CN102313783A - Method for measuring water-quality petroleum - Google Patents
Method for measuring water-quality petroleum Download PDFInfo
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- CN102313783A CN102313783A CN2010102224210A CN201010222421A CN102313783A CN 102313783 A CN102313783 A CN 102313783A CN 2010102224210 A CN2010102224210 A CN 2010102224210A CN 201010222421 A CN201010222421 A CN 201010222421A CN 102313783 A CN102313783 A CN 102313783A
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Abstract
The invention discloses a method for measuring water-quality petroleum. The method comprises the following steps of: extracting a sample, drying, adsorbing the dried extract, concentrating, and performing quantitative analysis on the concentrate by using a standard curve, wherein in the extraction process, the sample is respectively extracted for 2 to 5 times by using dichloromethane under an alkali condition and an acid condition, and extract liquor is mixed in a conical flask to perform the next operation. In the invention, the method for measuring the water-quality petroleum is accurate, effective, simple, convenient and practicable, meets the requirement of environment friendliness and is low in prices, and a scientific basis is provided for monitoring and controlling petroleum pollution in industrial sewage of oil refineries and environmental water bodies.
Description
Technical field
The invention belongs to water quality petroleum-type analysis technical field.The detection method that relates to oil-containing industrial water and environmental monitoring water body PetroChina Company Limited. class specifically is the analytical approach of a kind of methylene chloride liquid-liquid extraction/magnesium silicate purification/gas chromatography determination water quality petroleum-type.
Background technology
Along with oil industry rapid development, the development and utilization of petroleum products is increasingly extensive, and in the exploration of oil, accumulating, processing, use, the pollution of petroleum hydrocarbon is also extensively paid close attention to.Environmental Water PetroChina Company Limited. class is an important indicator of reflection ambient water quality quality, and it has important effect for the control of water treatment effect and the evaluation of surface water quality.Receive petroleum hydrocarbon contaminated water that the oil flavor is arranged, toxic to biology, especially aromatic hydrocarbons toxicity is stronger, and petroleum hydrocarbon can form oil film at the water surface, destroys its dissolved oxygen DO balance.Therefore, petroleum hydrocarbon is carried out measurement promptly and accurately, reliable Monitoring Data is provided, be the reflection environmental quality of comprehensive science, control is polluted provides scientific basis to have great importance.
At present, China's mensuration petroleum-type standard method of analysis is " the mensuration infrared spectrophotometry of GB/T 16488-1996 water quality petroleum-type and vegetable and animals oils ".One of reagent of the extraction solvent that the shortcoming of this method is to use-phenixin strong toxicity and genus international convention Montreal Protocol on Substances that Deplete the Ozone Layer limit production and use; This requirements of convention developed country to 1966 is year superseded fully, and developing country to 2010 year all stops using.Therefore this method will be eliminated.This method is about 0.1mg/L to heavy oil method detection limit, and light oil method detection limit is about 0.01mg/L.Present international standard method of analysis has EPA 418.1, ISO9377-2:2000, ASTM D7066-04 and EPA 8015D, and wherein EPA 418.1 is similar with GB/T 16488-1996, also uses the fluorochlorohydrocarbon of ozone pact forbidding to be extractant.The used extractant hexafluoro of ASTM D7066-04 tetrachloro butane (S-316) complex manufacturing costs an arm and a leg, and is difficult to promote.ISO 9377-2:2000 extractant n-pentane is difficult to obtain high purity reagent, and comparatively expensive, has limited the method application.EPA 8015D does not remove the non-hydrocarbon materials in the extract, and measuring the result is organism (DRO) in the diesel range.
Summary of the invention
Deficiency to prior art; The assay method that the purpose of this invention is to provide a kind of accurate and effective, self compliance with environmental protection requirements, simple and easy to do, cheap water quality petroleum-type is for refinery industrial waste water and the class pollution monitoring of environment water PetroChina Company Limited. and control provide scientific basis.
Mensuration process of the present invention is following: at first to sample extract, drying, then dried extract is adsorbed, concentrates, at last concentrate is carried out quantitative test with typical curve.Extraction process wherein is: sample is respectively extracted 2～5 times with methylene chloride under alkalescence and acid condition, and combining extraction liquid carries out next step operation in conical flask.
Following to sample extraction and drying process process in the mensuration process of the present invention: the water sample of measuring certain volume with graduated cylinder places the taper separating funnel; Regulate the sample pH value value with certain density sodium hydroxide solution and sulfuric acid solution respectively; Its methylene chloride with certain volume under alkalescence (pH>=11) and acid (pH≤2) or acid (pH≤2) and alkalescence (pH>=11) condition is respectively extracted 2～5 times, and combining extraction liquid is in conical flask.The consumption of methylene chloride is 5%～15% of a sample volume during sample extraction.Extraction process can extract 2～5 times under alkali condition earlier, under acid condition, extracts 2～5 times then; Also can under acid condition, extract 2～5 times earlier, under alkali condition, extract 2～5 times then.
Add anhydrous sodium sulfate in the extract after merging and carry out drying, till not luming to anhydrous sodium sulfate.Anhydrous sodium sulfate heats 20h down at 600 ℃ in advance.
Following in the mensuration process of the present invention: that above-mentioned extract is adsorbed through the magnesium silicate adsorbent to sample absorption and concentration process.Magnesium silicate heats 2h down at 500 ℃ in advance.During the magnesium silicate adsorbent is packed glass chromatography column into after treatment, fill certain altitude.The methylene chloride of the glass chromatography column that is filled with the magnesium silicate adsorbent with certain volume washed in advance, use the dichloromethane rinse of certain volume after waiting to adsorb again.Filtrating after the absorption is collected in the three ball K-D concentrating instruments.It is concentrated that collection filtrating makes it accomplish within a certain period of time at a certain temperature.
It is following in the mensuration process of the present invention sample analysis and typical curve to be prepared process: get the certain volume concentrate and inject the gas chromatograph analysis of being furnished with flame ionization detector, carry out quantitatively with typical curve.Choose additive-free 0 in the preparation of typical curve
#Diesel oil is as standard substance, adopts external standard method, with 4～50min integral area A (integration unit) to additive-free 0
#Diesel oil sample size (m) is done linear regression, makes a typical curve.
In the assay method of petroleum-type of the present invention, key is that (1) employing does not have the methylene chloride reagent of destruction under suitable process and condition, to carry out pre-treatment to ozonosphere.(2) this method can reflect the carbon number distribution and the fingerprint characteristic of petroleum-type, and monitoring and control for pollution source provides scientific basis.
Description of drawings
Fig. 1 is the glass chromatography column synoptic diagram that magnesium silicate is housed.
Among the figure: 1-magnesium silicate adsorbent, 2-glass wool, 3-glass chromatography column.
Embodiment
A kind of concrete grammar of the present invention below is described.
The preparation standard curve is a solvent with the methylene chloride, with additive-free 0
#Diesel oil is done standard specimen, takes by weighing 4.0002g additive-free 0
#Constant volume is as the standard stock solution in the 10mL volumetric flask for diesel oil, and its concentration is 4.00 * 10
5Ng μ L
-1Extract standard stock solution constant volume in the 10mL volumetric flask of different volumes respectively.Being mixed with concentration is 400ng μ L
-1, 800ng μ L
-1, 1.60 * 10
3Ng μ L
-1, 3.20 * 10
3Ng μ L
-1, 7.20 * 10
3Ng μ L
-1Standard solution, use external standard method, get above-mentioned standard solution 1 μ L respectively and in the flame ionization detector gas chromatograph, analyze, with 4～50min integral area A (integration unit) to additive-free 0
#Diesel oil sample size (m) is done linear regression, gets typical curve.
Gathered certain refinery aeration tank outlet and oxidation ditch outlet water sample respectively, measured the 1L water sample respectively in 2L taper separating funnel, used 10molL respectively with graduated cylinder
-1Sodium hydroxide solution and 1: 1 (v/v) sulfuric acid solution are regulated the sample pH value value, under alkalescence (pH>=11) and acid (pH≤2) condition, respectively extract three times, and each methylene chloride consumption is 60ml, and combining extraction liquid is in conical flask.Add in the extract after merging in advance and carry out drying, till not luming to anhydrous sodium sulfate at 600 ℃ of anhydrous sodium sulfates that heat 20h down.Extract after the drying is adsorbed through heating the 2h magnesium silicate down at 500 ℃ in advance, and the magnesium silicate adsorbent is seated in the glass chromatography column, packed height 80mm.The chromatographic column that the magnesium silicate adsorbent is housed is washed with the 30mL methylene chloride in advance, wait to adsorb the back and wash with the 50mL methylene chloride.Filtrating after the absorption is collected in the three ball K-D concentrating instruments, at 80～90 ℃ it is accomplished in 10～20min and concentrate, concentrated volume is 1mL.Get 1.0 μ L concentrates and inject the gas chromatograph analysis of being furnished with flame ionization detector, carry out quantitatively with typical curve.Measure result and China's GB/T 16488-1996 result comparison and see table 1.
Two kinds of methods of table 1 are measured the result relatively
Claims (10)
1. the assay method of a water quality petroleum-type, at first to sample extract, drying, then dried extract is adsorbed, concentrates, at last concentrate is carried out quantitative test with typical curve; It is characterized in that described extraction process is following: sample is respectively extracted 2～5 times with methylene chloride under alkalescence and acid condition, and combining extraction liquid carries out next step operation in conical flask.
2. according to the described method of claim 1, it is characterized in that: the consumption of methylene chloride is 5%～15% of a sample volume during sample extraction.
3. according to the described method of claim 1, it is characterized in that: the pH value of alkali condition is pH>=11, and the pH value of acid condition is pH≤2.
4. according to claim 1 or 3 described methods, it is characterized in that: alkali condition or acid condition adopt sodium hydroxide solution and sulfuric acid solution to regulate the sample pH value value.
5. according to the described method of claim 1, it is characterized in that: drying means carries out drying for adding anhydrous sodium sulfate in the extract after merging, till not luming to anhydrous sodium sulfate.
6. according to the described method of claim 1, it is characterized in that: dried extract adsorbs employing magnesium silicate adsorbent and adsorbs.
7. according to the described method of claim 1, it is characterized in that: it is following that sample analysis and typical curve are prepared process: get concentrate and inject the gas chromatograph analysis of being furnished with flame ionization detector, carry out quantitatively with typical curve.
8. according to the described method of claim 7, it is characterized in that: choose additive-free 0 in the preparation of typical curve
#Diesel oil is as standard substance, adopts external standard method, with 4～50min integral area to additive-free 0
#The diesel oil sample size is done linear regression, makes typical curve.
9. according to claim 1 or 3 described methods, it is characterized in that: under alkali condition, extract 2～5 times earlier, under acid condition, extract 2～5 times then.
10. according to claim 1 or 3 described methods, it is characterized in that: under acid condition, extract 2～5 times earlier, under alkali condition, extract 2～5 times then.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102224210A CN102313783A (en) | 2010-07-07 | 2010-07-07 | Method for measuring water-quality petroleum |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102224210A CN102313783A (en) | 2010-07-07 | 2010-07-07 | Method for measuring water-quality petroleum |
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| Publication Number | Publication Date |
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| CN102313783A true CN102313783A (en) | 2012-01-11 |
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| CN2010102224210A Pending CN102313783A (en) | 2010-07-07 | 2010-07-07 | Method for measuring water-quality petroleum |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105181922A (en) * | 2015-09-18 | 2015-12-23 | 上海昂林科学仪器有限公司 | Device for measuring animal and plant oil |
| CN109612958A (en) * | 2018-12-18 | 2019-04-12 | 海阳市启恒环保科技有限公司 | The method and device thereof of a variety of oils concentration in water can be measured simultaneously |
| CN110487733A (en) * | 2019-08-09 | 2019-11-22 | 南通化学环境监测站有限公司 | A kind of measurement surface water, underground water, in seawater petroleum-type measuring method |
-
2010
- 2010-07-07 CN CN2010102224210A patent/CN102313783A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 周艳红等: "气相色谱法测定水中萃取性石油烃", 《第十七届全国色谱学术报告会论文集》 * |
| 穆肃等: "气相色谱法测定水中总石油烃", 《第八次全国环境监测学术交流会论文集》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105181922A (en) * | 2015-09-18 | 2015-12-23 | 上海昂林科学仪器有限公司 | Device for measuring animal and plant oil |
| CN109612958A (en) * | 2018-12-18 | 2019-04-12 | 海阳市启恒环保科技有限公司 | The method and device thereof of a variety of oils concentration in water can be measured simultaneously |
| CN110487733A (en) * | 2019-08-09 | 2019-11-22 | 南通化学环境监测站有限公司 | A kind of measurement surface water, underground water, in seawater petroleum-type measuring method |
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Application publication date: 20120111 |