美国wilks红外测油仪萃取方法

10：1水中油萃取过程

1.1.1. Supplies needed for extraction in water  所需耗材

• 四氯乙烯（分析纯，高浓度样品使用）
• 正己烷（分析纯，普通样品使用）
• 125-ml Teflon wash bottle（125ml洗瓶） 
• 100-ml stoppered graduated cylinder or Sample bottle graduated in mL (ie: 125-ml graduated bottles)

带盖子和刻度的样品瓶（根据样品量选择100毫升或125ml）

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

（1:1比例稀释的盐酸或硫酸）

• pH indicator strips or pH meter（PH计或PH试纸）
• Silica gel anhydrous, 75-150 micrometers（无水硅胶，75-150um）Silica gel (无水硅胶)
• Glass funnel（玻璃漏斗）
• Whatman 40 filter paper, 11cm, or equivalent （40滤纸）
• Disposable polyethylene pipette or equivalent （一次性吸管）
• 100-microliter syringe

100ul注射器或移液枪（推荐使用100量程微升移液枪）

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

1.1.2. Considerations: 注意事项

• 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.  

确保器皿干净干燥，可使用萃取溶剂清洗容器，然后取60微升，放到设备中检测器皿的浓度。

• 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，因此尽量减少中间环节。可以将溶剂和样品在样品收集容器中混合，或者使用纯溶剂清洗样品收集容器。

• 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.

萃取溶剂比水重的和比水轻的，在操作中会有一点稍微的不同，但总体上两者是一样的。

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

总石油烃（萃取溶剂为四氯乙烯）的萃取方法——大于1%浓度样品使用方法

• 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.

将50毫升样品倒入到带刻度和盖子的样品瓶中。

• 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试纸检测水样的ph，使用盐酸或硫酸滴定（约3-5滴）确保它的ph在2以下。（这个操作一般针对的是隔夜样品）

• 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萃取溶剂到样品瓶中。

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

剧烈摇晃样品瓶2分钟。

• Allow the phases to separate.

静置样品，使其分层。

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

将滤纸放在漏斗中，放入1克（大概一勺）无水硅胶

• 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毫升下层溶剂，将下层溶剂通过放了无水硅胶的漏斗中。取过滤液进行检测。  

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

取60微升处理好的溶剂进行检测。（因为有机溶剂挥发性非常快，过滤过程应迅速完成，并应立即进行检测）

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

总油脂（萃取溶剂为正己烷）比水轻的萃取方法

• 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).

将50毫升样品倒入到带刻度和盖子的样品瓶中。使用ph试纸检测水样的ph，使用盐酸或硫酸滴定（约3-5滴）确保它的ph在2以下。（这个操作一般针对的是隔夜样品）。

• 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萃取溶剂到样品瓶中。

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

剧烈摇晃样品瓶2分钟。

• Allow the phases to separate.

静置样品，使其分层。

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

将滤纸放在漏斗中，放入1克（大概一勺）无水硅胶

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

取2-3毫升上层溶剂，将上层溶剂通过放了无水硅胶的漏斗中。取过滤液进行检测。  

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

取60微升处理好的溶剂进行检测。（因为有机溶剂挥发性非常快，过滤过程应迅速完成，并应立即进行检测）

• 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.

如果结果超过曲线量程，可以将样品稀释。如果浓度超过1%，建议使用四氯乙烯进行重新萃取，然后按照1.14高浓度检测流程进行检测。