1、 IT IS THE USERS RESPONSIBILITY TO ESTABLISH APPROPRIATE PRECAUTIONARY PRACTICES AND TO DETERMINE THE APPLICABILITY OF REGULATORY LIMITATIONS PRIOR TO USE. EFFECTIVE HEALTH AND SAFETY PRACTICES ARE TO BE FOLLOWED WHEN UTILIZING THIS PROCEDURE. FAILURE TO UTILIZE THIS PROCEDURE IN THE MANNER PRESCRIB
2、ED HEREIN CAN BE HAZARDOUS. MATERIAL SAFETY DATA SHEETS (MSDS) OR EXPERIMENTAL MATERIAL SAFETY DATA SHEETS (EMSDS) FOR ALL OF THE MATERIALS USED IN THIS PROCEDURE SHOULD BE REVIEWED FOR SELECTION OF THE APPROPRIATE PERSONAL PROTECTION EQUIPMENT (PPE). COPYRIGHT 1937, 1940, 1943, 1947, 1959, 1974, 20
3、07 UOP LLC. All rights reserved. Nonconfidential UOP Methods are available from ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA 19428-2959, USA. The UOP Methods may be obtained through the ASTM website, www.astm.org, or by contacting Customer Service at serviceastm.or
4、g, 610.832.9555 FAX, or 610.832.9585 PHONE. Doctor Test for Petroleum Distillates UOP Method 41-07 Scope This is a qualitative test for the presence of hydrogen sulfide, or mercaptans in the absence of hydrogen sulfide, in gasoline, jet fuel, kerosine and similar petroleum products. ASTM Test Method
5、 D 4952, “Qualitative Analysis for Active Sulfur Species in Fuels and Solvents (Doctor Test)” is similar. Reference ASTM Method D 4952, “Qualitative Analysis for Active Sulfur Species in Fuels and Solvents (Doctor Test),” www.astm.org Outline of Method The sample is shaken with a sodium plumbite sol
6、ution in a test tube. If hydrogen sulfide is present the following reaction occurs: Na2PbO2+ H2S PbS + 2NaOH The lead sulfide is black and readily visible. If this reaction does not appear, sulfur is added to the test tube and the mixture shaken again. If mercaptans are present, on shaking they unde
7、rgo a series of reactions, coloring the hydrocarbon layer first orange, then red and brown, and finally a black precipitate of lead sulfide appears. The overall reaction may be written: Na2PbO2+ 2RSH (RS)2Pb + 2NaOH (RS)2Pb + S RSSR + PbS The sodium plumbite (Doctor) solution may be prepared or purc
8、hased. Apparatus References to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used. Balance, readable to 0.01 g, for preparation of Doctor Solution 2 of 4 41-07 Flask, Erlenmeyer, with cap, 1000-mL, VWR, Cat. No, 10-041-6C, for preparation of D
9、octor Solution Funnel, filter, polypropylene, 150-mm top I.D., VWR, Cat. No. 30256-006 Pen, marking, resistant to water and hydrocarbons, VWR, Cat. No. 54848-150, for placing calibration marks on the test tube. Alternatively, a scriber may be used, VWR, Cat. No. 82024-590 Pipets, 5- and 10-mL, VWR,
10、Cat. Nos. 89003-348 and -350, respectively Pipet filler, VWR, Cat. No. 53497-053 Spatula, micro-spoon, stainless steel, glazed finish, VWR, Cat. No. 57952-311 Stopper, rubber, sulfur free, Size 5, VWR, Cat. No. 59589-212 Test tube, 25 x 150 mm, VWR Cat. No. 89000-490. Place permanent calibration mar
11、ks at 5 mL and 15 mL with marking ink. Place the marks by measuring the depth of 5 ml of water from a pipet followed by 10 mL. Timer, 60-minute, GraLab, VWR, Cat. No. 62371-001 Reagents and Materials References to catalog numbers and suppliers are included as a convenience to the method user. Other
12、suppliers may be used. Doctor solution, VWR, Cat. No. VW3547-1. The Doctor Solution may be purchased commercially, or it may be prepared as described under Procedure, Preparation of Doctor (Sodium Plumbite) Solution Filter paper, medium, Whatman Grade 40, 240-mm diameter, VWR, Cat. No. 28475-140 Lea
13、d (II) oxide (litharge), VWR, Cat. No. AA12220-36, for preparation of Doctor Solution Sodium hydroxide, VWR, Cat. No. EM-SX0590-1, for preparation of Doctor Solution Sulfur, VWR, Cat. No. EM-SX1225-1 Water, distilled Procedure The analyst is expected to be familiar with general laboratory practices
14、and with the equipment being used. Calibration of Test Tube Place permanent calibration marks on the test tube at 5 mL and 15 mL. 1. Pipet 5-mL of water into the test tube. Mark the level with marking ink or the scriber. 2. Pipet an additional 10-mL of water into the test tube. Mark the level with m
15、arking ink or the scriber. Preparation of Doctor (Sodium Plumbite) Solution Doctor Solution may be purchased already prepared, or it may be prepared as described below according to the following reaction: 3 of 4 41-07 2NaOH + PbO Na2PbO2+ H2O 1. Dissolve 125 g of sodium hydroxide in 1 L of distilled
16、 water. 2. Add 60 g of lead (II) oxide (litharge) and shake vigorously for 15 minutes. Let stand overnight. 3. Decant or siphon off the clear liquid. If the liquid does not settle clear, filter it through filter paper. 4. Keep the solution in a tightly-stoppered bottle away from sunlight. Refilter i
17、f it becomes cloudy. Sample Analysis 1. Fill the test tube to the first mark with Doctor Solution. 2. Fill the test tube to the second mark with sample. 3. Stopper and shake vigorously for 15 seconds. 4. Observe any appearance of black or brown lead sulfide precipitate. If this occurs, hydrogen sulf
18、ide is present. Stop the test. Report “Hydrogen sulfide present.” 5. In the absence of a brown or black precipitate, use a micro-spoon spatula to add a small amount of sulfur to the mixture in the test tube, not more than will just cover the interface between the hydrocarbon and Doctor Solution. Use
19、 only sufficient sulfur to form a thin film floating on the interface between the sample and the doctor solution. Approximately 40 to 100 mg of sulfur is appropriate. 6. Shake vigorously for 15 seconds and allow any precipitate and the sulfur to settle for one minute. 7. Observe again and report as
20、indicated in the next section. 8. Dispose of the solution, containing lead, in an environmentally safe manner according to local regulations. Report a) “Hydrogen sulfide present” (from Sample Analysis, Step 4). b) Sample sour. If a brown or black precipitate forms after the addition of sulfur, the s
21、ample contains a relatively high concentration of mercaptans and is reported “sour”. c) Sample borderline or sweet. If the mercaptan content of the sample is low, observe the sulfur layer and judge as follows: Discoloration of Floating Sulfur (from its original yellow color) Report Definitely discol
22、ored “sour” Barely discolored borderline Not discolored “sweet” Precision Since this is a qualitative test, no numerical precision is determined. 4 of 4 41-07 Time for Analysis The elapsed time and labor requirement for one analysis are identical, 0.5 hours. Suggested Suppliers VWR International, 1310 Goshen Parkway, West Chester, PA 19380 (610-431-1700)
