Document header for 61 Broadway records, 2002

NYC 9/11 Public Portal Document

FROM FAX NO. : Jan. 08 2000 10:34PM P18

LFAQ-kn Flame AAS Method 7 issue 2. dated 15 Auoust1®94 - Paea of7 a

Mark M lson. N10SH/DP9E and R. DeLon Hull, Ph.D., N1QSHI09SS; 9341 originally validated under N108H Contract CDC-947446: additional studies under MIOSH Contract x10-79-0068. James B, Perkins. David L. Wheeler, and Keith Nlchobaon, Ph.D., DtteChem Laboratories, Salt Lake City, UT, prepared the mlcv digestion procedure in the Appendbc. eve

APPENDIX - MICROWAVE DIGESTION Foie 61IIAO iN PAINT CHIPf1(AND OTHER MATRICES) This procedure Is an alternative to the procedure presented In the Sample Preparation asction of this method. It provides a rapid, complete acid digestion prior to analysis by flame atomic absorption (FAA), heated graphite furnace atomic absorptior(Hf3FAA), and Inductively coupled plasma speotresoopy (ICP) [101. . I[11.183 1. Microwave apparatus requirements a. The microwave uric provides programmable power with a minimum of 674 W and can be programmed to within ±10 W of the required power. b. The microwave unit Cavity Is won resistant as well as ventilated. All electronics are protected against corrosion for safe opso,ation, a. The system requires Teflon PFA digestion vessels (120-mt. capacity) capable of withstanding pressuresup to t 0.7 alert (I10 s 10 psi) and oapsbla of controlled pressure relief at pressures i.e

exceeding 7.6 a 0.1 stn: (110 ± 10 psi). d. A rotating tumtabis is employed ensure homogeneous distribution of microwave radiation within to

the unit. The speed of the turntable should be a minimum of 3 rpm. a. A safety concern rotates to the us®f sealed containers *01thout pressure relief valves In the unit. Temperatui is the important varlable controlling the reaction. Pressure is needed to attain e1.- meted temperatures W. must be safely c®ltaittad Jul.

f. Polymeric volumetric were In plastic (Teller or polyetllyione). 50• or 100-mL capacity. g. Disposable polypropylene filler funnel. h. Analyticai balance, 300-g capacity, end minimum z 0.001 g.

R 1. Nitrlo acid. concentrated, epacb2py grade. 2. ReegentWater. aagent water shall be interference free. All references to water in the method refer to reagent waits, that meets the AMTM Typo 2 standard. ocedure 1, Calibration of Microwave Equipment Calibrate microwave equipment in accordance with manufacturer's instructions. if ca instructions are not available, sue EPA Method 3031 111), libration 2, All digestion and be add washed rinsed with reagent Water. vessels

volurnetrlcwars

must oarelglly

and

Ail

digestion

vessels

be

Should

cleaned

minutes, rinsed With reagent water. and dried in a clean environment by

teaching with

(11)

hot

acid nitric

a for

of minimum

fifteen

3.

Sample

Digestion

a.

Tare the

PFA

Teflon

digestion

vessel,

b.

Weigh

out

0.1 a

chip

paint

the to

sample

nearest

into the

tared

PFA

Teflon 0.0010

sample

vessel.

With large

paint

chip

samples,

measure

a 2

out

weigh

the to

ciftpiaoe.

nearest

0.001 g.

and

quentilatively

it

transfer

to

Me

vessel.

c.

Add

6.0

*

0.1

mL

concentrated

to

nitrle acid

the

sample

a in vessel

fume

hood, It a

vigorous

ilrociion

ors, allow

the

readivn

to

before aapplahg

ft slop

Vessel. th e

Cap

the

vesuehd

torque

the

cap to 12

-lb `1e

Mum)

according

to

th e

manufacturers

direction.

The

vessel sample

may

be

to an connected

vverflaw

veesat

Teflon

using

PFA

contacting

tubes-

the

Plac

veseeis

th In e

microwave

carrousel.

the

Connect

vessels

overflow

the

to

center

well

unit. the

of

d.

the Place

vessels

evenly

in the

distributed

turntable

of

the

microwave unit

using

of

groups

two, six,

hIf0ni NiOSH

i

Aij al

Ma5ieds

Feum

QMAN .

11didcn

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