlorine in tar of the present invention, further, described calcination is carried out in muffle furnace.
Calcination isolation technics is by calcination by tar ashing, and chloride is deposited in ash content with the form of sodium chloride by organics removal.
Micro Amounts of Chlorine in tar comprises inorganic chloride and organochlorine, and inorganic chloride is again based on ammonium chloride, and the vapourizing temperature of ammonium chloride is at about 270 DEG C, and for ensureing the complete ashing of tar, calcination temperature must control more than 500 DEG C;
After sample is heated to uniform temperature, oil sample is liquid condition, and the sodium carbonate added in advance is dissolved among sample, and guarantee that sodium carbonate evenly and all absorb HCl gas, change into sodium chloride, organochlorine is also fixed after calcination is decomposed.All chlorine co-exists in residual ash with the form of sodium chloride and sodium carbonate.
The invention has the beneficial effects as follows: component chlorine tested in the analysis of tar Micro Amounts of Chlorine, by effective calcination isolation technics, is transferred in aqueous solution by the present invention quantitatively.Not only can shift inorganic chlorine, also effectively displaced organochlorine, test result can chloridely with actual chlorine in tar better be coincide.As can be seen from following test result, calcination method of separating and assaying of the present invention is more accurate than the conventional getable chlorinity of extraction separating method.
The analysis data measuring the technology of the Micro Amounts of Chlorine assay of tar product are compared as follows:
Sample: product in carbolineum AMO(tar distillation), the quantivative approach of use is the chromatography of ions.
Calcination separation determination result of the present invention: 0.0075%, 0.0085%
Extraction separating method measurement result: 0.0008%.
Embodiment
Embodiment 1
The mensuration of Micro Amounts of Chlorine in tar
(1) sample determination
After tar heating melts, take the sample of about 5 grams in silica dish, sample surfaces spreads one deck sodium carbonate (about 0.5 gram), after cooling, put into muffle furnace, design temperature is 600 DEG C, (sample calcination 3 hours is ashing time and determining per sample for calcination time 3 hours, 5g oil sample ashing time in muffle furnace, at 2 hours about 30 minutes, therefore determines calcination 3 hours, can decide calcination time in practical operation according to the kind of oil sample or sample weighting amount).Sample is ashed, and is cooled to room temperature, with the ash without chlorine distilled water or deionized water wash residual, and fixed rear constant volume after filtration.Adopt the chlorinity in ion chromatography solution.
Same sample is undertaken 5 times by above-mentioned steps and measures, result (CL): 0.0278%, 0.0268%, 0.0273%, 0.0275%, 0.0262%;
(2) recovery of standard addition test
The sample adopted is the same, and standard specimen uses the chlorine standard specimen of 100mg/L.Draw 1mL standard specimen, add in sample, measure by above-mentioned steps.
Recovery of standard addition result (5 times): 99.3%, 97.1%, 93.7%9,95.1%, in 92.1%(water with ion chromatography the method for chlorine require recovery of standard addition 90%)
Embodiment 2
The bottom product of SOP(tar distillation) in the mensuration of Micro Amounts of Chlorine:
After above-mentioned tar sample heating being melted, take the sample of 5 grams in silica dish, sample surfaces spreads one deck sodium carbonate (about 0.5 gram), and after cooling, put into muffle furnace, design temperature is 600 DEG C, calcination time 3 hours.Other are with embodiment 1.
The bottom product of SOP(tar distillation) measurement result: 0.0176%, 0.0162%.
Embodiment 3
The mensuration of Micro Amounts of Chlorine in raw tar:
After above-mentioned tar sample heating being melted, take the sample of 2,3,6 grams respectively in silica dish, sample surfaces spreads one deck sodium carbonate (about 0.5 gram), and after cooling, put into muffle furnace, design temperature is 600 DEG C, calcination time 3 hours.Other are with embodiment 1.
In raw tar, Micro Amounts of Chlorine measurement result is respectively: 0.046%, 0.043%, 0.047%.
Embodiment 4
The mensuration of Micro Amounts of Chlorine in raw tar:
After above-mentioned tar sample heating being melted, take the sample of 5 grams respectively in silica dish, sample surfaces spreads one deck sodium carbonate (about 0.5 gram), and after cooling, put into muffle furnace, design temperature is respectively 400,500,600 DEG C, calcination time 3 hours.Other are with embodiment 1.
In raw tar, Micro Amounts of Chlorine measurement result is respectively: 0.042%, 0.045%, 0.044%.
Component chlorine tested in the analysis of tar Micro Amounts of Chlorine, by effective calcination isolation technics, is transferred in aqueous solution by the present invention quantitatively.Not only can shift inorganic chlorine, also effectively displaced organochlorine, test result chloridely with actual chlorine in tar better can be coincide, improve test accuracy.
Claims (6)
1. the method for separating and assaying of Micro Amounts of Chlorine in tar, is characterized in that: the method comprises:
A. heat tar sample, after tar heating dissolves, at tar surface paving one deck sodium carbonate, the mass ratio of described sodium carbonate and tar is 1:8-15;
B. further calcination tar, by tar ashing, organics removal, described calcination temperature is more than 500 DEG C;
C. sample is ashed completely, is cooled to room temperature, and with the ash without chlorine distilled water or deionized water wash residual, fixed rear constant volume, adopts the chlorinity in ion chromatography solution after filtration.
2. the method for separating and assaying of Micro Amounts of Chlorine in tar according to claim 1, it is characterized in that, described in described sodium carbonate, the mass ratio of sodium carbonate and tar is 1:9-12.
3. the method for separating and assaying of Micro Amounts of Chlorine in tar according to claim 1, it is characterized in that, described calcination time is 1-10 hour.
4. the method for separating and assaying of Micro Amounts of Chlorine in tar according to claim 3, it is characterized in that, described calcination time is 2-5 hour.
5. the method for separating and assaying of Micro Amounts of Chlorine in tar according to claim 1, it is characterized in that, described calcination temperature is 550 DEG C-700 DEG C.
6. the method for separating and assaying of Micro Amounts of Chlorine in tar according to claim 1, it is characterized in that, described calcination is carried out in muffle furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310245102.5A CN104237424A (en) | 2013-06-19 | 2013-06-19 | Method for separating and measuring trace chlorine in tar |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310245102.5A CN104237424A (en) | 2013-06-19 | 2013-06-19 | Method for separating and measuring trace chlorine in tar |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104237424A true CN104237424A (en) | 2014-12-24 |
Family
ID=52225918
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310245102.5A Pending CN104237424A (en) | 2013-06-19 | 2013-06-19 | Method for separating and measuring trace chlorine in tar |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104237424A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109425682A (en) * | 2017-08-29 | 2019-03-05 | 中粮集团有限公司 | The method of edible oil pre-treating method and the chloride ion content in measurement edible oil |
| CN114487225A (en) * | 2022-01-20 | 2022-05-13 | 东莞理工学院 | Method for measuring sulfur and chlorine content in fly ash |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009137569A1 (en) * | 2008-05-07 | 2009-11-12 | Gary Lynn Emmert | Real-time, on-line analysis of haloacetic acid species and amounts thereof in drinking water supplies |
| CN102435691A (en) * | 2009-05-14 | 2012-05-02 | 上海宝钢化工有限公司 | C1 in phenol-containing samples-Content determination method |
-
2013
- 2013-06-19 CN CN201310245102.5A patent/CN104237424A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009137569A1 (en) * | 2008-05-07 | 2009-11-12 | Gary Lynn Emmert | Real-time, on-line analysis of haloacetic acid species and amounts thereof in drinking water supplies |
| CN102435691A (en) * | 2009-05-14 | 2012-05-02 | 上海宝钢化工有限公司 | C1 in phenol-containing samples-Content determination method |
Non-Patent Citations (4)
| Title |
|---|
| 刘建权等: "氧弹燃烧2离子色谱法测定煤中氯含量", 《分析化学》 * |
| 张丽珠等: "离子色谱法测定煤中的氯", 《岩矿测试》 * |
| 王宝凤等: "离子色谱法测定配煤、焦炭和焦油中的氯含量", 《煤化工》 * |
| 陈欣娟: "煤中氯的测定及赋存形态探讨", 《陕西煤炭》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109425682A (en) * | 2017-08-29 | 2019-03-05 | 中粮集团有限公司 | The method of edible oil pre-treating method and the chloride ion content in measurement edible oil |
| CN114487225A (en) * | 2022-01-20 | 2022-05-13 | 东莞理工学院 | Method for measuring sulfur and chlorine content in fly ash |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Ishikawa et al. | Re-evaluating digestion methods for highly siderophile element and 187Os isotope analysis: Evidence from geological reference materials | |
| CN105510548A (en) | Water quality real-time monitoring system instrument calibration method for complex water environment | |
| CN104237424A (en) | Method for separating and measuring trace chlorine in tar | |
| CN103940770B (en) | The quantitative analysis method of petroleum crude oil emulsification system emulsifiability and defining method | |
| CN104914090B (en) | Detection method for continuously measuring Ga, In and Ge In lead-zinc smelting smoke dust through microwave digestion-ICP-OES | |
| CN105606484A (en) | Method for measuring silicon elements in Fe-based amorphous alloy | |
| Fafet et al. | Characterization of acidic compounds in biodegraded oils | |
| CN105571550A (en) | Method of determining float cover plate glass flake tin surface thickness and tin surface tin contents | |
| CN113299350A (en) | Method for predicting chemical index of soda salt and alkali by using soil pH | |
| CN105842388A (en) | Method for measuring sodium carbonate in sintering synergist through acid-base titration | |
| CN109580605B (en) | Method for measuring sodium chlorate content in sodium hydroxide solution | |
| CN103728199B (en) | A kind of analyzing carbon-sulfure elements method in high purity copper | |
| CN108872200B (en) | Detection method for sulfur content adsorbed on coke surface | |
| CN104133036B (en) | The analysis determining method of alundum (Al2O3) in a kind of bauxite | |
| CN106442096B (en) | The measuring method of total organic carbon in a kind of sedimentary rock | |
| CN105223200B (en) | A kind of method of content of hydrochloric acid in Accurate Determining iron chloride etchant solution | |
| CN104655713A (en) | Method for measuring lithium isotope in fluid inclusion water | |
| CN108287155A (en) | A kind of method of phosphorus content in efficient detection copper alloy | |
| CN103323451A (en) | Determination method of marble and fluorite content in electrode coating | |
| CN110412113B (en) | Method for performing oil source comparison by using strontium isotope | |
| CN102435691B (en) | Cl in phenol-containing samples-Content determination method | |
| CN105300978A (en) | Method for detecting whether warm mix asphalt contains oil-soluble amine surfactant warm mix agent | |
| CN102507476A (en) | Method for measuring cadmium in plastic sample | |
| CN106840799B (en) | Method for determining anisidine value in dry emulsion | |
| CN101629910A (en) | Method for detecting diboron trioxide content in camsellite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20141224 |