PROGRAMS AND PLANS--National Hydrologic Benchmark Network: Fiscal Year 1996--October 1, 1995 to September 30, 1996


In Reply Refer To                                       December 4, 1995
Mail Stop 412


OFFICE OF WATER QUALITY TECHNICAL MEMORANDUM NO. 96.02

Subject: PROGRAMS AND PLANS--National Hydrologic Benchmark Network: 
         Fiscal Year 1996--October 1, 1995 to September 30, 1996

This memorandum contains an outline of Program status and protocol for 
operation of the Hydrologic Benchmark Network (HBN) for fiscal year (FY) 
1996. All personnel responsible for collecting HBN samples should read 
and have their own copy of this memorandum. Network data collection can 
be significantly enhanced when personnel responsible for field data 
collection are informed of changes in sample collection and processing 
procedures.

                     NETWORK OPERATIONS, FY 1996

HYDROLOGIC BENCHMARK NETWORK

Sampling frequency for all stations in the Benchmark Network will be 
QUARTERLY in FY 1996; this is subject to change depending on funding 
availability. The three stations that were discharge only 
(02178400--Tallulah River near Clayton, GA; 05014500--Swiftcurrent Creek 
at Many Glacier, MT; 06478540--Little Vermilion River near Salem, SD) are 
discontinued as part of the Benchmark Program as of October 1, 1995. 
Active stations are listed in Appendix A. Districts are encouraged to use 
the sample collection and processing protocol for filtered samples (OWQ 
Technical Memorandum 94.09) if they are equipped and ready to do so. 

Decreasing budgets and increasing costs continue to be a problem. 
Therefore, the Benchmark Program will be evaluated during FY 1996 and 
changes in the number of stations and the way they are operated are 
likely in FY 1997.

NOTES for FY 1996:

1. Field Alkalinity

The results of the National Field Quality Assurance proficiency tests 
show that field personnel continue to have problems determining 
alkalinity in the field, especially with the Hach titrator. The Hach 
titrator method for determination of alkalinity is documented in Appendix 
C. All individuals collecting Network samples should be familiar with the 
method.

2. Sediment Samples

Suspended-sediment concentration and sand-fine split are required for all 
NASQAN and Benchmark samples. Samples for sediment analysis are to be 
collected in a separate set of bottles (to be composited at the sediment 
lab), and are NOT to be taken from the churn splitter. If NAWQA samples 
are being collected at the same time as HBN samples, and a cone splitter 
is being used, the sediment sample can collected from the cone splitter. 
See Open-File Report 86-531 (Field Methods for Measurement of Fluvial 
Sediment by Edwards and Glysson) for details on collection of sediment 
samples.

3. Samplers

Tests of existing samplers to determine their acceptability for 
collection of trace-element samples have shown that all samplers, except 
the D-77 and frame samplers (with a teflon or polypropylene bottle and/or 
a teflon or Reynolds oven bag) and the DH-81 (with a teflon or 
polypropylene bottle), contaminate samples at levels that are significant 
at the microgram per liter (parts per billion) level. OWQ realizes that 
these samplers cannot accommodate all environmental conditions; the 
Instrumentation Committee (ICOM) has recommended development of 
additional, non-contaminating samplers and the Federal Interagency 
Sedimentation Project (FISP) is in the process of developing a 1-L 
non-contaminating sampler. 

All samplers being used for the collection of trace-element samples 
(including weighted-bottle samplers) are to be coated. The FISP now uses 
a Plasti-Dip coating on all new samplers. Older samplers can be recoated, 
if necessary. Contact Wayne O'Neal at FISP for more information. His 
phone number is 601-634-3735. 

4. Barometric Pressure

Barometric pressure is to be measured with a pocket altimeter-barometer 
and the value recorded on the field sheet and stored in the data base 
(parameter code 00025). Barometric pressure can be read and reported to 
the nearest 1 mm Hg, unless the barometer that is used is not 
sufficiently accurate. The barometers that are currently available from 
HIF are accurate to +/- 0.5 mm Hg. Make sure that the barometer is 
properly calibrated using the UNCORRECTED or STATION pressure that is 
obtained from the nearest National Weather Service office. Note that the 
pressure reported on radio and television is corrected to sea level.

5. Recording Field Measurement Information

The times that individual field measurements are made, the location of 
the measurements (from churn, side of stream, center of flow, point 
sample, depth-integrated sample), and the method used should be recorded 
on the field sheets. Because field measurements are often made some time 
before or after the chemical-quality sample is collected, it is important 
to note the time(s) (even though it cannot be stored in the NWIS I data 
base). Dissolved oxygen should be measured at the center of flow whenever 
possible. Use of the National Field Forms is recommended. They are 
available from the QW Service Unit in Ocala (edoc to OCALAMAN).

6. Bacteria

Every effort should be made to obtain bacteria counts in the ideal range. 
Keeping records of flow, volumes filtered, and counts in the field 
folder, and referring to them each time bacteria samples are processed 
should help in obtaining ideal counts most of the time. If counts are 
consistently low, and sediment does not interfere, volumes greater than 
100 mL can be filtered. See TWRI Book 5, Chapter A4 for correct methods 
for calculating bacteria counts. 

7. Storing Sampler Type in Data Base

In light of the concerns about potential contamination from samplers, it 
is very important that the type of sampler used be known. This 
information can be provided by storing SAMPLER TYPE under parameter code 
84164. Currently-available values for this code are given below. Because 
of the limitations of NWIS I, only the type of sampler used for 
collecting chemical samples needs to be stored. Note-- these are the 
correct codes; the codes on the National Field Form are incorrect.
84164  100.00VAN DORN SAMPLER                          
84164  110.00SEWAGE SAMPLE                             
84164  120.00VELOCITY INTEGRATED SAMPLE                
84164  125.00KEMMERER BOTTLE                           
84164 3001.00Sampler, US DH-48                         
84164 3002.00Sampler, US DH-59                         
84164 3003.00Sampler, US DH-75P                        
84164 3004.00Sampler, US DH-75Q                        
84164 3005.00Sampler, US DH-76                         
84164 3006.00Sampler, US D-43                          
84164 3007.00Sampler, US D-49                          
84164 3008.00Sampler, US D-49AL                        
84164 3009.00Sampler, US D-74                          
84164 3010.00Sampler, US D-74AL                        
84164 3011.00Sampler, US D-77                          
84164 3012.00Sampler, US P-46                          
84164 3013.00Sampler, US P-50                          
84164 3014.00Sampler, US P-61-A1                       
84164 3015.00Sampler, US P-63                          
84164 3016.00Sampler, US P-72                          
84164 3017.00Sampler, US U-59                          
84164 3018.00Sampler, US U-73                          
84164 3019.00Sampler, US PS-69                         
84164 3020.00Sampler, US PS-69TM                       
84164 3021.00Sampler, US CS-77                         
84164 3022.00Sampler, US PS-82                         
84164 3023.00Sampler, US BMH-53                        
84164 3024.00Sampler, US BMH-53TM                      
84164 3025.00Sampler, US BM-54                         
84164 3026.00Sampler, US BM-54TM                       
84164 3027.00Sampler, US BMH-60                        
84164 3028.00Sampler, US BMH-60TM                      
84164 3029.00Sampler, US RBM-80                        
84164 3030.00US DH-48 TM                               
84164 3031.00US DH-48 TM W/ TEFLON GASKET AND NOZZLE   
84164 3032.00US DH-59 TM                               
84164 3033.00US DH-59 TM W/ TEFLON GASKET AND NOZZLE   
84164 3034.00US DH-76 TM                               
84164 3035.00US DH-76 TM W/ TEFLON GASKET AND NOZZLE   
84164 3036.00US D-74 TM                                
84164 3037.00US D-74 AL-TM                             
84164 3038.00US D-74 AL-TM W/ TEFLON GASKET AND NOZZLE 
84164 3039.00US D-77 TM                                
84164 3040.00US D-77 TM MODIFIED TEFLON BAG SAMPLER    
84164 3041.00US P-61 AL-TM                             
84164 3042.00US P-61                                   
84164 3043.00US P-61 TM                                
84164 3044.00US DH-81                                  
84164 3045.00US DH-81 WITH TEFLON CAP AND NOZZLE       
84164 3050.00TEFLON BAG SAMPLER                        
84164 3060.00WEIGHTED-BOTTLE SAMPLER                   
84164 3070.00GRAB SAMPLE                               
84164 4010.00THIEF SAMPLER                             
84164 4020.00OPEN-TOP BAILER                           
84164 4025.00DOUBLE-VALVE BAILER                       
84164 4030.00SUCTION PUMP                              
84164 4035.00CENTRIFUGAL PUMP                          
84164 4040.00SUBMERSIBLE PUMP                          
84164 4041.00SUBMERSIBLE HELICAL ROTOR PUMP            
84164 4045.00SUBMERSIBLE GEAR PUMP                     
84164 4050.00SQUEEZE PUMP                              
84164 4060.00GAS RECIPROCATING PUMP                    
84164 4070.00GAS LIFT                                  
84164 4075.00PISTON PUMP                               
84164 4080.00PERISTALTIC PUMP                          
84164 4090.00JET PUMP                                  
84164 4095.00LINE-SHAFT TURBINE PUMP                   
84164 8000.00NONE                                      
84164 8010.00OTHER                                     

8. Storage of Sampling Method in Data Base

Data analysis requires as much knowledge about a sample as possible. 
Information on the method used to collect the sample is very useful. 
SAMPLING METHOD is to be stored under parameter code 82398. Values for 
this code are given below. 

   10.00EQUAL WIDTH INCREMENT (EWI)
   20.00EQUAL DISCHARGE INCREMENT (EDI)
   25.00TIMED SAMPLING INTERVAL
   30.00SINGLE VERTICAL
   40.00MULTIPLE VERTICALS
   50.00POINT SAMPLE
   60.00WEIGHTED BOTTLE
   70.00GRAB SAMPLE (DIP)
   90.00DISCHARGE INTEGRATED, CENTROID
  120.00VELOCITY INTEGRATED
 8010.00OTHER

9. Storing Sample Purpose Code in Data Base

A value for parameter code 71999 (Sample Purpose Code) is to be stored 
with all HBN samples. The following value is to be used:

        30.00 = Benchmark


Use of this code will allow identification and retrieval of Network 
samples for data analysis. If samples are collected at Benchmark stations 
for purposes other than National Network operations, the sample purpose 
code should not be 30.00.

10. Preservatives

The only preservative now required for National Network samples is nitric 
acid for the FA bottle. For schedules 176 and 177, The 1-mL glass or 
teflon ampoules containing ultrapure nitric acid are to be used. Handle 
ampoules carefully and dispose of them according to the method outlined 
in OWQ Tech Memos 90.01 and 92.11. This will reduce potential sample 
contamination. If a sample processing chamber is being used, the nitric 
acid preservation can be done in the chamber after all sample processing 
is completed. The chamber bag should then be disposed of.


11. Shipping Samples

Bottles for nutrient analyses (RCC and FCC -- 125 mL brown bottles) are 
to be shipped to the National Water Quality Laboratory in a cooler with 
plenty of fresh ice. The cooler should be lined with a plastic bag that 
is then tied or sealed at the top to prevent leakage. The nutrient 
samples are to be shipped to the lab immediately after sample collection, 
preferably from the field, by overnight delivery. The Analytical Services 
Request Form should be sealed in a zip-lock bag and included in the 
cooler (taped to the inside of the lid) with the sample bottles. A 
postcard requesting the arrival date and temperature of the sample can be 
placed in the zip-lock bag. Lab personnel will fill out the information 
and return the postcard to the District. This will enable you to 
determine that the samples remained chilled to about 4 degrees Celsius 
during shipping.

Although it is no longer necessary to separate the nutrient samples from 
other samples, all other samples can be shipped unchilled in a cooler or 
box. Make sure that each container has a separate Analytical Services 
Request Form (ASR). The latest revision of the ASR is in tablets with a 
blue cover. Books (of 50) forms can be obtained by sending edoc to 
DENSUPPL. There is no charge for the forms. Older versions of the ASR 
should not be used.

Shipping charges are paid by the Districts, either directly or billed by 
the laboratory. Information on shipping samples is contained in a 
memorandum dated September 17, 1991, from the Assistant Chief Hydrologist 
for Operations. A copy can be obtained from your District administrative 
officer.

12. Bottle Types

Following is a list of bottle types and the analyses that are done from 
each. Individuals processing Network samples should be aware of this 
information as means of preventing sample contamination. Note that the 
FAM bottle will not be required again this year.


Schedule 86 - Nutrients

     FCC - 125 mL, brown poly, filtered, chilled to 4oC

             Nitrogen, dissolved, NO2 + NO3 as N (00631)
             Nitrogen, dissolved, NH4 as N (00608)
             Nitrogen, dissolved, NO2 as N (00613)
             Phosphorus, dissolved, ortho as P (00671)
             Phosphorus, dissolved as P (00666)

     RCC - 125 mL, brown poly, chilled to 4oC
               
             Nitrogen, total, NH4 + organic as N (00625)
             Phosphorus, total as P (00665)


Schedule 1703 - Radiochemicals

     FAR - 2 L poly, acid rinsed, filtered, treated with 2 mL nitric acid
                (or amount necessary to obtain pH <2)

              Radium-226, dissolved (09511)
              Uranium, dissolved, ext, LIP, FF (22703)


Schedule 176 - Physical properties, common and trace dissolved inorganic 
constituents
              
     FA - 250 mL poly, filtered, treated with 1 mL nitric acid (glass 
ampoule)
             (or amount necessary to obtain to pH <2)

              Aluminum (01106)        Molybdenum (01060)
              Barium (01005)             Nickel (01065)
              Calcium (00915)           Potassium (00935)
              Cobalt (01035)             Selenium (01145)
              Iron (01046)                 Silver (01075)
              Lithium (01130)            Sodium (00930)
              Magnesium (00925)     Strontium (01080)
              Manganese (01056)     Vanadium (01085)


     FU - 500 mL poly, filtered, untreated

              Silica (00955)
              Sulfate (00945)
              Fluoride (00950)
              Chloride (00940)
              ROE at 180 C (70300)

     LC00050 - 125 mL poly, untreated

              Turbidity, NTU (00076)

     RU - 250 mL poly, untreated

              pH, laboratory (00403)
              Specific conductance, laboratory (90095)
              Alkalinity, total, laboratory (00417)


Schedule 177 - Physical properties, common and trace dissolved inorganic 
constituents
               
     FA - 500 mL poly, filtered, treated with 2 mL nitric acid (glass 
ampoule)
             (or amount necessary to obtain to pH <2)

              Aluminum (01106)      Molybdenum (01060)
              Barium (01005)        Nickel (01065)
              Calcium (00915)       Potassium (00935)
              Cobalt (01035)        Selenium (01145)
              Iron (01046)          Silver (01075)
              Lithium (01130)       Sodium (00930)
              Magnesium (00925)     Strontium (01080)
              Manganese (01056)     Vanadium (01085)


     FU - 500 mL poly, filtered, untreated

              Silica (00955)
              Sulfate (00945)
              Fluoride (00950)
              Chloride (00940)
              ROE at 180 C (70300)

     LC0050 - 125 mL poly, untreated

              Turbidity, NTU (00076)

     RU - 250 mL poly, untreated

              pH, laboratory (00403)
              Specific conductance, laboratory (90095)
              Alkalinity, total, laboratory (00417)


13. Water-Quality Field Techniques References

Below is a list of Office of Water Quality Technical Memoranda and 
additional references that describe the techniques that are to be used in 
the collection and processing of water-quality samples. These references 
should be available to all people collecting water- quality samples.

Office of Water-Quality Technical Memoranda

Number    Date     Subject

70.07   11-28-69   Quality control of water analyses: water-quality 
service units and mobile laboratories

71.04    1-13-71   Methods for collection and analysis of water samples
                   for dissolved minerals and gases (TWRI book 5, Ch. A1)

71.05    3-18-71   Sampling and analysis of water-quality constituents
                   associated with suspended solids

71.09    6-22-71   Guidelines for sampling and analysis of water-quality
                   constituents associated with solids

72.04   11-08-71   Instructions for use of sediment samplers for the
                   collection of samples to be analyzed for organic
                   substances

72.09    1-05-72   Preservation of water samples for chemical analysis
                   (superceded by 80.26)

72.13    2-28-72   Computations of fluvial-sediment discharge (TWRI book
                   5, Ch. C3)

73.02    9-11-72   Field determinations (superceded by 82.06)

73.07   10-26-72   Teflon sample splitters and plastic sleeves

73.16    4-23-73   Sampling procedures and problems in determining
                   pesticide residues in the hydrologic environment

74.11    2-28-74   Field instruction for NASQAN

75.09   12-26-74   Acceptable methods for collection of water-quality
                   data

75.15    3-13-75   Publication of water temperatures

75.25    6-19-75   Guidelines on sampling and statistical methodologies
                   for ambient pesticide monitoring

76.03  10-14-75    Water-quality field instrumentation

76.17    5-12-76   Sampling mixtures of water and sediment in streams

76.24-T  8-16-76   Sample splitter for water-sediment samples

77.01   12-13-76   Sample splitter for water-sediment samples (cleaning
                   instructions) (supplements 76.24T)

77.03    1-17-77   DH-75 suspended-sediment sampler

77.07    4-06-77   Guidelines for application of Helley-Smith bedload
                   sampler

77.08    5-06-77   Relationship of sediment discharge to streamflow

78.03    1-17-78   Churn splitters (supplements 76.24T and 77.01)

78.06    4-05-78   Field filtering of water samples for chemical analyses

78.13    7-10-78   Microbiological monitoring for water-quality
                   assessment

79.06   12-11-78   Shipment of hazardous material

79.08    3-07-79   Modification of the field chamber for the YSI
                   dissolved oxygen meter

79.10    3-14-79   Recommended procedures for calibrating dissolved
                   oxygen meters

79.15    9-11-79   Data networks; unique number identification for
                   federally funded stations

79.16    9-28-79   Quality assurance of temperature measurements

79.17   10-02-79   Use of Helley-Smith bedload sampler

80.03   11-19-79   Samplers--P-61 and P-63 point-integrating sediment
                   samplers

80.06    1-24-80   Color-coded nozzles for sediment samplers

80.07    2-05-80   Use of Helley-Smith sampler

80.16    6-02-80   Quality assurance program for sediment laboratories

80.17    7-03-80   New sample splitter for water-quality samples (cone
                   splitter)

80.18    6-13-80   Samplers-- problems with installation of plastic
                   nozzles on samplers

80.26    9-19-80   Preservation of nutrient samples by addition of
                   mercuric chloride

80.30    9-23-80   Significance of bottom material data in evaluating
                   water quality

81.02   10-16-80   Operation and availability-- D-77 water-quality
                   sampler

81.08    2-10-81   Electrodes for pH measurement in low-conductivity
                   waters

81.11    5-08-81   New tables of dissolved oxygen saturation values

82.01   10-27-81   Collecting water samples for stable isotope analysis

82.05   12-11-81   Provisional method for carbonate, dissolved;
                   bicarbonate, dissolved; and carbonate alkalinity,
                   dissolved; electrometric titration, incremental, field

82.06    1-22-82   Policy on publishing constituents with both field and
                   laboratory values

84.04   11-30-83   Technical information: briefing paper on mercury

84.18    9-28-84   Preservation and shipment of water samples for
                   determination of mercury

87.03    2-12-87   pH measurement in low conductivity waters

90.01   10-03-89   Sample preservation and ampoule disposal

90.07    2-02-90   Contamination from D-77 sampler equipped with
                   solenoid-actuated valves

91.01   10-29-90   "Methods for collection and analysis of aquatic
                   biological and microbiological samples," by L.J.
                   Britton and P.E. Greeson, editors, Techniques
                   Water-Resources Investigations (TWRI), Book 5, 
                   Chapter A4

91.02   12-05-90   "Methods for collection and processing of
                   surface-water and bed-material samples for physical
                   and chemical analysis," by Janice R. Ward and C.
                   Albert Harr, editors, Open-File Report 90-140

91.04    2-08-91   Office of Water Quality electronic memorandum system

91.08    8-07-91   "A primer on sediment-trace element chemistry" 
                   (second edition), by Arthur J. Horowitz

91.09    8-27-91   "Filtration of water-sediment samples for
                    determination of organic compounds," by Mark W.
                    Sandstrom

91.10    9-30-91   Dissolved trace element data

92.01   12-20-91   Distilled/deionized water for District operations

92.02   12-20-91   Field preparation of containers for aqueous samples

92.04    3-20-92   Revised statement regarding dissolved trace-element
                   data production

92.05    3-20-92   Quality of existing dissolved trace-element data

92.06   3-20-92    Report of committee on sample shipping integrity and
                   cost

92.08    3-27-92   Nutrient sample size reduction

92.10    7-13-92   Phosphorus methods and the quality of phosphorus data

92.11     7-16-92   Return of spent mercury and dichromate ampoules to
                    the National Water Quality Laboratory

92.12   7-17-92    Trace-element concentrations in deionized water
                   processed through selected surface-water samplers:
                   Study results and implications

92.13   7-17-92    Trace-element contamination: Findings of studies on
                   the cleaning of membrane filters and filtration
                   systems

93.01   10-05-92   National Water-Quality Networks: Fiscal year
                   1993--October 1, 1992 to September 30, 1993

93.03   10-29-92   Dissolved trace-element data

93.04   12-02-92   Discontinuation of the NWQL determinations for "total"
                   nitrite, "total" nitrite plus nitrate, "total"
                   ammonia, and "total" orthophosphate (using the
                   four-channel analyzer)

93.05    1-21-93   Evaluation of capsule filters

93.06    2-19-93   Trace-element contamination--Findings of study on the
                   cleaning of sampler caps, nozzles, bottles, and bags
                   for trace-element work at the part-per-billion level

93.09    4-16-93   Sample splitting devices

93.10    4-91-93   (1) Disposal of petri dishes containing bacteria
                   media, and (2) aspergillus

93.11   7-15-93    Implementation of the protocol for collecting and
                   processing surface-water samples for low-level
                   inorganic analyses

94.02  11-22-93   Discontinuance of field use of mercury liquid-in-glass
                  thermometers

94.06   1- 3-94   New custom analysis schedule (172) for blanks

94.09   1-28-94  Revision of new Division protocol for collecting and
                 processing surface-water samples for low-level inorganic
                 analyses

94.12   4-20-94  Changes in schedule 172

94.13   4-21-94  Evaluation of the churn splitter for inclusion in the
                 Division protocol for the collection and processing of
                 surface-water samples for subsequent determination of
                 trace elements, nutrients, and major ions in filtered
                 water

94.16   8- 5-94  New preservation techniques for nutrient samples


Additional References

Barnes, Ivan, 1964, Field measurement of alkalinity and pH: 
  U.S. Geological Survey Water-Supply Paper 1535-H, 17 p.

Britton, L.J., and Greeson, P.E., eds, 1989, Methods for collection and
  analysis of aquatic biological and microbiological samples: 
  U.S. Geological Survey Techniques of  Water Resources Investigations,
  book 5, chap. A4, 363 p.

Busenberg, Eurybiades, and Plummer, L.N., 1987, pH measurement of
  low-conductivity waters:  U.S. Geological Survey Water-Resources
  Investigations Report 87-4060, 22 p.

Edwards, T.K., and Glysson, G.D., 1988, Field methods for measurement of
  fluvial sediment: U.S. Geological Survey Open-File Report 86-531, 
  188 p.

Guy, H.P., and Norman, V.M., 1970, Field methods for measurement of
  fluvial sediment: U.S. Geological Survey Techniques of Water Resources
  Investigations, book 3, chap. C2, 59 p.

Hem, J.D., 1985, Study and interpretation of chemical characteristics of
  natural water: U.S. Geological Survey Water-Supply Paper 2254, 263 p.

Stevens, H.H., Jr., Ficke, J.F., and Smoot, G.F., 1975, Water
  temperature--influential factors, field measurement, and data
  presentation: U.S. Geological Survey Techniques of Water Resources
  Investigations, book 1, chap. D1, 65 p.

Sylvester, M.A., Kister, L.R., and Garrett, W.B.,eds, 1990, Guidelines
  for the collection, treatment, and analysis of water samples--U.S.
  Geological Survey Western Region field manual: U.S. Geological Survey,
  Western Region, internal report, 144 p.

Ward, J.R., and Harr, C.A., eds, 1990, Methods for collection and
  processing of surface-water and bed-material samples for physical and
  chemical analyses: U.S. Geological Survey Open-File Report 90-140, 
  71 p.

Wells, F.C., Gibbons, W.J., and Dorsey, M.E., 1990, Guidelines for
  collection and field analysis of water-quality samples from streams 
  in Texas: U.S. Geological Survey Open-File Report 90-127, 79 p.

Wood, W.W., 1976, Guidelines for collection and field analysis of
  ground-water samples for selected unstable constituents: U.S.
  Geological Survey Techniques of Water Resources Investigations, book 1,
  chap. D2, 24 p.

Yurewicz, M.C., 1981, Incremental field titration of bicarbonate: U.S. 
Geological Survey Water Resources Division Bulletin, October-December 
1981, (for WRD use only), p. 8-13. 

               Collection of Representative Samples

As in past years, the Office of Water Quality reminds all field personnel 
that the collection of a representative sample is of utmost importance. 
Procedures for the collection of a representative sample are well 
documented. As part of this effort, cross-section surveys (depth and 
width) of water temperature, pH, specific conductance, dissolved oxygen, 
and suspended sediment have been required activities at each site in the 
two networks. Over a period of years the data base of such data should 
include observations for various seasons and surface-water discharges. 
Cross-section surveys should include a discharge measurement so that each 
measured constituent can be associated with a weighted discharge value. 
The results of cross-section surveys should be stored in the 
WATSTORE/NWIS Water-Quality File. When entering such data, be sure to 
enter the cross section location - WATSTORE code 00009, CROSS-SECTION 
LOCATION, FEET FROM LEFT BANK, LOOKING DOWNSTREAM.

Contamination of trace-element samples in the field has become an 
important issue as laboratory methods continue to improve and reporting 
limits are lowered. Therefore, all individuals who are collecting 
water-quality samples need to be aware of the importance of keeping 
equipment and field vehicles clean and of using proper care when 
collecting and handling samples. All sampling equipment is to be 
thoroughly cleaned (the cleaning procedures are described in detail in 
Appendix D of this memo). Churn splitters and other equipment are to be 
stored in sealed plastic bags after they are cleaned and until they are 
used. Sample water should be poured carefully into the churn so that the 
water does not come into contact with hands or the cover of the churn. 
The churn is to be kept covered, when water is not being added to it (or 
modify the churn splitter by adding a cappable funnel as described in OWQ 
Technical Memorandum 94.09). In order to keep dirt off the outside of the 
churn, and dust from getting into the churn, it should be kept in a 
plastic bag which is opened only to allow access to the churn for 
emptying the sampler bottle. The "clean hands/dirty hands" technique is 
suggested where the "clean hands" person wears disposable gloves and 
handles only the sample bottle and the "dirty hands" person handles the 
sampling equipment (metal part of the sampler, reel, etc.) The "clean 
hands" person is careful not to touch metal objects or anything that 
could contaminate the sample, and changes gloves whenever this type of 
contact occurs.

Sample processing should be done inside the vehicle and away from dust 
and exhaust. Best results are obtained when samples are processed in a 
clean, metal-free chamber (a glove box or chamber built from wood and 
plexiglass). All bottles are to be stored in clean areas and uncapped 
bottles (other than the untreated bottles) should be discarded. Untreated 
bottles are to be rinsed with sample water (filtered water for filtered 
samples and unfiltered water for unfiltered samples), as described in OWQ 
Technical Memorandum 92.02. Disposable gloves are to be worn when 
handling preservatives (and changed between different types of 
preservatives), and when processing bacteria samples.

Periods for Sample Collection

The table below indicates the time periods for sample collection for 
stations sampled quarterly (four times per year). Sample collection 
frequencies for FY 1995 are shown in Appendix A. In order for the data to 
meet the objectives of the Benchmark program, it is important that the 
sampling schedule be adhered to.


                           QUARTERLY STATIONS 

first sample                   OCTOBER-NOVEMBER-DECEMBER

second sample                  JANUARY-FEBRUARY-MARCH

third sample                   APRIL-MAY-JUNE

fourth sample                  JULY-AUGUST-SEPTEMBER

Use of ICP

The inductively-coupled plasma (ICP) procedure is used for the analysis 
of selected dissolved common and trace inorganic constituents. The ICP 
procedure is not to be used whenever the specific conductance is greater 
than 2,000 uS/cm because the detection limits become greater. Schedule 
177 will be used in lieu of schedule 176 whenever the specific 
conductance is greater than 2,000 uS/cm. Based upon historical specific 
conductance data for each NASQAN and HBN Station, the percentage of 
samples with specific conductance values equal to or greater than 2,000 
uS/cm was computed and is given in Appendix A under the right-hand 
heading "PROBABILITY (%) THAT SPECIFIC CONDUCTANCE WILL BE EQUAL TO OR 
GREATER THAN 2,000 US/CM." These probabilities indicate the expected 
frequency of use schedule 177 will get at each site over a long period of 
time. Determination of specifically which schedule to request for a 
sample is based on the specific conductance value measured at the time of 
sampling.

Only schedule 176 is authorized for stations with zero probability of the 
specific conductance exceeding 2,000 uS/cm. Because of the uncertainty 
involved in predicting the number of samples that will exceed 2,000 
uS/cm, both schedule 176 and 177 are authorized for four uses at HBN 
stations where the value given in the right-hand column of Appendix A is 
greater than zero. The actual number of usages authorized between 
schedules 176 and 177 is however four, not eight.

District Water-Quality Specialists have the authority and responsibility 
to request schedules 176 versus schedule 177. Because use of schedule 176 
versus 177 is dependent solely upon the specific conductance of the 
sample, District Water-Quality Specialists should ensure that all field 
personnel are aware that a field specific conductance measurement is 
absolutely necessary whenever schedule 176 or 177 is to be utilized.

Unique Numbers

Districts are reminded that all samples (excluding suspended-sediment 
samples which are analyzed in District sediment laboratories for particle 
size and concentration) are to be sent to the U.S. Geological Survey 
National Water-Quality Laboratory in Arvada, CO, with appropriate 
National Laboratory unique numbers. Unique numbers are described in 
Quality of Water Branch Technical Memorandum 79.15 and can be obtained by 
station number through the SPN system on DCOLKA. New unique numbers are 
established at the beginning of the each water year and are to be used 
until September 30 of each water year. Personnel collecting HBN samples 
should keep a current listing of the unique numbers in their field 
folders.

Any National-Networks sample processed by the National Water Quality 
Laboratory without a unique number will result in the analytical costs 
being billed to the District default account instead of the appropriate 
National-Networks account. Correcting such billing errors after they 
occur requires a memorandum to the Coordinator, National Hydrologic 
Benchmark Program.



Analytical Services Request Form

Although the unique number, date, and time are all that are required on 
the Analytical Services Request Form, additional information such as 
station name, special sampling conditions, National-Networks program 
(Benchmark), etc., are helpful to the National Water Quality Laboratory 
personnel and District personnel processing the analytical results. All 
information coded in the comments section of the Analytical Services 
Request Form is stored in the Water-Quality File.

Uniform Data-Collection Program

Districts are reminded of the importance to ensure that all HBN samples 
be analyzed for the same measurements as specified later in this 
memorandum. In particular, all field measurements specified have to be 
done for every sample.


            HYDROLOGIC BENCHMARK DATA COLLECTION PROGRAM

Hydrologic Benchmark Network stations to be operated in FY 1996 are 
listed in Appendix A. Rain gages were installed at a number of stations 
during FY 1994. The rain gages should collect precipitation data at the 
same frequency as the stream gage. Changes in locations of sampling sites 
must be approved by the National Networks Coordinator.

All HBN stations will be sampled quarterly. Schedule 1904 will no longer 
be used. Analysis of radiochemicals will be on a semiannual basis (1 
high-flow and 1 low-flow sample).

The specific conductance is likely to exceed 2,000 uS/cm at only one HBN 
station - the Bear Den Creek at Mandaree, ND (06332515). Therefore, this 
station may require schedule 177 for analysis of quarterly dissolved 
common and trace inorganic constituents. All other stations will require 
use of schedule 176 for analysis of these constituents.

HBN Sampling Schedule for FY 1996

Please notify the Office of Water Quality if the District responsible for 
collection of samples for any HBN station has changed recently and is 
therefore incorrectly listed in Appendix A.

Hydrologic Benchmark Network Sampling Schedule

4 per year - Field Measurements:
        Instantaneous discharge (WATSTORE Code 0006l)
        Specific conductance (WATSTORE Code 00095)
        Water temperature, degrees C (WATSTORE Code 00010)
        Barometric pressure, mm Hg (WATSTORE Code 00025)
        pH (WATSTORE Code 00400)
        Carbonate, water, dissolved, mg/L (WATSTORE Code 00452)
        Bicarbonate, water, dissolved, mg/L (WATSTORE Code 00453)
        Alkalinity, water, dissolved, as CaCO3, mg/L
          (WATSTORE Code 39086)
        Hydroxide, water, dissolved, mg/L (WATSTORE Code 71834)
        Dissolved oxygen (WATSTORE 00300)
        Fecal coliform bacteria, 0.7 um (WATSTORE Code 31625)
        Fecal streptococcal bacteria, 0.45 um (WATSTORE Code 31673)
4 per year - Suspended sediment:
                Concentration (WATSTORE Code 80154)
                Percent finer than 0.062 mm, sieve diameter
                  (WATSTORE Code 70331)
4 per year - Nutrients, lab schedule 86
4 per year - Physical properties, common and trace dissolved
                 inorganic constituents: lab schedule 176
2 per year - Radiochemicals, lab schedule 1703

Cross-section surveys (depth and width) of temperature, pH, specific 
conductance, dissolved oxygen, and suspended-sediment concentration as 
needed to document cross-section homogeneity.

If any information in this memorandum prompts questions or comments, 
please call Kathy Fitzgerald whose current number is (703) 648-6902.



                                Janice R. Ward
                                for David A. Rickert

Attachments

This memorandum supersedes OWQ Technical Memorandum 95.01.

Distribution: A, B, S, FO, PO

Key Words: water quality, networks, sampling, Benchmark, FY 1996





                              APPENDIX A

This appendix contains the listing by District of all HBN stations. 
Copies of the appendix may be retrieved via anonymous ftp by issuing the 
following commands:


ftp 130.11.50.18
login: anonymous
password: your userid
cd pub/benchmark
type binary
get appendix.a.96.fm/
bye


This is a Framemaker 4.0 file. It must be opened in Framemaker to be 
printed. Choose the landscape option for printing.


                             APPENDIX B

 NUTRIENTS


      SCHEDULE   86 WN  OWNER:NQ
       COST:   77.80 CALCULATED

 LAB   WATSTORE
 CODE  CODE        INCLUDED PARAMETERS

 1688  00625    A  NITR. NH4+ORG AS N WWR
 1685  00666    B  PHOSPHORUS, DIS. JKA
 1686  00665    B  PHOSPHORUS, TOTAL JKA
 0160  00613    B  NITR DIS  NO2 AS   N
 0162  00671    B  PHOS DIS ORTHO  AS P
 0301  00608    B  NITR DISS  NH4  AS N
 0228  00631    B  NITR DIS NO2+NO3  -N

 REQUIRES

 0125      ml      OF  FCC
 0125      ml      OF  RCC


                           RADIOCHEMICALS

      SCHEDULE 1703 WR  OWNER:NQ
       COST:  305.00 FIXED

 LAB   WATSTORE
 CODE  CODE        INCLUDED PARAMETERS

 0794  09511    B  RADIUM-226, DISS. RN
 1386  22703    E  U.DIS,EXT,LIP,FF

 REQUIRES

 0002      liters  OF  FAR


PHYSICAL PROPERTIES, COMMON AND TRACE DISSOLVED INORGANIC
CONSTITUENTS

      SCHEDULE  176 WI  OWNER:NQ
       COST:  256.30 FIXED

 LAB   WATSTORE
 CODE  CODE        INCLUDED PARAMETERS

 0027  70300    A  ROE, DISS. AT 180 C
 0050  00076    A  TURBIDITY      (NTU)
 0054  00935    B  POTASSIUM, DISSOLVED
 0068  00403    A  PH (LABORATORY)
 0069  90095    A  SP. CONDUCTANCE LAB
 0070  90410    A  ALK TOT LAB.  CACO3
 0087  01145    A  SELENIUM, DISSOLVED
 0641  01005    C  BARIUM, DISSOLVED
 0644  01035    C  COBALT, DISSOLV.
 0645  01046    D  IRON, DISSOLV.
 0648  01056    C  MANGANESE, DISSOLVED
 0649  01060    A  MOLYBDENUM, DISS.
 0652  01080    B  STRONTIUM, DISSOLVED
 0653  01085    B  VANADIUM, DISSOLVED
 0659  00915    D  CALCIUM, DISSOLVED
 0663  00925    C  MAGNESIUM, DISSOLVED
 0664  01130    B  LITHIUM, DISSOLVED
 0667  00955    D  SILICA, DISSOLVED
 0675  00930    C  SODIUM, DISSOLVED
 1284  01106    E  ALUMINUM-DIS-DCP
 1552  01075    F  SILVER GFAA DIS
 1562  01065    F  NICKEL GFAA DIS
 1571  00940    J  CHLORIDE DIS IC
 1572  00945    G  SULFATE DIS IC
 1573  00950    E  FLUORIDE DIS IC

 REQUIRES
 0250      ml      OF  FA
 0250      ml      OF  RU
 0125      ml      OF  LC0050
 0500      ml      OF  FU


      SCHEDULE  177 WI  OWNER:NQ
       COST:  318.40 CALCULATED

 LAB   WATSTORE
 CODE  CODE        INCLUDED PARAMETERS

 0007  01005    B  BARIUM, DIS.
 0012  00915    C  CALCIUM, DISSOLV.
 0027  70300    A  ROE, DISS. AT 180 C
 0039  01130    A  LITHIUM, DISSOLV.
 0040  00925    B  MAGNESIUM, DISSOLV.
 0042  01056    A  MANGANESE, DISSOLV.
 0050  00076    A  TURBIDITY      (NTU)
 0054  00935    B  POTASSIUM, DISSOLVED
 0056  00955    C  SILICA, DIS.
 0059  00930    B  SODIUM, DIS.
 0062  01080    A  STRONTIUM, DIS.
 0068  00403    A  PH (LABORATORY)
 0069  90095    A  SP. CONDUCTANCE LAB
 0070  90410    A  ALK TOT LAB.  CACO3
 0087  01145    A  SELENIUM, DISSOLVED
 0110  01060    B  MOLYBDENUM, DISSOLV.
 0172  01046    C  IRON, DIS.
 1210  01085    D  VANADIUM, DIS. AUTO.
 1284  01106    E  ALUMINUM-DIS-DCP
 1552  01075    F  SILVER GFAA DIS
 1556  01035    F  COBALT GFAA DIS
 1562  01065    F  NICKEL GFAA DIS
 1571  00940    J  CHLORIDE DIS IC
 1572  00945    G  SULFATE DIS IC
 1573  00950    E  FLUORIDE DIS IC

 REQUIRES
 0500      ml      OF  FA
 0250      ml      OF  RU
 0125      ml      OF  LC0050
 0500      ml      OF  FU


                                APPENDIX C


                ALKALINITY - INCREMENTAL TITRATION METHOD
                             Hach Titrator


INTRODUCTION

Alkalinity is a measure of the buffering capacity of water against acid. 
Degasification, precipitation, and other chemical and physical reactions 
may cause the concentrations of carbonate and bicarbonate to change 
substantially within several hours or even minutes after sample 
collection. Consequently, field values for carbonate and bicarbonate or 
alkalinity usually are more reliable than values obtained in the 
laboratory (Wells and others, 1990).

Particulates can take up some strong acid by dissolution, adsorption, or 
ion exchange and, thereby, cause anomalously high measurements. For this 
reason, filtration through a 0.45 micron pore-size filter is required. In 
order to prevent contamination by wind-borne dust and loss of carbon 
dioxide due to warming by the sun, the analysis should be done in an 
enclosed vehicle (OWQ Technical Memorandum 82.05).

APPARATUS

1. pH meter with combination pH probe or equivalent.
2. Hach digital titrator.
3. Titrant acid cartridges (0.16 and 1.6 N) with straight- or bent-tube   
   delivery tubes. 
     (NOTE: Clear delivery tubes are now available from Ocala)
4. Magnetic stirrer.
5. Deionized water.
6. 50 mL and 100-mL volumetric pipets.


METHOD

1. Select the appropriate strength titrant, 0.1600 Normal (N) or 1.600N 
sulfuric acid, and sample volume from the following table, based on the 
expected alkalinity. Record the acid normality and sample volume on the 
field sheet.


       Expected Alkalinity         Sample Volume         Acid Normality

          <20                            100                 0.1600
          20-50                           50                 0.1600
          50-150                         100                 1.600
          >150                            50                 1.600


NOTE: The volumes and acid normalities in the above table are guidelines
      only. Inflection points will be better defined by using the 0.1600
      N acid.

2. Assemble the digital titrator:
    a) Insert the appropriate cartridge into the titrator and turning it
       1/4 turn to lock it in position.
    b) Remove the vinyl cap and insert a delivery tube into the cartridge
       tip. Delivery tubes cannot be interchanged between different
       normality cartridges and should be identified to avoid
       cross-contamination.
    c) Flush the tube by turning the delivery knob to release some of the
       titrant into a waste container. Make sure that a sufficient amount
       is released to assure that there are no bubbles or water in the
       tube.
    d) Gently blot any droplets that adhere to the end of the tube and 
       set the digital counter reading to ZERO.

3. Use a clean volumetric pipet or cylinder, rinse with sample water, and 
measure the appropriate sample volume into a clean beaker containing a 
Teflon-coated stirring bar.

4. Place rinsed pH probe (previously rinsed with sample water) into the 
sample and place the beaker on a magnetic stirrer.

5. Turn on stirrer and adjust stirring rate to LOW. Sample should be 
GENTLY stirred throughout the titration. Turn on pH meter, allow reading 
to stabilize and then read and record the initial pH value.

6. If sample pH is less than 8.3, then skip the next step (7).

7. If sample pH is greater than 8.3, add sulfuric acid by small 
increments (1 to 3 digital counts at a time) until the pH is less than 
8.0. The tip of the delivery tube should be below the sample surface 
(keep the tube clean to avoid contamination of the sample). Allow 15-20 
seconds for equilibration between incremental additions of acid. Record 
pH and digital counter reading after each addition of acid.

8. Titrate rapidly to pH 5.0 (5.5 for alkalinities of <20 mg/L). The tip 
of the delivery tube should be below the sample surface (keep the tube 
clean to avoid contamination of the sample). Allow 15-20 seconds for 
equilibration and record the digital counter reading.
 
9. From pH 5.0 (5.5) to 4.0, add acid by small increments (1 to 3 digital 
units at a time). Allow 15-20 seconds for equilibration between 
incremental additions of acid and record pH and digital counter reading 
after each addition of acid.
    
10. Calculations: (initial calculations should be done in the field)
     
     (a) Calculate the change in pH and the change in counter numbers and
         record these values on the field sheet.

     (b) Divide each change in pH by the change in the counter numbers
         and record the results on the field sheet.

     (c) The endpoints are the counter numbers where the maximum rates of
         change in pH per counter number increments occur. If a tie for
         the end point occurs, choose the last one (the one with the
         lower pH).

     (d) Calculate carbonate (00452).

           CO3 (mg/L as CO3) = A x F1/mL sample

     (e) Calculate bicarbonate (00453).

           HCO3 (mg/L as HCO3) = [B - 2(A)] x F2/mL sample

     (f) Calculate total alkalinity (39086).

           Total Alkalinity = B x F3/mL sample

     where:

     A = digital count from initial pH to endpoint near 8.3
     B = digital count from initial pH to endpoint near 4.5


                  0.1600N 1.600N
              F1     12.0   120
              F2     12.2   122
              F3     10.0   100


After completing the titration, remove the cartridge from the titrator 
and replace the vinyl cap immediately to avoid exposure of the contents 
to the air. Rinse the delivery tube with distilled water and blow out the 
remaining water with a syringe to avoid starting the next titration with 
water. Store the delivery tubes in a clean plastic bag.

REPORTING

Report total alkalinity, carbonate, and bicarbonate concentrations as 
follows: less than 1,000 mg/L, to whole numbers; 1,000 mg/L and above, 
three significant figures.

REFERENCES

Barnes, Ivan, 1964, Field measurement of alkalinity and pH: 
  U.S. Geological Survey Water-Supply Paper 1535-H, 17 p.

Quality Water Service Unit, 1990, Water-quality field techniques: 
  U.S. Geological Survey, Florida District, internal document, 164 p.

Sylvester, M.A., Kister, L.R., and Garrett, W.B., eds, 1990, Guidelines
  for the collection, treatment, and analysis of water samples--U.S.
  Geological Survey Western Region field manual: U.S. Geological Survey,
  Western Region, internal document, 144 p.

Wells, F.C., Gibbons, W.J., and Dorsey, M.E., 1990, Guidelines for
  collection and field analysis of water-quality samples from streams 
  in Texas: U.S. Geological Survey Open-File Report 90-127, 79p.

Branch of Water Quality Technical Memorandum 82.05: December 11, 1981.