ANALYZER System PPM RANGE for LUBRICATING OILS - Brochure

hydroscout ®For the Determination of Water ContentUser’s ManualVersion E34Copyright NoticeHydroScout User's Manual and other documentation copyright © 2001-2003 Dexsil Corporation. All rights reserved.DisclaimerDexsil Corporation makes no representations or warranties with respect to the contentshereof and specifically disclaims any implied warranties of merchantability or fitness forany particular purpose. Further, Dexsil Corporation reserves the right to revise thispublication and to make changes from time to time in the contents hereof withoutobligation of Dexsil Corporation to notify any person of such revision or changes.TrademarksHydroScout and Dexsil are registered trademarks of Dexsil CorporationDEXSIL CorporationOne Hamden Park DriveHamden, Ct. 06517Tel: (203) 288-3509; Fax: (203) 248-6523; http://www.dexsil.com HYDROSCOUTManualE34.RV1.wpd Version E34 Rev1 September 2008WARNING READ ALL CAUTIONS BEFORE USING THIS TESTONCE THE TEST IS INITIATED, CONTENTS OF THE TUBES ARE UNDER PRESSURE.SAFETY GLASSES MUST BE WORN AT ALL TIMES WHILE PERFORMING TESTS. DONOT REMOVE THE WHITE CAP AFTER THE TEST HAS BEEN PERFORMED.DO NOT USE THIS TEST ON CONCENTRATED ACIDS. THE EXCESSIVE HEATGENERATED MAY LEAD TO TUBE FAILURE.DO NOT USE 5 ML SAMPLES OF PHOSPHATE ESTER-BASED HYDRAULIC FLUIDS,GASOLINE OR SOLVENTS SUCH AS ACETONE. THESE SAMPLES WEAKEN THETUBES WHICH MAY RESULT IN TUBE FAILURE.THE TEST CONTAINS FLAMMABLE SOLVENTS AND PRODUCES HYDROGEN GAS;KEEP AWAY FROM OPEN FLAME.MAKE SURE THE BLACK SEPTUM IS FULLY INSERTED INTO THE NECK OF THE TESTTUBE AND THE WHITE CAP IS SCREWED ON TIGHTLY.SHAKE THE TUBE WHILE POINTING IT AWAY FROM YOURSELF AND BYSTANDERS.WHEN CRUSHING THE GLASS AMPULE, PRESS FIRMLY IN THE CENTER OF THEGLASS AMPULE. NEVER ATTEMPT TO RECRUSH BROKEN GLASS AS IT CANPENETRATE THE PLASTIC TUBE AND CUT FINGERS.THE GRAY AMPULE IN THE TUBES CONTAINS CALCIUM HYDRIDE WHICH IS AFLAMMABLE SOLID AND IS WATER REACTIVE.IN CASE OF ACCIDENTAL BREAKAGE OR SPILLAGE ONTO SKIN OR CLOTHING,WASH IMMEDIATELY WITH LARGE AMOUNTS OF WATER. DO NOT TAKEINTERNALLY, ALL OF THE CONTENTS ARE POISONOUS.KEEP OUT OF THE REACH OF CHILDRENREAD MATERIAL SAFETY DATA SHEETS BEFORE PERFORMING TEST.MANUFACTURER’S WARRANTYThis kit is warranted to be free of defects in material and workmanship until the expiration datestamped on the box. Manufacturer’s sole and exclusive liability under this warranty shall be limitedto replacement of any kit that is proved to be defective. Manufacturer shall not be liable for anyincidental or consequential damages.Reliable test results are highly dependent upon the care with which the directions are followed and,consequently, cannot be guaranteed.Table of ContentsIntroduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1Choosing the Correct Program . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1Table 1: HydroScout Analysis Program Information . . . . . . . . . . . . . . . . . . . . . . . 1Programs A & B - For Mid to High Range Water in Oil . . . . . . . . . . . . . . . . . . . . . 2Programs C, D & E - For Low Level Water in Oil . . . . . . . . . . . . . . . . . . . . . . . . . 2Program F - For Water in Soils and Solids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2Program G - For Water in Paint . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3Meter Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4Turning the Meter On . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4Making a Measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4Selecting a Program . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4Turning the Meter Off . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4Error Codes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4Table 2: Error Codes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5Interferences . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5Step by Step Instructions for Meter Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6Analysis Instructions for Each Sample Type and Analysis Program . . . . . . . . . . . . . . . . . 6Program A - Procedure for Testing Water Content up to 20% . . . . . . . . . . . . . . . . 6Program B - Procedure for Testing Water Content up to 100% . . . . . . . . . . . . . . . 7Program C, D & E - Procedure for Low Levels of Water (5 mL Sample Size) . . . 8Program F - Procedure for the Analysis of Water in Soils and Solids . . . . . . . . . . 9Program G - Procedure for Analysis for Water Content in Paint: . . . . . . . . . . . . . . 10-11Expected Water Content Less than 15% (No Dilution) . . . . . . . . . . . . . . . . . . . . 10Expected Water Content Greater than 15% (with Dilution) . . . . . . . . . . . . . . . . 11Appendix A: Comparison Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12-17Water in Used Oil (Programs A & B) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12Used Oil CRMs (Programs A & B) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12Low Levels in Turbine and Gear Oil (Program C) . . . . . . . . . . . . . . . . . . . . . . . . . 13Low Level Water in Other Oils (Program D) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14Low Level Water in Other Oils (Program E) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15Water in Soil (Program F) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16Water in Various Coatings [Paint] (Program G) . . . . . . . . . . . . . . . . . . . . . . . . . . . 17Appendix B: Meter Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 181IntroductionThe HydroScout™ system is designed to accurately and quickly measure the water content in a number of samplematrices. The test uses a specially formulated calcium hydride (CaH2) reagent to quantitatively convert all the watercontained in the sample to hydrogen gas (H2). The reaction is carried out in a sealed tube and the generated pressure ismeasured using a specially designed meter. Internal software converts the pressure into water content and the results aredisplayed directly in the appropriate units.The HydroScout meter is programed with seven different programs which are easily selected using the program menu.Each program is setup to cover a specific analysis range and matrix combination. Built into each program are all of theconversions necessary to convert the measured pressure into water content. The measurement programs compensate forsample size, dilutions, extractions, reaction efficiencies and conversion to the correct units.Choosing the Correct ProgramThe HydroScout meter is programed with seven unique measurement programs. The specific applications for each ofthe programs are tabulated below. Before beginning any measurements, choose the correct measurement program for thesample matrix and measurement range. Read throughly the specific instructions for the appropriate program to determinewhat specific reagents and preparation steps are necessary. Selecting the desired program is described below.Table 1: HydroScout Analysis Program InformationProgram Sample MatrixTypes Tested1Units MDL3 Maximum Reagents Needed SampleSizeA Used Oil/LiquidUsed Oil, Chemtool 250, Paint WasteVolumePercent0.15% (v/v) 20% (v/v) Standard ( HS-ORP) 0.25 mLB Used Oil/LiquidUsed Oil, Chemtool 250, Paint WasteVolumePercent5% (v/v) 100% (v/v) Standard +Dilution Vial(HS-ORP + HS-DVP)0.25 mLC Light Oil/LiquidExxon Terestic GT32, Mobil DTE Light,Shell Turbo T32, Ideal AW-32, Renolin T-32, Dupont Diamond Class 32, TexacoHavoline 80W-90 Gear Oilµg/mL 50 µg/mL 10,000 µg/mL PPM Reagents( HS-LRP)5 mLD Medium Oil/LiquidNAPA Non-Det. SAE 30, Amalie Non-Det.SAE 30, Valvoline Non-Det. SAE 30,Oilzum Non-Det. SAE 50, Gunk Heavy-Duty Brake Fluid, Shell Diala Aµg/mL 50 µg/mL 10,000 µg/mL PPM Reagents( HS-LRP)5 mLE Heavy Oil/LiquidExxon Superflo 10W-30, Mobil 1 10W-30,Quaker State Proline 10W-40, ValvolineSAE 50, John Deere Hydraulic Fluidµg/mL 50 µg/mL 10,000 µg/mL PPM Reagents( HS-LRP)5 mLF Soil/SolidsSand, Sandy Clay-Loam, Sea Sediment,Topsoil, Georgia Clay, Alabama Clay,Compost, Plant Materialmg H2O 0.25% (w/w) 100% (w/w)2 Standard+Extraction (HS-SEV)1-10gramsG PaintPaints and Coatingsmg H2O 0.15% (w/w) 100% (w/w)4 Paint ReagentsHS-LPTHS-HPT0.25 mL1 For comparison data, see Appendix A.2 Using a 1 gram sample.3 Method Detection Limit determined using procedure outlined in 40 CFR Ch. 1 Pt. 136, App. B.4 This method has been evaluated by the American Society of Testing and Materials (ASTM) Committee D01 over the rangeof 2% to 85% water content and is the basis of ASTM Method D 7358.2Programs A and B -> Mid to High Range Water in Oil (EPA Method 9001) Measurement Range: 0.15% to 100%Sample Matrix: Used Oil or LiquidsTypical Application: Used oil where moderate to high levels of water are expected.(Programs A and B are used for measuring water content in an oil/liquid matrix using a 0.25 mL sample.)Program A covers the range from 0.15% to 20% water content. When an ERROR Code of “Err 4” occurs when testingoil samples under this program, the water content is over 20% (v/v) and the sample must be retested as a diluted sampleusing Program B. The results for the method is displayed in volume/volume percent.Program B is used for oil/liquid samples with water concentrations in the 10% to 100% range. If a sample has previouslytested to be over 20% (v/v) or is suspected to contain over 20% (v/v) water, it must be run using a dilution solvent vial andProgram B. This procedure entails adding an initial 0.25 mL sample to the dilution solvent vial, mixing thoroughly, andintroducing a 0.25 mL sample of this mixture into a second sample tube which is part of the basic Reagent package Thissample is then processed under the basic test procedure. The results for the method is displayed in volume/volume percent.Programs C, D and E -> Low Level Water in OilMeasurement Range: 50 µg/mL to 10,000 µg/mLSample Matrix: Lube Oils, Hydraulic Oils, Brake Fluids, FuelsTypical Application: Condition monitoring for low levels of water in in-service oils.(Programs C, D and E are set up to measure low levels of water in an oil/liquid matrix using a 5 mL sample.)The results for programs C, D and E are reported in µg/mL (displayed as ppm) since the samples sizes are determined byvolume. The overall efficiency of the CaH2 reaction has been determined to be less than 100% with certain oil types dueto viscosity and solubility effects. However, since the pressure function is a linear parameter, the meter response value canbe corrected to produce accurate results on all oil types. The HydroScout response on low water level oils has beendocumented for a number of these oil types (See Appendix A). There are three major response groups among the oilstested. The recoveries for the lighter, non-additive, oils such as: turbine oils and diesel fuel are 100% and should be runon program C. Non-detergent motor oils, brake fluids and gear oils average approximately 87% recovery and should berun on program D. Multi-viscosity detergent motor oils and hydraulic fluids with polar additives average 63% recoveryand should be run on program E., The results obtained when using programs D and E are automatically corrected to yieldaccurate results that correlate with Karl Fischer.NOTE: Phosphate ester-based hydraulic oils and gasoline should be run using Programs A & B only.If the oil sample is a listed oil type, the corresponding program can be used for analysis. The correct program for oils notlisted can be determined by comparing the meter response on program C with a Karl Fischer analysis on the same oilsample. The ratio of the HydroScout result to the Karl Fischer result will determine the correct program to use for futuremeasurements. (NOTE: The HydroScout reports results in volume percent. Be sure to use the same units when comparingHydroScout results to Karl Fischer results.) If the ratio is near 1 (divide the Hydroscout program C result by Karl Fischerresult) continue using program C, for ratios between 0.95 and 0.85 use program D and for ratios near 0.6 use program E.(For further assistance in determining the correct program, contact Dexsil.)Program F -> Water in Soil and SolidsMeasurement Range: 0.25% to 100%Sample Matrix: Soils and Extractable SolidsTypical Application: Moisture content monitoring in agricultural soils.(Program F should be used to measure moisture content in soils.)This analysis requires that the soil/solid be extracted using the HydroScout extraction solvent. The extract is then sampledusing a standard sampling syringe and analysis procedure.3Program G -> Water in Paint (ASTM Method D 7358)Measurement Range: 2% – 85%Sample Matrix: Paints and CoatingsTypical Application: Quality control of paints and coatings.This method is designed to measure the water content of liquid samples over the range of 1% to 100% (w/w) water content.The reproducibility and repeatability of this method have been evaluated over the range 2% to 85% and are published inASTM Method D 7358. In order to achieve a result based on the weight of the sample, the sample must be weighed intothe reaction vessel. Not only does this allow for a weight based result, but it improves accuracy by eliminating theuncertainty of the volumetric sample size.If the sample to be analyzed is believed to contain less than 15% water, the sample should be introduced directly into thereaction tube following the procedure for “No Dilution”( See page 10). For samples containing more that 15% water thesample must be diluted and the diluted sample analyzed using the procedure for “”with Dilution” (See page 11).4Meter OperationThe HydroScout meter is fully factory calibrated and is ready to operate. Each time the meter is turned on, the micro-processor recalibrates the pressure transducer to zero and performs a QC check on the output voltage. While these checksare being preformed, relevant information on the meter will be displayed such as the software version loaded into memoryand the current selected measurement program. The meter also has other built-in QC checks to verify measurement integrity(see “Error Codes” below).Turning the Meter OnPress the key to turn the meter on. The software version will then be displayed for 5 seconds (-E28-,-E30-,etc.) followed by the currently selected measurement program (“A 0-20%”, “b 1-100%”, “c ind”, etc.). Whenthe meter has completed all QC checks, the display reads “tUbE”, indicating that the meter is ready to read asample (NOTE: It may take a few seconds to zero the sensor and for the display to read “tUbE”). Making a MeasurementThe factory default program is Program A. To make measurements using the default program or the currentlyselected program: insert the reaction tube into the bottom of the meter until it seats firmly, press the keyand allow the meter to stand upright until the result is displayed. The results are displayed in the units appropriateto the selected program, preceded by the program letter. NOTE: THE METER MUST BE KEPT UPRIGHTWHEN A MEASUREMENT IS MADE. INVERTING THE METER WHILE A TUBE IS INSERTED CANCAUSE DAMAGE TO THE PRESSURE TRANSDUCER.Selecting a ProgramTo select a new program, press the key once the meter has completed a reading or after the meter has beenturned on and has completed all QC checks (display reads “tUbE”). The display will change to the next programin the list after displaying the current program, e.g., “b 1-100%”, indicating that Program B has been selected.Press the key to scroll through the available programs from A to G followed by “OFF” and then, back to“A 0-20%” again. Press the key at any point to fix the selection at the displayed program or to turn themeter off when “OFF” is displayed. To begin using the selected program, press the key and the meterwill reset to zero and display “tUbE”. The meter is now ready to read a sample. NOTE: AN ERROR WILLRESULT IF THE METER IS TURNED ON OR THE PROGRAM IS CHANGED WHILE A REACTION TUBEIS IN THE METER.Turning the Meter OffThe HydroScout meter will turn off automatically after 5 minutes of non-use. To turn off manually, push the key until the meter displays “OFF” and then push the key.Error CodesThe HydroScout performs several QC checks each time the unit is turned on and during each reading to verify that thedisplayed result is valid. Each time the meter is turned on the pressure transducer output is measured and compared toacceptable values. A high voltage causes an “Err l” code to be displayed indicating that a tube has been left in the meterwhile turning it on. (An “Err l” displayed with no tube in place indicates that the transducer has been damaged.) A lowvoltage causes an “Err 2” code to be displayed indicating that the pressure transducer has been damaged and must beserviced. If the voltage is acceptable, the meter then sets zero and is ready to take readings by displaying the word “tUbE”.During readings of samples, the pressure is measured a number of times and the trends are analyzed. If the readings aretrending upward, the pressure is remeasured and re-analyzed. If this pattern continues, an “Err 3” code is displayedindicating that the reaction is not complete and the reading should be repeated. If the pressure is trending downward, an“Err 5” code is displayed indicating that the tube is leaking and that the sample testing should be re-run from the start. Oncea reading has stabilized, the result is calculated and displayed. If the pressure is outside of the linear range, an “Err 4” codewill be displayed indicating that the sample should be rerun using a smaller sample size or a dilution technique and adifferent program. (See Table 1)5Table 2: Error CodesError Code Explanation Likely Cause RemedyErr 1 Zero voltage too high. Reaction tube in place when turningmeter on or switching programs.Remove tube and re-selectprogram.Err 2 Zero voltage too low. Excessive drift in transducer outputcaused by damage.Call for service.Err 3 Pressure readingstrending up.Reaction has not gone tocompletion.Wait another minute and re-read.Err 4 Reading outside of linearrange.Water content greater than 20%(v/v).Re-run sample using dilutionvials and “Program B”.Err 5 Pressure too low duringsample reading.Leaking tube or cap.Tube squeezed while inserting graystopper.Re-run sample using newreaction tube. If problempersists call for assistance.Lo Pr Low Battery Low Battery Remove four screws. Replacebattery with 9V alkaline orlithium only.InterferencesIn addition to the testing the effectiveness of the HydroScout system in a number of matrices, extensive testing has also beenconducted to document possible interferences and/or cross reactivities due to additives or components in a sample matrix.The following compounds have been found to produce no measurable response to the HydroScout system and, therefore,cause no interference at levels up to 40%:Ethanol Dipropylene glycolMethanol Stearic acidAcetone* 2-Ethyl hexanoic acidMethyl ethyl ketone Lead oxide (II and III)Tetrahydrofuran Aluminum oxide (Brockman I)Diethylene glycol dimethyl etherEthylene glycol*Diethylene glycol*0.25 mL sample size program A and B When using the 5 mL sample size programs, i.e., programs C, D, or E, ethylene glycol and acids have been found to producea positive result. Ethylene glycol responds at approximately 7% of the volumetric equivalent.6Step by Step Instructions for Meter OperationStep 1. Press the Key.SCREEN: “-E34- ” is displayed followed by the currently selected program (i.e. “A 0-20%”) , thenflashes “-bL-”, and then “tUbE.”( “-E34-” is the current software version and “-bL-” indicates the instrument is undergoing internalcalibration.)Step 2. If Program “A” is not the desired program, press the key to change it by following the procedure describedin “Selecting a Program”.Step 3. With the meter held upright: Insert the reaction tube into the bottom of the meter until it seats firmly.Step 4. Press the Key.SCREEN: “CALC” flashes, then:SCREEN: “A XXXX ” (Where “A” is the letter designating the current program and “XXXX” is the reading in the units appropriatefor the current program.)Step 5. Record result, remove reaction tube and insert new sample.Step 6. Press the key.Step 7. Repeat steps 3-6 until all samples have been read.Step 8. Turn off meter manually or meter will turn off automatically after 5 minutes of non-use.NOTE: Meter is off when screen is blank.Analysis Instructions for Each Sample Type and Analysis ProgramProgram A –> Procedure for Testing Water Content up to 20%(Reagent System: HS-ORP)1. PREPARATION: Remove a sampling syringe and a white-capped reaction tube from the reagent box. Check thecontents to ensure that all items are present and intact. Remove the white cap and black septum from the reaction tube.Carefully remove a green water ampule from the cardboard carton and insert it fully into the top of the protectiveampule sleeve containing the grayish white ampule. Return the protective ampule sleeve to the reaction tube with thegrayish white ampule on the bottom and place the tube into the reagent box.2. SAMPLE INTRODUCTION: Work the plunger of the empty sampling syringe a few times to ensure that it slideseasily. Place the tip of the syringe into the oil sample to be tested (sample must be well mixed and representative) andslowly pull back on the plunger until it reaches the stop and cannot be pulled further. When drawing up the sample,make sure there are no air bubbles in the syringe. If not free of air bubbles, depress the plunger again and draw asecond sample slowly. Remove the syringe from the oil sample and wipe any excess oil from the outside of the syringewith a tissue wipe. Insert the sampling syringe into the reaction tube and dispense the oil sample by depressing theplunger. Replace the black septum (hole on top) by pressing down on the septum with your thumb while gripping thereaction tube firmly using a uniform pressure along the side of the tube and supporting the bottom. (NOTE: Squeezingthe tube to cause a deformation in the sides of the tube will result in an artificially low result.) Replace the white capTIGHTLY.3. REACTION: Break the bottom (grayish white) ampule in the reaction tube by compressing the sides of the tube. Mixthoroughly by shaking the reaction tube vigorously for 30 seconds. Allow the reaction to proceed for a total of 2minutes. DO NOT BREAK THE GREEN AMPULE.4. ANALYSIS: Press the key and make sure the meter is set for “A 0-20%” (NOTE: If changing the program, see“Selecting a Program” in the manual). Once the meter displays “tUbE”, insert the reaction tube into the opening atthe bottom of the meter. The hole in the white cap must be lined up with the metal pin extending from the inside ofthe hole of the meter. Push the reaction tube all the way into the meter. Press the key on the face of themeter. The display will flash the word “CALC,” and the results will be displayed in volume percent (v/v%) Recordthe results. KEEP THE METER AND REACTION TUBE UPRIGHT AT ALL TIMES.75. DISPOSAL: Carefully remove the reaction tube from the meter. Vent the reaction tube by inserting it completely intothe specially designed venting cap unit and remove slowly. REACTION TUBE AND CAP MUST BE UPRIGHTAND POINTED AWAY FROM USER AND BYSTANDERS. Tap the reaction tube on a hard surface to shake anyloose glass to the bottom of the tube, then break the top (green) ampule in the reaction tube by compressing the sidesof the reaction tube. Shake the tube for 15 seconds. After 5 minutes, vent the tube again. Discard the reaction tubeas laboratory waste. DO NOT REMOVE THE WHITE CAPProgram B –> Procedure for Testing Water Content up to 100%(Reagent Systems: HS-ORP + HS-DVP-12)1. PREPARATION: Remove a screw-capped dilution vial from the fluted cardboard carton, a sampling syringe and awhite-capped reaction tube from the reagent box. Check the contents to ensure that all items are present and intact.Remove the white cap and black septum from the reaction tube. Carefully remove a green water ampule from thecardboard carton and insert it fully into the top of the protective ampule sleeve containing the grayish white ampule.Return the protective ampule sleeve to the reaction tube with the grayish white ampule on the bottom and place thereaction tube into the reagent box.2. SAMPLE INTRODUCTION: Work the plunger of the empty sampling syringe a few times to ensure that it slideseasily. Place the tip of the syringe into the oil sample to be tested (sample must be well mixed and representative) andslowly pull back on the plunger until it reaches the stop and cannot be pulled further. When drawing up the sample,make sure there are no air bubbles in the syringe. If not free of air bubbles, depress the plunger again and draw asecond sample slowly. Remove the syringe from the oil sample and wipe any excess oil from the outside of the syringewith a tissue wipe.3. SAMPLE DILUTION: Remove the screw-cap from the dilution vial. Insert the sampling syringe into the dilutionvial and dispense the oil sample by depressing the plunger. Proceed to mix the solution thoroughly by repeateddrawing and re-dispensing of the solution into the dilution vial with the syringe (3 or 4 times). Using the samesampling syringe, draw up a sample from the diluted solution wiping any excess liquid from the outside of the syringe.Dispense the sample into the reaction tube. Replace the black septum (hole on top) by pressing down on the septumwith your thumb while gripping the reaction tube firmly using a uniform pressure along the side of the tube andsupporting the bottom. (NOTE: Squeezing the tube to cause a deformation in the sides of the tube will result in anartificially low result.) Replace the white cap TIGHTLY.4. REACTION: Break the bottom (grayish white) ampule in the reaction tube by compressing the sides of the tube. Mixthoroughly by shaking the reaction tube vigorously for 30 seconds. Allow the reaction to proceed for a total of 2minutes. DO NOT BREAK THE GREEN AMPULE.5. ANALYSIS: Press the key and make sure the meter is set for “b 1-100%” (NOTE: If changing the program,see “Selecting a Program” in the manual). Once the meter displays “tUbE”, insert the reaction tube into the openingat the bottom of the meter. The hole in the white cap must be lined up with the metal pin extending from the insideof the hole of the meter. Push the reaction tube all the way into the meter. Press the key on the face of themeter. The display will flash the word “CALC,” and the results will be displayed in volume percent (v/v%). Recordthe results. KEEP THE METER AND REACTION TUBE UPRIGHT AT ALL TIMES.6. DISPOSAL: Carefully remove the reaction tube from the meter. Vent the reaction tube by inserting it completely intothe specially designed venting cap unit and remove slowly. REACTION TUBE AND CAP MUST BE UPRIGHT ANDPOINTED AWAY FROM USER AND BYSTANDERS. Tap the reaction tube on a hard surface to shake any looseglass to the bottom of the tube, then break the top (green) ampule in the reaction tube by compressing the sides of thereaction tube. Shake the tube for 15 seconds. After 5 minutes, vent the tube again. Discard the reaction tube anddilution vial as laboratory waste. DO NOT REMOVE WHITE CAP.8Programs C, D & E –> Procedure for Testing Low Levels of Water in Oil Using a 5 mL SampleSize(Reagent System: HS-LRP)WARNING - DO NOT USE 5 ML SAMPLES OF PHOSPHATE ESTER BASED HYDRAULIC FLUIDS,GASOLINE OR SOLVENTS SUCH AS ACETONE. THESE MATERIALS WEAKEN THE REACTION TUBESWHICH MAY RESULT IN TUBE FAILURE.1. PREPARATION: Remove a sampling syringe and a white-capped reaction tube from the reagent box. Check thecontents to ensure that all items are present and intact. Remove the white cap and black septum from the reaction tube.Carefully remove a green water ampule from the cardboard carton and insert it fully into the top of the protectiveampule sleeve containing the grayish white ampule. Do not replace the protective ampule sleeve into the tube atthis time.2. SAMPLING: Using a clean polyethylene sampling pipette, pipette 5 mL of the oil to be tested into the reaction tube,e.g., up to 5 mL line marked on side of the reaction tube (NOTE: The protective ampule sleeve is not to be in thetube at this time.). Insert the protective ampule sleeve into the reaction tube with the grayish white ampule on thebottom. Replace the black septum (hole on top) by pressing down on the septum with your thumb while gripping thereaction tube firmly using a uniform pressure along the side of the tube and supporting the bottom. (NOTE: Squeezingthe tube to cause a deformation in the sides of the tube will result in an artificially low result.) Replace the white capTIGHTLY. NOTE: A homogeneous, representative sample of the oil being tested must be used to obtain accurateresults.3. REACTION: Break the bottom (grayish white) ampule in the reaction tube by compressing the sides of the tube. Mixthoroughly by shaking the reaction tube vigorously for 30 seconds. Allow the reaction to proceed for a total of 4minutes. The mixture will bubble and perhaps foam during this time DO NOT BREAK THE GREEN AMPULE.(NOTE: Some oils require a longer reaction time to achieve complete reaction. This is especially true for oils run onprogram C. If this is the case, shake the reaction tube again for 30 seconds and let stand for an additional 4 minutes.)4. ANALYSIS: Press the key once to activate the meter. Ensure the meter is set for the correct program C, D orE for the sample matrix being tested (See “Selecting a Program” for instructions on how to change programs.). Oncethe meter displays “tUbE”, insert the reaction tube into the opening at the bottom of the meter. The hole in the whitecap must be lined up with the metal pin extending from the inside of the hole of the meter. Push the reaction tube allthe way into the meter. Press the key on the face of the meter. The display will flash the word “CALC,” andthe results will be in micrograms of water per milliliter of sample displayed as ppm. Record the results. KEEPTHE METER AND REACTION TUBE UPRIGHT AT ALL TIMES.5. DISPOSAL: Carefully remove the reaction tube from the meter. Vent the reaction tube by inserting it completely intothe specially designed venting cap unit and remove slowly. REACTION TUBE AND CAP MUST BE UPRIGHTAND POINTED AWAY FROM USER AND BYSTANDERS. Tap the reaction tube on a hard surface to shake anyloose glass to the bottom of the tube, then break the top (green) ampule in the reaction tube by compressing the sidesof the reaction tube. Shake the tube for 15 seconds. After 5 minutes, vent the tube again. Discard the reaction tubeas laboratory waste. DO NOT REMOVE WHITE CAP.6. CALCULATION: The meter is programed to report the result in micrograms per milliliter and displayed as ppm.If a result is to be reported as a weight/weight value, divide the HydroScout result by the density of the oil sample.Water in Oil (µg/g) = R/dwhere:R = Meter reading in µg/mLd = Density of oil in g/mL9Program F –> Procedure for the Analysis of Water in Soils and Solids(Reagent Systems: HS-SEV)1. PREPARATION: Remove a sampling syringe and a white-capped reaction tube from the reagent box and theextraction solvent ampule from the colored-capped soil extraction tube. Check the contents to ensure that all items arepresent and intact. Remove the white cap and black septum from the reaction tube. Carefully remove a green waterampule from the cardboard carton and insert it fully into the top of the protective ampule sleeve containing the grayishwhite ampule. Return the protective ampule sleeve to the reaction tube with the grayish white ampule on the bottom,place the reaction tube into the reagent box. 2. SAMPLE EXTRACTION: Remove the colored cap from the soil extraction tube and tare on an electronic scale.Weigh 5-10 grams of soil to be tested into the soil extraction tube and record the weight. Add the contents of onebreak-top ampule of extraction solvent (white polypropylene top) to the soil extraction tube, re-cap and shake for 1minute. Allow soil in the soil extraction tube to settle for 2 minutes.3. SAMPLING EXTRACTED SAMPLE: Work the plunger of the empty sampling syringe a few times to ensure thatit slides easily. After soil has settled, draw up a sample from the extract layer with the sampling syringe ensuring thatthere are no air bubbles in the syringe. If not free of air bubbles, depress the plunger again and draw a second sampleslowly. Wipe any excess solvent from the outside of the syringe with a tissue wipe and dispense the sample into thereaction tube. Replace the black septum (hole on top) by pressing down on the septum with your thumb while grippingthe reaction tube firmly using a uniform pressure along the side of the tube and supporting the bottom. (NOTE:Squeezing the tube to cause a deformation in the sides of the tube will result in an artificially low result.) Replace thewhite cap TIGHTLY.4. REACTION: Break the bottom (grayish white) ampule in the reaction tube by compressing the sides of the tube. Mixthoroughly by shaking the reaction tube vigorously for 30 seconds. The mixture will bubble and perhaps foam duringthis time. Allow the reaction to proceed for 1.5 minutes. Shake the reaction tube again for 30 seconds and let standfor an additional 30 seconds. DO NOT BREAK THE GREEN AMPULE5. ANALYSIS: Press the key once to activate the meter. Ensure the meter is set for the “F SoiLmg.” program forthe sample matrix being tested (See “Selecting a Program” for instructions on how to change programs.). Once themeter displays “tUbE”, insert the reaction tube into the opening at the bottom of the meter. The hole in the white capmust be lined up with the metal pin extending from the inside of the hole of the meter. Push the reaction tube all theway into the meter. Press the key on the face of the meter. The display will flash the word “CALC,” and theresults will be displayed in milligrams of water in the sample. Record the results. KEEP THE METER ANDREACTION TUBE UPRIGHT AT ALL TIMES.6. DISPOSAL: Carefully remove the reaction tube from the meter. Vent the reaction tube by inserting it completely intothe specially designed venting cap unit and remove slowly. REACTION TUBE AND CAP MUST BE UPRIGHTAND POINTED AWAY FROM USER AND BYSTANDERS. Tap the reaction tube on a hard surface to shake anyloose glass to the bottom of the tube, then break the top (green) ampule in the reaction tube by compressing the sidesof the tube. Shake the tube for 15 seconds. After 5 minutes, vent the tube again. Discard the reaction tube and soilextraction tube as laboratory waste. DO NOT REMOVE WHITE CAP7. CALCULATION: The meter is programed to display the weight of the water, in milligrams, contained in the sample.Calculate the water content in weight percent using the following equation:Water in Soil, wt. percent = R/(10S1)where:R = Meter reading in milligrams of waterS1 = Weight of soil sample, in grams10Procedure G –> Procedure for the Analysis of Paints and Coatings(Reagent System: HS-LPT)Procedure for Expected Water Content Less than 15% (No Dilution)1. PREPARATION: Remove a sampling syringe and a white-capped tube from the box. Check the contents to ensurethat all items are present and intact. Remove the white cap and black septum from the reaction tube. Insert one greenwater ampule into the top of the polypropylene ampule sleeve containing the grayish-white ampule and replace theampule sleeve into the reaction tube with the grayish-white ampule on the bottom2. SAMPLE INTRODUCTION: Remove the cap from the sampling syringe. Work the plunger on the empty samplingsyringe a few times to ensure that it slides easily. Place the tip of the syringe into the paint sample to be tested andslowly pull back on the plunger until it reaches the stop and cannot be pulled further. Remove the syringe from thepaint sample and wipe any excess paint from the outside of the syringe with a tissue wipe. Place a syringe cap on thesyringe and weigh; record the weight (gross sample weight) to the nearest 0.1 mg. Dispense this sample into thereaction tube. Replace the syringe cap and reweigh the syringe and record the weight (sample tare weight). Thedifference in the two weights becomes the sample weight S1 to be used in equation 1 below. Replace the black septum(hole on top) by gripping the tube firmly and pressing the septum down with the thumb. (NOTE: Do not squeeze thesides of the tub while inserting the septum as this will cause a low reading.) Replace the white cap TIGHTLY, turningit until it cannot be turned further.3. REACTION: Break the bottom (gray) ampule in the tube by compressing the sides of the tube. Mix thoroughly byshaking the tube vigorously for 30 seconds. The mixture will be seen to bubble and perhaps foam. Allow the reactionto proceed for 2 minutes. Shake the reaction tube again for 10 seconds and let stand for an additional 1 minute.4. ANALYSIS: Press the key to activate the meter. Ensure the meter is set for "Program G" (See “Selecting aProgram” in the manual on how to change programs). Once the meter displays “tUbE”, insert the reaction tube firmlyinto the opening at the bottom of the meter. The hole in the white cap must be lined up with the metal pin extendingfrom the inside of the hole in the meter. Push the reaction tube all the way into the meter. Press the key onthe face of the meter. The display will flash the word "CALC," then the results will displayed in milligrams of waterin the sample. Record the results. KEEP THE METER AND TUBE UPRIGHT AT ALL TIMES.5. DISPOSAL: Carefully remove the reaction tube from the meter. Vent tube by inserting completely into venting capunit and remove slowly. REACTION TUBE AND CAP MUST BE UPRIGHT AND POINTED AWAY FROMUSER AND BYSTANDERS. Tap the tube on the bench top to shake any loose glass to the bottom of the tube, thenbreak the top (green) ampule in the reaction tube by compressing the sides of the tube. Shake the tube for 15 seconds.After 5 minutes, vent the tube again. Discard the reaction tube and vial as laboratory waste. DO NOT REMOVEWHITE CAP.6. CALCULATION: The meter is programed to display the weight, in milligrams, of the water contained in the sampleintroduced into the reaction tube (In this case the raw sample). Calculate the water content in the sample in weightpercent using the following equation:Water in paint, wt. percent = R/(S1x10) (1)where:R = Meter reading in milligrams of waterS1 = actual weight of whole paint sample, in grams11Procedure G –> Procedure for the Analysis of Paints and Coatings (cont’d)(Reagent System: HS-HPT)Procedure for Expected Water Content Greater than 15% (with Dilution)1. PREPARATION: Remove a dilution vial, two sampling syringes, two caps and a white-capped tube from the box.Check the contents to ensure that all items are present and intact. Remove the white cap and black septum from thereaction tube and the cap from the dilution vial. Insert one green water ampule into the top of the polypropyleneampule sleeve and replace the ampule sleeve into the reaction tube with the grayish-white ampule on the bottom.2. SAMPLE INTRODUCTION: Remove the cap from an empty sampling syringe. Work the plunger on the emptysampling syringe a few times to ensure that it slides easily. Place the tip of the syringe into the paint sample to be testedand slowly pull back on the plunger until it reaches the stop and cannot be pulled further. Remove the syringe fromthe paint sample and wipe any excess paint from the outside of the syringe with a tissue wipe. Place a syringe cap onthe syringe and weigh; record the weight (gross sample weight) to the nearest 0.1 mg.3. SAMPLE DILUTION: Remove the syringe cap and insert the sampling syringe into the dilution vial and dispense thepaint sample by depressing the plunger. (Do not allow the syringe to contact the dilution solvent when dispensing thesample.) Replace the syringe cap and reweigh the syringe and record the weight (sample tare weight). The differencein the two weights becomes the sample weight S1 to be used in equation 2 below. Replace the white cap on the dilutionvial and shake the vial vigorously for at least 10 seconds. Remove the vial cap and quickly, using a new samplingsyringe, draw up a sample from the solution. Wipe any excess solution from the outside of the syringe, cap with a freshcap and weigh the syringe. Record this weight (diluted sample gross weight). Dispense this sample into the reactiontube. Replace the cap and reweigh the syringe and record this weight (diluted sample tare weight). The difference inthe two weights becomes the sample weight S2 to be used in equation 2 below. Replace the black septum (hole on top)by gripping the tube firmly and pressing the septum down with the thumb. (NOTE: Do not squeeze the sides of thetube while inserting the septum as this will cause a low reading.) Replace the white cap TIGHTLY, turning it untilit cannot be turned further.4. REACTION: Break the bottom (gray) ampule in the tube by compressing the sides of the tube. Mix thoroughly byshaking the tube vigorously for 30 seconds. The mixture will be seen to bubble and perhaps foam. Allow the reactionto proceed for 2 minutes. Shake the reaction tube again for 10 seconds and let stand for an additional 1 minute.5. ANALYSIS: Press the key to activate the meter. Ensure the meter is set for "Program G" (See “Selecting aProgram” in the manual on how to change programs). Once the meter displays “tUbE”, insert the reaction tube firmlyinto the opening at the bottom of the meter. The hole in the white cap must be lined up with the metal pin extendingfrom the inside of the hole in the meter. Push the reaction tube all the way into the meter. Press the key onthe face of the meter. The display will flash the word "CALC," then the results will displayed in milligrams of waterin the diluted sample. Record the results. KEEP THE METER AND TUBE UPRIGHT AT ALL TIMES.6. DISPOSAL: Carefully remove the reaction tube from the meter. Vent tube by inserting completely into venting capand remove slowly. REACTION TUBE AND CAP MUST BE UPRIGHT AND POINTED AWAY FROM USERAND BYSTANDERS. Tap the tube on the bench top to shake any loose glass to the bottom of the tube, then breakthe top (green) ampule in the reaction tube by compressing the sides of the tube. Shake the tube for 15 seconds. After5 minutes, vent the tube again. Discard the tube and vial as laboratory waste. DO NOT REMOVE WHITE CAP.7. CALCULATION: The meter is programed to display the weight, in milligrams, of the water contained in the sampleintroduced into the reaction tube (In this case the diluted sample). Calculate the water content in the original paintsample in weight percent using the following equation:Water in paint, wt. percent = (R/S2)(1+(2.15/S1))/10 (2)where:R = Meter reading in milligrams of waterS1 = actual weight of whole paint sample, in gramsS2 = actual weight of diluted paint sample, in grams2.15 = Weight of the dilution solvent, in grams12Appendix A: Comparison DataDetermination of Water in Used Oil on Program A and B, w/w%Expected HydroScout1 Karl Fischer0 0.161 0.0610.1 0.148 0.1450.2 0.226 0.2550.5 0.458 0.5601.0 0.948 1.072.0 2.36 2.465.0 5.03 5.0510.0 9.82 9.9920.0 20.2 20.025.0 26.37 26.0550.0 50.01 50.611 HydroScout results converted to w% using sample densityAnalysis of Used Oil Certified Reference Materials on Programs A and B2CRM Certified Value, wt % HydroScout1, wt % Karl Fischer, wt %ERM-34 1.95 1.92±0.02 1.86±0.09ERM-35 5.86 5.91±0.61 5.82±0.79ERM-36 10.3 10.30±0.53 10.3±0.43ERM-41 87.4 88.4±6.7 86.4±6.61 HydroScout results converted to w% using sample density 2 ERM-34 to 41 Water Content in Used Oil Mixtures from Environmental Reference Materials, Inc.13Analysis of Low Levels of Water in Turbine and Gear Oils Using Program COil Type Karl Fischer (µg/mL) HydroScout (µg/mL) C.V.Exxon Teresstic Turbine Oil GT32 18.7 0 .169200 140 .124396 404 .023793 825 .019Mobil DTE Turbine Oil Light 26 53 .08236 202 .007448 410 .043838 778 .026Shell Turbo T32 23 34 .019220 223 .04433 403 .01825 800 .038Ideal Turbine Oil AW-32 39 43 .072210 208 .013400 435 .005759 842 .013Renolin Turbine Oil T-32 28 40 .067250 238 .024409 410 .039798 832 .01Dupont Diamond Class Turbine Oil 32 16 117 .056202 220 .048429 399 .03833 783 .011Texaco Havoline 80W-90 Gear Oil 285 250 .062510 460 .024721 659 .0111120 1037 .00814Analysis of Water Content in Various Fluids Using Program DFluid Type Karl Fischer (µg/mL) HydroScout (µg/mL) C.V.NAPA Non-Detergent SAE 30 0 17 .07388 117 .069176 217 .08351 303 .071702 661 .0641405 1450 .048Amalie Non-Detergent SAE 30 0 2 .05187 101 .038175 166 .057349 374 .009696 712 .0271397 1528 .015Valvoline Non-Detergent SAE 30 0 30 .05988 96 .042175 136 .061350 368 .028701 784 .021401 1497 .041Oilzum Non-Detergent SAE 50 0 76 .05189 126 .024177 212 .06355 404 .02707 799 .0091419 1595 .016Gunk Heavy-Duty Brake Fluid 3835 4123 .014318 4323 .0134586 4795 .0095136 5341 .002Shell Diala A 0 70 .03988 121 .054177 189 .055353 372 .012707 715 .0411413 1506 .01815Analysis of Various Fluids Using Program EFluid Type Karl Fischer (µg/mL) HydroScout (µg/mL) C.V.Exxon Superflo 10W-30 0 82 .08287 150 .014174 213 .029348 395 .009695 632 .0111390 1425 .037Mobil 1 10W-30 0 36 .04486 95 .035172 126 .047343 289 .035687 602 .0391374 1313 .015Quaker State SAE 30 0 7 .01888 105 .06176 183 .104352 333 .044703 597 .041406 1491 .018Quaker State Proline 10W-40 (Used) 0 26 .07989 195 .076178 294 .026357 409 .023714 801 .0101428 1370 .027Valvoline SAE 50 0 11 .04188 87 .047177 129 .039354 284 .035708 632 .0641415 1482 .021John Deere Hydraulic Fluid 0 0 .0388 145 .03176 233 .011352 330 .042704 664 .0371409 1597 .01316Analysis of Various Soil Types Using Program FSoil Type / Spiked Water Content (wt %) Average HydroScout Result (wt %) C.V. Composite Sandy-Clay-Loam0 0 -5.7 6.19 0.021910.1 10.65 0.038720.1 19.79 0.0236Sea Sediment0 0.08 -10.2 9.66 0.013120.0 18.68 0.018429.9 26.63 0.0081Topsoil0 0.21 -5.0 5.13 0.037710.1 10.33 0.024820.0 19.50 0.0026Sand0 0.22 -5.1 5.30 0.026610.1 10.30 0.027415.0 15.42 0.0304Clay Loam I0 0 -5.0 4.47 0.035410.2 10.50 0.003220.1 18.92 0.0041Clay Loam II0 0 -5.2 5.49 0.010410.1 10.19 0.006520.1 19.96 0.0038Georgia Clay0 0 -5.1 5.23 0.016810.0 10.17 0.023120.6 20.29 0.0281Alabama Clay0 0 -5.0 4.87 0.025910.1 10.14 0.002821.2 20.21 0.003017Calcium Hydride vs Karl Fischery = 0.9621x + 0.2562R2 = 0.980601020304050607080901000 20 40 60 80 100Water by Karl Fischer (%)Water by HydroSCOUT (%)Analysis of Various Coatings Using Program GData from the ASTM Inter-Laboratory Study of the Calcium Hydride Method D7358 comparing the HydroScout resultswith Karl Fischer. The coatings analyzed were:Fluid A: Clear Acrylic sealer Fluid B: Acrylic white tint baseFluid C: Acrylic stain Fluid D: Phenolic resin containing approximately 10% unreacted Phenol.Fluid E: Pigmented polyester polyol resin system containing MEK, Toluene, Ethyl Acetate, PM Acetate, and Ethyl3-Ethoxy Propionate. Fluid F: Phenolic coating containing approximately 5% unreacted Phenol as well as Ethyl Alcohol, PM Acetate, andDipropylene Glycol Monomethyl Ether.18Appendix B: Meter SpecificationsA/D Resolution: 12 bitMeasurement Range: Program and analyte dependantProgram MDL Max Linear RangeA 0.15% (v/v) 20% (v/v)B 5% (v/v) 100% (v/v)C, D& E 50 ug/mL 10,000 ug/mLF 0.25% (wt/wt)* 100% (wt/wt)**G 0.15% (wt/wt) 100% (wt/wt)* Using a 10 gram sample.** Using a 1 gram sample.Program Storage: Non-VolatileDisplay : 4 Digit 0.35 inch LCD with Program IndicatorBattery: One 9V Lithium (included) [Use only Alkaline or Lithium]Battery Life: 10,000 measurements or 10 year shelf-life (using 1200 mAh lithium battery)Operating Temperature: 4°C to 40°CDimensions: length - 5.9" (150 mm), width - 3.2" (81 mm), height - 1.8" (46 mm)Weight: 9.2 oz (261 g)