0 EDA United States	^u1Sm u 0fficeof

Environmental Protection Agency	Research and Development

National Human Exposure Assessment Survey

(NHEXAS)

Arizona Study

Quality Systems and Implementation Plan
for Human Exposure Assessment

The University of Arizona
Tucson, Arizona 85721

Cooperative Agreement CR 821560

Standard Operating Procedure	SOP-UA-L-1.2

Title: Calibration and Operation of NHEXAS Balances
Source: The University of Arizona

U.S. Environmental Protection Agency
Office of Research and Development
Human Exposure & Atmospheric Sciences Division
Human Exposure Research Branch

Notice: The U.S. Environmental Protection Agency (EPA), through its Office of Research and Development (ORD), partially funded
and collaborated in the research described here. This protocol is part of the Quality Systems Implementation Plan (QSIP)
that was reviewed by the EPA and approved for use in this demonstration/scoping study. Mention of trade names or
commercial products does not constitute endorsement or recommendation by EPA for use.


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S0P#UA-L-1.2

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Calibration and Operation of NHEXAS Balances

1.0 Purpose and Applicability

The purpose of this SOP is to describe the procedures used when calibrating and operating
Balances during the EPA NHEXAS and Border projects of the University of
Arizona/Battelle/Illinois Institute of Technology consortia, as well as future "Health in the
Environment" investigations.

2.0 Definitions

2.1	Control weight = An identified metallic object of a selected weight used to monitor
balance precision over time.

2.2	Down Equipment Area = Area in which defective equipment is placed to await either
repair in-house or shipment to a repair facility.

2.3	Down Equipment Label = Label which is attached to a defective piece of equipment to
identify it as being defective.

2.4	SOP = Standard Operating Procedure

2.5	Standard weight = A reference standard weight that has a known valid relationship
with a recognized national standard.

3.0 References

3.1	Model AE163 Operating Instructions, Mettler Instrument Corporation, Hightown, NJ,
1982.

3.2	Assuring Balance Accuracy, J. Weil, Cahn Instruments, Inc., Cerritos, CA, 1984.

3.3	Acculab, Model #V-1200 Operating Instructions, Acculab, Newton PA. No Date.

3.4	Mettler Toledo BalanceLink (V2.0) Software. Operating Instructions, Mettler
Instrument Corporation, Hightstown NJ, 1994.

4.0 Discussion

This procedure is directly applicable to the calibration and operation of balances used to weigh
a variety of materials during the NHEXAS and Border projects, as well as future "Health in
the Environment" investigations. The balances include; a Mettler AE 163 (UA ID# A195535)
with a readability set at 0 to 162 grams at 1+0.5 mg and 0 to 60 grams at 0.1+0.1 mg. This
balance is connected to a computer and readings are digitally transferred to the computer
screen during operation; a Mettler AE 166 (UA ID# A201335), with a readability set at 0 to
162 grams at 0.1± 0.02 mg and set at 0 to 31 grams at 0.01± 0.1 mg; and an Acculab #V-
1200 (ID# 50090339) with a readability of 0.1±0.1 g, set to 0 to 600 grams, and 0.1±0.2, set
to read 601 to 1200 g.


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Responsibilities

5.1	The Project Director will be responsible for:

5.1.1 Final review and approval of each procedure.

5.2	The Project Laboratory Supervisor is responsible for:

5.2.1	Insuring SOP procedures are followed by the Project Lab staff.

5.2.2	Notifying the appropriate technicians with needed repairs. In cases when
the item can not be fixed in house, Project Field Coordinator will generate
the appropriate paperwork, notify the appropriate vendor or company, and
ship the dysfunctional item.

5.2.3	Notifying and scheduling appropriate factory calibration for the item of
equipment.

5.3	The Project Lab Technicians will be responsible for:

5.3.1	Knowing and following the procedures described in this SOP.

5.3.2	Recording the information as directed in this SOP.

5.3.3	Notifying the Project Lab Supervisor with down equipment and repair
supplies needed (where applicable).

5.3.4	Providing the Project Lab Supervisor with down equipment label and
isolating the down equipment into the down equipment area.

5.3.5	Insuring proper labeling techniques of down equipment.

5.3.6	Repairing the item (where applicable) in a timely manner.

Materials and Equipment

6.1 Materials

6.1.1	Acculab #V -1200 balance (ID# 50090339)

6.1.2	Bachrach humidity/temperature recorder

6.1.3	Balance Log Book for the Mettler AE 163

6.1.4	Balance Log Book for the Mettler AE 166

6.1.5	Balance Log Book for the #V-1200 balance

6.1.6	Class "S" standard calibration weight 100 mg (#9800007)

6.1.7	Class "S" standard calibration weight 20 mg (#9800008)

6.1.8	Mettler model 163 balance (UA ID# A195535)

6.1.9	Mettler model 166 balance (UA ID# A201335)

6.1.10	Mettler Toledo BalanceLink Software (#ME410023)

6.1.11	Standard Brass calibration weight 1000 g (#9800009)

6.1.12	Standard Brass calibration weight 100 g (#9800010)

6.1.13	Standard Brass calibration weight 10 g (#9800011)

6.1.14	Standard Brass calibration weight 5g (#9800017)


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6.1.15	Standard Brass calibration weight 1 g (#9800018)

6.1.16	Teflon coated forceps

7.0 Procedure

7.1	Preparation

7.1.1	Siting Criteria

Not applicable

7.1.2	Reagents

Not applicable

7.1.3	Samples/Actions:

A. Balance Area Preparation

1. Wipe down working area of table adjacent to balance with damp towel.

7.2	Analyses/Procedures

7.2.1	Standards/Blanks

A. Control weights are the same as the "Standard Weights" in 7.2.2 (B)7
through 7.2.2 (B)12 and 7.2.2 (C)3 through 7.2.2 (C)7

7.2.2	Balance Preparation for Operation

A. Mettler Balances AE 163 and AE 166

1.	Check level of balance via the integral spirit level.

2.	Close all balance doors.

3.	Turn on balance, 20 minutes prior to use.

4.	Depress single control bar to turn display on; wait for 0.00000 to appear in
display on the AE 163 and 0.0000 on the AE 166.

5.	Set the balance to the lowest range. With the AE 163 the 30 g setting is
achieved by holding the control bar down until "rng" is displayed. Depress
the control bar to toggle between 30 g and 160 g. The AE 166
automatically switches to the higher mode if material heavier than 60 g is
placed on the weighing pan.

6.	Depress the control bar to set the following ranges for the greatest
weighing accuracy;

a.	Cal

b.	Int -3-

c.	ASd -1-

"CAL" is the calibration procedure discussed in 7.2.2.B.

7.	Release control bar when 0.00000 reappears on the AE 163 display and
0.0000 reappears on the AE 166 display.

8.	Record the start-up data in the balance logbook for the balance to be used,
and on the appropriate boxes on the weighing forms (figures 1 -6) to be
used during each weighing session.


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9. To setup the computer link with the AE 163 follow section 7.2.3.

B.	Calibration procedure for the Mettler Balances (AE 163 and AE 166):

1.	Depress and hold down control bar until "CAL" appears; then release the
bar.

2.	When "100.000" blinks on the display, slide CAL knob on lower right side
of balance to rear stop.

3.	When "Cal 0" blinks, return CAL knob to forward stop.

4.	The following displays should be observed:

a.	— (blinks)

b.	0.0000

5.	The balance is now zeroed; observe 0.0000

6.	Select one of the standard weights discussed in step 10 below, and place it
in the middle of the balance pan.

7.	Close all balance doors.

8.	Wait 5 seconds after stability indicator dot goes out before recording
displayed weight.

9.	Record observed weight and serial number of standard weight in the
respective calibration log book.

10.	Repeat steps 7-9 for each of the standard weights used with each scale.

a.	Class "S" 20 mg, serial #9800008 (AE 163)

b.	Class "S" 100 mg, serial #9800007 (AE 163)

c.	Standard brass calibration weight lOg, serial #9800011 (AE 166)

d.	Standard brass calibration weight 5g, serial #9800017 (AE 166)

e.	Standard brass calibration weight lg, serial #9800018 (AE 166)

11 For the calibration to be valid the recorded standard and control weights
will be + 5% of their recognized value (Table 1).

C.	Acculab #V-1200

1.	Push the "on/memory" button turning the balance on 20 minutes prior to
use.

2.	To Calibrate;

a.	Press and hold the "CAL" key until 1000.0 appears and flashes on the
display.

b.	Press the "tare" key and the display will read "CAL 0". Pausing for at
least two seconds, then place a 1000 g calibration weight gently on the
center of the tray top.

c.	The display momentarily shows "CAL F" and then returns to active
weighing. Calibration is complete when the display correctly shows the
calibration weight, 1000 g, and the display has stabilized.

d.	If "CAL E" appears instead of "CAL F", a calibration error is indicated


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and the calibration process must be repeated. "CAL E" can occur if the
calibration steps are not followed correctly or if an incorrect calibration
weight is applied.

e. Remove the calibration weight and press the tare key to reset the zero
point.

3.	Record the success of the calibration in the Acculab #V-1200 log book.

4.	Place a standard brass calibration weight on to the scale and wait for the
stability indicator to appear.

5.	Record the observed weight and serial number in the Acculab #V-1200
calibration log book.

6.	Repeat steps 4-5 for each of the following standard weights;

a.	Standard brass calibration weight, lOOg (#9800010).

b.	Standard brass calibration weight, lOg (#9800011).

c.	Standard brass calibration weight, 5g (#9800017).

d.	Standard brass calibration weight, 1 g (#9800018).

7.	If the standard weights are within 1% of their recognized value (Table 1),
the calibration is valid.

7.2.3	Computer Preparation

A.	Turn on the computer and login using your name and password.

B.	Type "cd\balance" to go to the "Balance" sub-directory.

C.	Once in the Balance subdirectory, type "Balink Numeric Stable Right" to
start and setup the balance program. Follow directions in UA-L-9.1 (7.1.2.A-
E; 7.5.1 A-J) for computer balance interface use.

7.2.4	Actions

A. General weighing procedure Mettler Balances (AE 163 and AE 166)

1.	Calibrate each scale prior to each operating session.

2.	Close all doors and zero the balance by momentarily depressing the left
side of the control bar. Observe 0.0000

3.	Pass the specimen over a static eliminator bar.

4.	Open the appropriate door and carefully place the sample in the center of
the pan.

5.	Close all doors and wait for the stability indicator dot to leave the display.

6.	Record onto the appropriate weighing backup form (figures 1-3, 6) the
specimen weight that is displayed 5 seconds after the stability indicator dot
goes out. On the AE163, which is connected to the computer, press the
hand-switch to transfer the weight to the computer screen. Check that it is
recorded with the appropriate sample ID#.

7.	Remove specimen, close all doors, and observe that the scale returns to
0.0000. If not, re-zero the balance between each weighing by momentarily
depressing the control bar. Specific quality control issues are discussed


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with each sample type (see UA-L-9.1).

8.	A control weight of known value is weighed and recorded between each 5
successive specimen weight determinations for accuracy assurance (figures
1-6). If the scale does not record the standard within 5% of its known
weight the equipment is labeled as defective and the scale must be
recalibrated. All samples that were weighed after the last good accuracy
assurance weighing must be re-weighed.

9.	Turn off balance display by momentarily lifting up on control bar when
finished.

10.	Return all supplies used during weighing operation to their designated

storage areas.

B. General weighing procedure for the Acculab #V-1200.

1.	Perform calibration procedure prior to each operating session.

2.	Place the material to be weighed onto the weighing pan, gently.

3.	Record the specimen weight that is displayed 5 seconds after the stability
indicator arrow appears on the display screen.

4.	Remove the specimen and observe that the scale returns to 0.0. Press the
"Tare" button to return the scale to 0.0 at any point during a procedure.

5.	A control weight of known value (5g, lOg or lOOg) is weighed and
recorded between each 5 successive specimen weight determinations for
accuracy assurance. If the scale does not record the standard within 5% of
its known weight (10+0.5 g or 100±5 g), the equipment is labeled as
defective and must be recalibrated. All samples weighed after the last good
accuracy assurance weighing must be re-weighed.

6.	Turn off balance display by pressing the "Off' button.

7.	Return all supplies used during the weighing operation to their designated
storage areas.

7.3	Calculations
Not applicable

7.4	Quality Control
7.4.1 Tolerance limits

A. Mettler Balance AE163

1.	At a weighing range of 0
0.02 mg.

2.	At a weighing range of 0
is 0.1 mg.

3.	A failure to reproduce standard weights within 5% of their recorded weight

to 31g. the reproducibility (standard deviation) is
to 162g. the reproducibility (standard deviation)


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constitutes an equipment failure and results in recalibration. Three
successive equipment failures and recalibration results in labeling the item
as "down equipment". A manufacturers representative is then consulted or
the equipment is returned for factory calibration.

B.	Mettler Balance AE166

1.	At a weighing range of 0 to 31 g the reproducibility (standard deviation) is
0.02 mg.

2.	At a weighing range of 0 to 162g the reproducibility (standard deviation) is
0.1 mg.

3.	A failure to reproduce standard weights within 5% of their recorded weight
constitutes an equipment failure and results in recalibration. Three
successive equipment failures and recalibration results in labeling the item
as "down equipment".

C.	Acculab # V-1200

1.	At a weighing range of 0 to 600g the reproducibility (standard deviation) is

2.	At a weighing range of 601 to 1200g the reproducibility (standard
deviation) is 0.2 g.

3.	A failure to reproduce standard weights within 5% of their recorded weight
constitutes an equipment failure and results in recalibration. Three
successive equipment failures and recalibration results in labeling the item
as "down equipment". A manufacturers representative is then consulted or
the equipment is returned for factory calibration.

7.4.2	Detection Limits

A. Mettler AE163 and AE 166

1. When the balance is set to a range of 0 to 30g it can be read to 0.01 mg.
When set at a range up to 160g it can be read to 0.1 mg

7.4.3	Corrective Actions

A.	Routine Maintenance (Mettler AE 163 and 166)

1.	A corporate representative will clean, adjust, and calibrate both balances

once a year.

2.	After the 3rd failure to reproduce the standard weights within the stated
variation, a corporate representative will be called to calibrate and adjust
the equipment.

B.	Acculab #V-1200

1. Failure to reproduce the standard weights within the stated variation 3
times will constitute a failure and the balance will be sent back to the
factory for calibration.

Records


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8.1	Data collected by this procedure.

8.1.1 Balance calibration data

A.	The date, calibration weight serial #, measured calibration weight and
operator's initials are recorded in each balance's respective log book at the
beginning of each weighing session.

B.	Standard weights measured during the weighing procedure will be recorded in
the data files containing the filter weights (UA-L-9.1; 7.5).

C.	Cleaning and Maintenance are recorded in the balance log book.

D.	Balance audits by an outside vendor are recorded in the balance log book, with
certificates of accuracy kept on file by the lab supervisor.

8.2	Location/Placement of Log Books and Forms

8.2.1	The "Balance Log Books" will be kept near each respective balance in the
weighing room and the wet lab.

A. Removal of a "Balance Log Book" will be recorded on a sign-out sheet kept
with each balance.

8.2.2	Blank sample weighing forms (figures 1-6) are kept in a stacked file located in
the lab (Room 130A). Completed forms are returned to the lab supervisor for
QA/QC checks and transfer to the data coordinator.


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Table 1. Standard weight values recorded during calibration of each of the balances. All values
reported in grams.



Mean

Standard

n





Deviation (10)



Scale #V-1200







#9800010

99.97

0.0455

229

#9800011

9.96

0.0486

229

#9800017

4.95

0.0603

175

Scale AE166







#9800011

10.008

0.00013

190

#9800017

5.000

0.00009

190

#9800018

1.004

0.00008

190

#9800007

0.100

0.00005

66

#9800008

0.020

0.00004

66

Scale AE163







#9800007

0.09996

0.00051

81

#9800008

0.01994

0.00055

81


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Figure 1. PM Filter Pre-Weighing Form

25mm and 37mm TEFLO FILTER PRE-WEIGHING BACKUP FORM

Equilibration Start Date 	/	/		Balance

Equilibration Start Time [ ][ ]:[ ][ ]	0AE163

Technician [ ][ ]		0AE166

Code Init.	0 #V-1200

Weighing Date	/	/	 Temperature [ ] [ ] °F

Technician [ ][ ]		Relative Humidity [ ] [ ] %

Code Init.

File Name: 	

All Weights Are Recorded In Grams (g).





Sample ID#









Weight







Status

QA/QC

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Standard Weight	g. Number	 0 0

Standard Weight	g. Number 		 0 0

Comments:

L-9.0-1.1


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Figure 2. PM Filter Post-Weighing Form

25mm and 37mm TEFLO FILTER POST-WEIGHING FORM

Equilibration Start Date
Equilibration Start Time

Technician [ ][ ]	

Code Init.

Weighing Date	/_

Technician [ ][ ]	

/

/

[][]:[][]

Balance
0 AE 163
0 AE 166
0 #V-1200

Temperature [
Relative Humidity [

][
][

] °F
]%

Code Init.

File Name:

All Weights Are Recorded In Grams (g).

Sample ID#
][

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Standard Weight
Standard Weight

Weight

Status

_g-
_g-

Number
Number

QA/QC
00
00
00
00
00

00
00
00
00
00

00
00

Comments:

L-9.0-2.1


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Figure 3. Sentinel Filter Pre-Weighing Form

SENTINEL FILTER PRE-WEIGHING BACK-UP FORM

Equilibration Start Date 	/	/		Balance

Equilibration Start Time [][]:[][]	0 AE 163

Technician [ ][ ]		0AE166

Code Init.	0 #V-1200

Weighing Date	/	/	 Temperature [ ] [ ] °F

Technician [ ][ ]		Relative Humidity [ ][ ]%

Code Init.

File Name: 	

All Weights Are Recorded In Grams (g).





Sample ID#









Weight



Status

QA/QC

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Standard Weight











g-

Number









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Standard Weight











g-

Number









00

Comments:

L-9.0-3.1


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Figure 4. Sentinel Filter Post-Weighing Form

SENTINEL FILTER POST-WEIGHING BACK-UP FORM

Equilibration Start Date 	/	/_

Equilibration Start Time [ ][ ]:[ ][ ]

Technician [ ][ ]	

Code Init.

Weighing Date	

Technician [ ][ ]

/

/

Temperature
Relative Humidity

Balance
0 AE 163
0 AE 166
0 #V-1200

[ ][ ]°F
[ ][ ]%

Code Init.

File Name:

All Weights Are Recorded In Grams (g).





Sample ID#









Weight



Status

QA/QC

[

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[ ][ ][ ][ ][ ][ ][ ] [ K U	M KM! MM	00

[ ][ ][ ][ ][ ][ M ] [ H ]¦[	MKM] I II 1	00

[ M ][ ][ ][ ][ M ] I II ]¦[	K H I I MM	00

[ ][ ][ ][ ][ ][ H ] I II ]¦[	I II K I I H 1	oo

Standard Weight	g.	Number		0 0

Standard Weight	g-	Number		0 0

Comments:

L-9.0-4.1


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Figure 5. Vacuum Dust Filter "Chain of Custody Form"



Sample Weights and Chain of Custody Sheet



NHEXAS Arizona







Vacuum Dust Sample











QA/QC

Sample ID# :







0 0

Filter Weight:

g. Tie Weight:

g. Filter + Tie Weight: g 0 0

Total Wt(#4) :

g. -- Filter + Tie Wt.(#3)

e. = Collected Wt.(#5) g. 0 0

Pesticide Aliquot ID#:





0 0

Split Wt.(#8)

g. — Weigh Paper(# 10)

g. = Aliquot Wt.(#12) g. 0 0

Metals Aliquot ID#:





0 0

Split Wt.(#9)

g. -- Weigh Paper(#l 1)

g. = Aliquot Wt.(# 13) g. 0 0



Standard Weight #:

Weight: g. 0 0

Custody Record

Relinquished

Signature

Date

Time

Action

or Received



mo./day/yr.





[Rel] [Rec]



/ /













[Rel] [Rec]



/ /

;











[Rel] [Rec]



/ /













[Rel] [Rec]



/ /

;











[Rel] [Rec]



/ /













[Rel] [Rec]



/ /













[Rel] [Rec]



/ /

;











[Rel] [Rec]



/ /





L-12.0-2.0


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Figure 6. Vacuum Dust Characterization Form

VACUUM DUST CHARACTERIZATION FORM	Balance

Technician	[ ][ ] Start Date	/ /	0AE163

Init. Code	0 AE 166

Samp. ID [ ][ ][ ][ ][ ][ ][ ] HHID [ ][ ][ ][ ][ ] F.S. [ ] Status [	] 0#V-1200

1. Total Sample

Total Wt.(#4)	g. - Filter + Tie Wt.(#3)	g. = Collected Wt.(#5)	g. 0 0

Total Wt.(#4)	g. - Dirty Filter + Tie Wt.(#6)	g. = Sample Wt.(#7)	g. 0 0

Screen Set [ ][ ] Archive Code [ ][ ]-[ ]-[ ][ ][ ][ ][ ]

2. Aliquots Pesticide Sample ID# [ ][ ][ ][ ][ ][ ][ ]

Split Wt.(#8)	g. - Weigh Paper Wt. (#10)	g. = Pest Samp. Wt.(#12)	g. 0 0

Metals	Sample ID# [ ][ ][ ][ ][ ][ ][ ]

Split Wt.(#9)	g.-Weigh Paper Wt. (#11)	g. = Pest Samp. Wt.(# 13)	g. 0 0

XRF Cup # [ ][ ] XRF Form Header Completed Y [ ] N [ ]

3. Other Fractions:

>10 Wt. (#14)	g. - Weigh Paper Wt. (#15)	g. = >10 Samp. Wt.(#16)	g. 0 0

10-230 Wt.(# 17)	g. - Weigh Paper Wt.(# 18)	g. = 10-230 Samp. Wt.(#l9)	g. 0 0

4. Standard Weights: ID#

Total Sample:	[	][	][	][	][	][	][	]	Weight	g	0

Aliquots:	[	][	][	][	][	][	][	]	Weight	g	0

Other Fractions:	[	][ ][	][	][	][	][	]	Weight—_	g	0

5. QA/QC Check	Total Screened Weight (#20)	_g-	°0

[(#7)	g. - (#20) 	g-] * 100 =	% 0 0

Sample Wt.	Total Screened Wt.	% Dust Loss

Total Sample Aliquots Other Fractions

Standard Wt. Number	 	 		® 0

Weight		g-	8-	S '

QA/QC Signature;	.		— Date;	/	/	

0 0

L-12.0-1.0


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