Test Procedure. I-9312 Starter Kit R-9310 Refill

Transcription

1 Test Procedure I-9312 Starter Kit R-9310 Refill Midland,VA USA WEB: TEL: (800) FAX: (540) Feb. 16, Rev. 19

2 Contents Section 1 Introductory Information 1.1 Test Method Response to Hydrocarbons... 2 Section 2 Test Instructions 2.1 Safety Information Sample Collection Operating Tips Test Procedure Dilution Procedure Alternative Test Procedure for High Range Hydrocarbon Soil Samples Generation of Standard Curve... 8 Section 3 Instrumentation 3.1 Photometer Battery Replacement Photometer Operating Tips Photometer Displays and Troubleshooting Photometer Specifications Photometer Menu Selection Calibrating the Balance Operating the Timer Balance Features Operating the Timer Timer Features Section 4 Warranty Information 4.1 Warranty Information Introductory Information 1.1 Test Method The RemediAid Total Petroleum Hydrocarbon Test Kit is a rapid, simple field test for measuring petroleum hydrocarbon contamination in soil. The patented test, developed in conjunction with Shell Research, 1,2,3 is based upon the Friedel Crafts reaction with one fundamental difference, the intermediate that is formed in the solvent is the colored species that is measured during the analytical finish. A pre-measured sample of soil is added to a reaction tube which contains anhydrous sodium sulfate, a drying agent. The drying agent is used to improve the subsequent extraction efficiency. The contents of a double point ampoule, 20 ml dichloromethane, is then added to the reaction tube. This organic solvent extracts the petroleum hydrocarbons from the soil sample. In order to remove polar hydrocarbons and color interferences, the soil extract is treated with Florisil. Finally, a vacuum sealed ampoule containing aluminum chloride draws in a predetermined volume of the hydrocarboncontaining solvent through a column containing filtering material that is mounted on the tip of the ampoule. The aromatic hydrocarbons in the solvent react with the aluminum chloride to produce a soluble yellow to brown colored product in direct proportion to the petroleum hydrocarbon concentration in the extract. The absorbance of the extract is measured in a portable, battery powered, LED based colorimeter and converted to mg/kg hydrocarbon in the soil by use of standard conversion values in the following formula: mg TPH/kg = [(A x S) - I] x V W SECTION 1 where, A = Absorbance S = Slope for a specific hydrocarbon mix, mg/l/a I = Intercept for a specific hydrocarbon mix, mg/l V = Extraction Volume; 20 ml (0.02 L) W = Weight of Soil Sample; 5 g (0.005 kg) 1. Shell Internationale Research, European Patent No , U.S. Patent No. 5,834, Roberts, R.M. Khalaf, A. A., Friedel Crafts Alkylation Chemistry; A Century of Discovery. Marcel Dekker, Inc., New York, pp Schmid, George H., Organic Chemistry, 1996, Mosby - YearBook, Inc., QD251.2S354, p

3 1.2 Response to Hydrocarbons The RemediAid Test Kit provides a quicker alternative to the more costly and time consuming standard laboratory methods, but one of the drawbacks to this type of test is that the chemistry is not selective for a particular hydrocarbon. Furthermore, most TPH chemistries are impacted, at least slightly, by various characteristics of the soil itself. Ultimately, the most accurate results are obtained when a site/hydrocarbon specific calibration is generated This kit is designed primarily to be a screening tool, allowing for a comprehensive site survey. Select samples should be sent to a laboratory for confirmatory testing and characterization The RemediAid Test Kit will respond to essentially all hydrocarbon products, as long as they contain some aromatic compounds. This covers nearly all products, with few exceptions (e.g.,household kerosene). The table below lists an average response factor that can be used if the identity of the hydrocarbon contamination in the soil sample is unknown. Calibration Information for SAM Photometers With Inspection Dates After October 10, Hydrocarbon Unleaded Gasoline Diesel Brent Crude Lube Oil BTEX Leaded Gasoline PAH (16 Component mixture) Unknown 1 Slope Intercept MDL (mg/kg) in Soil N/A Range (mg/kg) in Soil This response factor is supplied for use when the identity of the hydrocarbon contaminant in a particular soil sample is unknown. Test results generated using this factor are to be treated as estimates N/A Test Instructions 2.1 Safety Information Read MSDS before performing this test (availabe at Wear protective gloves and safety glasses while performing this test. Avoid inhaling dichloromethane fumes. Do not work in a confined space. Do not eat, drink, or smoke while performing this test. Wash hands thoroughly after performing this test. 2.2 Sample Collection SECTION 2 Methods of collection and sample size should be chosen to ensure that the sample is representative of the location from which it was taken. In many cases, contaminant composition can vary substantially over very short distances, even for relatively homogeneous soils. Sampling strategy will be guided by a number of factors such as prior knowledge of site activities and visual clues. Representativeness can be improved by taking large samples which are then well mixed immediately before being subsampled for analysis. However, sample size should be restricted to a size which can be mixed very quickly in the field so that volatile hydrocarbons are not lost. Any unnecessary agitation of samples should be avoided for this reason. Actual sampling of the soil should be carried out in the minimum possible time, with the least possible handling before the sample is sealed in a container. Samples should be collected in wide necked glass jars so that mixing can be carried out speedily. If possible, collection of an uncontaminated soil sample in close proximity to the sampling location is recommended. This sample would be analyzed according to the test procedure in section 2.4 and would potentially be used to correct for background in test samples, (refer to Section 2.3 under Soil Blank). To avoid cross contamination, care should be taken to ensure that all sampling equipment is decontaminated before each new sample is taken. In many cases, samples will be retained in case subsequent analysis is necessary. Error can also occur by poor labelling of samples. All sample vessels should be clearly labelled with sampling date, site or project identification, identification number, sampling depth and an identifier for the individual doing the sampling. A sampling log should be maintained which includes the sample details above and other details (e.g., sample appearance, color, smell, texture, or any other signs of hydrocarbon contamination). 3

4 2.3 Operating Tips Do not store this product at temperatures above 90 F (32 C). Keep Reagent Blank Ampoule out of direct sunlight. Avoid testing soil at high ambient temperatures (> 80 F or 27 C). CLOUDY TEST AMPOULE: After Step 13 of the test procedure, the ampoule contents should not be cloudy in appearance. Cloudiness is an indication that additional sodium sulfate was needed to remove excess moisture from the soil sample. A cloudy test ampoule will likely give false high test results. Repeat the test procedure using additional sodium sulfate. SOIL BLANK: If an absorbance value of > is obtained for the soil blank, then calculate a test result in mg/kg for the soil blank using the formula in Step 20 of the test procedure. Subtract this value from the result obtained for the sample to prevent positively biased test results caused by background color extracted from the soil. 2.4 Test Procedure 1. Add 5.0 g of the soil to be tested to a Reaction Tube (tube with natural cap). Whenever possible, exclude rocks and other non-soil debris. NOTE: Try to keep balance sheltered from wind. The reaction tube contains anhydrous sodium sulfate which is used to remove moisture from the soil. 2. Cap the reaction tube and shake it to mix the contents to a uniform mixture. NOTE: If the sample is too wet to form a granular, uniform mixture (as with clay soils), add up to 5 scoops of extra sodium sulfate and shake the tube vigorously until a uniform, free-flowing powder is obtained. If necessary, a clean spatula can be used to break up clumps of wet soil. 3. While holding the double-tipped ampoule in a vertical position over the reaction tube, snap the upper tip using the tip breaking tool. Carefully invert the ampoule and position the open end over the reaction tube. Snap the upper tip and allow the contents to drain into the reaction tube. 4. Cap the reaction tube and shake it vigorously for 3 minutes Allow the reaction tube to stand undisturbed while the soil settles to the bottom. This should take approximately 2 minutes. 6. Decant extract to an Extract Clean-up Tube (tube with green cap) using care not to transfer any soil to the clean-up tube. Cap the clean-up tube and shake it for 1 minute. Allow the florisil to settle for approximately 2 minutes. 7. Remove the cap from the clean-up tube and replace it with the Tube Plug/Snapper. This is a round, white plug that has a small hole in the center that will be used to snap the tip of the TPH ampoule. 8. Push a column onto the tip of the ampoule until it fits snugly. 9. Insert the column/ampoule tip assembly through the hole in the plug up to the scoremark on the ampoule tip. While holding the tube, gently pull the ampoule slightly out of the vertical orientation to snap the ampoule tip. The ampoule will slowly draw in liquid from the tube. When filling has stopped, withdraw the column/ampoule assembly from the tube. 10. Using a tissue, carefully remove the column from the tip of the ampoule. Wipe all liquid from the exterior of the ampoule. 11. Place a small silicone ampoule cap firmly onto the tip of the ampoule. 12. Over a period of 10 minutes, invert the ampoule periodically, allowing the bubble to travel from end to end each time. NOTE: Invert the ampoule several times every 1-2 minutes. 5

5 13. Allow the ampoule to stand undisturbed while the crystals settle to the bottom. This should take approximately 10 minutes. NOTE: If the ampoule appears cloudy after the 10 minute wait, wait an additional 5-10 minutes for the cloudiness to settle out of the ampoule. See Operating Tips for additonal information. 14. Insert the Reagent Blank Ampoule, flat end first, into the sample cell compartment of the photometer (with mild downward pressure to ensure that the ampoule is fully seated). 15. Place the light shield over the Reagent Blank Ampoule. 16. Press the Zero/Test Key. The TPH symbol will flash for approximately 8 seconds, then the display will show Insert the test ampoule, flat end first, into the cell compartment of the photometer (with mild downward pressure to ensure that the ampoule is fully seated). 18. Place the light shield over the test ampoule. 19. Press the Zero/Test Key. The TPH symbol will flash for approximately 3 seconds, then the sample absorbance value will appear in the display. 20. If the absorbance value is less than 1.00, then use the following formula to determine the TPH concentration: mg/kg soil = [(A x S) - I] x 4 where, A = Absorbance S = Slope for a specific hydrocarbon mix I = Intercept for a specific hydrocarbon mix If the instrument displays HI, then either the Dilution Procedure (Section 2.5) or the Alternate Test Procedure (Section 2.6) must be performed. 2.5 Dilution Procedure 1. Pipette 2.5 ml of the clear solvent extract from Step 6 into an Extract Clean-Up Tube. 2. Add the contents of a double-tipped ampoule to the Extract Clean-Up Tube. Cap the tube and shake it for 1 minute. Allow the florisil to settle for approximately 2 minutes. 3. Follow Steps 7-19 of the Test Procedure. 4. Use the following formula to determine the TPH concentration: mg/kg soil = [(A x S) - I] x D x 4 where, A = Absorbance S = Slope for a specific hydrocarbon mix I = Intercept for a specific hydrocarbon mix D = Dilution Factor: Alternative Test Procedure for High Range Hydrocarbon Soil Samples 1. Add 1.0 g of the soil to be tested to a Reaction Tube (tall tube with white cap). Whenever possible, exclude rocks and other non-soil debris. 2. Follow steps 2-19 of the Test Procedure. 3. Use the following formula to determine the TPH concentration: mg/kg soil = [(A x S) - I] x 20 where, A = Absorbance S = Slope for a specific hydrocarbon mix I = Intercept for a specific hydrocarbon mix 6 7

6 2.7 Generation of Standard Curve To improve accuracy or to determine a specific hydrocarbon product, a standard curve can be generated. Standard curves are generated from measurement of various hydrocarbon solutions in dichloromethane (DCM) covering the expected range of the test. For heavy hydrocarbons such as crude, lube oil, and diesel, prepare a stock solution (10,000 mg/l) by weighing out 1 g of the hydrocarbon and diluting to 100 ml in DCM. Prepare a series of diluted standard solutions as follows: 50 mg/l (0.5 ml stock in 100 ml DCM) 100 mg/l (1.0 ml stock in 100 ml DCM) 150 mg/l (1.5 ml stock in 100 ml DCM) 200 mg/l (2.0 ml stock in 100 ml DCM) 300 mg/l (3.0 ml stock in 100 ml DCM) 400 mg/l (4.0 ml stock in 100 ml DCM) For lighter (more volatile) hydrocarbons such as gasolines and pure BTEX, it is advisable to prepare the standards volumetrically rather than gravimetrically to reduce volatile losses. To make a particular concentration of dilute standard (e.g., 50 mg/l, which is 5 mg in 100 ml DCM) the needed volume is calculated by dividing the mass required (ex. 5 mg), by the density of the hydrocarbon. The calculated volume (Volume = Mass Density) is then injected into a 100 ml volumetric flask containing DCM. After preparing the appropriate standard solutions: 1. Add 20 ml of each standard to an Extract Clean-Up Tube (containing Florisil) and perform the Test Procedure beginning with Step 7. NOTE: When running standards in DCM, it takes at least 20 minutes for the crystals to settle in Step 13 of the test procedure. 2. Construct a calibration curve using the absorbance values for each standard. 8 Instrumentation 3.1 Photometer Battery Replacement Instrument Back Batteries Notch To ensure that the instrument is water proof: seal ring (A) must be in position battery compartment cover (B) must be fixed with the four screws 3.2 Photometer Operating Tips Upon start up, the photometer automatically proceeds to the zeroing process. Every time the photometer powers on, it must be re-zeroed. To re-zero the photometer, it must be turned off and back on again. A series of readings can be taken without re-zeroing, as long as the photometer stays on during the series. Protect photometer from extreme humidity, corrosive fumes and dusty areas. Store in a cool, dry place. Remove the batteries when photometer is not in use. If the batteries are removed for more than one minute the date and time menu starts automatically when the photometer is turn on the next time Photometer must be turned off and back on again for re-zeroing. However, re-zeroing is not necessary when reading a series of samples. Press the! key to turn the display back light on or off. When moving the photometer from one temperature extreme to another, wait at least 10 minutes to allow photometer to come to temperature equilibrium. Contamination of the transparent sample chamber will result in incorrect measurements. The sample chamber should be checked at regular intervals and cleaned as necessary. Use a soft moist cloth or cotton swab to clean. If the sample cell adapter has been removed, it must be replaced with proper orientation aligning the triangle on the adapter with the triangle on the photometer. 9 SECTION 3 Battery Compartment Cover (B) Seal Ring (A) Screws

7 3.3 Photometer Displays and Troubleshooting E01: Light absorption too great (dirty optics) E20/E21: Too much light reaching detector E22 or Battery Icon: Battery should be replaced btlo: Battery capacity is too low for the display backlight Hi/EO3: Measuring range exceeded or excessive turbidity Lo: Test result has a negative value E27/E28/E29: Instrument zeroed incorrectly, dirty optics or failing light source. 3.4 Photometer Specifications Auto Shut Off: After 15 minutes of non-use Optics: 430 nm LED/interference filter and photosensor in transparent sample chamber Operating Temp.: 5 to 40 C (41 to 104 F) Battery: 4 AAA batteries (approx. 5,000 tests or 17 hours) Waterproof: Floating, IP68 (1 hour at 0.1 meter) Wavelength Accuracy: ± 1 nm Photometric Accuracy*: 3% FS (T = 20 C - 25 C) / (T = 68 F - 77 F) Photometric Resolution: 0.01 A Ambient Conditions: Temperature 5-40 C / F Rel. humidity % (non-condensing) CE: Certificate of Declaration of CE-Conformity available upon request. * Measured with Standard Solutions 3.5 Photometer Menu Selection 1. Hold the Mode key down and press the On/Off key. Allow the 3 decimal points to appear in the display before releasing the Mode key. 2. Use the! key to toggle through 2 menu options: Store = recall stored data Date & Time = setting the date and time. 3. Press the Mode key to select the menu option that is indicated by the arrow. Note: If the instrument is already on, press and hold the! key for more than 4 seconds to access the recall menu. Recall of Stored Data The colorimeter shows the last 16 data sets in the following format: Sample Number: nxx (XX: 16, 15, 14,...1) Year: XXXX (i.e. 2009) Date: mm.dd (i.e ) Time: hh:mm (i.e. 12:05) Result: XX or XXX 10 The Zero/Test key repeats the current data set. The Mode key scrolls through all stored data. Quit the menu by pressing the! Key. Setting Date and Time The setting starts with the year (XXXX), then month (XX), then day (XX), then hour (XX), then minutes (XX). Increase value by pressing the Mode key. Decrease value by pressing the Zero/Test key. Proceed to the next setting by pressing the! key. After setting the minutes and pressing the! key, the display will show "IS SET" and return to measurement mode. 3.6 Calibrating the Balance For best results, calibrate at regular intervals, especially if the scale is in use for prolonged periods. 1. Press the On/Off button to turn the instrument on. 2. Press and hold the Unit/Cal button until the display shows CAL, then release. 3. Press the On/Off button. The display will show C When the display shows C 100 place the calibration weight on the platform. 5. Press the On/Off button. PASS will be displayed when calibration is complete. Note: If the calibration steps are not followed correctly or if the wrong weight is used, the display will show CAL E. Repeat the procedure. 3.7 Operating the Balance 1. Push the blue balance tray toward the back of the scale until it clicks into place. Pointers on the side of the tray will align with symbols on the bottom of the scale. 2. Place a reaction tube on the center of the balance tray. 3. Press the On/Off button and the display will show Proceed to weigh out the 5.0 g of soil needed in the Test Procedure. 3.8 Balance Features On/Off: Pressing this button turns the scale on. Pressing and holding this button turns the scale off. 11

8 Zero/On/Off: This key is also used to rezero the display when the scale is on. Unit/Cal: Press this button briefly to change the weighing unit. The following weight units may be selected: grams (g), ounces (oz), pennyweight (dwt) or troy ounces (oz t). Pressing and holding this button begins the calibration process. 3.9 Operating the Timer Note: The installed battery is insulated by tape to give maximum battery life. To use the timer, remove the tape from the battery compartment. 1. Press the CLOCK button until all channels display the timer mode. 2. Press and hold the CHANNEL button (1, 2, or 3) for three seconds. Display will flash. 3. Press the MIN (minute) button to set the countdown time required. Display will flash. 4. Press the CHANNEL button to confirm the entry. Display stops flashing. 5. Press the CHANNEL button (1, 2 or 3) to start countdown timing. 6. Press any button to silence the alarm Timer Features Each channel has a unique alarm to indicate which channel is alarming. Channel 1 emits a single beep, Channel 2 emits 2 beeps, etc. The ALL TIME button allows you to start or stop all channels simultaneously. The CLEAR button sets all stopped channels to 00:00:00. The ALARM DURATION switch, located in the battery compartment, allows for a choice between an alarm that sounds for 1 minute and then automatically shuts off and an alarm that sounds continuously until manually silenced There are two volume settings. Slide the VOL button to the upper position for high volume alarm, or to the lower position for low volume alarm. If the unit does not function properly for any reason install a new AAA alkaline battery Warranty Information SECTION 4 The TPH Photometer, Balance and Timer all carry an unconditional guarantee of freedom from defects in materials and workmanship for a period of one year from the date of the shipment. User access to the interior of these devices may impair their function and will void this warranty. Improper use, application, or servicing also voids this warranty. Manufacturer's liability shall not exceed cost of replacement of the device. The manufacturer generally warrants its products, other than instrumentation, to be free from defects in materials and workmanship for a period of two years from the date of the shipment. Return authorization must be obtained prior to returning any merchandise. If you have any questions concerning the operation and maintenance of the device or the reagent accessories, contact an authorized dealer for assistance. The manufacturer offers to replace any product which it manufactures in defective condition. This is the exclusive remedy for damages of any nature, including incidental and consequential, resulting from such products. THIS WARRANTY SHALL BE IN LIEU OF ALL OTHER WARRANTIES, EXPRESS OR IMPLIED, INCLUDING ANY IMPLIED WARRANTY OF MERCHANTABILITY OR FITNESS FOR A PARTICULAR USE. 13