IOP:012.4C IOP:012.3F IOP:012.5G IOP:012.0H. Spectrophotometers

IOP:012.4C IOP:012.3F IOP:012.5G IOP:012.0H Spectrophotometers IOP:012.4C Hach DR/2010 Spectrophotometer IOP:012.4C U.S. Fish and Wildlife Service...
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IOP:012.4C IOP:012.3F IOP:012.5G IOP:012.0H Spectrophotometers

IOP:012.4C Hach DR/2010 Spectrophotometer

IOP:012.4C U.S. Fish and Wildlife Service Marquette Biological Station 3090 Wright Street Marquette, Michigan 49855 U.S.A.

December 18, 2012

and U.S. Fish and Wildlife Service Ludington Biological Station 229 South Jebavy Drive Ludington, Michigan 49431 U.S.A. and Department of Fisheries and Oceans Sea Lamprey Control Centre 1219 Queen Street East Sault Ste. Marie, Ontario P6A 2E5 Canada

INSTRUMENT OPERATING PROCEDURE INSTRUMENT: Spectrophotometer MODEL: DR/2010 MANUFACTURER: Hach SERIAL AND PROPERTY NOS: Model number

Location

Serial number

Property number

Identifying number

DR/2010

MBS

000900019635

1522

#3

DR/2010

MBS

000900019687

1523

#4

PRECAUTIONS: POTENTIAL INTERFERENCES None listed in manual SAFETY No special safety precautions

PROCEDURES: I.

Background A.

The Hach DR/2010, the factory-suggested replacement for the DR/2000, is capable of direct readout of concentrations of TFM, however, this option does not support the requirements of methods of analysis developed for line-powered spectrophotometers.

B.

The procedures for analysis with the DR/2010 closely parallel those used with the Sequoia-Turner model 340 and Turner model SP-830 spectrophotometers.

C.

II.

1.

Similarities a. Pre-formulated standards with concentrations of 0, 4, 8, and 12 mg/L TFM are used. b. The slope of the instrument response is determined through measurement of the absorbance of the TFM standards. c. Base/Acid measurements of background absorbance are conducted to assure accuracy of analyses. d. Water samples are buffered to pH ~9.0 before measurement of absorbance. e. Water samples are filtered before measurement of absorbance. f. Record keeping requirements are the same.

2.

Differences a. The instrument wavelength setting is 400 nm versus 395 nm for dedicated, line-powered spectrophotometers. b. Water samples normally are not heated before analysis.

The accuracy of measurements depends to some degree on the comparative absorbencies of the optically-matched sample cells in each DR/2010 kit. The method of data interpretation used during TFM analyses demands that special attention is given to compensation for poor matches when they cannot be avoided.

Preparation A.

Set up the spectrophotometer in a shaded location. Always use the black outdoor light shield when making absorbance measurements.

B.

Use line power if available, however, use of this instrument is normally reserved for situations in which line power is not available.

C.

After all peripheral equipment for sample preparation is ready, press the POWER button. The instrument will conduct internal tests and will display SELF-TEST.

D.

When ENTER PROGRAM # is displayed press the SHIFT key and then the ABS key. P 0 ABS is displayed and the instrument is then operating in the absorbance mode.

E.

Adjust the wavelength control knob until the display indicates a wavelength of 400 nm. Always approach the desired wavelength from the high side for best accuracy and repeatability.

F.

Match the 25 mL sample cells 1.

Open a new 0.0 mg/L standard and rinse and fill two factory-matched 25 mL sample cells.

III.

IV.

2.

Place the first cell in the sample cell holder with the 25 mL mark facing to the right. Press the ZERO key. ZEROING will be displayed (flashing) until the instrument is zero calibrated. 0.000 ABS will appear on the display when the instrument is zero calibrated.

3.

Place the second cell in the sample cell holder with the 25 mL mark facing to the right. Press the READ key.

4.

The sample cell should produce an absorbance + less than 0.008 (considered an acceptable match; maximum ~ 0.05 mg/L error). If the difference is greater, clean the cell or check the absorbencies of spare sets of matched cells. If an acceptable match cannot be obtained and another matched set is not available, note the absorbance difference so absorbencies of standards can be corrected. The cell with the lesser absorbance is used as the blank.

Calibration–standards A.

Open the remainder of the new set of TFM standards. Do not allow the standards to sit in sunlight while in use and store the standards in the dark. If the standards are very cold (apt to fog), warm them in a water bath or in the hands.

B.

Insert the cuvette that contains the blank and press zero. Wait until 0.000 ABS is displayed.

C.

Insert the 0.0 mg/L TFM standard and press READ. The 0.0 standard may produce a reading other than 0.000 because of an imperfect match of cuvettes. If the cells are not suitably matched, subtract the difference due to cell mismatch (noted above) and record in log book.

D.

Again insert the cuvette containing the blank and press zero. Wait until 0.000 ABS is displayed, insert the 4.0 mg/L standard, and press the READ button. Again adjust the result for differences in absorbance between blank and sample cells if necessary. Record the corrected absorbance in the instrument log book. Repeat the procedure with 8.0 and 12.0 mg/L TFM standards

E.

Divide the recorded absorbance of each standard by the concentration of TFM (mg/L; 4.0, 8.0, and 12.0). Average the results and record the mean in the log book and on the analysis data sheet.

Calibration–stream water sample A.

Measure the background absorbance and B/A ratio of the stream water (TOP:018.x). Do not interchange the cells. Always use the same cell for the 0.0 standard (blank).

B.

Prepare the TFM-free water sample for analysis 1.

Add 1 mL sodium tetraborate buffer to a 250 mL stream water sample and shake.

2.

Filter the sample into the cuvette with a syringe filter. Generally syringe filters should be replaced after being used between 4 to 6 times. Filters can be used until resistance is felt which may be one use on a stream with high total suspended solids to many uses on a stream with low total suspended solids.

3.

Adjust the sample temperature by placing the 25 mL cuvette into a water bath or by holding in the hands.

V.

VI.

C.

Insert the blank into the sample cell holder.

D.

Press the ZERO key and wait until the instrument is zero calibrated.

E.

Dry the sample cuvette with a tissue and insert into the sample cell holder.

F.

Press the READ key.

G.

Note the measured result on the analysis form. This absorbance includes both the background absorbance of the stream water and the difference in absorbance between the blank and sample cells. Do not correct this value for differences between cells even if it is significant. If the difference between cells was considered significant when checked, compensation was made when producing the calibration curve.

H.

Determine the B/A ration for the stream water at the site according to procedures outlined in TOP:018.x.

Sample measurement A.

Collect a stream water sample containing TFM.

B.

Prepare the water sample for analysis. 1.

Add 1 mL sodium tetraborate buffer to a 250 mL stream water sample and shake.

2.

Filter the sample into the cuvette with a syringe filter.

3.

If problems with cuvette fogging occur, adjust the sample temperature by placing the 25 mL cuvette into the water bath or by holding in the hands.

C.

Insert the blank into the sample cell holder.

D.

Press the ZERO key and wait until the instrument is zero calibrated.

E.

Dry the sample cuvette with a tissue and insert into the sample cell holder.

F.

Press the READ key.

G.

Record the resulting absorbance on the lampricide analysis data sheet.

H.

Subtract the background absorbance (base blank on the data sheet) and record.

I.

Divide the resulting absorbance by the calculated slope of the calibration curve.

J.

Record the result as the concentration of TFM (mg/L) in the stream water sample.

Documentation 1.

Make entries into instrument log book each time instrument is used.

2.

Record results of analysis on LAMPRICIDE ANALYSIS data sheet (Appendix M).

MAINTENANCE: I.

Cleaning instrument -- Methods for cleaning the spectrophotometer and sample cell are described in Section 5.1.1, page 91 of the instrument manual.

II.

Replacing batteries -- Procedures for replacing batteries are found in Section 4.1, page 39, and Section 5.2.1, page 92 of the instrument manual.

III.

Replacing Lamp -- The procedure for replacing instrument lamp is found in Section 5.2.2 on pages 92 - 93 of the instrument manual.

IV.

Calibrating/adjusting lamp -- Instructions for lamp calibration are found in Section 5.3, page 94 of the instrument manual.

V.

Troubleshooting -- Section 6, page 95 - 96 of the instrument manual contains a guide for locating the cause of malfunctions in the DR/2010.

REFERENCE: Hach DR/2010 spectrophotometer instrument manual

This procedure has been reviewed and approved by the undersigned representative of the U.S. Fish and Wildlife Service.

REVIEWED/APPROVED______________________________ Field Supervisor (U.S.)

DATE____________

ATTACHMENTS

Log book for operation of the Hach Model DR/2010 spectrophotometer

SPECTROPHOTOMETER HACH MODEL DR/2010

SERIAL NUMBER

__________________

PROPERTY NUMBER __________________ UNIT NUMBER

__________________

LOCATION

__________________

Date

Time

Inits.

Stream

Std. number

mg/L

Absorb.

Slope

Remarks and maintenance

SEA LAMPREY CONTROL PROGRAM DOCUMENTATION OF INITIALS (All personnel trained to operate this instrument must sign and initial this form)

OPERATOR

INITIALS

IOP:012.3F

Thermo Electron Corporation Genesys 20 Spectrophotometer

IOP:012.3F U.S. Fish and Wildlife Service Marquette Biological Station 3090 Wright Street Marquette, Michigan 49855 U.S.A.

January 6, 2012

and U.S. Fish and Wildlife Service Ludington Biological Station 229 South Jebavy Drive Ludington, Michigan 49431 U.S.A. and Fisheries and Oceans Canada Sea Lamprey Control Centre 1219 Queen Street East Sault Ste. Marie, Ontario P6A 2E5 Canada

INSTRUMENT OPERATING PROCEDURE INSTRUMENT: Spectrophotometer MODEL: Genesys 20 MANUFACTURER: Thermo Electron Corporation SERIAL AND PROPERTY NOS: Model number

Location

Serial number

Property number

Identifying number

4001/4

MBS

3SGL326008

3001

G1

4001/4

MBS

3SGL340002

3002

G2

4001/4

MBS

3SGL326001

3003

G3

4001/4

MBS

3SGL340006

3004

G4

4001/4

MBS

3SGL340001

3005

G5

4001/4

MBS

3SGM268008

3090

G7

4001/4

MBS

3SGM268011

3091

G10

4001/4

MBS

3SGM268007

3092

G9

4001/4

MBS

3SGM268009

3089

G8

4001/4

SLCC

3SGL164016

08-17

08-17

Model Number

Location

Serial Number

Property number

Identifying number

4001/4

SLCC

3SGL165001

08-18

08-18

4001/4

SLCC

3SGL255016

08-26

08-26

4001/4

SLCC

3SGL255018

08-27

08-27

4001/4

SLCC

3SGL267009

08-30

08-30

4001/4

SLCC

3SGN020024

09-12

09-12

4001/4

LBS

3SGL339007

LFY09-065

65

4001/4

LBS

3SGL339008

LFY09-066

66

4001/4

LBS

3SGL339011

LFY09-067

67

4001/4

LBS

3SGL339005

LFY09-068

68

4001/4

LBS

3SGL339010

LFY09-070

70

4001/4

LBS

3SGL340008

LFY09-069

69

4001/4

LBS

3SGN096005

LFY10-176

76

4001/4

LBS

3SGN096006

LFY10-177

77

4001/4

LBS

3SGN096007

LFY10-178

78

PRECAUTIONS: POTENTIAL INTERFERENCES Suspended particulate matter in a sample produces an increased absorbance value. SAFETY No special safety procedures are required. PROCEDURE: I.

II.

Installation A.

Place unit on a flat, even surface away from sources of electrical interference.

B.

Connect the female end of the power cord into the A/C power connector on the back of the instrument, and then plug the power cord into a power outlet.

C.

Check that the cell holder is empty before turning on the instrument. Turn the power switch to ON (located next to the A/C power connector).

D.

A power-on, self-check sequence begins automatically. The sequence takes about two minutes to complete. The instrument must be allowed 30 minutes to warm up before use.

Controls and indicators A.

Soft keys 1 and 2: Represented by empty circles and of varying functions, depending on the screen.

B.

▲and▼ keys: Scroll keys used to scroll through menus and enter numeric values.

C.

nm ▲ and ▼ nm keys: Wavelength control keys used to increase and decrease the wavelength setting.

III.

IV.

D.

0 ABS/100%T key: Automatically sets instrument to zero absorbance.

E.

A/T/C key: Used to switch among absorbance, percent transmittance, and concentration modes.

F.

Utility key: Accesses instrument setup, diagnostics, and other functions.

G.

Print key: Sends currently displayed data to a selected printer.

Operation A.

Press A/T/C to select the absorbance mode. The current mode appears on the display.

B.

Press a wavelength control key nm ▲ or ▼ nm to set the wavelength at 395 nm.

C.

Insert a blank and close the sample door. Position the cuvette so a clear wall is facing the front of the instrument.

D.

Press 0 ABS/100% T to set the blank to 0 A.

E.

Match cuvettes that will be used in analysis. Fill a second cuvette with deionized water, wipe dry, and place in the cuvette holder. Close the sample compartment.

F.

The display will indicate the sample absorbance. If the display is + 0.002 units, repeat the process with additional cuvettes until a suitable match is found.

G.

Reinsert the blank and press 0 ABS/100% T.

H.

Fill the matched cuvette with filtered, buffered standard and replace the blank cuvette in the cuvette holder.

I.

The absorbance of the standard will be displayed on the LCD.

J.

Conduct analyses for TFM according to TOP:018.x.

Documentation A.

An instrument log book is assigned to each spectrophotometer (Attachment).

B.

Each day of operation of the spectrophotometer is documented in the book. 1.

Record the date, time, operator identity, and stream treatment during which the analyses will be conducted.

2.

Record the identity of the set of pre-packaged TFM standards.

3.

Absorbencies of the standards used for analysis are recorded.

4.

The slope of the response curve is calculated and recorded.

5.

The absorbance of a check standard is measured periodically during the day to confirm that instrument response has not changed this measurement is recorded.

MAINTENANCE: Consult the Maintenance and Troubleshooting section in the manual (page 10). I.

II.

III.

IV.

Routine care A.

Do not use or store the instrument in a corrosive environment.

B.

Gently wipe the outside of the instrument with a soft cloth to remove any dust or spills. Water, isopropyl alcohol and other common laboratory cleaning agents may be used if necessary.

C.

Clean up spills immediately to prevent or minimize damage to the instrument.

D.

Use water, isopropyl alcohol or other common laboratory cleaning agents to clean the keyboard. It is recommended that you clean spills off the keyboard as soon as they occur.

Changing the lamp. A.

Follow instructions on pages 10 – 12 of the operating manual to change the lamp.

B.

Always turn off and unplug the instrument before performing any maintenance.

Changing the fuse. A.

Follow instructions on pages 12 – 13 of the operating manual to change the fuses.

B.

Always turn off and unplug the instrument before performing any maintenance.

Error messages A.

The instrument recognizes two types of errors. With the first type, the instrument is still functional; with the second, the instrument is not functional until the condition is resolved.

B.

A listing of messages is found on pages 13 – 14 of the operating manual.

REFERENCES: Genesys 20 spectrophotometer instruction/maintenance manual.

This procedure has been reviewed and approved by the undersigned representatives of the U.S. Fish and Wildlife Service and Fisheries and Oceans Canada.

REVIEWED/APPROVED______________________________ Field Supervisor (U.S.)

DATE____________

REVIEWED/APPROVED______________________________ Division Manager (Canada)

DATE____________

ATTACHMENTS

Log book for operation of the Genesys 20 spectrophotometer

SPECTROPHOTOMETER GENESYS 20

SERIAL NUMBER

__________________

PROPERTY NUMBER __________________ UNIT NUMBER

__________________

LOCATION

__________________

Date

Time

Inits.

Stream

Std. number

mg/L

Absorb.

Slope

Bulb

Remarks and maintenance

SEA LAMPREY CONTROL PROGRAM DOCUMENTATION OF INITIALS (All personnel trained to operate this instrument must sign and initial this form) OPERATOR

INITIALS

IOP:012.5G

Hach DR/2800 Spectrophotometer

IOP:012.5G U.S. Fish and Wildlife Service Marquette Biological Station 3090 Wright Street Marquette, Michigan 49855 U.S.A.

February 4, 2014

and U.S. Fish and Wildlife Service Ludington Biological Station 229 South Jebavy Drive Ludington, Michigan 49431 U.S.A. and Fisheries and Oceans Canada Sea Lamprey Control Centre 1219 Queen Street East Sault Ste. Marie, Ontario P6A 2E5 Canada

INSTRUMENT OPERATING PROCEDURE INSTRUMENT: Spectrophotometer MODEL: DR/2800 MANUFACTURER: Hach SERIAL AND PROPERTY NOS: Model number

Location

Serial number

Property number

Identifying number

DR/2800

MBS

1404484

3164

5

DR/2800

MBS

1404482

3165

6

DR/2800

MBS

1404485

3166

7

DR/2800

MBS

1404283

3167

8

DR/2800

MBS

1257589

2192

3

DR/2800

MBS

1305958

3086

4

DR/2800

MBS

1305719

3088

1

DR/2800

MBS

1305217

3087

2

DR/2800

LBS

1285976

LFY09-076

1

DR/2800

LBS

1351327

LFY10-208

2

Model

Location

Serial Number

Property Number

Identifying Number

DR/2800

LBS

1404116

LFY11-047

3

DR/2800

LBS

1404279

LFY11-048

4

DR/2800

SLCC

1321174

09-17

09-17

DR/2800

SLCC

1321093

09-18

09-18

DR/2800

SLCC

1377283

10-61

10-61

DR/2800

SLCC

1376885

10-60

10-60

PRECAUTIONS: POTENTIAL INTERFERENCES None listed in manual SAFETY No special safety precautions PROCEDURES: I.

Background A.

The Hach DR/2800, the factory-suggested replacement for the DR/2400, is capable of direct readout of concentrations of TFM, however, this option does not support the requirements of methods of analysis developed for line-powered spectrophotometers.

B.

The procedures for analysis with the DR/2800 closely parallel those used with the Turner model SP-830 spectrophotometers.

C.

1.

Similarities a. Pre-formulated standards with concentrations of 0, 4, 8, and 12 mg/L TFM are used. b. The slope of the instrument response is determined through measurement of the absorbance of the TFM standards. c. Base/Acid measurements of background absorbance are conducted to assure accuracy of analyses. d. Water samples are buffered to pH ~9.0 before measurement of absorbance. e. Water samples are filtered before measurement of absorbance. f. Record keeping requirements are the same.

2.

Difference a. Water samples normally are not heated before analysis.

The accuracy of measurements depends to some degree on the comparative absorbencies of the optically-matched sample cells in each DR/2800 kit. The method of data interpretation used during TFM analyses demands that special attention is given to compensation for poor matches when they cannot be avoided.

II.

III.

Preparation A.

Set up the spectrophotometer in a shaded location. Always use the black outdoor light shield when making absorbance measurements.

B.

Use line power if available, however, use of this instrument is normally reserved for situations in which line power is not available.

C.

After all peripheral equipment for sample preparation is ready, press the POWER button on the back of the instrument. The instrument will conduct internal tests.

D.

The Main Menu will automatically be displayed once the status check is complete. Select the Single Wavelength option on the touch pad screen.

E.

With the Single Wavelength main screen active, check the wavelength for the desired wavelength of 395 nm for TFM.

F.

Match the 10 mL sample cells 1.

Open a new 0.0 mg/L standard and rinse and fill two factory-matched 10 mL sample cells.

2.

Place the first cell in the sample cell holder with the 10 mL mark facing to the right and close the black outdoor light shield. Press ZERO on the touch pad screen. “ZEROING...” will be displayed until the instrument is zero calibrated. 0.000 ABS will appear on the display when the instrument is zero calibrated.

3.

Place the second cell in the sample cell holder with the10 mL mark facing to the right and close the black outdoor light shield.

4.

Press READ on the touch pad screen.

5.

The sample cell should produce an absorbance + less than 0.008 (considered an acceptable match; maximum ~ 0.05 mg/L error). If the difference is greater, clean the cell or check the absorbencies of spare sets of matched cells. If an acceptable match cannot be obtained and another matched set is not available, note the absorbance difference so absorbencies of standards can be corrected. The cell with the lesser absorbance is used as the blank.

Calibration–standards A.

Open the remainder of the new set of TFM standards. Do not allow the standards to sit in sunlight while in use and store the standards in the dark. If the standards are very cold (apt to fog), warm them in a water bath or in the hands.

B.

Insert the cuvette that contains the blank and press zero. Wait until 0.000 ABS is displayed.

C.

Insert the 0.0 mg/L TFM standard and close the black outdoor light shield. The 0.0 standard may produce a reading other than 0.000 because of an imperfect match of cuvettes. If the cells are not suitably matched, subtract the difference due to cell mismatch (noted above) and record in log book.

IV.

V.

D.

Again insert the cuvette containing the blank and close the black outdoor light shield. Wait until 0.000 ABS is displayed, insert the 4.0 mg/L standard, and close the black outdoor light shield. Press READ on the touch pad screen. Again adjust the result for differences in absorbance between blank and sample cells if necessary. Record the corrected absorbance in the instrument log book. Repeat the procedure with 8.0 and 12.0 mg/L TFM standards

E.

Divide the recorded absorbance of each standard by the concentration of TFM (mg/L; 4.0, 8.0, and 12.0). Average the results and record the mean in the log book and on the analysis data sheet.

Calibration–stream water sample A.

Measure the background absorbance and B/A ratio of the stream water (TOP:018.x). Do not interchange the cells. Always use the same cell for the 0.0 standard (blank).

B.

Prepare the TFM-free water sample for analysis 1.

Add 1 mL sodium tetraborate buffer to a 250 mL stream water sample and shake.

2.

Filter the sample into the cuvette with a syringe filter. Generally syringe filters should be replaced after being used between 4 to 6 times. Filters can be used until resistance is felt which may be one use on a stream with high total suspended solids to many uses on a stream with low total suspended solids.

3.

Adjust the sample temperature by placing the10 mL cuvette into a water bath or by holding in the hands.

C.

Insert the blank into the sample cell holder.

D.

Press the ZERO key and wait until the instrument is zero calibrated.

E.

Dry the sample cuvette with a tissue, insert into the sample cell holder, close the black outdoor light shield, and press READ on the touch screen.

F.

Note the measured result on the analysis form. This absorbance includes both the background absorbance of the stream water and the difference in absorbance between the blank and sample cells. Do not correct this value for differences between cells even if it is significant. If the difference between cells was considered significant when checked, compensation was made when producing the calibration curve.

G.

Determine the B/A ration for the stream water at the site according to procedures outlined in TOP:018.x.

Sample measurement A.

Collect a stream water sample containing TFM.

B.

Prepare the water sample for analysis. 1.

Add 1 mL sodium tetraborate buffer to a 250 mL stream water sample and shake.

2.

Filter the sample into the cuvette with a syringe filter.

3.

VI.

If problems with cuvette fogging occur, adjust the sample temperature by placing the 10 mL cuvette into the water bath or by holding in the hands.

C.

Insert the blank into the sample cell holder.

D.

Press the ZERO key and wait until the instrument is zero calibrated.

E.

Dry the sample cuvette with a tissue and insert into the sample cell holder.

F.

Close the black outdoor light shield, and press READ on the touch screen.

G.

Record the resulting absorbance on the lampricide analysis data sheet.

H.

Subtract the background absorbance (base blank on the data sheet) and record.

I.

Divide the resulting absorbance by the calculated slope of the calibration curve.

J.

Record the result as the concentration of TFM (mg/L) in the stream water sample.

Documentation A.

Make entries into instrument log book each time instrument is used.

B.

Record results of analysis on LAMPRICIDE ANALYSIS data sheet (Appendix M).

MAINTENANCE: I.

Cleaning instrument -- see page 73, Section 7.1 in the instrument manual.

II.

Replacing batteries -- See page 74, Section 7.2 in the instrument manual.

III.

Replacing Lamp -- See page 76, Section 7.3 in the instrument manual.

REFERENCE: Hach DR/2800 Spectrophotometer Instrument Manual

This procedure has been reviewed and approved by the undersigned representative of the U.S. Fish and Wildlife Service.

REVIEWED/APPROVED______________________________ Field Supervisor (U.S.)

DATE____________

ATTACHMENTS

Log book for operation of the Hach Model DR/2800 spectrophotometer

SPECTROPHOTOMETER HACH MODEL DR/2800

SERIAL NUMBER

__________________

PROPERTY NUMBER __________________ UNIT NUMBER

__________________

LOCATION

__________________

Date

Time

Inits.

Stream

Std. number

mg/L

Absorb.

Slope

Remarks and maintenance

SEA LAMPREY CONTROL PROGRAM DOCUMENTATION OF INITIALS (All personnel trained to operate this instrument must sign and initial this form)

OPERATOR

INITIALS

IOP:012.0H Hach Colorimeter

IOP:012.0H U.S. Fish and Wildlife Service Marquette Biological Station 3090 Wright Street Marquette, Michigan 49855 U.S.A.

April 16, 2010

and U.S. Fish and Wildlife Service Ludington Biological Station 229 South Jebavy Drive Ludington, Michigan 49431 U.S.A. and Fisheries and Oceans Canada Sea Lamprey Control Centre 1219 Queen Street East Sault Ste. Marie, Ontario P6A 2E5 Canada

INSTRUMENT OPERATING PROCEDURE INSTRUMENT: Colorimeter MODEL: Pocket colorimeter 11 (420) MANUFACTURER: Hach SERIAL AND PROPERTY NOS: Model number

Location

Serial number

Property number

Identifying number

Pocket Colorimeter 11 Pocket Colorimeter 11

MBS MBS

08110E113828 08100E112719

3008 3007

#1 #2

PRECAUTIONS: POTENTIAL INTERFERENCES None listed

SAFETY No special safety precautions PROCEDURES: I.

Background A.

B.

II.

The procedures for conducting analyses with the Pocket Colorimeter are similar to those for analyses with the DR/2000/2010/2800 spectrophotometers. Some exceptions in procedures and equipment result from the requirement of portability. 1.

Sample bottle size, filter type, and size differ.

2.

The addition of sodium borate is done drop-wise with an eye dropper.

The Pocket Colorimeter operates at a wavelength of 420 nm and is not adjustable. This wavelength is slightly out of the desired range for analysis of TFM (395 – 400 nm). This fact along with increased variability in wavelength caused by requirements of size and portability limit the use of this instrument to certain applications: 1.

Beaver pond or backwater applications

2.

Estimations of TFM concentration in a lampricide block for determining flow timing

3.

Remote application sites where a DR 2000/2010/2800 spectrophotometer would be unreasonably difficult to transport

Preparation A.

Set up the spectrophotometer in a shaded location. Always use the light shield when making absorbance measurements.

B.

Ready all peripheral equipment and reagents for sample preparation.

C.

Remove the light shield from the end of the instrument and place it over the cell compartment. Press the POWER button (bottom center black button with bulb icon). The instrument will display either a flashing “0” or last reading.

D.

Check the absorbance match between the 10 mL sample cells: 1.

Fill the two pre-matched sample cells with 0.0 mg/L TFM standard.

2.

Place the first cell in the sample cell holder with the diamond mark facing forward (toward the keypad). Replace the light shield. Press the ZERO key (blue button with “0” icon). 0.000 will appear when the instrument is zero calibrated.

3.

Place the second cell in the sample cell holder with the diamond mark facing front. Press the READ/ENTER key (green button with check icon).

4.

The difference in absorbance between the sample cells must be less than 0.010. If the cells cannot be cleaned so the difference is less than 0.010, than measurements must be corrected by the difference. The cell with the lesser absorbance is used as the blank.

III.

IV.

V.

Calibration–standards A.

Open the remainder of the new set of TFM standards. Do not allow the standards to sit in sunlight while in use and store the standards in the dark. If the standards are very cold (likely to fog), warm them in a water bath or in the hands.

B.

Insert the sample cell that contains the blank and press ZERO. Wait until 0.000 ABS is displayed.

C.

Insert the 4.0 mg/L standard, and press READ/ENTER (green button). Adjust the result for any significant difference in absorbance between blank and sample cells if necessary. Record the corrected absorbance in the instrument log book. Repeat the procedure with 8.0 and 12.0 mg/L TFM standards

E.

Divide the recorded absorbance of each standard by the concentration of TFM (mg/L; 4.0, 8.0, and 12.0). Average the results and record the mean (slope) in the log book.

Calibration–stream water sample A.

Measure the background absorbance and B/A ration of the stream water by the following steps. Do not interchange the cells. Always use the same cell for the 0.0 standard (blank).

B.

Prepare the TFM-free stream water sample for analysis 1.

Add 6 drops sodium tetraborate buffer to a 60 mL stream water sample and shake.

2.

Place a 2.4 cm filter into the syringe filter holder. Filter the buffered stream water sample into the sample cell with the syringe filter.

3.

Zero the instrument on the blank then read the stream water sample. Record the result on an analysis form.

4.

Measure the absorbance of an acidified stream water sample for determining the B/A ratio by adding 2 drops of 10% sulfuric acid to the cell and recording the result.

Sample measurement A.

Collect a stream water sample containing TFM.

B.

Prepare the water sample for analysis. 1.

Add 6 drops sodium tetraborate buffer to the 60 mL stream water sample and shake.

2.

Filter the sample into a sample cell with a syringe filter.

C.

Insert the blank into the sample cell holder.

D.

Press the ZERO key and wait until the instrument is zero calibrated.

E.

Dry the stream water sample cell with a tissue and insert into the sample cell holder.

F.

Press the READ key.

VI.

G.

Record the resulting absorbance on the lampricide analysis data sheet.

H.

Subtract the background absorbance (base blank on the data sheet) and record.

I.

Divide the resulting absorbance by the calculated slope of the calibration curve.

J.

Record the result as the concentration of TFM (mg/L) in the stream water sample.

Documentation A.

Make entries into instrument log book each time instrument is used.

B.

Record results of analysis on LAMPRICIDE ANALYSIS data sheet (Appendix M).

MAINTENANCE: No recommended maintenance REFERENCE: Hach Pocket colorimeter 11 instruction manual

This procedure has been reviewed and approved by the undersigned representative of the U.S. Fish and Wildlife Service.

REVIEWED/APPROVED______________________________ Field Supervisor (U.S.)

DATE____________

ATTACHMENTS

Log book for operation of the Hach Pocket Colorimeter II

SPECTROPHOTOMETER HACH POCKET COLORIMETER II

SERIAL NUMBER

__________________

PROPERTY NUMBER __________________ UNIT NUMBER

__________________

LOCATION

__________________

Date

Time

Inits.

Stream

Std. number

mg/L

Absorb.

Slope

Remarks and maintenance

SEA LAMPREY CONTROL PROGRAM DOCUMENTATION OF INITIALS (All personnel trained to operate this instrument must sign and initial this form)

OPERATOR

INITIALS