Lancaster SOP - Mercury

382 Pages·2009·7.6 MB·English

Lancaster Laboratories
MC-10-014
2425 New Holland Pike. Lancaiter. PA 17601
Revision 08
Supersedes Date: 07130108
Effective Date: r ~ 0a4 20~10
Page 1 of I6

Vapor Generation for Cold Vapor Mercury
Method Using the Leeman Labs PS200 and Hydra II Mercury Analyzer
Approvals:
. .
Prepared, by: Date:
- Approved by Date: }2-)7.b9
..
.... . 4 ~ -
Approved by: Date:
COMPANY CONFIDENTIAL
Level 3 Document
MC-10-014
Revision 08
Supersedes Date: 07130108
Effective Date: QAN g) 4 201Q
Page 2 of I 6

Revision Log:
Revision Log
Title New instrument covered under this Changed title to add and Hydra II Mercury Analyzer
snp
Reference Clarifcation Changed references to be actual titles
Purpose New nstrLment covered under this Added Hydra II Mercury Analyzer
SOP
Current practice Changed the codes for hotkeys
Current practice Removed tne steps for changing tne orylng tube, aaoed
steps for changing dehydrator tube.
Procedure A.1 .a Current practice Updated colors of tubes and tabs
Procedure A.1 .a Current ~ractice Removed instructions 2 system conditioning procedures
and replace with "Turn on the flow rate and let it pump
rinse and reductant for 5-10 minutes."
Current practice Deleted optimization section
New instrument Added section to address ~eemanL abs Hydra II Merc~ry
Analyzer
Procedure B. 'New instrument Added section to address Leeman Labs Hydra II Mercury
Analyzer
Procedure B.2.a Current practice Revised directions for recalibration
Procedure Current practice Changed flushmg solut~onfr om de~onizedw ater to 0.1 5%
C.l.b.(5) HN03
Procedure C.2. New instrument Added section to address Leeman Labs Hydra II Mercury
Analyzer
Procedure D. Current practice Revised entire section
COMPANY CONFIDENTIAL
Level 3 Document
4l? Lancaster La.b oratories
MC-10-014
2425 hen no ma I're .a-<em %I ' 6.
Revision 08
Supersedes Date: 07/30/08
Effective Date: 6)4 20,0
Page3of I 6

I I
LOM-SOP-LAB901
Document I Formattina reauirements per I Placed sections in order
COMPANY CONFIDENTIAL
Level 3 Document
Lancaster Laboratories
2425 New Holland Pike. tancarter. PA 17601 MC-10-014
Revision 08
Su~ersedesD ate: 07130108
~GectiveD ate:
:JAN 0 4 2010
Page 4 of I6

Reference:
The method described in this maintenance and calibration is adapted from the following
references.
1. Method 7470A (waters) and 7471A (solids), Test Methods for Evaluating
Solid Waste, USEPA SW-846, modified, September 1994.
2. USEPA CLP SOW ILM04.0, Exhibit D, CLP-M, D4.
3. USEPA CLP SOW ILM05.2, Exhibit DIMercury.
.
4. Method 245.1, Methods for Analysis of Water and Wastes,
USEPA 60014-79-020, Rev. March 1983.
5. Method 245.1, Methods for the Determination of Metals in Environmental
Samples, Supplement I, EPA-600lR-941111, May 1994.
6. Leeman Labs PS200 Automated Mercury Analyzer Manual.
7. Leeman Labs Hydra I1 Automated Mercury Analyzer Manual.
Cross Reference:
Document Document T~tle
SOP-10-005 Quality Control Procedures for Mercury
SOP-10-007 Preparation of Standards and Solutions
SOP-IO-011 Inorganic Analysis Safety and Waste Handling Procedures
COMPANY CONFIDENTIAL
Level 3 Document
4?
Lancaster Laboratories
2425 l!rr no ;no Pee. .a-<axe: FA /bL 1 MC-10-014
Revision 08
Su~ersedesD ate: 07130108
~iectiveD ate: 'JAN 0 4 201D
Page5of I 6

Purpose:
The purpose of this procedure is to outline the proper techniques for the operation,
calibration, and maintenance of the Leeman Labs, PS200 Automated Mercury Analyzer
and Hydra II Mercury Analyzer.
Scope:
-
The Leeman Labs Mercury Analyzers utilize continuous flow technology with drying of
the sample vapor for the analysis of mercury by automated vapor generation. The dry
vapor enters one path of a heated double path optical cell, which has been optimized for
fast response (small diameter), and sensitivity (long length). Merctlry is measured using
a solid state detector with a wide dynamic range and a mercury source that delivers a
stable source of emission at 254 nm. The signal is referenced to the simultaneous
absorbance of the pure carrier gas flowing through the second optical path under
identical conditions. This procedure offers advantages in sensitivity and precision over
conventional CV-AAS systems by a factor of approximately 10 times.
This procedure is applicable to the determination of mercury in waters, wastewaters,
leachates, and soils by vapor generation.
Safety Precautions and Waste Handling:
Refer to SOP-10-01 1.
Personnel Training and Qualifications:
Personnel performing this procedure must have documentation of reading,
understanding and agreeing to follow this version of the SOP. They must have a
documented Demonstration of Capability for this or an equivalent procedure.
All personnel that are responsible for operating the Mercury Analyzers must have a
working knowledge of both operating and maintenance procedures for the instrument.
COMPANY CONFIDENTIAL
Level 3 Document
Lancaster La.b oratories
2425 1.er ro 3-0 Pre a-cater PA '?&?I MC-10-014
Revision 08
Su~ersedesD ate: 07130108
~fiectiveD ate: 'JL~N0 4 2010
Page 6 of 16

Training to achieve this knowledge will consist of reading related departmental SOPS
and instrument operations manuals as well as hands-on experience. A trainee will first
observe a trained analyst perform the functions; then the trainer will supervise and
review the trainee's performance and data.
Reagents and Standards:
Refer to SOP-10-007.
Procedure:
A. Instrument setup
1. Leeman Labs PS200 Automated Mercury Analyzer
The Leeman Labs PS software has been set up using "hotkeys" to help with
moving around in the software and macro utilization. (Macros are small
programs used to operate the instrument.) The hotkeys are the capitalized
letters that are highlighted in red on the computer screen.
a. System conditioning
If the instrument and computer are off, turn ON the power to the
instrument (green button). Also turn ON the power to the computer and
printer. Double click the PS icon on the desktop. This will initialize the
PS instrument software. The system is now ready for the initial setup.
If the instrument was shut down completely, the optical cell must be
reconnected. To reconnect the optical cell, remove the front cover from
the instrument by sliding the cover up and lightly pulling it out. Remove
the two screws from the retaining brackets and carefully slide the cell
out of its holder. Connect the gas lines on the left side of the cell to their
respective connections. Check that all connections are secure for the
COMPANY CONFIDENTIAL
Level 3 Document
ql?
Lancaster Laboratories
2425 (.en -'o'a-o I're a-:anv PA '760' MC-10-014
Revision 08
Supersedes Date: 07130108
Effective Date: (j,\~ 2010
Page 7 of I6

gas, lamp, detector, and cell heater. Place the cell in its holder and
tighten the retaining brackets to hold the cell in place. Replace the front
cover to the instrument.
Turn ON the power to the mercury lamp (blue button). The lamp will
take approximately 20 minutes to stabilize. Press F10 to stop and exit
any previously running macro. Press F1 to go to the Main menu. Use
hotkeys by typing "I" to select Instrument and then by typing " 0to
select Operation. Type "M" to turn the mercury lamp on or off. Type "R"
to turn the rate flow on and off. Remove the sample trays and the rinse
tank from the autosampler. Rinse the rinse tank with deionized water
several times and refill the rinse tank with a 0.15% nitric acid solution
(1% HN03).
Change the dehydrator tube if it needs to be replaced. It is across the
front of the instrument along the top of the face plate.
Replace the rinse tank and sample racks on the autosampler. Press F1
for Menu, then type "I" for Instrument, "0fo r Operations, and then
"T" for Tip to Rinse. This will lower the autosampler tip into the rinse
tank. Check the pump tubing for excessive wear by flipping the locking
hub down and lifting up on the pump cassette. Visually check the tubing
for excessive wear. Under normal daily operation, the tubing should last
approximately 1 week. To replace the tubing, disconnect old tubing and
discard and obtain a new set of tubing from the parts drawer. All tubing
should be replaced together. The pump tubing is color coded for easy
replacement. The sample tubing is clear with a blue tab, the reductant
tubing is clear with a red, orange, or yellow tab (0.16 cclm), and the
2 waste tubes are clear with a blue tab (1. OO cclm). The tubes are
placed in separate cassettes with the sample tube closest to the
instrument, followed by the reductant tube and finally the 2 waste tubes.
To secure the tubing to the pump head, slide the tubing through the
COMPANY CONFIDENTIAL
Level 3 Document
Lancaster La.b oratories
MC-10-014
2L;5 hen nc ma Pre .a".mter ?A 1761'
Revision 08
. Supersedes Date: 07130108
Effective Date: 'j#d 0 4 2010
Page 8 of I6

plastic clips at the bottom of the cassette until the tab is secure. Hold
the tube taut (not stretched) and slide the loaded cassette onto the
pump head.
Lock the clamp by pulling the locking hub up. Repeat for the remaining
tubes and connect the ends to the respective connections. Turn on the
flow rate and let it pump rinse and reductant for 5 to 10 minutes.
The system is now ready to be optimized for automated analysis.
b. Run setup
Once the cell has been optimized, the instrument is ready for sample
analysis. Press F1 for Menu, type " Pf or Protocol, and "G" for Get.
It will ask you for a protocol name. The protocols have been set up for
those operating the instrument as initials-employee number
(e.g., JKG-201). A default protocol has been set up as TEST. Type in
the protocol name and press ENTER. It will prompt you for a folder
name. The folder name is the file where the run information will be
stored. Type in the folder name as follows and press ENTER: year,
day, run number (e.g., 9403201 for the first run of day 032 of 1994).
Press F1 to return to the Main menu.
c. Autosampler setup
..
To set up the autosampler, type "A" for Autosampler and "Rnf or Rack
Entry. It will prompt you for a rack name. There are 2 sample racks
called stations, which hold 44 samples each. The standards and check
standards are located on their own rack. If less than 44 samples are to
be used, only one station is required to be defined. Enter a distinctive
rack name such as the day number and 01 or 02 and press ENTER.
The INSERT key is used to move between the entry modes. The
3 entry modes are single cells down ("cell entry"), single cell across
("row entry"), and full column ("column entry"). The current entry mode
COMPANY CONFIDENTIAL
Level 3 Document
Lancaster Laboratories
2425 1.1 ro a-0 :.<e.. armne. PA 176)' MC-10-014
Revision 08
Supersedes Date: 07130108
Effective Date: 0 4 2019
Page9of I 6

is displayed at the bottom right corner of the computer screen. In cell
entry mode, move the cursor to the cup ID column using the arrow key.
Enter the labels, up to 10 characters, and press ENTER. Enter PBW or
PBS for blanks, LCSW or LCSS for lab controls, and sample numbers
followed by a space then U, D, R, or M for background, duplicate, spike,
or matrix spike duplicate, respectively. Once the sample labels have
been entered, the extended ID must be entered. The extended ID
includes Me initial weights or volumes and batch numbers. In the
column entry mode, type " R f or Range and enter the range of samples
for the first batch. Type "E" for Extended ID (the full range that was
selected will be highlighted). Enter the most common initial weight or
volume followed by a space and then the full batch number and press
ENTER (e.g., 8 mL 940250821001). To edit values in either sample or
extended ID columns, select either cell or row entry mode and move the
cursor to the cell to be edited. Delete the value to be changed, retype
the corrected value and press ENTER. Once the entries for all samples
and batches are complete, return to the Main menu by pressing F1. The
defined sample rack must be loaded into the autosampler setup to be
run. Type "A" for Autosampler, "S" for Setup, and 1 for Station Rack
Nyrnber 1 or 2 for Station Rack Number 2. You will be prompted for a
rack name, enter the rack name, which corresponds, to the sample IDS
you will be running. Enter the beginning cup position and the end cup
position. Return to the Main menu by pressing F1. Load the standards,
check standards, and samples into the appropriate locations (see
Figure 1).
2. Leeman Labs Hydra II Mercury Analyzer
The Leeman Labs Envoy software is a windows based program to help
navigate the software.
COMPANY CONFIDENTIAL
Level 3 Document
4?
Lancaster Laboratories
MC-10-014
?C:5 ye., -om3 PL~.a m:w PA 176CI
Revision 08
Supersedes Date: 07130108
Effective Date: 'JAN 0 q 2010
Page 10 of I 6

a. System conditioning
If the instrument and computer are off, turn ON the power to the
instrument (switch in the back). Also turn ON the power to the
computer. Ensure that Argon supply is set to 15 psi. Double click the
Envoy icon on the desktop. This will initialize the instrument software.
The system is now ready for the initial setup. Loosen all the peristaltic
pump cassettes. Place levers to the 1 o-clock position. This will avoid
the pump from stalling. Check that rinse and reductant bottles are full
and Luer connections are tight. Only a 'light' finger tightening is
required. Clicking the start icon on the Tool Bar will turn on the
peristaltic pump and set the gas flow to method programmed conditions.
Check to see that the lamp, pump and gas turn on. If any of them is not
on open the Methodllnstrument Control Panel and turn them on and set
appropriate parameters. Once pump is turning, tighten the cassettes by
lowering the levers to a horizontal position. Allow 10 minutes for lamp
and pump equilibration. Inspect all system connections for leaks.
The system is now ready to be optimized for automated analysis.
b. Autosampler and Run setup
Click on the Sequence Tab to display the automated sequence page.
Click the Sequence menu item on the Menu bar and select Create from
the displayed options. A spreadsheet of empty locations will be added
to the display. This consists of 3 racks each with sample locations equal
to the rack capacity (24, 60 or 90). Each row represents a cup location
on one of the racks and its graphical representation will be updated in
the lower 'Rack' graphic whenever the Update button is clicked. Only
samples are entered into the sample list table. The standards and QCs,
will be programmed in the method. When all samples are entered click
the Update button to populate the navigation tree to the left with the
proposed run sequence.
COMPANY CONFIDENTIAL
Level 3 Document