Standard Operation Procedure of
Total Organic Carbon Analyzer In Prof. Wyman’s Wyman’s Laboratory 701
This is a simplified instruction of the operation hen the c atalyst and others or! ell. "ore detailed instruction and troubleshootin# could be found in the $ser’s "anual. %% The li&uid sample TO' ran#es from 0()00ppm* solid sample +dry ei#ht, 0(100 m# ith TO' )0(-0 currently. To To &uantify samples out of this ran#e/ further e&uilibrium of the catalyst and ne calibration ill be needed.
0. The check list for both liquid and solid samples analysis before you start: a. To fill fill the 'ooler 'ooler rain 'ontainer 'ontainer ith ith Water Water.. +o not bend drain drain tubin#/ tubin#/ as this may preent drain dischar#e., b. To fill the 2umidifier ith Wa Water ter c. To prepare prepare ilution ilution Water ater and needle rinsin# rinsin# ater ater d. To prepare prepare 2ydrochlo 2ydrochloric ric acid acid +34 for for 4PO' 4PO' and and T', T', e. To emp empty ty as aste te conta contain iner er f. To chec! chec! O5y#e O5y#en n pressu pressure re +at +at leas leastt 100 psi, psi,
6i#ure 1. 2umidifier/ rinsin# ater/ and to ri#ht
ilution Water and needle aste container from left
1. Liquid sample
analysis
I.
Standard
and Sample preparation
a. "a!e the ith TO' )00 prepared ith
standard #lucose solution ppm. This could be 0.1 #lucose standard solution by dilution
number 10. b. stimate the solution based dissoled in dilution Prepared by Taiying Zhang
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c. $se I ater to dilute dilute the solution solution ith ith pipet and balance balance into into the dry and clean clean sample ials ith the olume of )0 ml. d. Load the the samples samples into into the autosampl autosampler er as shon shon in middle middle of of 6i#ure 6i#ure 1. II.
Sample Analysis
a. Start. Start TO'('ontrol 8 from the Windos Windos Start menu/ and clic! the Sample Table Table ditor button. +The Sample Table Editor can also be started directly from the Windows Start menu and from the shortcut icon created on the desktop.)
The Sample Table ditor application starts up.
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b. Creating a Sample Table . 'lic! in the Sample Table tab of the file ieer/ or clic! on the toolbar. 1.
The Select 29W Settin#s indo is displayed.
3. Select the System to be used and enter a comment if necessary. :. 'lic! O;. < ne Sample Table is created/ and opened in the Sample Table ditor.
c. Creating a Calibration Curve File . < calibration cure file is created to set the analysis parameters for measurin# !non standard solutions and #eneratin# a calibration cure.
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1
'lic! New in the 'alibration 'ure tab of the file ieer. +The Calibration Curve Wizard (a!e ") System #nformation pa!e can also be displayed by selectin! $ile % &ew % Calibration Curve. The 'alibration 'ure Wi=ard +Pa#e 1, System Information pa#e is displayed.
3
Select the system confi#uration to be used.
:
'lic! Net. The 'alibration 'ure Wi=ard +Pa#e 3, 'alibration 'ure Type pa#e is displayed.
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)
nter the type of calibration cure. Note: ilution cannot be performed for I' measurement ith the TO'8 'P4. Since i. Standard Solutions 9 6i5ed ilution and i.Standard Solutions +auto correction of dilution factor, are not enabled/ select ilution from Standard Solution.
>
'lic! Net. The 'alibration 'ure Wi=ard +Pa#e :,
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analy=ed.
-
nter the basic analysis parameters.
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'lic! Net. The 'alibration 'ure Wi=ard +Pa#e ), 'alibration "easurement Parameters pa#e is displayed +default settin#s,.Su##ested 4o. of in?ection is :9> for hi#her accuracy. The unit shall be the same as
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that of the samples to be analy=ed. Su##ested unit is ppm.
@
nter the adanced parameters. ependin# on the
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B
'lic! Net. The 'alibration 'ure Wi=ard +Pa#e >, 'alibration Points List pa#e is displayed.
10 nter the adanced parameters for each calibration point. ependin# on the settin#s/ some items may not be displayed.
11 'han#e the calibration point parameters as necessary usin# the dit 'alibration Point Parameters dialo# bo5. ependin# o n the settin#s in the 'alibration 'ure Wi=ard +Pa#e 3, 'alibration 'ure Type pa#e/ the contents of the dit 'alibration Point Parameters dialo# bo5 may differ. ilution from Standard Solution is the su##ested method.
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The dit 'alibration Point Parameters dialo# bo5 is displayed as follos if the dilution settin# is i. Standard Solutions +auto correction of dilution factor,.
13 'lic! O! . The 'alibration 'ure Wi=ard +Pa#e >, 'a libration Points List pa#e is displayed.
1: 'lic! Net
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1) nter the remainin# parameters. Su##est to use the default settin#s.
1> 'lic! "inis#. The calibration cure file is saed. d. Creating a Method. 1 'lic! New in the "ethod tab of the file ieer. The "ethod Wi=ard +Pa#e 1, System Information pa#e is displayed. The 'ethod Wizard (a!e ") System #nformation pa!e can also be displayed by selectin! $ile % &ew % 'ethod.
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3
Select the system to be used.
:
'lic! Net. The "ethod Wi=ard +Pa#e 3,
)
nter the basic method information.
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>
'lic! Net. The "ethod Wi=ard +Pa#e :, 'alibration 'ures pa#e is displayed.
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Select the calibration cure files that ill be incorporated into the method. $p to : calibration cure files can be selected. If multiple calibration cure files are selected/ the softare selects the most suitable calibration cure durin# the analysis. 6or information on this function/ refer to the folloin# pa#e.
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7
'lic! Net.
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@
Set the adanced analysis parameters. ependin# on the
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B
'lic! Net. The "ethod Wi=ard +Pa#e >, Pea! Time Parameters pa#e is displayed.
10 nter the pea! detection parameters.
11 If there is a 4e5t button at the bottom of the pa#e/ clic! it and repeat this procedure from step -. Note: If the
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e. Editing the Sample Table.
1. Insert the calibration cure +standard solutions, into the Sample Table. ra# the calibration cure file from the 'alibration 'ure tab of the file ieer.
3. Insert the un!non samples into the Sample Table. ra# the method file from the "ethod tab of the file ieer.
When analy=in# multiple samples usin# the same cond itions/ the inserted sample can be reproduced by copyin# and pastin#. Select the inserted sample/ ri#ht(clic! in the cell at the left end of the ro/ and clic! 'opy.
Select the ros in the Sample Table correspondin# to the number of samples to
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set/ ri#ht(clic! in the cell at the left end of the ro/ and clic! Paste.
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:. 'lic! $ial number in the Sample Table.
). nter the ial numbers. nter a number in a 8ial column cell/ clic! on the loer ri#ht part of the cell/ and dra# donard to enter a series of sample ial numbers all at once. >. 'lic! O; to close the indo and automatically set all of the ial numbers in the Sample Table. f. Run the Samples Analysis
1
Open the Sample Table/ and connect to the Instrument by clic!in# Connect. Turn on carrier gas %oygen &' psi(
The ready state of the instrument is shon at the ri#ht end of the toolbar.
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3 :
) >
'hec! the bac!#round. Aun the analysis by clic!in# Start.
Select the procedure to be performed hen the analysis se&uence is complete. C ;eep runnin#D The instrument remains in the Aead y state at the completion of the analysis se&uence een after analysis is completed. C Shut don instrumentD The instrument automatically turns off at the completion of the analysis se&uence. C SleepD The instrument enters the sleep state/ and restarts at a specified date and time. Su##est to !eep runnin#. 'lic! Start to be#in the analysis se&uence. 8ie and Output the
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The sample indo is displayed. ach of the sample analyses can be reieed.
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Output to a 6ile. 'lic! 6ile E
7
ndin#
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Select the appropriate shutdon process. C Shut don instrumentD The instrument poer turns off after about :0 minutes. C SleepD The instrument enters a sleep state/ and restarts automatically at a specified date and time.
Su##ested to leae it on unless it ill be idle for lon#er than to ee!s or poer outa#e.
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1I. Solid sample analysis %% Solid sample analysis includes to modulesD T' and I'/ hich re&uire different treatments of sample boats and Fuart=(#lass filter paper. Note: ue to the potential loss of crystal solid durin# the combustion/ recommend to use the standard solution other than solid/ especially ithout Fuart=(#lass filter paper. The stand used to hold sample boats durin# analysis should be made of an inor#anic material/ such as ceramic/ #lass/ or metal/ ith a surface free from contamination.
a. Sample Boats, Measurement Tools, and Quartz!lass "ilter #aper 2eat the sample boats in a furnace to o5idi=e any carbon content. $se an electric furnace of the type normally used in a laboratory. Note: Tee=ers are supplied to handle sample boats. 2eat the tip of the tee=ers that contacts the sample boat to red hot in the furnace or ith #as burner to o5idi=e any attached carbon #rocedure for T$ %nalysis ". 2eat the sample boat in the furnace at appro5imately B00G' for 30 minutes. 2eat the &uart=(#lass filter paper in the furnace at appro5imately -00G' for 30 minutes. . Store the heat(treated sample boat/ &uart= #lass filter paper and tee=ers in a clean container or case.
a. Sample #reparation $sin# a ne sample boat for each sample is recommended. 2oeer/ a sample boat may be reused if the sample analy=ed does not contaminate/ modify/ or de#rade the sample boat material. o not reuse the &uart=(#lass filter paper.
Sample Boat $leanin! #rocedure &T$' 1. Aemoe as much of the sample remainin# in the used sample boat as possible. 3. $se a brush or the tip of a scraper to scrape off pieces adherin# to the bottom of the sample boat. :. Soa! the boat in appro5imately 3" sulfuric acid or hydrochloric acid for about 10 minutes. ). Wash under runnin# tap ater for seeral minutes. >. Ainse the tap ater off the boat ith de(ioni=ed or distilled ater. ry the boat. -. Ha!e the dried sample boat in a furnace at appro5imately B00G' for 30 minutes. Note: • aluate hether a sample boat can be reused b y runnin# a blan! test +an analysis ith no sample in the boat, to determine the amount of residual carbon. • 6or some samples/ it may not be possible to reuse the sample boat een after performin# the aboe treatment procedure. In these cases/ use a more appropriate method to remoe the residual material from the sample boat or use a ne sample boat.
$eramic "iber 'eramic fiber can be reused in cases here a pure product/ such as #lucose/ is measured as the standard.
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The combustiono*idation reaction (TC analysis) and the carbonate acidification reaction (#C analysis) are more efficient when the sample particles are smaller in size.
(ryin! the Sample Solid samples may be ei#hed and measured directly after samplin# or they can be dried before they are ei#hed and measured. The folloin# three methods are used to dr y samples before ei#hin#. 1, heatin# ith an electric isothermal dryer 3, air(dryin# oer a spread(out sample :, free=e dryin# Select the appropriate method for the analytical ob?ecties.
Note: 8olatile or#anic components contained in a sample may be lost durin# dryin#. Solid Samples Wei#hin# accuracy is directly reflected in the accuracy of the analysis results. To reduce errors associated ith ei#hin#/ use an analytical balance or microbalance to carefully ei#h the sample directly into a tared heat(treated sample boat. Note: • Aeduce the effects of poor distribution/ hich commonly occur ith solid samples. • Aeduce the ei#hin# error. • Aeduce the impact of e5ternal contamination/ by choosin# a sample a mount that ill produce a result close to the upper limit of the instrument +about :0m# ',. Note: 'onsider the combustion characteristics of each indiidual sample hen determinin# the amount of sample. ue to a lac! of o5y#en durin# combustion/ samples that burn e5tremely rapidly tend to burn less completely ith increasin# sample si=e.
Analyzing Crystalline Samples Suc# as Oalic Acid or )lucose 'oer the sample boat because these samples ma y scatter durin# combustion. If part of the sample scatters out of the sample boat durin# combustion/ artificially lo and inaccurate results ill be obtained. $se the supplied ceramic fiber to coer the sample. 'eramic fiber allos #ood entilation and is unaffected by heat and o5y#en. 6ashion a lon#/ thin coer from ceramic fiber to rou#hly coer the openin# of the sample boat/ and place it oer the sample. o not coer the sample boat for I' analyses.
)iquid Samples The folloin# to samplin# methods are aailable for li&uid samplesD
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1, Wei#hin# the sample ith a balance 3, "easurin# the olume of the sample ith a microsyrin#e or pipette Note • The ma5imum measurable mass of a li&uid sample is 0.># for T' and 0.:# for I'.
b. Sample table and analysis To edit the sample table is the same as the li&uid sample ith
With SS"/ the sample could be loaded one b y one manually as shon in the folloin# fi#ures.
Note • The O(rin# is easy to pull out hen the lid is pushed too closely/ so the nut shall be loosen enou#h before slidin# the lid.
6i#ure 3.Solid sample module close +left, and op en +ri#ht, The in?ection number and sample amount are not shon in the sample table/ hich as input as selectin# repeat or ne5t sample durin# the test.
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The reie and output of the results could be performed in the same ay as the
I' process need be deeloped later since e hae not tested it yet. #rocedure for *$ %nalysis. ". Soa! the sample boat in 3 or :" hydrochloric acid for about 10 minutes. . Ainse ell ith purified ater and dry in an oen. #reparin! the $eramic "iber When analy=in# a sample that may scatter durin# combustion/ cut off a suitable amount of supplied ceramic fiber and coer the sample ith it. 2eat the ceramic fiber in the furnace/ as described for the sample boat. +eat the $eramic "iber ". 'ut off a suitable amount of ceramic fiber for a sin#le an alysis +appro5. )0 to -0m#,. . Shape the ceramic fiber to about :>mm lon# 5 10mm ide. +. 2eat the ceramic fiber/ as described for the sample boat. ,. $se the heat(treated tee=ers to insert the heat(treated ceramic fiber into a clean container or case for stora#e.
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*$ %nalysis of $arbonates
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List o* Aut#orized +sers o* TOC If you name is not on this list/ please contact responsible user to set up a trainin#. I 1
$ser name +please type,
Si#nature
ate authori=ed
4ote
Taiyin# han#
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responsible user
3
2on#?ia Li
@(3:(3010
responsible user
:
eepti Tan?ore+J,
@(3:(3010
)
Fin# Fin#
@(3:(3010
> 7 @ B 10 11 13 1:
-esponsible users Taiyin# han#/ B>1(7@1(>7@0+o,/ :1B(>)1(:)@)+cell,/ taiyin#Kcert.ucr.edu 2on#?ia Li/
To boo! any spot to use the TO'/ please do it by #oo#le calender. If you hae no access to it/ please email Taiyin#.
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