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Methods Manual 2011 - Natural Resource Ecology Laboratory

1. 4 Ziplock style freezer bags garbage 4 Safety pins Keep several sizes Topper sponges Different sizes Triangular bandages or Cravats i Any dressing that can be used for absorbing large quantities of 2 Surgical dressings lg sanitary napkins blood is acceptable 8 4 x4 sterile dressings Telfa Assorted Band Aids Keep different styles on hand Moleskin Useful for blisters 2 Roller bandages 3 or 4 1 Roller bandage 2 1 Roll of adhesive tape Athletic tape works well 2 SAM splits wire ladder or other splint 2 Tongue depressors 1 Accident release form Used if aid is declined by patient 2 Butterfly closures Useful for deep incisions 1 2 Packets of sugar honey or glucose Used for diabetics 1 Pen light 1 CPR mask with one way valve 1 Suction device e g a modified turkey baster Most people use a specially made tip and tail for a ski If you 1 Traction application gear don t have these make sure you have something as effective a nice new alternative is the Kendrick traction device 1 Windlass for traction 6 wood dowel 6 Avalanche cord For use in pulling traction 1 Trauma shears 1 package Antiseptic wipes e g PAWS Basic Equipment for your Backpack Quantity Item Comments 1 Pliers Leatherman type 1 Screwdriver Combo Phillips amp flat head 1 Knife Pocket knife or Leatherman which combines all 3 of t
2. DE aii i Ki LANN AA AN bn D n gt z Sos 170 ES AS NAS Wan lternate route involves a very steep descent into the Lost Meadow Basin Travel with caution Loch Vale Watershed Methods Manual 68 AAA Glacier Gorge to Loch Outlet via Alberta Falls 250 te ural Lin Ji 15m Cam 004 104 Um Am l Um im 14 Summer Trail liln r 7 f i 7 NAF DNI S 5 B S E T 69 Loch Vale Watershed Methods Manual Glacier Gorge to Loch Outlet via Chaos Creek ZE ve Gr a Am AA Um n Li m u Lt fw 11 mi Ddw im 00m Wim Wim gw Im Mw 0 w 100 ural Gat HIN 2 e E Wi NN 5 NOOO NON t5 3 E DAN 1 KC ANN S 70 Loch Vale Watershed Methods Manual PS Glacier Gorge to Loch Outlet via Chaos Creek Fire Trail S a le 8 E OU Set Si E SS E 2 ei a si Si E E i E N Si RS Ke Si z sos aS gt E ER 71 Loch Vale Watershed Methods Manual Appendix B Sampling Schedule Table B1 LVWS surface water sampling schedule for active sites Name Sampling Frequency Analyses Andrews Creek 1 month summer RU FU DOC DOP DON Emerald Outlet 1 year fall RU FU DOC DOP DON Haiyaha Outlet 1 year fall R
3. Before starting up the trail to LVWS ensure your radios are functioning properly To do this turn on radio by turning volume knob clockwise Then adjust squelch by turning squelch knob clockwise until static is heard Turn squelch down counterclockwise until static is no longer audible Turn channel selector knob to channel one Listen to make sure there is no other radio traffic you would be interrupting Once you are sure the channel is clear key the transmit switch and say ROMO Researcher Baron Radio check Release key They will answer Researcher Baron loud and clear You then say Copy Researcher Baron clear If ROMO cannot hear you there will obviously be no reply to your call Repeat your initial call two more times spaced by 30 seconds apiece If no contact is made say No contact VIP Researcher clear Loch Vale Watershed Methods Manual 8 Channels one and two are the primary channels used by RMNP personnel within the park Channel 11 is recommended for communication between LVWS staff while in the field Keep your radio set on ROMO i e channel one or two while traveling as a group that way you can assist if an incident occurs elsewhere If you encounter an incident do not hesitate to call for help You should not have any trouble reaching ROMO from anywhere in the LVWS You may have to move to higher ground to increase quality of transmission If your group separates at some point use channel 11 fo
4. and total phosphorus TP dissolved organic phosphorus DOP can be calculated by simple subtraction Be sure the test tubes and threads are free of chips and cracks since contents may be lost during autoclaving Set autoclave for liquid cycle 250 F 50 min using only the cycle 4 button If system is set for a different cycle please see Dan Reuss lab manager 1 Pipette 5 ml of standards samples washes and duplicates into acid washed and oven dried borosilicate glass test tubes 2 Add 1 ml of potassium persulfate oxidizing solution to each tube 12 5 g potassium persulfate to volume in a 250 ml volumetric adjust recipe depending on sample size 3 Tightly cap the tubes with acid washed linerless caps and arrange in autoclavable racks Loch Vale Watershed Methods Manual 50 With remaining persulfate make up a 1 5 mixture of potassium persulfate to di in 1000 ml flasks 80 ml persulfate to 400 ml di Two flasks should be enough for 1 run of 90 samples or 2 smaller runs This is to be used in place of di in the sampler wash line Be sure to leave plenty of head space 1 2 of flask so oxidant does not overflow in autoclave Use foil and autoclave tape to seal the flasks Place racks with tubes and sealed flasks in metal pans in autoclave Fill the pans with a di water bath to the depth of the solution in the flasks and tubes This will minimize leaks due to rapid changes in temperature and pressure Turn on the power to the au
5. 5 All boxes to be shipped should be placed in or near the out going mail box near the NREL elevator Loch Vale Watershed Methods Manual 65 REFERENCES Allstott E J M A Bashkin and J Baron 1999 Loch Vale watershed project quality assurance report 1995 1998 U S Geological Survey Open File Report 99 111 23 p Botte J A and J Baron 2003 Loch Vale watershed project methods manual 2003 Natural Resource Ecology Laboratory Colorado State University Fort Collins Colorado 80 p Botte J A and J Baron 2004 Quality assurance report Loch Vale watershed 1999 2002 U S Geological Survey Biological Resources Discipline Open File Report 2004 1306 17 p Clesceri L S A E Greenbery and A D Eaton eds 1998 Standard methods for the examination of water and wastewater 20t ed American Public Health Association Washington D C 1 325 p Denning A S 1987 Quality assurance report 1982 1987 Loch Vale watershed project Natural Resource Ecology Laboratory Colorado State University Fort Collins Colorado 19 p Dosset S R and V C Bowersox 1999 National Trends Network site operation manual National Atmospheric Deposition Program Office Illinois State Water Survey NADP Manual 1999 01 Champaign Illinois 99 p Edwards R L 1991 Quality Assurance Report Loch Vale Watershed Study 1989 1990 Natural Resource Ecology Laboratory Colorado State University Fort Collins Colorado 22 p Newkirk B K 199
6. relationship to be correct Check frequently especially during high flows and remove any obstructions The pen carriage rails in the Stevens Recorder may need to be cleaned so the pen can move smoothly along the time axis Sometimes problems that appear as clock malfunction can be attributed to dirty rails Lubricate with dry graphite or WD 40 Usually the Stevens gage pen will last 2 3 seasons Make sure there are spares in the supply bag located in the Stevens stilling well Loch Vale Watershed Methods Manual 89 Winter Lake Sampling Discontinued in 2002 a Introduction The lakes in the LVWS freeze over sometime in October In the field book note the date and percentage of ice cover of the Loch until frozen completely Also note the percentage of ice cover and date each week in the spring until the Loch is ice free Due to minimal flow after freezing lakes become nearly closed basins until the following spring When ice covered lake water thermally stratifies and in lake biological processes are more likely to influence water chemistry than under summer flow conditions Take water samples from upper surface and lower hypolimnion water layers of Sky Pond and the Loch after boring through ice bi monthly during ice covered period Equipment and Supplies Hand crank peristaltic pump 10 meters of acid washed DI rinsed tubing Sink weight and duct tape Orion conductivity temperature meter Butyl glo
7. sampling period Record the field blank storage location Note any unusual site conditions in the REMARKS section Each sampler is labeled with a unique two letter code on the bottom of the sampler Packing and shipping exposed sampler s ensure the shipping bag with the citric acid filter paper is sealed and place it in the shipping box Include the top white copy of the field form Seal the box with tape affix the prepaid shipping form and send to N Q ON wm Phyllis Ballard Central Analytical Laboratory Illinois State Water Survey 2204 Griffith Dr Dock B Champaign IL 61820 7463 Loch Vale Watershed Methods Manual 19 f Be Aware Beware of ammonia contamination Be sure to store all samplers in the NREL freezer while they await deployment to the field or shipment to CAL This will minimize sampler contamination Be sure to wear the vinyl gloves provided by NADP whenever handling a NH sampler If the sampler falls onto the ground or another surface but remains intact simply pick it up ensure the flexible tubing is firmly attached to the cartridge and deploy or pack the sampler as you would normally Make a note on the field form If in doubt contact the CAL for guidance AMON Site Liaison Telephone 800 952 7353 toll free Email amon isws illinois edu Loch Vale Watershed Methods Manual 20 Measuring Conductivity a Introduction The conductivity of a solution is its ability to conduct an
8. 66 APPENDICES ia RIE A GO EAS 67 Appendix A Sampling Locations dE 67 Appendix B Samipling E EE 72 Appendix C Quality Assurance Quality Control Samples ENEE 74 Appendix D Lak errereen kt Eege 75 Appendix NN 76 Appendix Ts SUP PUSS eneee Eeer gebei E eE E ae e SEEE tabu e ES EE ea Seet ta 80 Appendix G Radio Channels in Rocky Mountain National Park AAA 82 Appendix H Database WiAanag eminent e 83 Appendix I Historical Field and Laboratory Procedures eva acopiar dida 84 Appendix LV VV SW atershecd EE 95 Loch Vale Watershed Methods Manual 2 FIELD PROCEDURES General Introduction Weekly field procedures in LVWS include 1 collection of precipitation for chemical analysis 2 measurement of precipitation amount and 3 sampling of surface waters for chemical analysis The National Atmospheric Deposition Program NADP monitoring site CO98 was established within the LVWS in 1983 NADP is a national network of precipitation monitoring sites The network is a cooperative effort between many different groups including the State Agricultural Experiment Stations USGS U S Department of Agriculture and other governmental and private entities The objective of the network is to provide data on the amounts trends and geographic distributions of acids nutrients and base cations in precipitation Samples from each station are collected weekly using clean handling procedures and sent to the Central Analytical Laboratory CAL in Champaign
9. C 1mlN 1mlN 20 ml 2M HCl 40 ml 2M HCl And fill to meniscus with DI And fill to meniscus with DI d Procedures Use the following procedures when working from the template sample table 1 Each row will be assigned a specific sample and must be named according to the sample site and date For example LO_NORM_031215 refers to a Loch O normal sample from Dec 15 2003 Be sure to name all samples washes and checks in the empty sample name column The vial number is the sample table must correspond with the location of the sample in the sample tray 2 Prepare the first twelve sample vials in the sample tray according the following table These vials will be used to wash the machine and determine calibration curves Vial Contents DI Calibration Std Calibration Std DI Calibration Std Calibration Std Check Std DI Check Std DI Check Std DI pa elle dl ts CAE pa o m eN m N 3 Fill the 40 ml sampler vials with at least 15 ml of analyte and note the position of each sample in the tray Cover all sampler vials with parafilm to prevent evaporation and contamination Along with field blanks field dupes and an occasional lab dupe every Loch Vale Watershed Methods Manual 53 20 samples be sure to insert a DI wash and check 3C 2N after every 10 samples DI wash and check samples should be included in the template file End the run witha wa
10. Contact the NREL admin office to request a Stockroom user card To make a purchase via Kuali login to the Campus Administrative Portal CAP via the CSU website Once logged into CAP click on Kuali Financial System KFS One in Kuali click on Shop Catalogs and browse to the company and supplies you need Add the desired supplies to your basket click Review check that the shipping address is correct and fill out the form as appropriate For the Object type 6201 for supplies Consult Karen Adleman kadleman nrel colostate edu or someone else in the NREL admin office NESB A202 if you need assistance navigating Kuali To fill out a Purchase Request Form visit the NREL website On the website click on Internal Resources and login Navigate to a blank Purchase Request Form by clicking on Procedures and Guidelines Consult the NREL reallocater in the admin office or Program Manager if you are unfamiliar with Purchase Request Forms New field supplies can be purchased from either Ben Meadows or Forestry Supply after filling out a Purchase Request Form Any purchase over 500 requires approval from the Principal Investigator All purchases require a justification statement Some frequently ordered supplies are listed below NADP National Atmospheric Deposition Program 75 1 uS cm Specific Conductance Standard SCS solution from NADP 1442 uS cmt Quality Control QC check solution from NADP Field Observer Report Forms Packing
11. Empty the PO waste into the container in the acid cabinet in A258 Empty and discard the sample cups and tubes Rinse the sampler racks with DI water and set on the bench to dry Loch Vale Watershed Methods Manual 49 8 Refrigerate the standards if the instrument will be used the next day or freeze them if it will be longer 9 Wipe down the instrument and benches with a moist sponge Switching the AlpKem from NH4 NOz to PO 1 Make sure the NH waste container is empty The waste goes in the bottle on the floor by the sink 2 Disconnect the NH waste from spec line from the outflow tube of the channel 3 PO NHa detector and connect the PO waste from spec line in its place 3 Disconnect the NH to spec line from the bottom connection on the debubbler on the channel 3 detector and replace it with the POs to spec line 4 Disconnect the NH from debubbler line from the top connection on the debubbler and replace it with the PO from debubbler line 5 Turn the NH heater off and the PO4 heater on 6 Disconnect the sampler line from the T where the NH4 sample line and the NO3 sample pull thru line meet and connect it to the pump tube labeled PO sample Total Phosphorus Methods for total phosphorus are taken from the Hedin lab at Cornell This is a modification of the total nitrogen method with a few slight differences By analyzing samples for orthophosphate PO4
12. Illinois for chemical analysis Aerochem Metrics samplers collect precipitation samples for analysis of water chemistry Concentrations of solutes in precipitation water can be multiplied with precipitation volume to estimate chemical deposition Methods for operating precipitation collectors and raingages are found in the NADP National Trends Network Site Operation Manual Dosset and Bowersox 1999 An Alter shielded Belfort raingage measured precipitation volume for CO98 from August 1983 to August 2010 NADP updated CO98 with an electronic NOAH IV raingage in June 2007 An additional or co located NADP site was installed in October 2010 under the name CO89 CO89 consists of an Aerochem Metrics precipitation collector and NOAH IV electronic raingage After recording three years of co located data with the CO98 NOAH IV the CO98 Belfort was removed from the Loch Vale NADP site on August 9 2010 A Parshall Flume with stilling well was installed at the Loch Outlet in 1983 Prior to August 2006 stage was measured with a float within the stilling well Stream levels were recorded with a Campbell Scientific CR500 stream recorder and a Leupold and Stevens strip chart recorder served as a backup for the Campbell Stage data were then converted to discharge values me Operation of the Loch Outlet stream gage was transferred to the USGS Water Resources Division WRD in August 2006 Stage is currently monitored with a depth transducer and data logger
13. N Tap on the Connect button to connect to CO98 raingage No 0 Once Connected is displayed on the screen check the gage information Tap on Download to move to Download page 10 Select start date and time i e bucket on from previous week tap on Download 11 Tap on Data to move to Data page 12 Select Sample Start i e bucket on from previous week and End dates i e bucket off for current week then set Network to NTN 1 and tap View to view daily precipitation totals RECORD THE DAILY PRECIPITATION TOTALS IN THE FIELD BOOK 13 Tap X to close window 14 15 At Raingage page Tap Refresh Note voltage and bucket depth 16 Tap Collectors then Refresh and note status of both CO98 NTN 1 and CO89 MDN 2 collectors 17 Tap Disconnect to move to Disconnect page then tap Disconnect and Exit Navigate to Raingage page by tapping Time and then Raingage and Exit again Download data from CO89 NOAH IV Precipitation Gage a k a MDN 2 and NPX3 Repeat steps 1 17 from above but use CO89 MDN 2 and NPX3 for gage and collector references Turn off PDA Transfer data files to NADP Archive folder and email to NADP 1 Back in the office connect the PDA to the computer 2 Navigate to the folder where the data files are stored on the PDA 3 Copy new files to data baron NADP_Archive year site There should be two f
14. NREL A254 and the plastic bottles and caps are in NREL A235 Plastic bottles and caps various sizes from 2 L to 60 ml 10 by volume HCI acid bath see recipe in Appendix E DI water Plastic dishpans Lab coat goggles rubber gloves and closed toe shoes Sodium bicarbonate to neutralize acid spills Estimated time to complete procedure Allow one half hour for the first 12 bottles and 15 minutes for each additional set of 12 bottles Preparation 1 2 Make sure you are aware of safety procedures for dealing with strong acids The NREL lab manager must certify you for safe laboratory practices Bottles to be washed should have no visible dirt or oil If necessary wash them in hot water and Alconox detergent before acid cleaning making sure all detergent has been thoroughly rinsed off with tap water The bottles and caps should have a final DI rinse before entering acid bath Remove any tape or labels on bottles before placing in the acid bath The acid will alter the labels causing them to fragment and dirty the acid bath as well as make them much harder to remove from the bottle The acid baths are good for about six months depending on how heavily they are used Replace the acid baths if there is substantial particulate material in it or if the acidity has decreased Acid must be neutralized before disposal Consult a lab manager for assistance neutralizing the acid after which is can be poured down the drain with copious
15. Raingage Collector Figure 2 Wiring diagram for the Loch Vale NADP sites CO98 and CO839 each site is wired independently Loch Vale Watershed Methods Manual 13 The dry side bucket is changed monthly and the foam lid seal is changed twice a year DI rinsed dry side buckets should be carried to the NADP the first Tuesday of every month Replace the dry side buckets before replacing wet side buckets The CAL will send new lid seals necessary Follow installation instructions that come with the lid seal If you have concerns or problems with any NADP equipment contact the NADP Site Liaison Matt Layden immediately The CAL contact for all questions and problems is Matt Layden NADP Site Liaison Telephone 217 244 0372 Email ntn sws uiuc edu Loch Vale Watershed Methods Manual 14 NOAH IV Raingage a Introduction An Alter shielded NOAH IV electronic raingage egage was installed at the CO98 NADP site in June 2007 The ETI NOAH IV Total Precipitation Gage provides accurate and unattended measurements of rain and snow precipitation over a full range of temperatures and environmental conditions An additional egage was installed at the LVWS NADP site in October 2009 when the co located CO89 NADP site was established Site operators are required to download precipitation data from both NOAH IVs every Tuesday Raingages are kept in a winterized state all year requiring the catch buckets to be emptied periodically Detailed
16. Routine sampling of precipitation chemistry surface water chemistry hydrology and meteorological conditions and began in 1983 Since then all samples and data have been analyzed according to accepted and published methods e g Clesceri et al 1998 U S Environmental Protection Agency 1987 Collection and analyses methods for all data have been rigorously tested Quality assurance methods and results are described in reports produced by LVWS personnel Denning 1988 Edwards 1991 Allstott 1995 Allstott et al 1999 Botte and Baron 2004 and Richer and Baron 2011 Loch Vale Watershed Methods Manual 1 Table of Contents CHEM 1 NIETO TT 1 TAILS Contents ae 2 FELD PROCEDURES a a ence re bide EET ld 3 General OO UCA AAA A A as 3 Field Eeer Aere ie 4 Snow Stability EE 5 Radio E 8 PERSE ATU E 10 Basic Equipment for your Backpack arado IA SCENE SE 10 Precipitation SAMPUN oanet ea rarae used caverns rebonsh ES EA Eea ESEE EA ELETE DEERE S SEE ENNE CEEE SECES 11 NOAH IV Rail A E EE 15 Ambient a een Ee 18 Measuring TEE 21 DUE LACE Water ee A ar exon EE i ae E e EE E zune Ee 23 Collection Permits and Fee WalVerS sonaba iban dai taci n 26 LABORATORY PROCEDURES atascado don 27 General IO UCA consent ea Ee 27 Filtration for Major ET 29 Filtration for DOC DON and DOP ao dns 33 ET 36 PDR e 39 CHAT AU LOGS ULES ee ee 52 LECO CN peter 57 Acid washing E EE 61 SHIPPING SAMPLES iaa OA R N AR aia 63 Surface EE 63 Ier en EI 64 REFERENCES o idad
17. amounts of tap water Loch Vale Watershed Methods Manual 61 e Procedures 1 Submerge bottles and caps except for the green Teflon lined caps used for amber borosilicate bottles these caps get soaked and rinsed with DI water only in acid bath Be sure bottles have been DI rinsed before entering bath Bottles must be completely immersed in the acid bath for at least three hours prior to removal and DI rinses Wear all protective gear available when submerging bottles being careful not to splash or drip acid outside the acid bath Sodium bicarbonate and water can be used to neutralize and clean up any acid spills After gently pouring acid back into bath place bottles and caps into a plastic dishpan Again be careful not to spill or drip acid Rinse all outside surfaces briefly with DI water Place the caps into a large mouthed jar or beaker and fill shake and dump DI seven times to rinse caps Set aside in jar filled with DI until needed Fill each bottle of 1 3 full with DI water shake and empty Repeat 6X to remove any residual acid After seventh rinse fill bottle with DI water and screw on rinsed cap of appropriate size Store washed bottles under the lab bench in NREL A235 Check conductivity of water in the bottles before use see page 34 for instructions on how to measure conductivity Rewash any bottle with a conductivity value gt 2 uS cm1 Be Aware Protective clothing must be worn when working with str
18. and fill a vial with the sample to be measured Immerse probe in the sample vial and wait for stable measurement Once the pH has stabilized to the hundredths place record measurement on lab sheet notebook Remove probe from the sample vial and thoroughly rinse with DI water Blot excess water from probe tip with Kimwipe Rinse the stir bar with DI blot dry and transfer to next sample vial Repeat steps 6 through 8 for each additional sample If measuring more than five samples re measure QC sample after every fifth cup samples to check for drift If QC sample is not 4 90 0 15 re measure last five samples if possible Be Aware The plastic body of the pH electrode is fragile Be careful not to crack or scratch it Be especially careful not to allow anything solid to touch the spherical glass membrane at the tip of the probe It is easily scratched which ruins the electrode The electrical potential being measured is in the millivolt range therefore the equipment is extremely sensitive to static charge Stand back and keep motions to a minimum when attempting a measurement Loch Vale Watershed Methods Manual 94 Appendix J LVWS Watershed Staff The LVWS Watershed Project staff is made up of a Principal Investigator co Principal Investigator s Program Manager technicians programmers graduate students undergraduate students and collaborators Principal Investigator Jill Baron Ph D U S Geological Survey Natural Re
19. cartridge and connect the two ends together Be careful to minimize the amount of air let into the column Connect the to column and from column lines together Press the run stop button on the pump to restart the flow Move the NOs lines to the NOs rinse bottle and the NH lines to the NH4 manifold startup solution bottle Let pump about 10 minutes Disconnect all the lines and let the system pump until all the liquid is out of the instrument about 15 minutes Press the run stop button to stop the pump and turn off the main power switch to the instrument Push the engaging levers on all the pump platens to horizontal and disconnect one end of each platen from the pump Empty the NH4 waste into the proper hazardous waste container 10 Empty the NOs waste into the proper hazardous waste container 11 Empty and discard the sample cups and tubes Rinse the sampler racks with DI water and set on the bench to dry 12 Return the NOx color reagent and NH4 salycilate nitroferricyanide bottles to the fridge 13 Refrigerate the standards if the instrument will be used the next day or freeze them if it will be longer 14 Wipe down the instrument and benches with a moist sponge 15 Turn off the ball valve on the compressed air Loch Vale Watershed Methods Manual 45 Switching the AlpKem from PO4 to NHa NOzx 1 2 Make sure the PO4 waste container is empty The waste goes in the bottl
20. cup away and wipe the bench with a wet sponge The NOs buffer contains NH which can contaminate your samples Connect the cadmium column to the instrument 1 Make sure there are no bubbles in the nitrate cartridge about 10 minutes after moving the NOs buffer line to the buffer bottle Press the run stop button on the pump press the mode button 4 times the display should read 2 0 press the run stop button again this puts the pump speed to minimum Break the connection in the line between the to column and from column ports on the NOs cartridge Break the tubing connection on the column and note which end will connect to the line from the to column port on the cartridge Elevate the other end of the tubing until a drop of liquid forms at the end Wait until a drop forms on the end of the to column line and connect it to the column without introducing any air Connect the other end of the column to the from column line on the cartridge Press the run stop button on the pump press the mode button 3 times the display should read 50 0 press the run stop button again this puts the pump speed back to normal Move the NOs color reagent line to the color reagent bottle Move the NH reagent lines to their respective reagent bottles Make sure the line from the sampler is completely clear of all other lines and the reagent bottles so the sample probe can
21. filter box lid 2 Flame forceps with Bunsen burner and douse with DI water 3 Using forceps remove rubber ring from filter holder and set it on a clean surface e g a Kimwipe or inside of filter box lid 4 Use forceps to remove paper over filter and carefully remove one filter Isopore 0 4 um from box Filters rest in box upside down Turn filter over from its position in box and Loch Vale Watershed Methods Manual 30 place directly into of filter holder If filter is not centered carefully adjust its position by pulling on edge with forceps Be careful handling filters as any contact between the filter and forceps in any area except its extreme outer edge will result in contamination or damage to the filter Do not use any filter you think may be punctured or contaminated Replace the rubber ring on top of filter and carefully secure in filter head by pushing into outer groove of filter holder with forceps Screw filter holder back into the filter head and rinse the assembly with more DI water 10 seconds is sufficient Filtering sample 1 x KI N xr Take tube out of DI water bottle walk away from bench and spin tube to remove all DI water Place tube into sample bottle and attach to stopcock Turn pump on to a forward setting of 3 to purge all DI water and allow tubing and filter to be rinsed with sample Watch bubbles from the sample as they move through the pump tubing
22. gage stilling well cover combo 16 18 24 Remove ice from stilling well when Outlet stage height is just greater than 0 1 foot This is achieved by carefully chopping with an ice axe or spud bar and by melting with approximately one gallon of boiling water heated with a backpacking stove Place float and weight in the stilling well with the cable passing over the external pulley on the Stevens Recorder The float goes on the left as you are looking towards the creek Make sure the little balls on the cable fit into the holes in the pulley Place the D battery in the blue clock Movement of the balance wheel should be visible through the inspection window Place clean chart paper on the drum in the recorder Position the drum and the pen such that the pen writes the stage height on the horizontal axis and the day time on the vertical axis Make sure you write the date time and stage height reading at the beginning of the chart as well as in the flume notebook If flow is on the rising limb of the hydrograph early season position the drum so the whole chart is available for recording This reduces the possibility that the pen will have to skip over the edges of the chart paper After flow becomes less flashy you should start the pen in the middle of the chart Loch Vale Watershed Methods Manual 88 5 Replace the recorder cover Close and lock the cover to the stilling well Weekly maintenance for Stevens gage 1 Visually r
23. in about 70 ml DI water in a 100 ml volumetric flask Dilute to 100 ml with DI water Check sampler wash waste reservoir under bench to right of instrument Empty into sink if more than half full Turn on main power switch and make sure PO heater is on Loch Vale Watershed Methods Manual 46 7 Open Winflow 4 0 software If software is already open exit and reopen This causes the sample probe to go into the wash reservoir 8 Lock down the pump platens and pull the engaging levers straight up for all the pump tubes labeled PO plus to sampler wash and from sampler wash 9 Press the run stop button on the pump the display should read 50 0 10 Connect the sampler wash line to the port labeled sampler wash on the large DI water bottle Connect the PO color reagent line to the port labeled NOs carrier on the large DI water bottle be sure to connect to the ports as listed the sampler wash will not flow properly if connected to the port labeled NOs carrier 11 Connect the POs Dowfax line to the dowfax bottle 12 Let the system pump for 15 minutes and check for leaks 13 Prepare the color reagent by adding the following stock solutions to the color reagent bottle IN ORDER and mixing after each addition 150 ml 5N sulfuric acid 15 ml antimony potassium tartrate solution 45 ml ammonium molybdate solution 90 ml ascorbic acid solution 14 If there are no leaks move the PO4 color reagent line to the co
24. maintenance and repair procedures can be found in the NOAH IV Total Precipitation Gage Technical Manual The manual is located in NREL A223 Equipment and Supplies Personal Digital Assistant PDA and downloading instructions are kept in NREL A223 be sure to fully charge the PDA prior to leaving for the field Antifreeze and funnel are kept in the storage box at the NADP site Estimated time to complete procedure It takes around five minutes to download data from each NOAH IV an additional 20 30 minutes if either catch bucket is full To prevent overflow consider a bucket full when bucket depth reaches 10 inches Preparation Charge the PDA the day before going in the field Be sure there is an adequate supply of antifreeze at the NADP should you need to empty and winterize one of the egages Make sure you have enough empty antifreeze or Nalgene containers to accommodate the volume of precipitation waste from the raingage Procedures Download data from CO98 NOAH IV Precipitation Gage a k a NTN 1 1 Stand next to the CO98 NOAH IV raingage and turn on PDA 2 Tap the Bluetooth key to open the Bluetooth Manager 3 Double tap the CO98 icon to establish the connection 4 Close the Bluetooth Manager tap on the X in the upper right corner Loch Vale Watershed Methods Manual 15 al Tap the NADP Rain key to start the NADP Rain program on Tap on the Retrieve Data from Raingage button
25. move freely 10 Let the system pump at least 30 minutes before beginning a sample run Loch Vale Watershed Methods Manual 42 Setting up a sample run Press the sample table button on the main tool bar in Winflow4 WY hh Type in cup name and type for each sample and standard to be analyzed Refer to the typical sample table on the page 7 and the notes below Cup Numbers Positions 1 20 are the large tubes at the back of the sampler and are used for standards checks and baselines washes The instrument can sample from these cups up to 6 times each There are 3 racks for the 2 ml sample cups The one on the left closest to the sampler wash cup holds cup numbers 101 190 The middle rack holds cup numbers 201 290 and the rack on the right holds number 301 390 These cups should only be sampled one time each Sample Name Sample names can be anything that fits in the field However the standards used in the calibration curve anything labeled C in the type column must be named exactly the same as they are named in the calibrant table in the method file To view the calibrant table click the edit method button on the main toolbar click file open and select the correct method file Consult the lab manager for the correct method file The calibrant table is the last page of the method file The format for naming calibration standards is X Y where X is the concentration of NH4 and Y is th
26. on the amount of particulate matter in the sample d Preparation All glassware and glass fiber filters GF F must be baked in the muffle furnace in NREL A121 before use Rinse equipment in DI water and cover all orifices with aluminum foil Place in muffle furnace for five hours at 500 C one hour to reach temperature and four hours at full temperature Temperature in the furnace must not exceed 500 C If it does the glass will deform Allow oven to cool overnight to lt 150 C before opening furnace and removing glassware otherwise it may crack from sudden cooling e Laboratory Procedures Total Phosphorus 1 Rinse one 120 borosilicate amber bottle 3X with sample and then fill to shoulder Label the bottle Total P be sure to include site name sample type and date on the label Add two drops of 37 HCl to the Total P bottle invert and shake vigorously Repeat for each sample site Store sample bottles in walk in cooler in appropriate location i e with other Total P bottles DOC DON DOP Rinsing filter tower 1 3 4 Assemble filtration apparatus by placing filter support on flask center a single filter over fritted glass on filter support using forceps center funnel on filter support and clamp support funnel together with clamp Do not connect to vacuum line yet Add 20 ml of sample to funnel Swirl to rinse sides of funnel and then connect vacuum line to port on flask Disconnect vacu
27. repeater communications M7 Dirct East amp West Radio to radio direct Maintenance division M8 Prosp East side Radio to Prospect Maintenance division long Mtn repeater distance communications F9 Dirct East amp West Radio to radio direct Fire ane PE pur adin iO Tadig direct F10 Twin East side Radio to Twin Sisters Fire and Resource long distance Fire repeater communications Ch11 Work East amp West Radio to radio direct ROMO work channel L12law E RE channel LE Rangers Only E13 Meadow Southeast Radio to Meadow Long distance communications Mtn repeater in Wild Basin area Long distance communications E14 Hagues ee EE in North Fork and Hagues Creek Northwest repeater ee Transmit only as necessary on all channels except for 11 Work Channel 11 is open to work related conversation Although you may talk freely on this channel please keep conversation brief and concise Emergency radio transmissions should go out to ROMO E1 first Protocols are described on in the Radio Protocol section If ROMO E1 cannot be reached try channel 2 and then either channel 9 or 10 Loch Vale Watershed Methods Manual 82 Appendix H Database Management 1 All LVWS databases should be updated annually Ensure that all new data have passed QA QC procedures prior to adding data to the LVWS master databases See LVWS Quality Assurance reports for QA QC methodology Denning 1988 Edwards 1991 Allstott 1995 Allstott et a
28. sampler s and travel blank e Prepaid return shipping tag e Vinyl gloves e Sample field form LVWS field book with pencil c Estimated time to complete procedure Once on site approximately 10 minutes are required to change the NHs sampler s d Preparation A set of new unexposed samplers will be shipped to you in advance of each change date Upon arrival open the outer box to verify that the sampler s and QA travel blank arrived in good condition The samplers should be sealed in two glass jars Notify CAL of any problems with the shipment and also note any issues with the shipment in the REMARKS section of the field form Once you verify the sampler s and travel blank are okay close the box and store it in the NREL freezer Sampler s and travel blanks should be stored in Loch Vale Watershed Methods Manual 18 the NREL freezer at all times to minimize NH3 contamination excluding transportation to and deployment in the field e Procedures 1 Once on site inspect the sampler s and shelter for any contamination e g bird droppings or dirt or other conditions that might affect sample integrity If necessary clean the sample shelter with DI water Retrieve the exposed sampler s put on clean vinyl gloves provided by NADP Detach the sampler s from the holder one at a time Handle the samplers by the flexible tubing only Place the sampler s with the attached flexible mounting tube into the glass jar that they were shi
29. samples must be either duplicate DUPE or blank BLANK samples Repeatability and accuracy of analysis is tested with duplicate sample results Bias is assessed by analyzing blank samples Instructions for conducting QA QC sampling are in Appendix C b Equipment and Supplies Field notebook and pencil Orion conductivity temperature meter Butyl or neoprene sampling gloves 20 ml plastic vial of Lugol s solution with 2 ml disposable pipette for monthly phytoplankton sample see recipe for Lugol s solution in Appendix E Bottle set this set is repeated for all locations unless otherwise noted 1 500 ml translucent HDPE acid washed bottle for filtered analysis 1 250 ml brown HDPE acid washed bottle for raw unfiltered sample 1 60 ml translucent HDPE acid washed bottle for SiO2 1 480 ml baked borosilicate bottle for DOC DON and DOP 1 125 or 250 ml baked borosilicate bottle collected monthly at Loch Outlet only for phytoplankton sample mi a Oe c Estimated time to complete procedure Once on site it will take 15 minutes to collect all samples Loch Vale Watershed Methods Manual 23 d Preparation All supplies needed for surface water sampling are located in the cabinet below the lab bench in NREL A223 or in the boxes underneath the lab bench Instructions for ordering new supplies are located in Appendix G Orders are frequently filled within a few days but can also take weeks so
30. suitable for long hikes warm socks plus an extra pair light to medium weight long underwear warm pants and sweater fleece works well headlamp or flashlight knife compass map emergency blanket well stocked food bag bring more than you think you ll eat water drink at least 2 liters per day and a well stocked first aid kit with the knowledge of how to use it Summertime hazards include lightning hail snowstorms and hypothermia Winter hazards include avalanches blizzards hypothermia and frostbite There is danger of serious injury broken bones cuts concussions etc in all seasons Ground squirrels in LVWS can be carriers of bubonic plague so do not approach or feed them Mountain lions have also been sighted in the area If confronted by a lion raise your hands high above your head and slowly back away Fight back if attacked Make sure all group leaders have a working two way radio All group leaders should also be certified in first aid and CPR It is best to start the day with a clear plan of action Know all your sampling points routes between them and how long you expect the work to take at each point Reevaluate the plan and your progress within the plan frequently throughout the day It is best to hike out while there is still light in the sky Plan accordingly Never go to the field alone and never go out in a group without someone in town knowing where you plan on going and when you are expected to ret
31. taps until column fractured Q quality of shear depth from the surface of the fracture depth of the isolated column Shear Quality Q1 Clean planar smooth and fast shear surface Slab typically slides easily into the snow pit can break like its spring loaded Q2 Shear surface appears smooth but slab does not slide as readily as Q1 Shear surface may have some irregularities but not as irregular as Q3 The entire slab does not slide into the snow pit Q3 Shear surface is non planar uneven irregular and rough Shear fracture typically does not occur through the whole slab weak layer interface being tested After the weak layer fractures the slab moves little or may not move at all even on slopes steeper than 35 Radio Protocol Radios are your lifeline to the outside world in the event of an emergency They also provide communication between separate groups in LVWS In either case you should use proper radio etiquette Itis very important to keep communications with ROMO dispatch brief and to the point since the rest of ROMO staff also uses these frequencies Make sure radios have charged batteries and are in good physical condition before going to the field Batteries need to be on the charger for at least four hours for a complete charge An optimum charge can only be attained if the batteries are periodically drained of all charge Do this by leaving power on overnight to the weather channel
32. to be taken to the field Two clean buckets and lids leave in plastic bags LVWS field book with pencil c Estimated time to complete procedure Once on site approximately 10 minutes are required to change the buckets and check the sensors If there are problems that require trouble shooting or repair or if the weather is bad the time spent at the NADP site can increase substantially d Preparation Buckets and lids for the Aerochem are shipped to and from the CAL in 6 packs Within each 6 pack there should be six buckets lids 1 L sample bottles and boxes for shipping sample bottles to CAL Each 6 pack should also include a supply of Field Observer Report Forms FORFs Two to three 6 packs are stored in NREL A223 When six used buckets and lids have been accumulated a used 6 pack of buckets and lids should be assembled and shipped to CAL CAL will automatically ship a clean replacement 6 pack when they receive a used 6 pack of buckets and lids When picking up mailers from the mailroom at NREL be careful not to confuse LVWS boxes with those used at other sites Loch Vale Watershed Methods Manual 11 e Procedures Carry two new buckets and lids still in their plastic bags to the LVWS NADP site each Tuesday Once on site check the foam lid seal to ensure good contact with the sample buckets There should be no gaps or openings Check the temperature of sensors by touching a finger to the sensor plate not on the rib
33. yearly for collecting permits We must also file an Investigator s Annual Report after each year of research or the privilege to work in the park will be revoked We renew our Scientific Research and Collecting Permits every 1 2 years depending on the expiration date The project title for our primary research permit is Long term Ecological Research and Monitoring in the Loch Vale Watershed Research permits are renewed through the NPS Research Permit and Report System Application and renewal instructions are found at https science nature nps gov research ac ResearchIndex Existing LVWS permits can be viewed and renewed by searching for last name Baron with the Investigator Lookup during the application process Every person must be pre approved by RMNP Natural Resources staff to collect samples of any kind in the park Each December submit the names of all those projected to be working in LVWS the following summer to Judy Visty judy_visty nps gov Make sure that fee waiver permits are requested at the same time as collection permits Fee waivers can be used for free entry at all RMNP entrance stations Keep the list to a minimum number of people Be sure to bring the LVWS Scientific Research and Collecting Permit to the field with you every week for entry to the park Loch Vale Watershed Methods Manual 26 LABORATORY PROCEDURES General Introduction The NREL laboratories are shared among a number of different projects
34. 0 minutes to process sample fill out FORF and ship the bottle d Preparation The sample bucket and lid must be weighed on the balance in NREL A231 All precipitation samples of any volume must be transferred to the 1 liter sample bottle See the NADP field procedures for further details e Procedures 1 Enter all necessary information in the Field Observer Report Form Remove the pink copy which is added to the NADP Field Forms notebook in NREL A235 2 Place used bucket back into plastic bag label as Used NTN Sampling Material and place into used 6 pack i e large boxes located in A223 Once six used buckets and lids have accumulated the used 6 pack should be shipped to CAL Loch Vale Watershed Methods Manual 64 3 Place the white and yellow copies of the FORF in the sample box with the 1 liter sample bottle Seal the box with packing tape which can be ordered from NADP by requesting additional supplies on the FORF and write you name above the return address You must also include the appropriate CSU account number on the box in the upper right hand corner Consult the Program Manager or Principal Investigator if you do not know the correct account number 4 For shipping used 6 pack back to CAL after checking that there are six used buckets and lids in the large card board box seal the box and place a NADP shipping label on the box lid Write your name and appropriate CSU account number on the shipping label
35. 30 minutes if the Belfort catch bucket is full To prevent overflow consider bucket full when the chart reads 7 inches Preparation Include a new chart with Tuesday s sample set Make sure all required supplies are present in the gage shell each Tuesday If some are missing make sure they are replaced by the following Tuesday Procedures To change charts open the sliding access door Move the pen up and down to mark the end of the week s record Move pen away from chart with the pen shift bar Remove drum and chart by lifting drum up off the clock gears Write the time date off in appropriate Loch Vale Watershed Methods Manual 84 places on chart Install new chart on drum Fold edge at end of week and slip it under the beginning portion of the chart Mark the station ID CO98 date and time on chart Return drum and new chart to clock making sure gears are properly meshed Rotate the drum so pen rests on the current day and time Refill the pen nib with ink if needed usually a small drop is sufficient The pen can usually go 2 4 weeks between refills Do not over fill the pen ONLY FILL THE PRECIPITATION PEN WHICH IS THE BOTTM PEN The top two pens are no longer used after installation of the NOAH IV electronic raingages Mark the beginning of the week s record by moving pen up and down against the chart paper f Be Aware The catch bucket in the Belfort should be emptied when chart reads 7 inches otherwise the bucket
36. 5 Loch Vale watershed methods manual 1995 Natural Resource Ecology Laboratory Colorado State University Fort Collins Colorado 124 p Richer E E and J S Baron 2011 Loch Vale Watershed Long term Ecological Research and Monitoring Program Quality Assurance Report 2003 09 U S Geological Survey Open File Report 2011 1137 22 p Thermo Electron Corporation 2003 Spectronic 20 Series Spectrophotometers User s Guide Thermo Electron Scientific Instruments Corporation Madison WI 53711 U S Environmental Protection Agency 1987 Handbook of methods for acid deposition studies Laboratory analysis for surface water chemistry U S Environmental Protection Agency Acid Deposition and Atmospheric Research Division Office of Research and Development Washington D C EPA600 4 87 026 376 p Loch Vale Watershed Methods Manual 66 APPENDICES Appendix A Sampling Locations and Trails FEA de ESS i ee LD Gi pe AS AWA Ay A Va Dk ANNAN with su Loch Vale Watershed Methods Manual d bstectt SITES AS Ki D f EZ Pi E OY 67 S SC d cael WMG Bear Lake Parking Lot f Y Ge A if f f Ji DoH Y iii 1 e y LUV INSI SC TI Y 1 d H JAAS IO He ASNO ZA Ge eee E SIN NAC a MY ag ZANNA S NX to Pingree Park lt e E Tak dy NS NOR 0 9 Louise Outlet 9 Z 2 E SS to Dunraven Trailhead NM gt R S TEES EN lt
37. A red stop sign should appear next to the first standard This will stop the analysis temporarily after the last blank sample Blank Calibration If the carbon values vary by less than 0 04 and the nitrogen values vary by less than 0 02 you may proceed with the calibration If not continue running blanks until the values stabilize After the blanks have finished running and the machine is in pause mode choose the blanks you wish to use for the blank calibration by highlighting the appropriate group of blanks left click and drag or left click and use control to select individual blanks Select Configuration from the main menu click Blank From the General Blank window Include both Nitrogen and Loch Vale Watershed Methods Manual 59 Carbon if necessary using the Include Exclude button Click Ok After the blank calibration restart the analyses by clicking the Analyze button or F5 Standard Calibration Select the appropriate standards you want to use in calibration Select Configuration from the main menu click Drift from the next menu click Drift again Include both Nitrogen and Carbon if necessary using the Include Exclude button Click OK 8 Running Samples Run one blank and one standard immediately after calibration to ensure the values are correct If the values are out of range run a few more blanks and or standards checking to see if they stabilize in the correct range Contact the Lab Manager if values are still q
38. ANSMITTANCE by pressing the MODE key until the appropriate LED is lit Adjust the display to 0 Transmittance using the knob on the front left side of the instrument Make sure that the sample compartment is empty and the cover is closed Loch Vale Watershed Methods Manual 36 6 7 8 9 Set the display mode to ABSORBANCE by pressing the MODE key until the appropriate LED is lit Fill a clean cuvette with DI and wipe the cuvette with a Kimwipe to remove liquid droplets dust and fingerprints Place the DI filled cuvette in the sample compartment and align the guide mark on the cell with the guide mark at the front of the sample compartment Press the cell firmly into the sample compartment and close the lid Adjust the display to 0 0 Absorbance 0 0 Absorbance 100 Transmittance with the Transmittance Absorbance Control knob on the right side of the instrument 10 Remove the cuvette from the sample compartment Matching cuvettes 4 Allow samples and standards to reach room temperature Fill each cuvette with 10 ml of DI water Wipe each cuvette with a Kimwipe as any scratches or marks will skew results After wiping a cuvette insert it into the sample compartment and note the absorbance in the lab notebook All matching cuvettes should have absorbance values lt 0 002 Set cuvettes that do not match aside Keep all that do match d Procedures Standard curves 1 2 3 Begin by running a s
39. CR500 is in operating order do test runs in office Also ensure the Stevens gage is in good shape with no visible corrosion WD 40 and graphite dust work well to care for and prevent corrosion The area around the flume throat and stilling well must be dug out of the snowdrift This is usually accomplished over several weeks beginning in early April There should be no obstructions De snow in the flume e Procedures Initial Set up for CR500 1 The CR500 should be set up in mid to late April Open the CR500 stilling well lid it s the big PVC tube Remove ice from the stilling well by gently chopping with an ice axe or spud bar and by melting with water heated with a backpacking stove when the outlet stage height is just greater than 0 1 foot Be VERY careful not to crack or move the PVC barrel The link from it to the flume is a point of instability Fasten the EnviroSystems shaft encoder to platform inside stilling well Place float and weight in the stilling well with the metal pulley tape passing over the external pulley of the shaft encoder The float goes on the left and weight on right as you look towards the creek Make sure the spikes on pulley mate with holes in pulley tape Attach screw cap connection to shaft encoder Connect wires to right hand white panel on CR500 red 12V white C2 P3 black G and clear G Boot computer and start PC208 Connect battery pack to CR500 Attach CR500 to the computer using serial cab
40. Cl 2 NOT filtered but TOTAL P Total P NREL transferred into pre refrigerator baked 120 ml amber borosilicate bottle AND acidified with 2 drops of 37 HCl Table 2 Summary of laboratory procedures for processing LVWS monthly surface water samples Bottle Set for Treatment Label Analysis Destination Surface Water 500 ml HDPE acid Filtered with peristaltic ARCHIVE F U As needed NREL washed bottle pump into 250 ml freezer brown HDPE acid FORT washed bottle freezer Pre baked 250 ml Stained with 1 2 ml of PHYTO Species richness NREL amber borosilicate Lugol s solution in the and abundance refrigerator bottle field then algal taxonomist Loch Vale Watershed Methods Manual 28 Filtration for Major Ions a Introduction Solutes present in surface waters are primarily derived from precipitation inputs and geochemical weathering Because samples must be delivered to laboratories for chemical analysis it is important that the original chemical composition remains unchanged before and during transport Particulates in a sample can affect chemical results as well as clog lines of sensitive instrumentation Biological activity in the sample can alter chemical composition Therefore we filter to remove particulate materials spores and bacteria from sample water to minimize their effect on chemical analysis Samples that have been filtered with the peristaltic pump are lab
41. It is important to follow general laboratory practices of safety and cleanliness All lab users must complete the lab safety training with a lab manager If you have any questions or concerns do not hesitate to ask the lab manager Make sure all LVWS personnel including volunteers are properly trained for the tasks they are asked to perform The following procedures are used both in preparation for field collection and for the processing of samples after returning from the field Refrigerate all water samples upon return from field in walk in cooler not the freezer All samples should be processed by noon the day following collection Surface water samples were previously analyzed for pH and specific conductivity at NREL Currently specific conductivity is measured in the field at each sampling location for all stream and lake water samples Specific conductivity and pH measurements in the NREL laboratory were discontinued in 2010 due to redundancy with conductivity and pH measurements that are obtained during water chemistry analyses at the Rocky Mountain Research Station RMRS and NADP Central Analytical laboratories Samples are still filtered preserved as directed and refrigerated at NREL before delivery to the appropriate analytical laboratory A note on cleanliness Since LVWS waters are extremely dilute you must assume any surface you touch is sufficiently contaminated to affect the outcome of analysis Therefore be very careful
42. Loch Vale Watershed Long term Research and Monitoring Program Methods Manual 2011 Eric Richer Jorin Botte and Jill Baron Natural Resource Ecology Laboratory Colorado State University Fort Collins Colorado USA NATIONAL PARK MZ USGS University science for a changing world MA Forward This manual is intended to serve as a guide for technicians students and other participants in the Loch Vale Watershed LVWS long term ecological research and monitoring program in Rocky Mountain National Park and others like it Procedures are described for sample collection analyses quality assurance and database management This is a living document so we welcome suggestions and questions This document was most recently revised on July 28 2011 Please forward comments to Jill Baron 970 491 1968 or Eric Richer 970 491 2153 Introduction The National Park Service NPS initiated the LVWS monitoring program in 1983 with funding from the Aquatic Effects Research Program of the National Acid Precipitation Assessment Program Initial research objectives were to understand natural variability and the processes that mitigate or accelerate the effects of atmospherically deposited pollution on soil and surface water chemistry and to build a record in which long term trends could be identified The project is currently a cooperative effort between the NPS U S Geological Survey USGS and Colorado State University CSU
43. O98 and CO89 do not get confused Record any other relevant information i e contamination malfunction etc in the field notebook Load sample buckets into the bottom or onto the outside of your pack It is best to have two people carry one bucket each f Be Aware The Aerochem collectors can malfunction in many ways but the most consistent problem is power loss during prolonged snow storms Each Loch Vale NADP site is independently powered by solar panels Be sure to remove snow from the solar panels and trample down snow that accumulates in front of the solar panels Wiring for the solar power system is detailed in Figure 2 The solar power systems are designed for three days of autonomy Power to the collectors and raingages will automatically disconnect when battery banks drop below 40 50 capacity In the summer the solar panels batteries and wiring must be checked and repaired if needed Also check connections to the Aerochem motor box and tighten any loose screws and nuts especially those related to the movement of the roof and lid seal Loch Vale Watershed Methods Manual 12 Wiring Diagram for Loch Vale NADP Site Equipment 12 volt system Two 60 watt solar panels Sola r wired in parallel to create a 120 watt solar Pa ne panel array a va Batteries SAR Three 100 AH batteries wired in parallel for a 300 AH battery bank Charge Controller 20 amp SunSaver D Batter y NOAH IV Precipitation
44. Surface water samples are analyzed for chemical concentrations Five sites are currently sampled within the LVWS as well as five others within Rocky Mountain National Park RMNP Sampling locations are shown in Appendix A Sampling frequency ranges from weekly at the Loch Outlet to annually for Emerald Haiyaha Louise and Husted lakes A detailed sampling schedule is listed in Appendix B As stream and lake waters in the Loch Vale Watershed Methods Manual 3 LVWS are chemically dilute sampling protocols need to be followed carefully to avoid contamination Weather conditions were measured at a Remote Area Weather Station RAWS near the Loch Vale NADP site from 1983 to 1998 The RAWS was shut down on November 24 1998 Details of the decommissioning process can be found in the LVWS Quality Assurance Report for 1995 1998 Allstott et al 1999 The Main Loch Vale Weather station was established in 1991 approximately 30 meters from the location of the RAWS and is operated and maintained by the USGS WRD Field Safety LVWS is a remote basin that can be demanding of advanced fitness and survival skills Never consider a trip to LVWS to be a simple day hike Field days can be very long and stormy even in the summer Be prepared with appropriate gear to keep warm and dry during inclement weather Gear should include but are not limited to a good waterproof and windproof shell warm hat two pairs of warm gloves comfortable waterproof boots
45. Technical Manual for detailed maintenance procedures Service Mode should be enabled prior to and during all maintenance procedures Contact the NADP Site Liaison Matt Layden phone 217 244 0372 email ntn sws uiuc edu immediately if there are any problems with the egages Loch Vale Watershed Methods Manual 17 Ambient Ammonia Sampling a Introduction LVWS CO 98 is part of the NADP Ammonia Monitoring Network AMoN Passive Diffuse Ammonia NH3 Samplers are exposed for a 14 day sampling period Exposed samples are removed and new samples installed on Tuesday mornings in accordance with the AMON sampling schedule NH3 monitoring entails the use of two samples 1 a travel blank and 2 sampler for field deployment In most cases a single sampler is deployed Periodically triplicate samplers will be deployed as part of network quality assurance The procedure for deploying the samplers is the same regardless of whether there is a single sampler or triplicate samplers Additional information and detailed procedures are provided at the NADP AMON website You must be familiar with AMON procedures before handling a NH sampler The following instructions provide a brief synopsis of appropriate methods b Equipment and supplies to be taken to the field To be retrieved NHs sampler box containing e travel blank e Prepaid return shipping tag e Vinyl gloves e Sample field form To be deployed NH sampler box containing e NH
46. U FU DOC DOP DON Husted Surface 1 year fall RU FU DOC DOP DON Loch Outlet 1 week year round RU FU DOC DOP DON Phyto Archive Loch Inlet 1 month summer RU FU DOC DOP DON Louise Inlet 1 year fall RU FU DOC DOP DON Louise Outlet 1 year fall RU FU DOC DOP DON Sky Outlet 1 month summer RU FU DOC DOP DON Sky Inlet South 1 month summer RU FU DOC DOP DON Phytoplankton samples are collected once a month at the Loch Outlet Archive samples are collected once a month from the Loch Outlet Archive samples are filtered with the peristaltic pump into brown 250 ml HDPE bottles and stored in the NREL freezer The frozen archive samples are transferred from the NREL freezer to the LVWS chest freezer at the USGS Fort Collins Science Center FORT laboratory once a year Synoptic sampling occurs once a month during the summer starting in June and ending in September Synoptic sampling entails collecting surface water sample at Sky Inlet South Sky Outlet Andrews Creek and Loch Inlet in addition to the regular weekly sampling at the Loch Outlet A sampling schedule should be prepared by the Program Manager prior to the beginning of a new calendar year Ten percent of the total number of samples collected must be quality assurance samples i e DI field Blanks or field Duplicate samples Around 80 samples Normal Blanks and Duplicates are collected yearly To obtain 10 quality assurance a Blank or Duplicat
47. a number of pre cut acid washed pieces of Antlia silicone replacement tubing ready Disassemble the pump tubing head to replace the old piece of tubing with a new piece of tubing Wrap the outlet side of silicone tubing with strapping tape to prevent ballooning under filtration pressure Pump assembly is easier if the pump rotor is rotating slowly do this by hand with screwdriver while the tubing is held in place and the plastic pump head halves are gradually pushed together New tubing for pump is located in drawers under lab bench Any other pump related supplies can be bought from VWR Loch Vale Watershed Methods Manual 32 Filtration for DOC DON and DOP a Introduction Dissolved organic carbon DOC is created in natural systems by leaching of soil organic matter or from decomposition of algal biomass DOC is operationally defined as organic carbon that passes through a 0 45 um filter Therefore we filter water samples prior to analyzing DOC Proper washing baking is essential to remove all surface contaminants most importantly carbon Proper washing and baking will also prolong the useful life of the filtration apparatus Methods for analyzing DOC are detailed in the Schimadzu section of the LVWS Methods Manual Dissolved organic nitrogen DON is determined by calculating the difference between Total Dissolved Nitrogen TDN and Total Inorganic Nitrogen TIN TIN is calculated by converting nitrate NOs to nitrate expressed as
48. ale Watershed Methods Manual 35 Measuring Silica a Introduction Read Silica High Range Method adapted by Hach from Clesceri et al 1998 If necessary make new standards and keep in refrigerator Use Hach s 10 mg L SiO standard to make standards range of 0 0 0 1 0 5 1 0 2 0 5 0 mg L using formula C1V1 C2V2 where C1 is the initial concentration V1is the initial volume C2is the desired concentration and V2is the desired volume Refer to the Spectronic 20 Series Spectrophotometer User s Guide Thermo 2003 for trouble shooting and additional operating procedures b Equipment and Supplies found in walk in refrigerator and NREL A256 Thermo Spectronic 20D spectrophotometer in NREL A256 Vortex Genie 2 stirrer in NREL A258 Timer or clock Wide mouth flat bottom optically matched cuvettes 10 ml automatic pipette and clean pipette tips Hach High Range Silica Test Kit 10 mg L SiO solution for standards Acid Reagent Powder Pillows Molybdate Reagent Powder Pillows Citrate Acid Pillows Samples for analysis c Preparation Zero the absorbance 1 x x xw get x Turn on the spectrophotometer turning the Power Switch knob on the left side of the instrument clockwise Allow the spectrophotometer to warm up for at least 15 minutes After the warm up period set the analysis wavelength to 420 nm by rotating the Wavelength Control Knob Set the filter lever to 340 599 nm Set the display mode to TR
49. alimnion Bi monthly winter RU FU DOC DOP DON Phyto Loch Surface Bi monthly winter RU FU DOC DOP DON Phyto Louise Hypolimnion Variable summer RU FU DOC Louise Metalimnion Variable summer RU FU DOC Louise Surface Variable summer RU FU DOC Sky Inlet North 1 month summer RU FU DOC DOP DON Sky Hypolimnion Bi monthly winter RU FU DOC DOP DON Phyto Sky Metalimnion Bi monthly winter RU FU DOC DOP DON Phyto Sky Surface Bi monthly winter RU FU DOC DOP DON Phyto Loch Vale Watershed Methods Manual 73 Appendix C Quality Assurance Quality Control Samples Blank samples are taken in the following manner 1 When taking a blank sample a normal Loch Outlet sample is taken at the same time Prepare two normal bottle sets for the Loch Outlet in the lab 2 On the day of sampling fill a 1 liter acid washed rinsed plastic bottle with conductivity tested DI water from the lab Conductivity of this water must be lt 2 uS cm Notify lab manager if it is not and postpone the blank sample 3 After taking normal Loch Outlet sample rinse and fill each bottle in the blank sample set from the 1 liter DI water bottle using the same methods as described in the Surface Water Sampling section of the LVWS Methods Manual only pouring DI into sample bottles instead of dipping into stream 4 Process the sample just as you would a normal sample Label the blank s
50. amples bottles with sample type BLANK instead of NORM Duplicate samples are taken in the following manner 1 A duplicate sample is simply that a duplicate of a normal sample from the Loch Outlet Take two identical sets of samples according to the methods detailed in the Surface Water Sampling section of the LVWS Methods Manual Label one bottle set NORM and the other DUPE 5 Process the sample just as you would a normal sample Label the bottles with sample type DUPE instead of NORM Loch Vale Watershed Methods Manual 74 Appendix D Lake Bathymetry N A Z THE LOCH E SC wt Ss o 25 0 eo PO 100 METERS a 150 200 300 FEET EXPLANATION ci JU LIME OF COUAL WATER DEPTA interval craters is venabis o 5 METERS a S gt o 53 109 150 FEET EXPLANATION 0 LME DF EQUAL WATER DEPTH ircerval n metere is sanable Loch Vale Watershed Methods Manual 75 Appendix E Recipes Lugol s Fixative Solution Dissolve 10 g Iz pure iodine caution toxic and 20 g KI in 200 ml distilled water and 20 ml concentrated glacial acetic acid Store in amber borosilicate bottle Transport to field in 20 ml plastic vial Acid Baths To make new acid baths add one part concentrated HCl to nine parts water under a fume hood Make sure you use safe procedures for working with strong acids add acid to water NOT water to acid NADP Quality Control Check Sample QC pH 4 9 0 15
51. ansport e Procedures 1 Place one or two blue ice packets in the cooler 2 Make sure all sample bottles are sealed tightly 3 Pack samples into cooler 4 Deliver samples to the USFS RMRS laboratory and place them in the Sample Drop Off location in the walk in cooler Loch Vale Watershed Methods Manual 63 Precipitation Samples a Introduction A 1 liter sample bottle is sent to the Central Analytical Laboratory CAL of the National Atmospheric Deposition Program NADP for chemical analysis of the precipitation sample Following is a brief synopsis of procedures Detailed instructions are given in the NADP NTN Site Operation Manual Dosset and Bowersox 1999 The person responsible for shipping the precipitation sample should be certified as an NADP site operator Precipitation samples are weighed in the bucket Subtract lid and bucket weight written on each bucket and lid from the total weight of lid bucket and sample to find the sample volume Decant the sample from the bucket into a clean NADP 1 liter HDPE Nalgene bottle and send to the NADP Central Analytical Laboratory CAL in Champaign Illinois for complete chemical analysis b Equipment and Supplies NREL A223 and NREL A235 1 liter bottle for precipitation sample Precipitation sample in white plastic bucket with snap on lid Card board box for 1 liter sample bottle Field Observer Report Form FORF c Estimated time to complete the procedure Allow 3
52. be sure you are collecting filtered sample and not DI rinse water Samples that have been refrigerated overnight will be colder than the DI rise water When you feel colder water coming through the filter you know that sample water is passing through the pump Filtering pressure must be less than 15 Ibs in so that the filter does not rupture This corresponds to a setting of 3 on pump motor control Rinse bottles three times with filtrate before filling a few ml per rinse is sufficient If sample contains enough matter to clog the filter before the F U bottle is filled it may be necessary to stop change the filter and resume filtering Remember to rinse the new filter with sample before beginning to fill bottle again Be sure to collect an Archive sample from the Loch Outlet once a month Change filters between samples Follow filter rinsing procedure as previously directed Also rinse and spin inked tube with DI water between samples After all samples have been filtered give the unit a final rinse with DI water at least 1 liter to purge all sample water Be sure there is no water left in the filter tubing Rinse inked tube with DI water and place back into box in clean drawer Store the 60 ml F U sample bottles in the walk in cooler before delivery to analytical laboratory Store the monthly Archive sample from the Loch Outlet in the NREL freezer Loch Vale Watershed Methods Manual 31 a Be Aware It is a good idea to have
53. calibrated prior to taking it into the field The conductivity meter should be checked against standard solutions weekly and calibrated as necessary The meter must also be calibrated every time the battery is replaced Calibration procedures are detailed in the Thermo Orion Instruction Manual in the LVWS lab drawer The nominal cell constant for the conductivity probe is 0 475 cmt Check the amount and date of the standard and QC solutions prior to calibration Recipes for the NADP QC solution pH 4 9 0 15 conductivity 14 2uS Loch Vale Watershed Methods Manual 21 cm1 and SCS pH 4 9 0 15 conductivity 14 2uS cm1 can be found in Appendix E Standard conductivity solutions can also be ordered from NADP and VWR e Procedures To check the meter for accuracy 1 Turn meter on 2 Rinse conductivity cell and all vials to be used with DI water under faucet Fill a vial with 10 ml of DI dip probe and record value in lab notebook 3 Rinse conductivity cell and all vials to be used with DI water under faucet Shake vials dry and rinse first one 3X with 14 2 uS cm QC conductivity solution Fill a vial with 10 ml QC conductivity solution dip probe and record value in lab notebook 4 Rinse another vial 3X with 75 1 uS cm SCS conductivity solution Fill a vial with 10 ml SCS conductivity solution dip probe and record value in lab notebook 5 If the conductivity values are outside of the acceptable range calibrate the m
54. conductivity 14 2 uS cm1 To make this quality control check sample get 0 5 liters of DI water stirring in a 1 liter volumetric flask on a stir plate Slowly add 4 00 g NaCl and 0 78 ml HNOs Bring volume up to 1 liter Dilute 1 ml of this solution to 1 liter Freeze remainder of original liter for later use This standard does not need to be refrigerated but it should be stored in a dark cupboard and shaken before use NADP Specific Conductance Standard SCS pH 5 62 0 20 conductivity 74 1 uS cm1 To make this conductivity standard first dry 100 e of KCl crystals at 105 C for gt 5 hours Then dissolve 93 2 g of the dried KCl in a 1 L volumetric flask to create a 1 25 M KCl stock solution Dilute 0 40 ml of this stock solution to 1 L to make the 5 0 x 104 M KCL SCS Alpkem Reagents Prepare all recipes in their written order When filtering is necessary use 8 0 um membrane filters located in NREL A256 For NH Channel Manifold Startup Solution Add 0 5 ml BRIJ or other surfactant to 1L DI NH Buffer 12 g NaOH 29 g Na Citrate 50 g disodium EDTA Bring up to 1000 ml with DI water Filter through 8 0 um polycarbonate membrane Add 6 drops Dowfax to actual dispensing container Salicylate 0 6 g Na Nitroferricyanide 300 g Na Salicylate Bring up to 1000 ml with DI water Loch Vale Watershed Methods Manual 76 Filter through 8 0 um polycarbonate membrane Store in refrigerator in dark glass bottle Hypochlorite 24
55. d Contents 18 Ethylene Glycol 2 Transmission Fluid 80 Water Include start and stop dates on the label for each jug These jugs are found in NESB A101A ask the Laboratory Manager for keys to A101A Dispose of waste through the CSU Hazardous Waste Office x1 6745 Replace D cell batteries in the clock at least twice a year mandatory each November and March Loch Vale Watershed Methods Manual 85 Measurement of Hydrologic Discharge Transferred to USGS WRD in 2006 a Introduction Operation of the Loch Outlet stream gage was transferred to the USGS WRD in August 2006 LVWS personnel are no longer responsible for measurement of hydrologic discharge within the LVWS Icy Brook carries most surface water out of LVWS A Parshall Flume with a four foot throat was installed in Icy Brook approximately 100 meters downstream from the Loch during the fall of 1983 The flume is rated so that a given water level in the flume can be directly related to a discharge volume rate A Campbell Scientific CR500 stream recorder recorded stage height in a stilling well and a Leupold and Stevens chart recorder served as a backup for the Campbell Water level data from both gages were converted to instantaneous flow and cumulative flow m s When the USGS WRD assumed responsibility for operation of the flume at the Loch Outlet a depth transducer was installed to measure water levels and a stage discharge was developed for the flume The stilling we
56. d turn off the TTT85 Be sure to hit the reset button on the circuit breaker to restore power 3 Rinse the stir bar with DI water and blot dry on a Kimwipe Add the stir bar to the scintillation vial containing the pH 7 00 buffer Set the stir plate to the lowest setting and place the vial on the stir plate Insert the pH probe into the vial so that the red eye is completely submerged 4 Press the pH key on the TTTS85 5 Press the CAL key 1 CAL TEMP XX X C appears on the display 6 Press the CAL key again pH X XXX BUF1 Y YYY appears on the display If necessary change the pH value of buffer 1 Y YYY i e SHIFT 7 0 0 0 and STORE 7 Wait for a stable measurement As we record pH to two decimal places e g 4 52 a measurement is considered stable when the hundredths place does not fluctuate This could take some time gt 15 minutes Don t worry if the meter says that the pH is not 7 00 The calibration procedure will reset the meter Once a stable measurement is obtained press the CAL key ZERO pH X XXX CAL1 appears on the display for a short period then Z CAL TEMP X XX C will be displayed 8 Rinse the pH probe and stir bar with DI water Blot dry with Kimwipe 9 Place the stir bar in the pH 4 00 buffer vial Put the vial on the stir plate and insert the pH probe into the buffer solution 10 Press the CAL key again pH X XXX BUF2 Y YYY appears on the display If necessary change the pH value of bu
57. e concentration of NOs No leading zeros on values less than 1 and no decimal points except for fractional concentrations Type SYNC This is always the first cup in a run it is a high standard usually top standard which will yield a large peak to let the software know the sample peaks have started C indicates a calibration standard to be included in the calibration curve Do not use this for internal standards or checks unless you want them included in the calibration curve RB indicates a baseline wash The instrument will use these peaks to correct for baseline drift so they should always be a 0 ppm standard U unknown Should be used for all samples checks and internal standards Loch Vale Watershed Methods Manual 43 After the calibration curve the basic pattern should be 10 samples 1 standard 10 samples and 1 baseline Repeat to a maximum of about 80 samples Larger sets should be broken into multiple runs Sample runs should always end with a baseline Other columns in the sample table R Number of replicate samples to be taken from the cup Should be set to 1 Dil dilution factor of the sample usually 1 Wt weight of the sample usually 1 After the sample table is prepared be sure to save it Starting a sample run 1 Click the collect data button on the main toolbar The software will ask for an operator name and ID type in your initials for both The software will then ask for a sample table
58. e on the bottom shelf of the acid cabinet in room A258 Disconnect the PO waste from spec line from the outflow tube of the channel 3 PO4 NHa detector and connect the NH waste from spec line in its place Disconnect the PO to spec line from the bottom connection on the debubbler on the channel 3 detector and replace it with the NH to spec line Disconnect the POs from debubbler line from the top connection on the debubbler and replace it with the NH from debubbler line Turn the PO4 heater off and the MNHA heater on Disconnect the sampler line from pump tube labeled PO sample and connect it to the T where the NH sample line and the NO3 sample pull thru line meet Orthophosphate Total Phosphorus Directions Orthophosphate 1 2 5 6 All glassware and bottles used should be acid washed before beginning Check that the instrument is configured to run PO4 The line from the sampler should be connected to the pump tube labeled POs sample and lines labeled PO to spec and PO from debubbler should be connected to the channel 3 debubbler If not see the section Switching the AlpKem from NH4 t NOs to PO Empty the large DI water bottle and fill with 1 2 M HCI from the acid bath Let it sit for at least 15 minutes Carefully pour the acid back into the acid bath rinse 6 times with DI and fill with DI Dissolve 1 8 grams ascorbic acid
59. e sample should be collected from the Loch Outlet every 6 7 weeks QA sampling at the Loch Outlet should alternate between field Blanks and field Duplicates Details of taking processing these samples are found in Appendix C Loch Vale Watershed Methods Manual 72 Table B2 Historical LVWS sampling sites that are no longer actively sampled Name Sampling Frequency Analyses Andrews Tarn 1 year summer RU FU DOC Andrews Tarn Inlet 1 year summer RU FU DOC Emerald Inlet Variable summer RU FU DOC Emerald Hypolimnion Variable summer RU FU DOC Emerald Metalimnion Variable summer RU FU DOC Emerald Surface Variable summer RU FU DOC Glass Inlet Variable summer RU FU DOC Glass Hypolimnion Variable summer RU FU DOC Glass Metalimnion Variable summer RU FU DOC Glass Surface Variable summer RU FU DOC Glass Outlet 1 month summer RU FU DOC DOP DON Haiyaha Hypolimnion Variable summer RU FU DOC Haiyaha Metalimnion Variable summer RU FU DOC Haiyaha Surface Variable summer RU FU DOC Husted Inlet Variable summer RU FU DOC Husted Hypolimnion Variable summer RU FU DOC Husted Metalimnion Variable summer RU FU DOC Husted Lake Surface Variable summer RU FU DOC Husted Outlet Variable summer RU FU DOC Little Loch Creek 1 month summer RU FU DOC DOP DON Loch Hypolimnion Bi monthly winter RU FU DOC DOP DON Phyto Loch Met
60. ead the water level along the staff gage ft in the flume averaging the high and low water surges Record the value and any adjustments or repairs made to the recorder or flume in the flume notebook Remove the Stevens recorder cover Tilt pen back and remove chart drum Replace the chart paper on the drum and reposition the drum in the recorder Slide pen carriage back so that the pen will begin recording at the correct time Each line is equal to two hours Position the cylinder so the pen will be unlikely to be hung up passing over chart ends and lock in place Write the date time and stage height on the end of the old chart and the beginning of the new chart Record the date time and stage height in the flume notebook Annual Shut Down for Stevens gage 1 2 3 Temperatures will become increasingly colder later in October After a point water in the stilling well will freeze A drop in stage height below 0 1 feet usually accompanies this In either case it is time to shut down the gage for the year First perform the weekly maintenance as above except do not replace the chart paper Remove the battery from the clock Bring all supplies back to the lab except for the gage float weight and cable Remove the float cable and weight from the stilling well and place next to the recorder Close and lock the stilling well cover f Be Aware The opening and throat of the flume must be clear for the stage height discharge
61. electrical current and is the reciprocal of its electrical resistance It is an indicator of the ionic strength of a solution As with all other analyses we perform conductivity measurements are susceptible to contamination Conductivity of tap water can be 50 times greater than that of surface waters in LVWS Make sure that everything that may contact sample waters has been thoroughly rinsed with DI before attempting any measurement The conductivity and temperature of all stream and lake samples are measured in the field prior to sample collection Previously precipitation samples were analyzed for conductivity at NREL NADP no longer requires that conductivity be measured prior to shipment of precipitation samples Therefore laboratory conductivity measurements for precipitation samples are no longer collected as of 2010 b Equipment and Supplies found in NREL A235 Field notebook Orion Conductivity meter Model 105A Deionized DI water VWR Traceable Conductivity Standard 10 uS cm Catalog 23226 567 VWR Traceable Conductivity Standard 100 uS cm Catalog 23226 589 75 1uScm Specific Conductance Standard SCS solution from NADP 14 2uScm Quality Control QC check solution from NADP Kimwipes c Estimated time to complete procedures Allow 5 minutes for measurement of conductivity and temperature in the field d Preparation Be sure the conductivity meter has sufficient battery power and is
62. eled F U Filtered Untreated and are used to determine the concentration of major ions An ARCHIVE sample is collected from the Loch Outlet once a month This sample is filtered with the peristaltic pump into a brown 250 ml HDPE bottles labeled as ARCHIVE F U and stored in the NREL freezer Archive samples are transferred from the NREL freezer to the LVWS chest freezer in the USGS Fort Collins Science Center FORT laboratory once a year Equipment and Supplies Equipment and supplies are located in the NREL A235 Bottle s with sample Peristaltic pump with Antlia filter holders Millipore Isopore 0 4 um membrane filters Catalog HTTP04700 Clean forceps Deionized DI water Waste beaker Clean 60 ml HDPE bottle labeled with site name date sample type amp F U Clean 250 ml brown HDPE bottle labeled with site name date sample type amp ARCHIVE F U collected once a month from the Loch Outlet Estimated time to complete procedure Allow approximately 15 minutes per sample although filtering times may vary greatly depending on the amount of particulate matter in the sample Preparation All pump apparatus should be acid washed once a month This can be done on the lab bench To clean fill a one liter bottle with 10 HCl from acid bath run acid through pump Loch Vale Watershed Methods Manual 29 as you would a regular sample only without the filter membrane allow acid to s
63. er and another line labeled NH to spec If not see the section Switching the AlpKem from PO4 to NH4 NOs Remove NOs color reagent and NH4 salicylate nitroferricyanide bottles from the fridge Place the NOs color reagent in a warm water bath to warm up to room temperature Check that the sampler wash waste is flowing into the sink Turn on compressed air at round black knob on bottom of regulator Turn on main power switch and make sure NH4 heater is on Let the sampler initialize Open Winflow 4 0 software If software is already open exit and reopen This causes the sample probe to go into the wash reservoir Empty and refill the large DI water bottle Loch Vale Watershed Methods Manual 40 8 Lock down the pump platens and pull the engaging levers straight up for all the pump tubes labeled NH and NO plus to sampler wash from sampler wash and sample pull through 9 Press the run stop button on the pump the display should read 50 0 10 Connect the sampler wash and NOs carrier lines to the large DI wash bottle be sure to connect to the ports as labeled the sampler wash will not flow properly if connected to the port labeled NOs carrier 11 Connect the NH lines buffer hypochlorite and salycilate to the NH4 manifold startup solution 12 Connect the NOs lines color reagent and buffer to the NOs rinse bottle 13 Let pump for 10 minutes and check for leaks 14 Discard old h
64. es foil for analyzer cups blanks and standards i e Mixed Meadow Grass plant or Sidhigh soil c Preparation 1 Separate plant or soil samples by site and date 2 Grind oven dried samples to a fine powder using the ball mill grinder for soil or Wiley mill for plants in downstairs lab 3 Place each ground sample in a well labeled scintillation vial and store according to date site and treatment e Procedures 1 Check gases Compressed Air should read 40 psi Helium and Oxygen should read 35 psi on the left gage Consult a Lab Manager if the pressure on the Oxygen or Helium tanks is less than 300 400 psi regulator closest to the tank 2 Check furnace temperature the temperature should be close to 950 C 3 Check to see if crucible is in the furnace same procedure used to change crucible Carefully lift off sampler carousel and gently set aside Loosen the 3 main screws on the loading head very carefully remove the loading head and set it on its side on top of the machine Loch Vale Watershed Methods Manual 57 Screw the lance extractor tool into the lance tube carefully remove the tube and place in the tray next to the machine THE LACE TUBE IS EXTREMELY HOT Replace crucible with tongs if necessary don t forget to reset the counter if you replace the crucible Replace the lance tube use a Kimwipe to clean any grit from the O ring Replace the loading head by very carefully lining up the connectin
65. eter and repeat steps 3 4 until both readings are accurate 6 Turn meter off rinse probe with DI and discard vials 7 Put meter away in drawer To measure conductivity and temperature of surface waters in the field 1 At each site conductivity and temperature are measured prior to collecting water samples 2 Turn on the meter and submerge the probe in the stream lake Agitate the probe until Ready is displayed 3 Record the time conductivity and temperature in the field book 4 Turn the meter off Loch Vale Watershed Methods Manual 22 Surface Water Sampling a Introduction Surface water samples are collected from flowing streams lake inlets and lake outlets throughout the year see sampling schedule in Appendix B Stream samples are analyzed for pH specific conductance i e conductivity major ions silica DOC DON DOP and phytoplankton Samples from the Loch Outlet are used in conjunction with precipitation chemistry to calculate chemical budgets and for long term trend analysis Samples taken elsewhere in the watershed are useful for analyzing processes and trends Stream and lake waters in LVWS are chemically dilute Therefore it is crucial that sampling protocols are carefully followed to avoid contamination Three types of samples are collected from the Loch Outlet normal duplicates and blanks Quality control samples must be collected on a regular schedule Appendix B Ten percent of all LVWS
66. ffer 2 Y YYY i e SHIFT 4 0 0 0 and STORE 11 Wait for a stable measurement X XXX and then press the CAL key SENS XX X amp CAL2 appears on the display briefly after 3 CAL TEMP XX X C is displayed The sensitivity should be between 97 5 and 102 5 If not re calibrate starting with the pH 7 00 buffer 12 Press the pH key to return to a measuring state Be sure to rinse the probe and stir bar between samples Loch Vale Watershed Methods Manual 93 Check solution and sample measurement Rinse a vial with DI then rinse the vial with QC check solution before filling with QC check solution Be sure to rinse the probe and stir bar with DI and then blot dry Immerse the pH probe in the QC check solution and wait for stable measurement If stable pH is 4 90 0 15 record it If pH is outside of this range rinse probe with DI water and check QC check solution expiration If the QC check solution is good repeat calibration Measured pH of check solution must be 4 90 0 15 before any samples are measured If you cannot get a good reading on check solution the QC check solution likely needs to be replaced Cleaning and troubleshooting procedures are described in NADP Site Operation Manual If a probe is not able to read the check solution properly consult the Lab Manager Remove probe and stir bar from check solution vial and thoroughly rinse with DI water Blot excess water from probe tip and stir bar with Kimwipe Rinse
67. formed Click No if maintenance was not performed Return to the Counter window to ensure the proper item was reset 6 Leak Checks Before running any samples it s in your best interest to check for leaks Select Diagnostics from the main menu then click Leak Check Select Whole O2 click Start wait until Passed or Failed appears in the Results column If Passed appears be sure the value is less than 2 0 mbars Select Whole He click Start wait until Passed or Failed appears in the Results column If Passed appears be sure the value is less than 2 0 mbars Contact a Lab Manager if either of the leak checks fails Loch Vale Watershed Methods Manual 58 7 Calibration Initial Blanks First make sure the next available i e empty cell on the spreadsheet has been selected Select Samples from the main menu then click Login From the Sample window use the drop down arrow next to Sample Name to select Blank The Mass must be 1 0000 which is the default select 4 repetitions Using the drop down arrow at the end of the Method line select the appropriate Method Material Method Standard Weight Carbon Nitrogen Check Range g Range Range PLANT 10ML 0 1000 Plant LOOP Mixed Grass 0 1100 10 8 100 0 62 8 5 f SOIL 10ML e 0 2000 Soil LOOP Sidhigh 0 2100 0 62 5 3 0 065 0 55 Note The organic soils collected for the ongoing fertilization experiment in Loch Vale are high in bot
68. g pins and stems NOTE you should hear compressed gas is seated properly this is normal and will stop once the loading head is tightened Carefully push down on the loading head and then tighten the bottom right hand screw first until you feel resistance Tighten the other two screws until you feel resistance and then fully tighten each screw by rotating among the screws 4 Balance Turn on the balance Use the 29 button to switch display to 0 0000 g Press the CAL 2059 button to calibrate the balance 5 Counters Select Configuration from the menu bar to access the counter window then click on Counters The Warn column indicates the maximum number of samples that should be run before that item needs replacement or maintenance The Count column will increase by 1 each time you run a blank standard or sample Make sure that the Count column will not exceed the Warn value during your run NOTE It is especially important that the crucible Count is not exceeded Overfilling the crucible can result in expensive damage to the machine and considerable downtime Please consult the Lab Manager if you are uncertain if the crucible needs to be replaced Resetting the Counters if necessary After changing the crucible or performing other maintenance please reset the Count to 0 To access this window select Maintenance then click Login select the item that maintenance has been performed on click OK Click Yes if maintenance was per
69. h Carbon and Nitrogen and are therefore analyzed with the PLANT 10ML LOOP method Enter your name or supervisor s name on the Operator line The other Attributes should be left blank in most cases Click OK to add the Blanks to the sample list Click Cancel if necessary to close the Sample window Four blanks should have been added to the sample table To help keep track of your samples change the numbers in the Location column to match the numbers on the sample carousel Initial Standards Select Samples from the main menu and click Login Drift Samples Select the appropriate method using the drop down arrow and the associated calibration standard will appear in the Drift Standards box along with the weight range your standards must be within this range see table above Select 4 repetitions The standards appear after the blanks on the spreadsheet Note The weights in the Mass column for the standards will appear with a symbol this is just to remind you of the approximate weight you should use The actual weights will replace the reminder weights as you enter them using the Print button on the balance To start the analysis click the Analyze button of press F5 to start analyzing the blanks and standards To halt the machine after the blanks in order to run the blank calibration first left click on the row containing the first standard then right click select Pause from the Samples menu choose Manually from the drop down list
70. he above 1 Notepad amp Pencil 1 Plastic whistle 1 Space blanket 1 Razor knife 2 40 gallon 2 ply trash bags Glove liners Sunscreen Lip balm 1 1 4x3 bolt amp nut Ski repair equipment 1 Shovel Suitable for digging through avalanche debris 1 Avalanche Beacon Mandatory 1 Headlamp Loch Vale Watershed Methods Manual 10 Precipitation Sampling a Introduction The LVWS is part of the National Atmospheric Deposition Program NADP precipitation chemistry monitoring network Aerochem Metrics collectors capture precipitation samples that are collected weekly for chemical analysis at the Central Analytical Laboratory CAL in Champaign IL The Aerochem collector lid covers a clean plastic bucket when it is not raining The lid opens when precipitation activates a sensor The sensor is heated so water evaporates when precipitation stops which closes the lid back over sample bucket Sample buckets are collected for the LVWS co located NADP sites CO98 and CO89 every Tuesday morning Detailed sampling and maintenance procedures are provided in the National Trends Network Site Operation Manual Dosset and Bowersox 1999 located in NREL A223 You must be familiar with these procedures before operating a collector Training in NADP procedures is offered yearly and should be taken by all regular operators of the LVWS NADP site The following instructions are given as a brief synopsis of appropriate methods b Equipment and supplies
71. hods can be found in JIS K 0102 Industrial Waste Water Testing JIS K 0551 Total organic carbon TOC testing methods for ultra pure water U S Pharmacopoeia 23 EPA 415 1 EPA 9060A ASTM D2575 Standard Methods for Examination of Water and Waste Water 5310B Refer to the Schimadzu user manual in A256 b Equipment and Supplies located in room A256 Schimadzu TC TN Auto Analyzer Filtered acidified DOC DON DOP samples Calibration standard 6 ppm C 2 ppm N Check sample 3 ppm C 1 ppm N 2MHCl 40 ml clear sampler vials Parafilm c Preparation 1 Allow samples and C and N stocks to reach room temperature by setting on counter while setting instrument up 2 Open the two valves on the air tank main valve to tank and the on off valve connected to the blue air line which goes to instrument 3 Turn on the power to the instrument bottom right corner Loch Vale Watershed Methods Manual 52 4 Load the correct template file consult the lab manager for the correct template file and save as a new file with today s date e g lvws_2010Mar18 Connect the instrument to the PC and allow to warm up by clicking on the lightning bolt button 5 Make up fresh calibration standard check sample and carbonate removal check sample Calibration Standard 6 ppm C 2 ppm N Check Sample 3 ppm C 1 ppm N In 500 ml volumetric flask add In 1000 ml volumetric flask add 3 ml organic C 3 ml organic
72. ial across a glass membrane The pH meter is simply a voltmeter that measures this potential A stable pH reading is operationally defined as one that does not change by more than 0 01 units in 30 seconds There are extensive notes on pH measurement and specific hints on the Broadley James electrode contained in the Instruction Manual for NADP NTN Site Operation Equipment and Supplies located in the NREL A235 Lab notebook pH meter ITT85 Broadley James pH electrode Calibration buffers pH 4 00 and pH 7 00 Quality Control QC Check Solution pH 4 90 0 15 Fresh deionized DI water in squeeze bottle 2ml plastic scintillation vials Kimwipes Waste beaker Estimated time to complete procedure Allow 30 minutes for calibration and 1 or 2 samples Add 5 15 minutes for each additional sample whether open cup or closed chamber Preparation 1 All solutions to be measured including standards and check samples should be at room temperature within a few degrees 2 Check amount and expiration dates of the standard buffers and QC solution If needed order more from the NADP Central Analytical Laboratory by contacting the NADP Site Liaison It may take several weeks for them to arrive Loch Vale Watershed Methods Manual 92 e Procedures Calibration 1 Unplug the LVWS Broadley James pH electrode from the meter on the LVWS bench Rinse the probe copiously with DI water 2 Swap probes an
73. iles for each NOAH IV Example file names for CO98 site name CO98 20091027T1543CO98 txt CO9820091027T1543 xml Example file names for CO89 site name NPX3 20091027T1548NPX3 txt NPX320091027T1548 xml 200991027T1548 Year 2009 Date 1027 Time T1548 4 Send all four files to nadp precip isws illinois edu Subject CO98 CO89 NOAH IV Files Include local download time plus start bucket on and stop bucket off dates Loch Vale Watershed Methods Manual 16 f Be Aware The catch buckets in NOAH IV raingages can hold a maximum of 14 inches Buckets should be emptied and winterized when bucket depth reaches 10 inches You can check the current bucket depth with the PDA by navigating to the Raingage page within the NADP Rain program using procedures detailed above Once on the Raingage page click Refresh to view the current bucket depth To empty the bucket you will first need to place the egage in Service Mode Once you navigate to the Raingage page on the PDA you must click Service Mode Service Mode will time out after 300 seconds As it will likely take longer than five minutes to empty and winterize the gage you will need to click Refresh to extend Service Mode prior to automatic time out While in Service Mode you will need to remove the collection chamber First remove the inlet orifice and set aside be sure to clean any debris off the O ring before re installing the office Gently remove the collection chamber b
74. in a file name and press OK The software will not allow you to overwrite or append and existing file The data collection window will appear on the screen Press the play button to start the data collection At this point the software will monitor the baselines for 60 minutes and then start sampling Debubble the flow cell by pinching and releasing the outflow tubing Repeat until no bubbles appear Pour standards and samples into the cups and place in the sampler Get at least 20 cups poured before starting the sampler Check baselines for stability and drift should be less than 500 micro absorbance units If there are any peaks or jumps in the baseline traces Press the stop button The software will ask if you want to stop press yes Press the rewind button and then the play button Press the fast forward button to begin sampling Instrument shutdown 1 Move the POs color reagent line to the NOs carrier port on the large DI water bottle Let the system pump for about 10 minutes Disconnect all the lines and let the system pump air for about 15 minutes or until all the liquid is out of the instrument Press the run stop button to stop the pump and turn off the main power switch to the instrument Push the engaging levers on all the pump platens to horizontal and disconnect one end of each platen from the pump Pour the unused color reagent into the PO4 waste container
75. it in tubing for 4 hours then copiously rinse with DI water at least 10 liters Conductivity of the rinse water should be lt 2 uS cm even after sitting in the pump for several hours pH paper can be used to check that the pH of the DI rinse water did not change as it passed through the peristaltic pump i e that all acid has been removed from the pump Make sure there are enough filters on hand to process all samples Filters may take several weeks to be delivered from scientific supply houses so plan ahead Plastic bottles must be acid washed before use see acid washing section Bottles are stored filled with DI water Check the conductivity before using any bottle A bottle with a conductivity gt 2 uS cm should be taken out of rotation and re cleaned e Procedures for filtering sample Rinsing pump 1 Geta piece of clean tubing from the Tupperware box in the LVWS clean drawer Handle tubing on the end marked with ink Rinse inside and out with DI water 2 Place non inked end of tube in 1 liter bottle of DI water 3 Attach inked end of tube to the stopcock on peristaltic pump 4 Place waste beaker under filter holder 5 Open stopcock Turn pump on forward to a setting of 3 Rinse pump tubing with 1 liter of DI before working with sample 6 Turn pump off Loading filter 1 Being careful not to touch any of its inner surfaces remove bottom half of filter holder Place on clean surface e g a Kimwipe or inside of
76. l 1999 Botte and Baron 2004 and Richer and Baron 2011 For new surface water chemistry data arrange quality assured data from the RMRS laboratory so that fields i e columns are consistent with the LWWS surface water chemistry master database Ensure that all data field are in the correct order and units and that all site names are consistent with those in the master database Copy and paste the new data into the master database Be sure all values that are below published detection limits are stored appropriately for each variable i e if the detection limit is 0 02 mg L then all values less than 0 02 should be stored as lt 0 02 Values of 0 should not be entered into the database All missing data should be reported at 999 The path to the LVWS surface water chemistry master database is data nrel colostate edu baron LVWS_master data LVWS_masterdata_surfacewaterch emsitry xlsx New precipitation data should be obtained from the National Atmospheric Deposition Program website and added to the LVWS database as outlined in step 2 above The path to the LVWS master precipitation database is data nrel colostate edu baron LVWS_master data New climate data should be obtained from the Water Energy and Biogeochemical Budgets program and added to the LVWS database as outlined in step 2 above The path to the LVWS master climate database is data nrel colostate edu baron LVWS_master data Be sure
77. le SC32A and an RS232 cable blue It goes from the CS I O port on the CR500 to the data logger port on the SC32A The terminal printer port on the SC32A is linked to the printer port on the laptop with the serial cable Click the Connect button on the PC208 menu bar Go to tools Make sure the associated program is LOCHO DLD Click connect button on tools window When connected send the program to the data logger Go to the numeric display window Enter the observed level reading from staff gage meters in the offset window Monitor display to make sure readings are updated on the frequency set by program Loch Vale Watershed Methods Manual 87 7 Disconnect the link to laptop Close and lock shelter lid Weekly service for CR500 1 2 Attach SM192 to CS I O on CR500 with blue RS232 cable Wait ten minutes and then detach cable and close all enclosures Annual Shut Down for CR500 1 2 Temperatures will become increasingly colder as fall progresses After a point water in the stilling well will freeze A drop in stage height below 0 1 feet usually accompanies this In either case it is time to shut down the gage for the year First perform the weekly maintenance as above Disconnect all equipment listed in section b Equipment and Supplies Load everything carefully into pack and return to lab Initial Set up for Stevens gage 1 The Stevens gage should be set up in mid to late April Open Stevens
78. les standards washes TP 1 ml pipette and tips for oxidizing solution TP AlpKem Reagents NH NOs PO43 TP KCI DI Carrier DI Carrier PO4 Color Reagent NHa Working Buffer NOs Color Reagent Dowfax Sodium Salicylate Sodium NOs Buffer NH4Cl check DI Carrier Nitroferricyanide filter for clogs Hypochlorite use fresh bleach Cadmium Reduction Column Potassium Persulfate Loch Vale Watershed Methods Manual 39 c Preparation 5 Allow samples and standards to reach room temperature by setting on counter while setting instrument up Make sure all of the reagents are full and your standards reagents and DI are fresh Turn on the computer from the power strip and follow the set up procedures detailed below The water and NH4 NOs waste must be collected and disposed of as hazardous waste Consult the lab manager if you questions regarding hazardous waste disposal DO NOT ALLOW THE PINK AND GREEN WASTES TO MIX UNDER ANY CIRCUMSTANCES Mixing these substances will produce noxious gasses Be sure the correct channels are set up for your particular needs d Procedures Ammonium Nitrate Directions 1 Check that the instrument is configured for NH4 NOs The line from the sampler should be connected to the T where the NH sample line and the NOs pull through line meet The debubbler on the channel 3 detector NH4 PO should be connected to one line labeled NH from debubbl
79. lls can only function when sufficient flow is present Generally this is from late April to late October Winter flow is a small proportion of the annual total and was estimated prior to installation of the depth transducer in 2006 Although stage has been recorded during the winter since 2006 these measurements may be affected by ice formation within the flume Equipment and Supplies Flume field notebook and pencil Campbell Scientific CR500 stream recorder Eight D cell batteries for CR500 EnviroSystems encoder w Gulley wheel pulley tape float and counter weight Laptop computer with PC208 program RS232 cable and a SC32A converter A9to 25 pin serial cable Data storage module SM192 One D cell battery for Stevens gage Stevens gage w pulley line float and counter weight Strip chart paper Stevens gage pen and cylinder kept in lab over winter Cylinder paper spring and rubber bands kept in lab over winter Estimated time to complete procedures Initial set up of the gages requires about an hour at the site not including time to dig snow from around the flume For weekly service allow 20 30 minutes to download data change Loch Vale Watershed Methods Manual 86 chart record the current stage height and make minor adjustments Closing down the flume for the winter requires only slightly more time than the weekly service d Preparation For initial set up make sure the
80. lor reagent bottle 15 Let the system pump 15 minutes before running samples Setting up a sample run Press the sample table button on the main tool bar in Winflow4 Type in cup name and type for each sample and standard to be analyzed Refer to the typical sample table on the page 5 and the notes below Cup Numbers Positions 1 20 are the large tubes at the back of the sampler and are used for standards checks and baselines washes The instrument can sample from these cups up to 16 times each Loch Vale Watershed Methods Manual 47 There are 3 racks for the 2 ml sample cups The one on the left closest to the sampler wash cup holds cup numbers 101 190 The middle rack holds cup numbers 201 290 and the rack on the right holds number 301 390 These cups can be sampled up to 4 times each Sample Name Sample names can be anything that fits in the field However the standards used in the calibration curve anything labeled C in the type column must be named exactly the same as they are named in the calibrant table in the method file To view the calibrant table click the edit method button on the main toolbar click file open and select the appropriate method Consult the lab manager for the correct method The calibrant table is the last page of the method file Type SYNC This is always the first cup in a run it is a high standard usually top standard which will yield a large peak t
81. m Molybdate Solution 60 ml Stock Ascorbic Acid Solution Add reagents in order Filter through 8 0 um polycarbonate membrane Prepare daily Stock 1000 mg L P 1L 4 393 g Potassium DI hydrogen Phosphate KH2PO4 Dissolve into 900 ml DI water Bring up to 1000 ml with DI water Intermediate Calibrant 100 mg L P 100 ml Using a volumetric pipette add 10 ml Stock to 80 ml DI Bring up to 100 ml with DI water Working Calibrants 100 ml Use CiVi C2V2 to measure out desired range of standards Bring up to 100 ml with DI water Loch Vale Watershed Methods Manual 719 Appendix F Supplies Order new supplies glassware bottles instruments etc from the VWR catalog via the Kuali Financial System website CSU gets a contract pricing rate 40 of list from VWR so it is much less expensive to get new things from them versus other lab supply houses Check with NREL s purchasing administrator about what to do if VWR does not stock an item you need Purchases through Kuali do not require a Purchase Request Form For all other purchases you must fill out a Purchase Request Form on the NREL website Supplies can also be obtained from the CSU Chemistry Stockroom in the Chemistry building on campus Purchases from the Chemistry Stockroom do not require a Purchase Request Form but do require a CSU Chemistry Department Stockroom Card The LVWS Program Manager should have a Stockroom Card and be able to make purchase for other LVWS personnel
82. ml bleach Bring up to 400 ml with DI water Be sure to use fresh bleach opened within the week For NO3 Channel NOs Color Reagent 100 ml H3PO4 40 g sulfanilamide 2 g N 1 Naphthylethylenediamine Add to 800 ml DI water Bring up to 1000 ml with DI water Filter through 8 0 um polycarbonate membrane Store in refrigerator in dark glass bottle NOs Buffer 638 g NH4Cl 0 75 g disodium EDTA Bring up to 7 5 liters with DI water Filtered inline from dispensing bottle NH4 NO3 Standards Use the formula Ci Vi C2V2 to make ammonium nitrate working standards from a 1000 mg L stock solution For Orthophosphate Analysis Stock Sulfuric Acid 5N 140 ml concentrated H2504 Slowly added to 800 ml of DI water in a cool water bath Bring up to 1000 ml with DI water Stock Antimony Potassium Tartrate Solution 3 g Antimony Potassium Tartrate Dissolve into 500 ml DI water Bring up to 1000 ml with DI water Store at 4 C in a dark glass bottle Loch Vale Watershed Methods Manual 77 Stock Ammonium Molybdate Solution 40g Ammonium Molybdate Dissolve in 800 ml DI water Bring up to 1000 ml with DI water Store at 4 C in polyethylene bottle Stock Ascorbic Acid Solution 1 8 g Ascorbic Acid Dissolve into 70 ml DI water Bring up to 100 ml with DI water Stable for 1 week at 4 C POs Color Reagent 100 ml Stock Sulfuric Acid 5N 10 ml Stock Antimony Potassium Tartrate Solution 30 ml Stock Ammonium Molybdate Solution 60 ml Stock A
83. n hand before sample day 2 Clear any loose ice out of open water in the hole with shovel and or rubber gloves 3 Measure the depth of lake and ice with tube to make sure you are over the deepest point of lake Be careful not to disturb sediments If you choose a site that is less than half as deep as the deepest point of the lake abandon it and drill another hole 4 Measure temperature profile of the lake by taking readings every meter Also take a reading just above and below the ice layer Record all data in the field notebook 5 Holding on to one end drop sample tube into the water through hole Weight the end of pump tubing so it falls in a straight line a small bottle filled with sand duct taped to bottom of tube is easy to carry and works very well ON wm Collect two water samples from the lake The first should be labeled surface and is collected from just below the bottom of the ice The second should be labeled hypolimnion and is collected 0 25 0 5 m above lake bottom Before drawing sample flush pump with at least 45 revolutions of pump handle Rinse all bottles and syringe 3X before filling see rinsing procedures in Surface Water Sampling section To collect the phytoplankton sample rinse the bottle 3X fill dispense 1 ml of Lugol s solution with a disposable 2 ml pipette and then cap While one person operates the pump the other person fills sample bottles The person holding tube and bottles should wear ins
84. name and a method name Consult the lab manager for the correct method Select the correct file names and press OK The software will ask for a filename for the results with the default being the same as the sample table with an rst extension Select or type in a file name and press OK The software will not allow you to overwrite or append and existing file The data collection window will appear on the screen Press the play button to start the data collection At this point the software will monitor the baselines for 60 minutes and then start sampling Debubble both flow cells by pinching and releasing the outflow tubing Repeat until no bubbles appear Pour standards and samples into the cups and place in the sampler Get at least 20 cups poured before starting the sampler Check baselines for stability and drift should be less than 500 micro absorbance units If there are any peaks or jumps in the baseline traces Press the stop button The software will ask if you want to stop press yes Press the rewind button and then the play button Press the fast forward button to begin sampling The first NO3 peak will appear about 75 seconds after the first sample is drawn The first NH4 peak will appear after about 250 seconds Loch Vale Watershed Methods Manual 44 Instrument shutdown 9 Press the run stop button on the pump to stop the reagent flow Disconnect the cadmium column from the NOs
85. ne gloves to prevent cold hands and minimize sample contamination Rinse all bottles three times with sample before filling To rinse dip bottle to depth of 0 2 0 5 m with bottle mouth upstream fill to one third of capacity replace cap shake vigorously uncap and pour water from bottle over threads of cap and from cap over threads of bottle Make sure you pour rinse water downstream or away from eventual sample point When finished rinsing fill bottles to shoulder and replace cap Follow the same procedure for all bottles except for the phytoplankton bottle which is rinsed 3X and filled to shoulder before adding 1 2 ml of Lugol s solution Loch Vale Watershed Methods Manual 24 f Be Aware Make sure no person or animal is disturbing the stream immediately upstream of the sampling site You do not want any sediment in the sample If necessary wait until water has cleared before sampling Streams flow at very low levels underneath the snow in the wintertime If you have to dig away snow or chop out ice in order to sample choose a spot with sufficient flow Wait for water to clear of snow ice and sediment before sampling An igloo or other shelter built just upstream from the throat of the flume at the Loch Outlet works well to minimize shoveling snow during winter Loch Vale Watershed Methods Manual 25 Collection Permits and Fee Waivers Our presence in RMNP is a privilege granted yearly by park staff and as such we apply
86. nitrogen NO3 N and ammonium NH4 to ammonium expressed at nitrogen NH4 N Once nitrate and ammonium concentrations are expressed as nitrogen they can be summed to get TIN Methods for analyzing TDN are detailed in the Schimadzu section of the LVWS Methods Manual Dissolved organic Phosphorus DOP is estimated by calculating the difference between Orthophosphate PO4 and Total Phosphorus TP Methods for analyzing PO4 and TP are detailed in the AlpKem Section of the LVWS Methods Manual PO4 samples are filtered but TP samples are not b Equipment and Supplies Equipment and supplies are located in drawers below the LVWS lab bench in NREL A235 480 ml amber borosilicate bottle filled with sample from cooler Whatman GF F filters pre baked at 500 C for 5 hours see instructions below Forceps Pre baked filtration apparatus ground fitted glass 1000 ml flask ground glass 47 mm fritted glass filter support ground glass 47 mm funnel amp clamp Vacuum line lt 15 Hg vacuum 2 Pre baked 120 ml amber borosilicate bottles Once bottle should be labeled DOC DON DOP and the other bottle should be labeled Total P Both bottles labels should include the site name sample type and date 37 concentrated hydrochloric acid HCl Loch Vale Watershed Methods Manual 33 c Estimated time to complete procedure Allow 10 min per sample although filtering times may vary greatly depending
87. o let the software know the sample peaks have started C indicates a calibration standard to be included in the calibration curve Do not use this for internal standards or checks unless you want them included in the calibration curve RB indicates a baseline wash The instrument will use these peaks to correct for baseline drift so they should always be a 0 ppm standard U unknown Should be used for all samples checks and internal standards After the calibration curve the basic pattern should be 10 samples 1 standard 10 samples and 1 baseline Repeat to a maximum of about 80 samples Larger sets should be broken into multiple runs Sample runs should always end with a baseline Other columns in the sample table R Number of replicate samples to be taken from the cup Should be set to 1 Dil dilution factor of the sample usually 1 Wt weight of the sample usually 1 After the sample table is prepared be sure to save it Starting a sample run 1 Click the collect data button on the main toolbar The software will ask for an operator name and ID type in your initials for both The software will then ask for a sample table name and a method name Consult the lab manager for the correct method Select the Loch Vale Watershed Methods Manual 48 7 correct file names and press OK The software will ask for a filename for the results with the default being the same as the sample table with an rst extension Select or type
88. of what you sample bottles and lids come in contact with during lab work Wash hands frequently with DI water Latex gloves are available in the lab however the gloves themselves are not completely clean and they become very slippery when wet To minimize the potential for sample contamination the LVWS lab bench at NREL is used exclusively for processing LVWS water samples Clean the bench top before starting lab work and continually sponge away any water that accumulates during lab work Leave the area clean for the next user Procedures for processing and storage of surface water samples are summarized in Tables 1 and 2 Loch Vale Watershed Methods Manual 27 Table 1 Summary of laboratory procedures for processing LVWS weekly and synoptic surface water samples Bottle Set for Treatment Label Analysis Destination Surface Water 500 ml HDPE acid Filtered with peristaltic F U Ge Filtered Ion concentrations RMRS lab washed bottle pump into 60 ml Untreated translucent HDPE acid washed bottle 250 ml brown None R U Ge Raw ANC pH and RMRS lab HDPE acid washed Untreated specific bottle conductivity 60 ml translucent None SiO2 SiO2 Concentration NREL HDPE acid washed refrigerator bottle Pre baked 480 ml 1 Filtered with baked DOC DON DOP DOC TDN and NREL amber borosilicate glass filter tower into PO refrigerator bottle pre baked 120 ml amber borosilicate bottle AND acidified with 2 drops of 37 H
89. ong acid solutions Bottles may soak longer than three hours but should not remain in the acid bath for longer than three days It is easiest to fill acid bath with fresh bottles after rinsing a batch then you are ready to rinse another set when needed Dirty bottles are returned to us from the analytical laboratory they are stored in NREL A254 until needed Loch Vale Watershed Methods Manual 62 SHIPPING SAMPLES Surface Water Samples a Introduction Deliver surface water samples weekly to the USFS Rocky Mountain Research Station water chemistry analytical laboratory 417 2394 piersond usgs gov for chemical analysis within 24 hours of collection When Wednesday s lab work is complete simply walk the R U and FU samples over to the USFS building and place them in the appropriate refrigerator DOC samples were previously delivered to George Aiken 303 541 3057 at the USGS WRD in Boulder every other week 3215 Marine Street Suite E 127 DOC is now analyzed at NREL so DOC samples are no longer shipped b Equipment and Supplies Equipment and supplies are located in NREL A223 and NREL A235 The following supplies are used in the shipment of surface water samples as necessary Small plastic cooler Ice pack Packing material c Estimated time to complete procedure Allow 15 30 minutes for delivering samples to the RMRS laboratory d Preparation Samples must be filtered and stored in the walk in cooler until ready for tr
90. otential avalanche terrain based on slope alone is shown in Figure 1 South facing aspects are generally more stable during the colder winter months while north facing slopes are generally more stable in the spring and summer Dry slab avalanches are the primary danger during winter months The recipe for a dry slab avalanche is a more consolidated layer of snow on top of a less consolidated layer when combined with slopes over 25 degrees and a trigger i e YOU these avalanches can be fatal Be aware of runout angles when you are below steep terrain Stay far enough away from steep terrain above you to keep the top of the potential avalanche path at less than 20 from you to it When traveling in avalanche terrain all parties must carry an avalanche beacon probe and shovel Your partner or group is responsible for saving your life should you become buried in an avalanche and vice versa There is no substitute for proper avalanche awareness training There are many avalanche awareness courses offered throughout the fall and winter Awareness of all major contributing factors is the first and possibly best means of staying out of harm s way The following tests can be used as tools in your evaluation of how safe a zone is for travel but they are not your only tools Loch Vale Watershed Methods Manual 5 LVWS Potential Avalanche Terrain Based on Slope Legend Weather Stations Loch Outlet Streams Trails Lakes Glaciers Slo
91. pe degrees T Safest lt 25 E Less Safe 25 30 zy Greatest Danger 30 45 LC Danger gt 45 2 Kilometers Figure 1 Potential avalanche terrain within the Loch Vale Watershed bases on slope alone Note Other factors besides slope contribute to avalanche risk The Hasty Pit The pit provides information to evaluate the questions Are there slab layers How large and extensive are the slabs Approximately how well are the slabs bonded to other layers What might it take to make a slab fail In the pit you will be able to identify snow layers snow types layer cohesiveness and snow density Pits can be used to identify buried surface hoar and faceted snow layers Never dig a hasty pit where you might trigger a slide The site should be safe and representative of the slopes you are really evaluating Your pit site should have the same elevation slope angle and aspect as the slopes of interest A hasty pit can be dug and analyzed in 15 20 minutes with practice Make the pit about 3 feet wide Dig to ground if practical but go at least 4 to 6 feet deep The actual digging of your pit will give you information about the layering of the snow so pay close attention Make the uphill face vertical and smooth Observe this face for layers by brushing the face with your glove Check hardness of the layers by pressing into the snow If you can easily push in your fist the snow is Very soft four fingers is Soft one finger is Medi
92. plan ahead Check with a supervisor prior to making a purchase to ensure you have the correct account number Assemble a bottle set for each site Fill appropriate number of gallon sized Ziploc bags with contents listed in Bottle set section above Label each bag with the site name sample type De NORM DUPE BLANK and collection date YYMMDD Do not forget to pack the conductivity meter and field notebook Be sure the conductivity meter has been calibrated recently and that the battery has adequate charge All HDPE bottles are acid washed and stored filled with DI to minimize sample bottle contamination Prior to inclusion in a bottle set the conductivity of the water inside each HDPE bottle must be tested If the conductivity is lt 2 uS cm the bottle may be included in a sample set If the conductivity is gt 2 uS cm the bottle must be removed from rotation and acid washed again prior to use e Procedures 1 Begin sampling at a given site by recording site name weather conditions time of sampling and names of technicians in the field notebook 2 For the Loch Outlet be sure to record a stage reading from the staff gage inside the flume at the time of sampling 3 Turn on conductivity temperature meter Immerse probe in stream until reading stabilizes Ready should be displayed once the values stabilize For all sites record sampling time conductivity and temperature in the field notebook 4 Wear rubber or neopre
93. pped in Seal the jar and wrap the jar with bubble wrap to protect it during transportation and shipment Place the wrapped sealed sampler jar and its corresponding wrapped sealed travel blank into the shipping bag for return shipment to CAL Leave the citric acid impregnated filter paper in the shipping bags The citric acid filter paper acts as an ammonia scavenger Record the Sample Off date and time Install the new sampler s remove and save the bubble wrap from the new sampler jar Remove a single new sampler from the jar Handle the sampler buy its flexible tubing only DO NOT TOUCH THE BLUE TUBE i e radiello diffusive sampler body Attach the sampler onto the mounting bolt inside the shelter Ensure that the sampler is secure Reseal the now empty glass jar and wrap it in bubble wrap Place the resealed empty jar in the bag containing travel blank and citric acid filter paper Record the sample start date time Repeat installation procedure for any remaining samplers 4 Samper Storage bring the two sampler boxes i e for the retrieved sampler and the newly installed sampler back to NREL Store the box for the newly installed sampler with its travel blank in the NREL freezer Complete the field form for the retrieved sampler and ship the complete box to CAL 5 Completing the field form record the NADP site ID i e CO98 your name initials and the sample start and end dates times Report site conditions applying to the
94. pslope dimension that is deep enough to expose potential weak layers on the smooth walls of the column A depth of 100 120 cm is usually sufficient as the compression test rarely produces fractures in the deeper weak layers e Completely isolate the column on all sides e If the snow surface slopes remove a wedge of snow to level the top of the column e Place a shovel blade on top of the column o Tap 10 times with fingertips moving hand from wrist While tapping if the upper part of the column slides off or no longer evenly supports further tapping on the column remove the damage part of the column level the new top of the column and continue tapping o Tap 10 times with fingertips or knuckles moving forearm from elbow o Hit the blade 10 times with open hand or fist moving the arm from the shoulder e Record when the column fractures and note characteristics of snow layer below fracture Term Description Reporting Risk Very Easy Fractures during cutting CTV Q Red Easy Fractures within 10 light taps using finger tips CT1 10 Q Red only Moderate Fractures within 10 moderate taps from the CT11 20 Yellow elbow using fingertips Q Hard Fractures within 10 firm taps from whole arm CT21 30 Green Loch Vale Watershed Methods Manual 7 using palm or fist Q No Fracture Does not fracture CIN Green Recording CT Q cm test depth cm CT number of
95. r communication RMNP will provide a volunteer to assist with winter time sampling This volunteer is generally responsible for all radio communication but all LVWS staff traveling to the field should be familiar with radio operation and etiquette When traveling with a Park Service volunteer you must file a back country travel plan at the Resource Management Office at park headquarters When filing this plan we must include call signs for all parties in the group Park Service volunteers will use a call sign of VIP e g VIP Messina LVWS staff should use a call sign of Researcher All frequencies programmed into radios except the USGS line of sight channel are not intended to be used unless necessary and if they are used proper radio etiquette must be followed This consists of brief concise transmissions A typical call would resemble the following Us ROMO Researcher Baron Them Researcher Baron Us I have a 28 year old male with possible femur fracture Break Them Go ahead Us Patient is breathing and responsive no external bleeding vitals steady Break Them They will lead conversation from this point Loch Vale Watershed Methods Manual First Aid Kit Item Comments Quantity 2 Pairs of nitrile or latex gloves Non latex gloves are best in order to prevent allergic reactions Can be used for used dressings bandages miscellaneous
96. ration box 1 in the Auto Dilution box and OK Continue this process using 6 as the Standard Solution Concentration and by increasing the Auto Dilution box number to dilute the four top standards to the ones listed above Select to use default settings and do not enable history log Repeat the above steps for the TN curve The injection volume should read 150 wl From top to bottom TN standards should read 0 0 25 0 5 1 2 This is accomplished by clicking add typing 1 in the Standard Solution Concentration box 1 in the Auto Dilution box and OK Next type 2 in the Standard Solution Concentration box 2 in the Auto Dilution box and OK Continue this process using 2 as the Standard Solution Concentration and by increasing the Auto Dilution box number to dilute the 1 top standard to the concentrations listed above This set up allows the instrument to pull 6 and 3 for NPOC from vial 2 1 5 and 0 75 Loch Vale Watershed Methods Manual 54 for NPOC from vial 3 0 and 0 for NPOC and TN from vial 4 0 25 and 0 5 for TN from vial 5 and 1 and 2 for TN from vial 6 Setting up method WY hh Select file new method For analysis choose NPOC TN and name the method For example LVS031215 for stream samples or LVPPT031215 for precipitation samples Browse for the NPOC calibration cur
97. s suspended above the plate It should be cool but above freezing Sprinkle a few drops of water or snow onto the ribs above sensor plate to open the wet side bucket If the lid does not open consult the NADP Site Operation Manual Dosset and Bowersox 1999 for troubleshooting procedures Peer into the wet side bucket from the downwind side i e northeast Note any contamination in the field book Using the plastic bag as a glove seal the clean lid onto the sample bucket Ensure the lid is firmly sealed on the bucket Check the sensor heater again it should now be warm Remove the sealed wet side sample bucket from the Aerochem Install the clean bucket using the bag as a glove Blow any remaining water off the sensor and away from wet side bucket or wait for the heater to evaporate remaining water on the sensor Observe the lid seal as it covers the newly installed wet side bucket If the seal is not complete airborne particulates could contaminate the sample Notify the NADP Site Liaison 217 244 0372 if lid does not seal completely Place the sample bucket into the plastic bag from the clean lid or clean bucket Label the plastic bag with the collector ID either CO98 or CO89 DO NOT WRITE ON THE BUCKETS Record the bucket change time and date in the field book and note the bucket weight written on the side of each bucket by CAL CAL bucket weights can be used to identify each bucket back in the lab and ensure precipitation samples for C
98. scorbic Acid Solution Add reagents in order Filter through 8 0 um polycarbonate membrane Prepare daily Stock 1000 mg L P 1L 4 393 g Potassium DI hydrogen Phosphate KH2PO4 Dissolve into 900 ml DI water Bring up to 1000 ml with DI water Intermediate Calibrant 100 mg L P 100 ml Using a volumetric pipette add 10 ml Stock to 80 ml DI Bring up to 100 ml with DI water Working Calibrants 100 ml Use CiVi C2V2 to measure out desired range of standards Bring up to 100 ml with DI water For TP analysis Potassium Persulfate Oxidizing Solution Dissolve 5g K2520s into 90 ml DI water using stir bar and low heat Bring up to 100 ml with DI water Stock Sulfuric Acid 5N 140 ml concentrated H2504 Slowly added to 800 ml of DI water in a cool water bath Loch Vale Watershed Methods Manual 78 Bring up to 1000 ml with DI water Stock Antimony Potassium Tartrate Solution 3 g Antimony Potassium Tartrate Dissolve into 500 ml DI water Bring up to 1000 ml with DI water Store at 4 C in a dark glass bottle Stock Ammonium Molybdate Solution 40 g Ammonium Molybdate Dissolve in 800 ml DI water Bring up to 1000 ml with DI water Store at 4 C in polyethylene bottle Stock Ascorbic Acid Solution 1 8 g Ascorbic Acid Dissolve into 70 ml DI water Bring up to 100 ml with DI water Stable for 1 week at 4 C POs Color Reagent 100 ml Stock Sulfuric Acid 5N 10 ml Stock Antimony Potassium Tartrate Solution 30 ml Stock Ammoniu
99. sh and check Fill a brown 480 ml acid washed borosilicate bottle with check solution and insert the small tube protruding from the front left corner of the Schimadzu into the bottle This is vial number 0 Once the sample table has been set up and everything looks in place start the machine by hitting the start button which looks like a traffic light signal Click shut down instrument standby OK external acid addition OFF and start Use the following procedures if you need to set up a sample table from scratch Setting up calibration curves Set up the calibration curves File new calibration curve for NPOC Choose edit calibration points manually and dilution from a standard solution Change analysis to NPOC select zero shift off multiple injections on and name the curve according to the run date and particular curve For example 031215NPOC Choose NPOC acid addition to be 2 0 There is no acid addition for the TN method Create NPOC calibration curve using Edit Calibration Point Parameters page The injection volume should be changed to 150 ul From top to bottom standards should read 6 3 1 5 0 75 0 This is accomplished by clicking add typing 0 in the Standard Solution Concentration box 1 in the Auto Dilution box and OK Next type 6 in the Standard Solution Concent
100. source Ecology Laboratory Colorado State University 1499 Campus Delivery Fort Collins CO 80523 1499 970 491 1968 jill nrel colostate edu Program Manager Eric E Richer Natural Resource Ecology Laboratory Colorado State University 1499 Campus Delivery Fort Collins CO 80523 1499 970 491 2153 eericher nrel colostate edu Loch Vale Watershed Methods Manual 95
101. tandard curve to get the respective absorbencies Perform a linear regression to find the equation that describes the relationship between the standard concentrations and their absorbencies A new standard curve is necessary for every 2 3 runs and for each new day s run s If the R is gt 0 99 proceed to the next step If not check date on standards and either rerun the standards or make new ones Loch Vale Watershed Methods Manual 37 Running samples 1 2 9 Check that the pipette is dispensing the correct volume of sample De 10 00 ml Once pipette is calibrated begin pipetting standards and samples into 12 cuvettes Keep a written log of what sample or standard goes into each cuvette in the silica lab notebook Each group of 12 cuvettes should contain a standard blank and duplicate Rinse cuvettes with a few ml of sample or standard three times before dispensing 10 ml of analyte After analytes are pipetted into cuvettes add 1 Acid Reagent Powder Pillow to each cuvette Use the Vortex Genie to stir the reagent in with the analyte This speeds dissolution greatly Add 1 Molybdate Reagent Powder Pillow to each cuvette and use Vortex Genie to dissolve reagent wait 10 minutes before next step Add 1 Citrate Acid Pillow to each cuvette and use Vortex Genie to dissolve reagent Wait two minutes before placing cuvette into meter Wipe the outside of each cuvette with a Kimwipe before placing in
102. tape Loch Vale Watershed Methods Manual 80 Plastic bottles 60 ml 250 ml square brown 500 ml amp 1000 ml HDPE Nalgene Glass amber borosilicate bottles with green Teflon caps 120 ml 240 ml amp 480 ml Millipore Isopore 0 4 um membrane filters Catalog HTTP04700 Whatman GF F glass fiber filters 47 mm 0 7 um 47 mm all glass filter tower all glass funnel and support 1000 ml flask Kontes pH buffers 4 00 and 7 00 Specimen cups Scintillation vials VWR Traceable Conductivity Standard 10 uS cm Catalog 23226 567 VWR Traceable Conductivity Standard 100 uS cm4 Catalog 23226 589 10 mg L SiO standard solution Silica method 8185 Silicomolybdate method high range 0 100 0 mg L SiO2 Acid Reagent Powder Pillows Molybdate Reagent Powder Pillows Citrate Acid Pillows Loch Vale Watershed Methods Manual 81 Appendix G Radio Channels in Rocky Mountain National Park List of channels available on LVWS Bendix King Radios Channel Area Action Use E1 Dirct East side Radio to radio direct 1 5 miles E2 Twin East side Radio to Twin Sisters East side long distance repeater communications E3 Tundr East amp West Radio eS Trail Ridge above treeline repeater W4 Dirct West side Radio to radio direct 1 5 miles W5 Red Westside Radio to Red Mtn West side long distance repeater communications W6 Shdo Westside Radio to Shadow West side long distance Mtn
103. the start vial number Clear the sample name field and click OK Each row will be assigned a specific sample and must be named according to the sample site and date For example LO031215 refers to Loch O from Dec 15 2003 Be sure to name all samples washes and checks in the empty sample name column Loch Vale Watershed Methods Manual 55 8 Along with field blanks field dupes and an occasional lab dupe every 20 samples be sure to insert a di wash and check 3 ppm C 1 ppm N after every 10 samples Also be sure to end the run with a wash and check 9 Once the sample table has been set up and everything looks in place hit the start button which looks like a traffic light signal Be sure to check the external acid addition off Loch Vale Watershed Methods Manual 56 LECO CN Analyzer a Introduction The LECO TruSpec CN carbon and nitrogen analyzer is a non dispersive infrared microcomputer based instrument designed to measure the carbon and nitrogen content in a wide variety of organic compounds For LVWS purposes the LECO is used for the analysis of percent carbon C and nitrogen N on finely ground soil and plant samples b Equipment and Supplies located in Rm A253 LECO TruSpec CN analyzer plant soil samples ground and stored in well labeled scintillation vials ball mill soil tissue grinder Room A127A inside Room A121 microbalance to weigh sampl
104. to meter Record the absorbance reading from spectrophotometer in the silica lab notebook 10 Run 2 to 3 sets of 12 samples before running a new standard curve 11 Use the standard curve equation to convert absorbance to concentration Enter the absorbance as the x variable Loch Vale Watershed Methods Manual 38 AlpKem Procedures The Alpkem is an instrument that colorimetrically analyzes aqueous solutions for concentrations of different chemicals NREL s AlpKem can be configured to run ammonium NH nitrate NOs and orthophosphate DCH Technicians must have proper training from a laboratory manager before attempting to use this instrument a Introduction Please refer to the Flow Solution Manual IV by OI Analytical 2001 for NH4 NOs PO and total phosphorus TP persulfate digest methods This manual is located in NREL A256 Modifications to the TP method are supplied by the Hedin lab and are described below b Equipment and Supplies located in Rm A256 OI Analytical AlpKem Spectrophotometer Samples for NH4 NO3 PO4 Total Phosphorus KCL DI matrix Standards KCI DI matrix 2 ml analyzer cups and racks KCI DI squeeze bottles 8 micron membrane filters Reagents recipes are described in Appendix E Test tubes TP Linerless caps TP Oxidizing solution Potassium Persulfate for TP Autoclave TP 5ml pipette and tips for samp
105. to plot all new data to ensure units and formatting are correct and note all data that are preliminary and subject to change Loch Vale Watershed Methods Manual 83 Appendix I Historical Field and Laboratory Procedures These procedures are no longer used to collect and analyze samples from the LVWS but are provided as a reference for past methods Belfort Raingage Discontinued in August 2010 a Introduction An Alter shielded Belfort raingage was used in LVWS to measure precipitation amount from August 1983 to August 2010 The Belfort recorded cumulative precipitation depth as well as frequency and length of precipitation events The Belfort was initially installed in 1983 and removed on August 16 2010 The CO98 Belfort and CO98 NOAH IV provide a continuous precipitation record for the Loch Vale NADP site Detailed sampling and maintenance procedures for the gages are provided in the NADP NTN Site Operation Manual Dosset and Bowersox 1999 and in the Belfort Equipment Manual Both manuals can be found in NREL A223 Equipment and Supplies Raingage charts cylinders cylinder clips rubber bands dashpot oil D cell batteries and pencils are kept in the NREL lab and or inside shell of Belfort Antifreeze and transmission fluid are kept in the storage box at the NADP site Raingage ink is kept inside the Belfort Estimated time to complete procedures It takes five to ten minutes to change charts an additional 20
106. toclave and allow to warm up for 10 min Press the 4 button twice to start the autoclave cycle Once cycle is finished crack door 1 inch and allow slow cool for 10 min 10 Use caution when taking samples and flasks from autoclave as solutions are extremely hot Allow samples to cool to room temperature for immediate run or place in cooler and run within 24 hours 11 Follow same procedures to run samples on AlpKem as for Orthophosphate only difference is instead of di for sampler wash use 1 5 persulfate solution from autoclave Loch Vale Watershed Methods Manual 51 Schimadzu Procedures For the analysis of non purgeable organic carbon NPOC and total nitrogen TN in stream lake and precipitation waters a Introduction The Schimadzu TOC V instrument measures the amount of total carbon TC inorganic carbon IC and total organic carbon TOC in water Non purgeable organic carbon NPOC can also be measured when the POC accessory is installed Oxidative combustion infrared analysis is a widely used TOC measurement method that has been adopted by the JIS and other international standards By installing the optional TN unit total water borne nitrogen TN can be measured using the principles of oxidative combustion chemiluminescence As LVWS water samples are filtered prior to analysis the resultant concentrations are operationally defined as dissolved organic carbon DOC and total dissolved nitrogen TDN Met
107. uestionable and enter a Pause at the beginning and end of the calibration check Standard Carbon 5 Nitrogen 5 Mixed Grass 43 78 41 59 45 97 2 53 2 40 2 65 Sidhigh 2 589 2 460 2 718 0 269 0 255 0 282 Enter the sample name in the Name column Weigh the appropriate amount of sample for the method and press the Print button on the balance the sample weight should appear next to the name you just entered Run a blank and or standard every 10 samples to ensure the machine is running properly At the end of your run DO NOT shut off the machine and DO NOT close the software Change the crucible if necessary select and download your data and fill out the log book 9 Exporting Data Select the sample you want to download by clicking and dragging in the row column Go to Samples on the main menu bar and click on Text Export Data Enter a filename and the appropriate drive click Save 10 Printing Data Select the rows containing the samples you want to print Select Samples on the main menu bar click Print click OK Loch Vale Watershed Methods Manual 60 Acid washing Procedures a Introduction All plastic bottles and tubing used for collection processing and storage of water samples must be cleaned in 10 HCl acid prior to use This cleaning removes any contaminants adhered to the walls of bottles that can affect sample quality Equipment and Supplies Acid baths are located in
108. ulated rubber gloves to keep hands warm and to prevent contamination of sample Keep bottles insulated if they are in danger of freezing Record the sample depths sample times and names of field technicians in the field notebook f Be Aware Water inside the pump will freeze if not constantly flowing Once started pumping do not stop Difficulty of turning handle and diminished flow is evidence that freezing has begun You may be able to thaw it by pumping more vigorously from the lake bottom If this does not work drain tube put in plastic bag and thaw inside your parka Prolonged exposure to cold and wind can lead to frostbite or hypothermia Come prepared with adequate warm clothing wind protection hand warmers and food Do not ever endanger yourself or the party for a sample If anyone is in doubt of the party s safety pack it up and go Loch Vale Watershed Methods Manual 91 Measuring pH Discontinued in 2010 a Introduction LVWS staff discontinued pH measurement for precipitation and surface water samples at NREL in 2010 The CAL and USFS laboratories measure pH for precipitation and surface water samples respectively Therefore pH measurements at NREL were considered redundant and discontinued An important characteristic of water is its acidity pH is defined as the negative log of the hydrogen ion activity The standard method for pH measurement uses an H ion specific electrode that generates an electrical potent
109. um a pencil is Hard a knife blade is Very hard snow The hasty pit is not a complete stability evaluation Informed decisions can only be reached by combining input Loch Vale Watershed Methods Manual 6 from weather terrain snowpack skier capabilities and information provided by your hasty pits The Shovel Shear Test Isolate a column of snow about the width and depth of a shovel blade from your smooth face Cut both sides and the back to isolate the column from the surrounding snowpack This lets us evaluate the shear strength of the layers since that is all that is now holding them together Insert the shovel 1 2 feet vertically behind the column Do not lever the shovel If the column fails without pressure this is a very easy shear If failure occurs with light horizontal pressure this is an Easy shear These are indicators of unstable snow The rating then goes to Medium Hard and Very hard as you exert progressively more force The force you exert is relative to your own technique therefore so are these ratings When a layer shears examine the snow at the shear plane to identify the sliding layer and the failure source e g buried surface hoar ice lens faceted snow The shear test in a hasty pit will identify many weak layers Examining crystals along these planes may help explain the source of instability The Compression Test e Diga hasty pit e Isolate a column of snow 30 cm wide and with a 30 cm u
110. um line just as rinse water completely leaves funnel before significant amount of air passes through the filter otherwise trapped particles may fracture and be washed into the sample Shake and swirl filtrate around in flask and then pour into waste vessel Rinse two more times Loch Vale Watershed Methods Manual 34 DOC DON DOP Filtering sample 1 Pour remaining sample into funnel attach vacuum line and pull sample into flask If there is substantial amount of suspended material in the sample filtering will be very slow If the sample appears to contain substantial suspended material only pour half of the sample into the filter tower so that the filter can be changed midway through sample Once the sample has been filtered rinse a 120 borosilicate amber bottle 3X with sample and then fill to shoulder Label the bottle DOC DON DOP be sure to include the site name sample type and date on the label Add two drops of 37 HCl to the DOC DON DOP bottle invert and shake vigorously Repeat all steps for each sample Be sure to rinse the filter tower with DI between samples and use a new filter for each sample Store sample bottles in the walk in cooler in appropriate location After processing samples rinse all glassware thoroughly with DI water Cover all orifices with aluminum foil and bake as previously described Bake glassware on either Friday or Monday so it is ready for use by Wednesday morning Loch V
111. urn Once back in town make sure you contact the person s awaiting your return Loch Vale Watershed Methods Manual 4 The bottom line is to never endanger yourself or anyone else for a sample In the best conditions a park led rescue will take a minimum of 5 hours If the weather is bad a rescue can take over a day even during summer Stay safe Snow Stability Evaluation Avalanche danger is a serious concern in LVWS A good rule of thumb is that if a slope can be skied it can also produce an avalanche Standard routes to the most frequently visited sampling sites in LVWS involve relatively little avalanche danger In spite of this the trip leader needs to be constantly aware of present and changing snow conditions When traveling to a non standard sampling point during the winter snow stability is your primary concern If after careful evaluation of snow stability someone in the group is in doubt of the party s safety TURN AROUND The loss of a sample is inconsequential compared to injury or death Be sure to call the Colorado Avalanche Information Center CAIC hotline 970 498 5311 before traveling to the mountains or check the CAIC website at http avalanche state co us index php Know what to expect before leaving town Weather terrain and snow conditions all influence avalanche danger Be wary of slopes with angles greater than 25 degrees after new snowfall especially when accompanied with winds greater than 15 mph P
112. ve you just created and open You can go through the injection parameters wizard or choose to skip this option Do not check USEPA or History Log Repeat these steps to locate and select the TN calibration curve Setting up sample table 1 YW hh From blank sample table with cursor on row 1 select insert auto generate choose method you just created select 3 samples for the number of samples box make sure start vial is 1 change sample name to DI and click next Click next on the Perform Calibrations page and Insert Control Samples page without changing any options From the Sparging Acid Addition page make sure to change the vial column related to the 3 DI samples to read 1 This will tell the instrument to pull 3 samples of DI from vial 1 Click OK WY Mh From the next blank row choose insert calibration curve choose NPOC curve you recently set up for the run click open and change the vial numbers column to 2 2 3 3 4 Click OK WY hh From the next blank row choose insert calibration curve choose TN curve you recently set up for the run click open and change the vial numbers column to 4 5 5 6 6 Click OK WY hh From the next blank row choose insert auto generate select the method you just created and add the number of samples you will run and
113. ves ice axe ice auger with spare blades snow shovel 20 ml plastic vial of Lugol s solution see recipe for Lugol s solution in Appendix E One 2 ml disposable pipette Sampling set for each sampling point 1 500 ml translucent HDPE acid washed for chemical analysis 1 60 ml translucent HDPE acid washed for SiO2 1 250 ml brown HDPE acid washed for raw unfiltered sample 1 480 ml baked borosilicate bottle for DOC DON and DOP 1 125 ml baked borosilicate bottle for monthly Loch outlet phytoplankton sample 1 30 ml syringe for pH for closed cell pH Estimated time to complete procedures For one site allow 15 minutes to drill hole in ice and 30 additional minutes to collect samples and conductivity temperature data Preparation Acid wash the pump tubing before each use instructions for acid washing on page 50 Make sure tubing is thoroughly rinsed in DI water To rinse tube run DI at full blast through it for at least 5 minutes Drain and spin as much water out of the tubing as possible so it will not freeze during the trip to sampling site Loch Vale Watershed Methods Manual 90 e Procedures 1 Go to the deepest spot of lake See bathymetric maps of lakes in Appendix D for locations Start a hole in the ice with an ice axe Finish the hole with ice auger The ice is usually about a meter thick so do not give up Sharp blades are necessary Either have them sharpened or have a new set o
114. will likely overflow during a major storm event The gage works best in the range of 2 6 inches When emptying bucket funnel waste into empty antifreeze containers most other containers will leak Containers of used antifreeze should be brought down from the station immediately in a plastic bag to protect pack against leakage Add two inches of fresh antifreeze to the empty bucket and just enough transmission fluid to cover surface area of antifreeze 0 5 cups Return bucket to scale The mechanical linkages of the Belfort are sensitive to water oil dirt dust and abuse of any kind Be careful to keep the internal area clean Do not to allow the catch bucket to overflow with precipitation see section on changing antifreeze above Calibration of the Alter shielded Belfort must be checked once a year Complete procedures are given in the Belfort manual Advanced Technology Systems Inc provided a better set of instructions in 1999 These procedures are included as loose leafs in the Belfort manual Procedures are quite tricky so if adjustment is required the process should be thoroughly understood before attempting The antifreeze mixture brought down from the weather station should be carried in antifreeze jugs and Nalgene containers not milk jugs Milk jugs are not durable enough to withstand the abuse they will receive on the trip down the trail Back at NREL funnel waste antifreeze into the five gallon metal jugs labeled Un Regulate
115. y lifting the bucket straight up Make sure the collection chamber is not dropped onto the platform This could cause irreversible damage to the load cell To empty the collection chamber funnel waste into empty antifreeze or Nalgene containers Containers of used antifreeze should be brought down from the station immediately in a plastic bag to protect against leakage Add two inches of fresh antifreeze to the empty chamber Return the collection chamber to the inside of gage housing and onto the platform Again be careful not to drop it onto the platform Make sure the alignment guideposts are inserted into the alignment ring on the bottom of the chamber Align the black mark on the collection chamber with the black alignment mark between the two LED emitters The emitters must have an unobstructed view of the detectors through the opening in the chamber Finally place the black inlet orifice over the housing and press down on the inlet orifice until it sits securely on the housing The antifreeze mixture brought down from the weather station should be carried in antifreeze jugs or Nalgene containers Back at the lab funnel waste antifreeze into the five gallon metal jugs labeled Un Regulated Contents 20 Ethylene Glycol 80 Water Include start and stop dates on the label for each jug These jugs are found in NESB A101A Dispose of waste through the CSU Hazardous Waste Office x1 6745 Refer to the NOAH IV Total Precipitation Gage
116. ypochlorite solution and make fresh 12 ml bleach and 178 ml DI water 15 Move the NOs buffer line to the buffer bottle Condition the cadmium column 1 Place the column syringe with tube to fit column open specimen cup of NOs buffer and open cup of 0 2 CuSO3 on the bench within easy reach 2 Draw about 1 ml of buffer into the syringe and remove all air bubbles from the tube Break the tubing connection on the column and elevate the connector end slightly until a drop of liquid appears at the tube end 3 Hold the syringe plunger end up and depress the plunger until a drop of buffer appears at the connector end 4 Connect the syringe to the column without introducing any air 5 Place the free end of the column into the buffer cup and slowly depress the plunger to expel the air from the free end of the column 6 Transfer the free end to the cup of CuSO and draw up about 2 4 ml 7 Depress the plunger slightly to release any tension on the liquid in the column and transfer the end to the cup of buffer Loch Vale Watershed Methods Manual 41 8 9 Draw up 3 5 ml of buffer and then depress the plunger slightly to release any tension on the liquid in the column Remove the end from the buffer place the column tubing and syringe flat on the bench then disconnect the syringe and connect the two ends of the column together 10 Take the column and syringe to the sink and rinse with DI water Put the buffer and CuSO

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