TSSSOP

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STANDARD OPERATING PROCEDURE

for determination of

Total Solids, Total Suspended Solids

and Total Dissolved Solids

in Aquatic Systems

(SM19-2540)

Environmental a!oratory59 "olle#e Avenue

$%&% $esleyan "olle#e'ucannon* $& 2+201-2995

,evision . /

ate. 4-9-00

a! Suervisor.

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1.0 SCOPE AND PURPOSE6atural 7aters contain varyin# amounts of solid materials in a 7ide ran#e of

si8es% issolved su!stances include individual molecules* ions* atoms and colloids(te smallest clay articles)% articulates or susended solids are lar#er articles ofmineral or or#anic material from lar#e clays u to sand% otal solids (S) refers to te

mass er unit volume of dissolved and susended solids% otal dissolved solids (S)refers to te mass er unit volume of solids tat can ass trou# a 2%0 µm filter% otal

Susended Solids (SS) is te mass er unit volume of solids tat are retained !y a

2%0 µm filter%

2.0 ATERIA!S AND E"UIPENTEquiment

ryin# oven tat can !e set to :0* 95 and 105°"

Analytical !alance (measures do7n to 0%0001# ; 0%1 m#)&acuum umMa#netic stirrer

Materials150- or 250-m !eaers (/ er samle)mem!rane filters (#lass fi!er filters< 4=mm< $atman 9/4A>< / er samle)t7o desiccators 7it desiccant100-m #raduated cylinders50-m #raduated cylinder 10-m ietsiet !ul!s or ums

stir !ar forcesmem!rane filter funnels500- or 250-m sidearm flasston#s or insulated #loveslar#e aluminum 7ei#in# dises (/ er samle)500-m olyetylene samlin# !ottles* la!eled%

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#.0 SAP!ING PROCEDURE• Samle !ottles sould !e made of an inert material lie i#-density olyetylene

(>E)* lo7-density olyetylene (E) or olyroylene ()% $ide-mout!ottles are essential for collectin# samles for sediment analysis% All samle !ottlessould !e 7ased 7it soay (osate-free soa?) 7ater* rinsed in ta 7ater*soaed in 5@ >"l for at least 10 minutes and rinsed four times 7it ultra-ure

($) 7ater%

• A field !lan sould !e included 7it eac !atc of samles% Bill a samle !ottle

7it ultra-ure ($) 7ater and carry it 7it te oter samle !ottles 7ile you aresamlin#%

• e amount of sediment !ein# measured can !e minute* terefore any

contamination of te interior of te !ottles or cas !y soil* fin#errints* or even dustcan alter te test results% Cee !ottles caed until you are ready to collect tesamle% ,elace te ca immediately after fillin# te samle !ottle%

• Dust !efore collectin# te samle* fill out te la!el on te !ottle% Eac !ottle la!el

sould contain te date* time (24-r)* samlin# location* samle num!er* andcollectors name%

• $en collectin# te 7ater samle* try to samle as close to te middle of te

stream as ossi!le% A simle samlin# ole can !e constructed from a !room sticand an adFusta!le duct clam%

• ,emove te ca* su!mer#e te !ottle in te 7ater 7it te !ottle oenin# facin#

ustream% Mae sure any art of you tat is in te 7ater is do7nstream from te!ottle% "ollect 7ater from te uer 10 cm of te stream% f te stream is sallo7*do your !est to avoid stirrin# u sediment% ry not to #et !u#s* leaves* stics* etc%in te !ottle%

• lace te filled !ottle in an ice cest 7it ice acs to !rin# te temerature of te

samle as close to 4" as ossi!le% ,efri#erate te samles as soon as ossi!le toslo7 do7n decomosition of or#anic matter%

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$.0 SAP!E PREPARATION$.1. P%e&'ei()in( t)e *ea+e%s -o% TDS and TS onl/ $as te !eaers if necessary% a!el te !eaers usin# tae and ermanent

marer% lace in oven at 105" for at least one our%

,emove from oven and lace in desiccator to cool% nce cool* 7ei# to te nearest

0%0001 # (; 0%1 m#) and record te 7ei#t as ea+e% p%e&'ei()t in SS la!note!oo%

Store uside-do7n in a clean* dry* covered container until ready to use%

$.2. P%e&'ei()in( t)e -ilte%s -o% TSS, TDS and TS/ a!el te #lass fi!er filter aers 7it num!ers (eac samle 7ill !e filtered tree

times)% lace in aluminum !oats in oven at 105" for at least 2 ours% Mae surevent on oven roof is oen%

,emove from oven and lace on clean rac in desiccator to cool% nce cool* 7ei#to te nearest 0%0001 # (; 0%1 m#) and record te 7ei#t as ilte% p%e&'ei()t inSS la! note!oo%

Store in a clean* dry* covered container until ready to use%

.0 ANA!3SIS.1. ilt%ation

Sae samle !ottle vi#orously to susend any sediment tat as settled on te!ottom% lace samle !ottle on ma#netic stirrer and add a stir !ar% Set stir seed sotat all articles are susended%

Assem!le filter aaratus (vacuum um* side arm flas and funnel !ase)% Gsin#forces lace one of te re7ei#ed filters on te funnel !ase% Attac te funnelto% urn on vacuum and rinse 7it a!out 20 m of 7ater to moisten te filter%iscard filtrate%

,emove samle from te stirrer and raidly add approximately 200 m of samle tote funnel and allo7 to filter% ransfer te filtrate to a re-rinsed* #raduated cylinderand record te sa4ple volu4e% ,eassem!le te filter aaratus and rinse te

funnel and filter aer 7it aroHimately /0 m of 7ater% "ontinue suction for /minutes after filtration is comlete% Add tese 7asin#s to te samle filtrate%ransfer filtrate to one of te re-7ei#ed !eaers%

Gsin# forces transfer te filter aer to a la!eled aluminum 7ei#in# dis%

$as filter aaratus and dises%

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.2. easu%in( D% ass

lace !eaers 7it filtrate in an :0°" oven and eat until all te liquid as

evaorated% nce te 7ater as !een removed* increase oven temerature to105" for at least t7o ours% lace in desiccator to cool !efore 7ei#in#% $ei# to

nearest 0%0001# (0%1 m#) and record as ea+e% post&'ei()t in SS la!note!oo%

lace aluminum dises 7it filters in :0°" oven for at least 24 ours% ,aise

temerature of oven to 105°" for at least t7o ours (tis recaution revents filters

from sticin# to te aluminum dis)% lace in desiccator to cool !efore 7ei#in# tefilter aer only% ,ecord mass as ilte% post&'ei()t in SS la! note!oo%

iscard filters% urn off oven%

5.0 Cal6ulations, Units and Data Re6o%din(

otal issolved SolidsS (m# -1) ; ('eaer ost-$ei#t (m#) - 'eaer re-$ei#t (m#))I1000

Samle &olume (m)

otal Susended SolidsSS (m# -1) ; (Bilter ost-$ei#t (m#) - Bilter re-$ei#t (m#))I1000

Samle &olume (m)

otal SolidsS (m# -1) ; S (m# -1) J SS (m# -1)

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7.0 "UA!IT3 ASSURANCE8"UA!IT3 CONTRO!7.1. P%e6ision C)e6+ Dupli6ate/ Sa4ples

Bor every 10 samles analy8ed* include a P%e6ision C)e6+ samle.

a% After analy8in# 10 samles* rocess a dulicate samle% A dulicate is asecond su!samle removed from a samle !ottle and carried trou# te

entire analysis% ,ecord te result in te K" section of te a!oratory'enc Seet%

!% After te rocedure as !een comleted* fill in te recision "ontrol"art% "alculate te SS (and S and S* if alica!le) for te samleand for te dulicate usin# te equation in section +%0% en* calculatete a!solute value of te difference (D) !et7een te 2 dulicate samles%

c% Bind te recision "ontrol "art for SS in te SS a!oratory6ote!oo% Bill in te neHt ro7 on te cart 7it te date and dra7 a dotso7in# te value of te difference (D) you Fust calculated%

d% f D is 7itin te $ on te cart* te analysis is acceted%

f D eHceeds $* !ut not " and if te revious oint 7as !elo7 $* teanalysis is acceted%

f D eHceeds te "* analy8e anoter dulicate as soon as ossi!le% fte reeat is 7itin te "* te ori#inal analysis is acceted< if it stilleHceeds "* determine te source of error and reanaly8e all te samles%

f t7o out of te last tree oints on te #ra eHceed $* analy8eanoter dulicate as soon as ossi!le% f te reeat is less tan $*accet te analysis< if it still eHceeds $* determine te source of errorand reanaly8e all te samles%

7.2. A66u%a6 C)e6+Bor assessin# A66u%a6 te annual erformance Evaluation ata 7ill !e usedand reorted in te a!oratory 6ote!oo%

7.#. et)od lan+sBor every 10 samles include a DDI9 *lan+ samle% Bilter it Fust as you 7ould

a normal samle% Su!tract te !lan value from all samle values%

7.$. ield lan+s

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7ice a year* include a -ield *lan+% Add $ to a clean samlin# !ottle andcarry it into te field durin# samlin#% en analy8e it as if it 7ere a samle%,ecord te results in te K" section of te a!oratory 6ote!oo%

7.. D!s

e et)od Dete6tion !i4it D!/ is determined once er year !y rocessin#several lo7 concentration samles trou# te comlete analytical metod(includin# filterin#* stora#e* di#estion* dilution* addition of reservatives orrea#ents* etc%)%

a% "ollect 2 liters of river or stream 7ater% ae seven 200-m su!samlesfrom tis samle and rocess eac trou# te entire analysis% "alculatete standard deviation (s) of te = values% Estimate te M in tefollo7in# manner.

M for SS (m# -1) ; t I s

7ere t is te t-value from a one-sided t distri!ution at te 99@ level and +de#rees of freedom (t ; /%14/)% nclude tese results in te a!oratory6ote!oo and reort te M in all la!oratory reorts%

7.5 P%e6ision Cont%ol C)a%tnce eac year construct a P%e6ision Cont%ol C)a%t% "ollect from reviousanalyses* te most recent 20 airs of values reresentin# recision "ecsamles% Alternatively* collect 20 samles of stream 7ater (durin# i# flo7)and erform dulicate analyses on eac% Enter te 20 airs of num!ers into terecision $orseet on EL"E (in m# -1)% "alculate te difference () of eacair* ten te Mean ifference and te standard deviation of te 20 differences%"alculate te 7arnin# limit ($) and te control limit (") as follo7s.

$ (m# -1) ; Mean ifference I 2%51

" (m# -1) ; Mean ifference I /%2=

e $ aroHimates te 95@ confidence limits for differences !et7eendulicates% at is* on avera#e only 1 out of 20 dulicate analyses souldeHceed te $% e " aroHimates te 99@ confidence limits* meanin# tatno more tan 1 out of every 100 dulicate analyses sould eHceed te "% Gse

tese values alon# 7it te Mean ifference to construct a recision "ontrol"art eac year (see KA lan for eHamle)%

=

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:.0 Re-e%en6es

American u!lic >ealt Association% 1995% Solids.2540 In (A%% Eaton* %S% "lesceriand A%E% reen!er#* eds%) Standard Metods for te EHamination of $ater and$aste7ater% 19t ed% A>A* $asin#ton* "% section 2* % 5/%

G%S% Environmental rotection A#ency% 19:/% Metods for "emical Analysis of $aterand $astes% Environmental Monitorin# and Suort a!oratory* "incinnatti* >%EA-+0034-=9-020%

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