美國wilks紅外測(cè)油儀萃取方法

10：1水中油萃取過程

1.1.1. Supplies needed for extraction in water  所需耗材

• 四氯乙烯（分析純，高濃度樣品使用）
• 正己烷（分析純，普通樣品使用）
• 125-ml Teflon wash bottle（125ml洗瓶） 
• 100-ml stoppered graduated cylinder or Sample bottle graduated in mL (ie: 125-ml graduated bottles)

帶蓋子和刻度的樣品瓶（根據(jù)樣品量選擇100毫升或125ml）

• Hydrochloric (HCl) or sulfuric acid (H₂SO₄)(dilute with water 1:1)

（1:1比例稀釋的鹽酸或硫酸）

• pH indicator strips or pH meter（PH計(jì)或PH試紙）
• Silica gel anhydrous, 75-150 micrometers（無水硅膠，75-150um）Silica gel (無水硅膠)
• Glass funnel（玻璃漏斗）
• Whatman 40 filter paper, 11cm, or equivalent （40濾紙）
• Disposable polyethylene pipette or equivalent （一次性吸管）
• 100-microliter syringe

100ul注射器或移液槍（推薦使用100量程微升移液槍）

• 5-mL syringe (for use with prescription bottles and solvents heavier than water) 5ml注射器（使用四氯乙烯萃取時(shí)使用）

1.1.2. Considerations: 注意事項(xiàng)

• Make sure glassware for use in analysis is clean.  Any residual hydrocarbons in the glassware and sampling containers will be extracted and added to the TOG or TPH reading.  To check the glassware, rinse with solvent then put 60 microliters on the ATR crystal to test for cleanliness.  

確保器皿干凈干燥，可使用萃取溶劑清洗容器，然后取60微升，放到設(shè)備中檢測(cè)器皿的濃度。

• Oil and grease tends to adhere to the surfaces it comes in contact with.  Use the entire sample collected.  Either mix the solvent and sample in the sample collection container or rinse the sample collection container with a portion of the solvent to be used for extraction.  

油和脂容易沾到容器表面，因此盡量減少中間環(huán)節(jié)?？梢?/span>將溶劑和樣品在樣品收集容器中混合，或者使用純?nèi)軇┣逑礃悠肥占萜?/span>。

• The mechanical details of the extractions are a little different depending on whether the solvent is lighter than water (hexane) or is heavier than water (Vertrel MCA) but in all other respects the methods are identical.

萃取溶劑比水重的和比水輕的，在操作中會(huì)有一點(diǎn)稍微的不同，但總體上兩者是一樣的。

1.1.3. Total Petroleum Hydrocarbon (TPH)  from Water for Solvents Heavier than Water (ie: Vertrel MCA)

總石油烴（萃取溶劑為四氯乙烯）的萃取方法——大于1%濃度樣品使用方法

• Pour measured sample into separatory funnel.  Rinse the sample collection container and graduated cylinder with a portion of the solvent to be used for extraction.  If using a graduated bottle with a septa cap, solvent can be mixed directly in the bottle without using the separatory funnel.

將50毫升樣品倒入到帶刻度和蓋子的樣品瓶中。

• Adjust the pH to less than 2 with Hydrochloric acid or Sulfuric Acid (typically 3-5 drops depending on buffers in sample).

使用ph試紙檢測(cè)水樣的ph，使用鹽酸或硫酸滴定（約3-5滴）確保它的ph在2以下。（這個(gè)操作一般針對(duì)的是隔夜樣品）

• Add one tenth of the sample size of solvent to the sample collection container to rinse interior surfaces and cap. (With the 177-ml prescription bottle, it is convenient to collect 140 ml of sample and add 14 ml of solvent). Pour this solvent into separatory funnel containing sample or if a septa cap is used, the sample can be mixed and extracted from the bottle.

加入5ml萃取溶劑到樣品瓶中。

• Shake the separatory funnel or bottle vigorously for 2 minutes with periodic venting to release excess pressure.

劇烈搖晃樣品瓶2分鐘。

• Allow the phases to separate.

靜置樣品，使其分層。

• Place a filter paper in a filter funnel and add approximay 1 gram (1Tablespoon) of Silica gel anhydrous. 

將濾紙放在漏斗中，放入1克（大概一勺）無水硅膠

• Drain the solvent (lower) layer from the separatory funnel through the sodium sulfate into a clean container (10-mL graduated cylinder can be used). With the prescription bottle, invert the bottle so that the solvent layer fills the neck. Using a 5 ml syringe withdraw 45_mL of the solvent layer and deliver through the Silica gel anhydrous into a clean container.

取2-3毫升下層溶劑，將下層溶劑通過放了無水硅膠的漏斗中。取過濾液進(jìn)行檢測(cè)。  

• Eject 60 microliters of solvent extract using a syringe onto the center of the ATR crystal and select “Run”.  

取60微升處理好的溶劑進(jìn)行檢測(cè)。（因?yàn)橛袡C(jī)溶劑揮發(fā)性非?？?，過濾過程應(yīng)迅速完成，并應(yīng)立即進(jìn)行檢測(cè)）

1.1.4. Total Petroleum Hydrocarbon (TPH)  Extraction from Water for Solvents Lighter than Water (ie: hexane, pentane, cyclohexane) 

總油脂（萃取溶劑為正己烷）比水輕的萃取方法

• Pour sample into a stopper graduated cylinder and measure. Rinse the sample collection container with a portion of the solvent to be used for extraction.   If using a graduated bottle solvent can be mixed directly in the bottle.  Adjust the pH to less than 2 with Hydrochloric acid or Sulfuric Acid (typically 3-5 drops depending on buffers in sample).

將50毫升樣品倒入到帶刻度和蓋子的樣品瓶中。使用ph試紙檢測(cè)水樣的ph，使用鹽酸或硫酸滴定（約3-5滴）確保它的ph在2以下。（這個(gè)操作一般針對(duì)的是隔夜樣品）。

• Add one tenth of the sample size of solvent to the sample collection container to rinse interior surfaces and cap. (With the 177-ml prescription bottle, it is convenient to collect 140 ml of sample and add 14 ml of solvent). Pour this solvent into graduated cylinder containing the sample.

加入5ml萃取溶劑到樣品瓶中。

• Shake the graduated cylinder or graduated bottle vigorously for 2 minutes with periodic venting to release excess pressure. 

劇烈搖晃樣品瓶2分鐘。

• Allow the phases to separate.

靜置樣品，使其分層。

• Place a filter paper in a filter funnel and add approximay 1 gram (1Tablespoon) of sodium sulfate.

將濾紙放在漏斗中，放入1克（大概一勺）無水硅膠

• Withdraw 45_mL of the solvent layer and deliver through the sodium sulfate into a clean container.

取2-3毫升上層溶劑，將上層溶劑通過放了無水硅膠的漏斗中。取過濾液進(jìn)行檢測(cè)。  

• Eject 60 microliters of solvent extract using a syringe onto the center of the ATR crystal and select “Run”.  

取60微升處理好的溶劑進(jìn)行檢測(cè)。（因?yàn)橛袡C(jī)溶劑揮發(fā)性非?？?，過濾過程應(yīng)迅速完成，并應(yīng)立即進(jìn)行檢測(cè)）

• If the result is above the calibration range, see section 4.5 for dilution procedure or create/select a second calibration for the higher range.

如果結(jié)果超過曲線量程，可以將樣品稀釋。如果濃度超過1%，建議使用四氯乙烯進(jìn)行重新萃取，然后按照1.14高濃度檢測(cè)流程進(jìn)行檢測(cè)。