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text:
I went out to eat the other night, and while I am not a complainer, I was a bit annoyed when I didn't get my silverware until like, 10 minutes after I got my food.
That got me thinking, what was the worst dining experience you ever had?
I'm actually pretty pissed off that springs ruined my good time last night. Godzilla was totally abandoned.
I know it may look like I was being like a bitch, but that's only because I was acting like a bitch.
We had a server once that couldn't take his eyes off the big screen TV on the wall that had a football game on. Not while he was taking our orders, or bringing our drinks, or our food.... and that was pretty much the only time he came to our table. He was too busy standing in the middle of the room watching the game. I think we left him a 14c tip.
There's been a few times when servers asked us if we wanted change, but like a pp said, it was always at a cheap place and never over $5. I don't really consider it rude in those circumstances, since it's a pretty laid-back atmosphere in the first place, but I would be pretty shocked if our server asked for a $14 tip.
Let your NADs enjoy the refreshing taste of Debate Team Chat!
I was just wondering if it was a tactic. Yeah I could see tips depending on the place, but this was Texas Roadhouse. A chain where I'm sure she would've made plenty not asking for change. It was kinda stupid really.
I just assumed if you were banned, you were banned. I guess not everyone is stupid enough to announce that they were banned. "Look at my new SN!"
"Welcome to the shit show." ~ Nurse Jackie
Long time server here. I never ask if the customer needs change. I do say, "I will be right back with your change", giving them a chance to say they don't need change. If it's not busy I don't say anything, bring change. If I am slammed, I say be right back line just in hopes to have one less thing to do if they don't need it back. If I saw a $50 down for a $36 bill, I would bring change back without saying a word.
Welcome back Springs. Oh, and cutting in line was a punk ass move.
screw you guys you'll never figure out who i am
ETA I am glad I have provided ample entertainment for your weekend.
I'm an adult? When did that happen and how can I make it stop?
I think I need to spend more time on BHB to fully understand what is going on.

subset: commoncrawl


text:
I'm sure I'm not the only one...
I had my first loss back in Februay at 16 weeks and my most recent one on 12.23 at 20 weeks.,
I want to crawl in a hole with a case of wine....
"Nothing in this world is more dangerous than sincere ignorance and conscientious stupidity" ~ MLK
2 baby boys in heaven and a little girl on Earth.
I've had 5 losses, 2 of which happened in December. I'm having a very difficult time of it. I should be holding a 4 month old right now. >.< Ugh. Is it 2013 yet?
Me: Teri, 37 DH: Anton, 31 TTC since June 2010 w/ PCOS, Hashimotos, MTHFR, Septum. Mom to 6 angel babies.
I hear you all. Sometimes I want to throw a shoe at the television and all the happy endings, it seems so insensitive sometimes to those that are going through losses. Hope and prayers for a better 2013 to us all!
I was so happy when I found this board, it is nice to know that there are other women who are struggling to concieve and have miscarriages. I just wish we all met under better circumstances!
"Nothing in this world is more dangerous than sincere ignorance and conscientious stupidity" ~ MLK
2 baby boys in heaven and a little girl on Earth.
definitely NOT the only one. Hugs!
We delight in the beauty of a butterfly, but rarely admit the changes it has gone through to achieve that beauty. ~Maya Angelou
Wow....5 losses. I am so sorry. I am having my 3rd and I'm devastated. This is one of the hardest struggles I have ever had in my life. Hugs to all.
Emily-34 DH-34 DD 7-16-09 DS 4-3-14
Forever missing 4 angels.
Right there with you...2012 was not my year thats for sure. Just had our 3rd loss week before Christmas, and was still going through all of the physical aftermath throughout Christmas. Happy to be with loved ones, but having to "hide" the physical pain and discomfort was a downer. Although this is the third this year, this one was the most difficult as before we were hoping it was just "coincidence" and now we have to face reality that there may really be a problem...Hoping and praying that this year will bring rainbows!!!
TTC#2: (3 losses) BO April '12, mc Aug '12 (12 weeks), mc December '12 (9 weeks)


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Edited by Lady Shade, 13 November 2013 - 12:15 AM.
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A room in our new house
Creepy feeling in new homescary emf creepy
Started by Lady Shade , Nov 13 2013 12:14 AM
Started by Lady Shade , Nov 13 2013 12:14 AM
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|Republic of Iceland
Lýðveldið Ísland
|Anthem: Lofsöngur
Location of Iceland (dark green)
on the European continent (dark grey) — [Legend]
and largest city
|National language
|Ethnic groups (2013[1])
|Unitary parliamentary constitutional republic
|Ólafur Ragnar Grímsson
|Prime Minister
|Sigurður Ingi Jóhannsson (acting)
|Speaker of the Althing
|Einar Kristinn Guðfinnsson
|9th century
|Union with Norway
|Danish monarchy
|5 January 1874
|Kingdom of Iceland
|1 December 1918
|17 June 1944
|103,001 km2 (108th)
39,770 sq mi
|Water (%)
|1 January 2015 estimate
|329,100[a] (182nd)
|3.2/km2 (233rd)
8.29/sq mi
|2012 estimate
|$12.831 billion[2]
|Per capita
|GDP (nominal)
|2012 estimate
|$13.654 billion[2]
|Per capita
|Gini (2010)
low · 1st
| 0.906[3]
very high · 13th
|Icelandic króna (ISK)
|Time zone
|Summer (DST)
|not observed (UTC)
|Drives on the
|Calling code
|Internet TLD
|^ "Statistics Iceland:Key figures". Statistics Iceland. 1 October 2002. http://www.statice.is/?PageID=1390. Retrieved 2011-07-02.
|^ "CIA – The World Factbook – Field Listing – Distribution of family income – Gini index". United States government. https://www.cia.gov/library/publications/the-world-factbook/fields/2172.html#Govt. Retrieved 14 September 2008.
Iceland (Icelandic: Ísland) is an island country in the North Atlantic, between Greenland and Norway, formerly a possession of Denmark. It is culturally considered to be part of Europe. Iceland is 300 kilometres east of Greenland and 1000 kilometres west of Norway. There are about 329,100 people who live in Iceland. Iceland has an area of 103,000 km².
History[change | change source]
The first people who lived on Iceland are thought to have been Irish monks. They came to Iceland around the year 800.
In the 9th century, Norsemen went to live in Iceland. The first Norseman who lived in Iceland was Flóki Vilgerðarson. He was also the one who gave Iceland its name. Ingólfur Arnarsons
, a chieftain from Norway went to live in South West Iceland. He founded the city of Reykjavík.
In 930, the Icelandic rulers wrote a constitution. They created the Althing, a kind of parliament in a place called Þingvellir. Therefore, Iceland is the oldest existing republic.
In 985, Erik the Red was sent away from the island because he had killed someone. He sailed to the west and discovered Greenland. Eric's son Leif Ericson discovered America in the year 1000. He called it Vinland. The voyages of Eric, Leif and others were written down in the sagas (long stories).
In 1262, Iceland became part of Norway. This lasted for 400 years. In 1662, it became part of Denmark. In the 19th century, many Icelanders wanted to be independent from Denmark. In 1918, Iceland got many powers of its own, but the king of Denmark was still king of Iceland.
When Germany took over Denmark on April 9 1940, the Althing decided that Icelanders should rule the country themselves, but they did not declare independence yet. British and later American soldiers occupied Iceland to prevent it from being attacked by the Germans. In 1944, Iceland finally became fully independent.
After World War II, Iceland became a member of the North Atlantic Treaty Organisation (NATO), but not of the European Union. Between 1958 and 1976, there were three debates between Iceland and the United Kingdom about the rights to catch codfish. They were called the Cod Wars.
In 1980, Vigdís Finnbogadóttir was elected president of Iceland. She was the first woman ever to be elected president of a country.
Politics[change | change source]
Iceland has a multi-party system. Since the 2013 election, the centre-right Independence Party and Progressive Party are the biggest political parties in Iceland. Other powerful parties in Iceland include the centre-left Social Democratic Alliance and Left-Green Movement. See also: List of political parties in Iceland.
Iceland is a representative democracy and a parliamentary republic. Iceland has a president (Ólafur Ragnar Grímsson) and a prime minister (Sigurður Ingi Jóhannsson). The parliament, Althing, has 63 members and each member can only be in there for four years[4]. The president is elected by Icelanders, and is in government for four years. The president can be elected an unlimited amount of times.
Iceland has no standing army. The United States Air Force had a base near Reykjanesbær, but they left in 2006. Since 2008, NATO nations have occasionally had their air force patrol Iceland. This was requested by the Icelandic government[5][6].
Economy[change | change source]
Fishing and fish processing is the main economic activity in Iceland.[7] Despite effort to diversify, particularly into the travel industry, seafood exports continue to account for nearly three-quarters of merchandise exports and approximately half of all foreign exchange earnings.
Geothermal Energy produces the vast majority of Electrical Power consumed on Iceland, due chiefly to the island's position atop the Mid-Atlantic Ridge and exhibits plentiful hot water reservoirs and geysers. This has the effect of drastically reducing the price of electricity in Iceland, and has attracted several energy-intensive industries.
Aluminum Smelting (The reduction of Aluminum ores to Aluminum metal) is the largest energy-intensive manufacturing sector in Iceland, and the country produced over 800,000 Metric Tonnes per Year in 2013,[8] making it the 10th largest producer of Aluminum metal worldwide.
Geography[change | change source]
Iceland is very geologically active and combined with large amounts of rain and snow caused by the warm waters of the gulf stream current which flow toward it, many interesting and unusual geographic features have developed which make it different from any other island so close to the Arctic Circle.
Some of these features are Iceland's numerous mountains, volcanoes, hot springs, rivers, small lakes, waterfalls, glaciers, and geysers. The word geyser is, in fact, derived from Geysir, the name of a particularly famous geyser on the southern side of the island. Glaciers cover approximately 11% of the island and the largest, Vatnajökull, is up to 1 km thick and, by far, the largest glacier in Europe.
Iceland, though considered to be a European country, sits partly in North America since it straddles the Mid-Atlantic Ridge which marks the boundary between the Eurasian and North American tectonic plates. The ridge runs directly through the populated Reykjavik and Thingvellir historic areas, and the tectonic activity of these plates separating is the source of the abundant geothermal energy in the region.
Towns and cities[change | change source]
Reykjavík is the capital city of Iceland. Reykjavík is also the most important port in Iceland. Other important towns in Iceland are Akureyri, Kópavogur, Hafnarfjörður, Keflavík, Seyðisfjörður and Vestmannaeyjar.
People[change | change source]
The people in Iceland are mostly of Scandinavian origin. The language they speak is Icelandic. The language has not changed much in 1,000 years, so Icelanders are still able to read the sagas about the Vikings without many problems. Most people in Iceland are Christian. Most of them are Lutheran.
Icelandic people are considered to be the happiest people on Earth.[9] Iceland has the highest birth rate in Europe, highest divorce rate and the highest percentage of women working outside their home.[9]
Names[change | change source]
There are no real surnames on Iceland. Children get the first name of their father (sometimes mother) with -s+son if it's a boy, and -s+dóttir if it's a girl. For example, a man named Jón Stefánsson has a son named Fjalar. Fjalar's last name will not be Stefánsson like his father's, it will become Fjalar Jónsson. The same goes for women. Jón Stefánsson's daughter Kata would not have the last name Stefánsson, she would have the name Jónsdóttir. In most countries people use to call other people by their surname, but in Iceland people call other people by their first name. So when people talk about Halldór Ásgrímsson they do not call him Ásgrímsson, but Halldór.
References[change | change source]
|The Simple English Wiktionary has a definition for: Iceland.
- ↑ "Population by country of citizenship, sex and age 1 January 1998-2013". Reykjavík, Iceland: Statistics Iceland. http://www.statice.is/Statistics/Population/Citizenship-and-country-of-birth. Retrieved 3 April 2013.
- ↑ 2.0 2.1 2.2 2.3 "Iceland". International Monetary Fund. http://www.imf.org/external/pubs/ft/weo/2013/01/weodata/weorept.aspx?pr.x=60&pr.y=9&sy=2009&ey=2012&scsm=1&ssd=1&sort=country&ds=.&br=1&c=176&s=NGDPD%2CNGDPDPC%2CPPPGDP%2CPPPPC%2CLP&grp=0&a=. Retrieved 2013-04-17.
- ↑ "Human Development Report 2013". United Nations. 2013. http://hdr.undp.org/en/media/HDR2013_EN_Complete.pdf. Retrieved 14 March 2013.
- ↑ "Government & Politics". Iceland.is. http://www.iceland.is/government-and-politics/. Retrieved 10 February 2010.
- ↑ "French Air Force in Iceland". Ministry for Foreign Affairs. 5 May 2008. http://www.mfa.is/speeches-and-articles/nr/4240. Retrieved 2 October 2010.
- ↑ "Air Policing". NATO Air Command Operations. http://www.aco.nato.int/page142085426.aspx. Retrieved 2 October 2010.
- ↑ "Iceland economy". http://www.fisheries.is/economy/fisheries-impacts/employment/. Retrieved December 16, 2013.
- ↑ Hjalti Jóhannesson. "Aluminium overtakes fish in Iceland". Nordregio website. http://www.nordregio.se/en/Metameny/About-Nordregio/Journal-of-Nordregio/Journal-of-Nordregio-no-2-2011/Aluminium-overtakes-fish-in-Iceland/. Retrieved 10 August 2014.
- ↑ 9.0 9.1 "No wonder Iceland has the happiest people on earth". The Guardian.com. http://www.theguardian.com/world/2008/may/18/iceland. Retrieved September 24, 2013.


text:
f/8 and Be There
Fred Lynch has captured images for the Southeast Missourian since 1975, in that time moving from black-and-white to color, from film to digital and to video. The blog title is a nod to an earlier era of news photography and the 4x5 Speed Graphic: It's more important to be there for the shot than to worry about technical details.
Midweek Mystery: Frony's Shadow
Posted Wednesday, September 8, 2010, at 7:30 AM
We don't know anyone in this group, but we can certainly identify the shadow.
G.D. Fronabarger could not avoid the sun behind him as he took the picture in front of the Hotel Marquette on Broadway in Cape Girardeau. The date is unknown.
- Parker helps establish SEMO campus museum (05/04/16)
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- Modern scoreboards at Capaha Field (04/27/16)
- Wayne & Eva Rust mark 48 years in business (04/25/16)
- Tourist train begins operation in Jackson (04/20/16)
- State College swim team 1971 (04/18/16)
- R.B. Potashnick builds lake for Boy Scouts (04/13/16)
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- -- Posted by redpen on Wed, Sep 8, 2010, at 7:36 AM
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text:
Official: 2 suspects in French standoff came out shooting
Officials say the brothers died in the assault.
Sponsored by:
Officials say the brothers died in the assault.
Charged with raping and killing his high school math teacher want to have his police confession dismissed as evidence.
A sweeping proposal that would make higher education as accessible as a high school diploma.
Terrorists linked to each other seized hostages at two locations around Paris on Friday.
The man opened fire in the kosher market, near Paris' Porte de Vincennes, and declared "you know who I am."
President pays respects to those killed in Paris attack.
US trying to break a 28-year games "drought".
The father of a 5-year-old girl pulled his daughter from the back seat of his car and then threw her off a bridge.
Connecticut Supreme Court rules teen must continue to undergo chemotherapy against her will.
Michigan family terrified as they're dragged 16 miles after rear-ending tractor-trailer.
Cold snap brings record-setting temperatures to much of the nation.
A tour bus crashed Thursday near the Arizona-Mexico border, injuring more than 20 people.
Collapsed at a school during a recreational soccer practice.
Calling his attorney "God" and asking her to translate a Bible in Swedish.
Fort Bliss increased random vehicle searches and checks of proper registration Wednesday.
Europe's resurgent far-right and anti-immigrant parties trumpeted a unified message: I told you so.
It was located off the coast of Punta Leona.
When a sick little girl wanted a fireworks show, people in her northeast Missouri community found a way to grant the wish.
Police say the dad pulled the girl from the back seat of his car and tossed her over a bridge.
Massive I-80 wreck shots down freeway for most of the day.
Dealers will apply a corrosion-fighting wax to a brake line connector at no cost to owners.
Now, the French are trying to understand why.
Wet gloves, socks or boots speed up the process.
The goal is to prevent disease caused by contaminated water supplies.
Snake was found in San Diego office building.


text:
Searched for: "master your domain windows server active directory domain services"
Content Types
About 115 results for "master your domain windows server active directory domain services"
Five budget-friendly open source storage servers
Open source servers are a good choice for many enterprise storage needs. Here are five excellent tools that are ready to help you build and deploy.
How to automate workflow tasks with DeployStudio
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Pro tip: How to configure a Golden Triangle
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Publishing Chrome in a Citrix virtualized environment
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Top iPad apps for IT managers
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DIY: LDAP user management with LAM
Jack Wallen has tried a lot of LDAP administration tools, and he says they all pale in comparison to LDAP Account Manager. Get details about this powerful tool.
The easiest way to set up Samba for file-sharing
Samba is directly compatible with Windows and allows for a lot of configuration, but if you just want a stand-alone Samba server on your network, it's an easy setup. Vincent Danen shows you how.
10 tips for effective Active Directory design
The way you design your Active Directory can make a huge difference in how well your network functions and how easy it is to administer. These best practices will help you maximize efficiency, simplif...
How do I configure RSync on FreeNAS to sync shares with a Windows NAS device?
Donovan Colbert illustrates how to create a suitable, inexpensive data replication solution for a small office or data center on a limited budget.


text:
To slow down or even stop these "Short term or Day Traders". The ones that don't let a stock get to it's full price potential should be assessed a substantial penalty.
Something along these lines:
Shares held less then 30 days---------------80% Capital Gaines Tax on profits.
Shares held longer then 31 days but less then 75 days---------#$%$ Capital Gaines Tax on profits.
Shares held longer then 76 days but less then 120 days---------------40% Capital Gaines Tax on profits.
Anything after 121 days ------------------Include gain as part of their Gross Income.
Any loss would be treated as it is now and can be used against their future stock purchases.
Short term trades and "shorting" are not evil enough to warrant the kind of confiscatory tax rates you are suggesting and as often promoted by various Obama/Biden sidekicks. I'm sure you don't want to be associated with the latter.
These sales are all classed as short term capital gains and are tax like ordinary income from 10% to 35%. Capital gains are the profits from a a capital sale. If there is a loss it is classified as a capital loss. Equities held over 1 year get the favorable capital gains tax rate of 15%. Any equity held one year or less the gains are treated as ordinary income.
That 2nd one should be 50%


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text:
Unmasking anti-endomysial antibodies in coeliac subjects positive for anti-smooth muscle antibodies
Article first published online: 2 JAN 2007
DOI: 10.1111/j.1651-2227.1999.tb01141.x
Acta Paediatrica
Volume 88, Issue 4, pages 462–464, April 1999
Additional Information
How to Cite
Lasagni, D., Ferrari, R. and Lapini, M. (1999), Unmasking anti-endomysial antibodies in coeliac subjects positive for anti-smooth muscle antibodies. Acta Paediatrica, 88: 462–464. doi: 10.1111/j.1651-2227.1999.tb01141.x
Publication History
- Issue published online: 2 JAN 2007
- Article first published online: 2 JAN 2007
- Received March 3, 1998. Accepted in revised form Nov. 3, 1998
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text:
- 544Promote
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text:
|ESPN.com: NFC North
|[Print without images]
Reading between the lines, it sounds as if New York Giants coach Tom Coughlin won't go overboard with his veterans Sunday at the Metrodome.
This will come as good news to Minnesota, who need a victory over the Giants to clinch the NFC North, and bad news to Chicago. The Bears are hoping for a Giants victory, combined with a win of their own at Houston, to grab the NFC North division title for themselves.
But if you read my colleague Matt Mosley's take over on the NFC East blog, you'll see Coughlin talking about "medical people" and doing "the best thing for our football team."
Coughlin insists that "we play every game to win" and that "we have always believed at this time of the year it is important to be playing your best football." But ultimately, Coughlin said: "We would like to continue to do that but we will do the right thing and the smart thing [for] our team."
It's not as if the absence of a few Giants starters would guarantee a Vikings victory. But the mentality of sitting or limiting starters tends to permeate the rest of a roster. According to Brad Biggs of the Chicago Sun-Times, Bears coach Lovie Smith made it clear he hopes the Giants play a normal game but added:
''We shouldn't have to think about what someone else is doing or hope someone does something to help us.''
This will be a topic of conversation all week, but I think it's pretty clear we'll see the likes of quarterback Eli Manning, tailback Brandon Jacobs and defensive end Justin Tuck on the sidelines pretty early Sunday at the Metrodome.
Continuing a look around the NFC North on Christmas Eve morning:


text:
Federal prosecutors and the attorneys representing the former head of Jamaica Hospital's parent company are now waiting for a judge to determine the administrator's fate in his bribery and corruption trial.
Both sides gave their final arguments in Manhattan federal court Friday in David Rosen's bench case in which he has been accused of illegally paying off and hiring several state legislators, including the late state Assemblyman Anthony Seminerio, in return for favorable legislation for Jamaica Hospital.
The prosecutors contended that the evidence against Rosen, who used to be the chief executive officer of MediSys, which runs Jamaica, Flushing and Peninsula hospitals, showed a clear example of corruption.
"Sophisticated men commit sophisticated crimes," Assistant U.S. Attorney Michael Bosworth said during his long summation. "[Rosen] was particularly sophisticated when it came to politics. That's how he was able to build a health care empire."
Rosen has been accused of paying hundreds of thousands of dollars to Seminerio; Assemblyman William Boyland (D-Brooklyn), a former MediSys employee; and state Sen. Karl Kruger (D-Brooklyn) from 2001 to the time of his arrest. He allegedly paid Seminerio $390,000 for favorable legislation that would support Jamaica Hospital, according to prosecutors.
Boyland and Kruger are awaiting their own corruption trials in the court.
Seminerio died in federal prison earlier this year after he pleaded guilty to setting up a consulting firm that was used to take money for his corrupt hospital deeds.
Bosworth reminded Judge Jed Rakoff that Rosen never told the FBI that he hired Seminerio as a paid consultant when they questioned him during the investigation into the elected officials.
But Scott Morvillo, Rosen's lawyer, countered that the U.S. attorney's office does not have a clear-cut case. Morvillo played up Rosen's 40 years of experience in the Queens health care system and said that his dealings with the elected officials was not illegal in any shape or form.
"There is no proof on the record that comes close to establishing that," he told Rakoff. "It's totally circumstantial evidence."
The judge did not deliver his verdict following the summations and as of press time Tuesday afternoon, no decision had been made. The court indicated that he might submit a written verdict at a later date.
Reach reporter Ivan Pereira by e-mail at ipereira@c
©2011 Community News Group
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text:
Settings.bundle, I have a text input with the identifier
ViewController.m, and my storyboards I have a
UIWebView set up that displays a url from the Settings:
- (void) updateBrowser {
NSString *fullURL = [[NSUserDefaults standardUserDefaults] stringForKey:@"url_preference"];
NSURL *url = [NSURL URLWithString:fullURL];
NSURLRequest *requestObj = [NSURLRequest requestWithURL:url];
[_EmbeddedBrowser loadRequest:requestObj];
This works.
When the URL in the Settings is changed, however, the
UIWebView does not update to reflect the new URL.
By disallowing the app to run in the background, the problem of not reflecting updated URLs is solved. However, a new problem arises: sessions are not preserved if the URL in Settings is left unchanged.
UIWebView should only update if the
url_preference is changed.
I've been attempting to use
applicationWillEnterForeground in
AppDelegate.m to force the
UIWebView to reload, however I'm having trouble.
In the ViewController, I can run:
- (void)viewDidLoad {
[self updateBrowser];
But it doesn't update when I try to run the same thing in the App Delegate:
- (void)applicationWillEnterForeground:(UIApplication *)application
ViewController *vc = [[ViewController alloc]init];
[vc updateBrowser];
(I also included
- (void) updateBrowser; in
ViewController.h, and
#import "ViewController.h" in
Thank you.


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text:
News Headlines
- Mon, May 02
- From Software lineup reel teases a PlayStation VR title for 2017
- Mighty No. 9 goes gold, receives a new release date of June 21 for everyone but 3DS and Vita
- Call of Duty: Infinite Warfare blasts off this November 4 on PC, Xbox One, and PlayStation 4
- Fri, Apr 29
- Kimishima: Nintendo to reduce Wii U production this fiscal year, 800,000 units expected to ship
- Mighty No. 9 is now a summer 2016 release according to EB Games
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text:
|Publication number
|Publication type
|Application number
|Publication date
|Dec 11, 2007
|Filing date
|Oct 26, 2005
|Priority date
|Oct 26, 2005
|Fee status
|Also published as
|Publication number
|Geetha Murthy, Daniela Fritter, Robert J. Iliff, Paula Ann Sanchez
|Original Assignee
|The Clorox Company
|Export Citation
|BiBTeX, EndNote, RefMan
|Patent Citations (37), Referenced by (2), Classifications (18), Legal Events (4)
|External Links: USPTO, USPTO Assignment, Espacenet
1. Field of the Invention
The present invention relates to thickened oxidant compositions, having both viscous and elastic properties, and in particular to thickened bleach compositions which are formulated to pour easily and flow through a narrow orifice or trigger spray bottle. The compositions also provide improved cling to vertical surfaces, such as toilet bowls.
2. Description of the Related Art
Hard surface cleaners are often thickened to provide to the consumer some control over the product during application, and to cling to the surface for some time after application in order to increase the contact time of the cleaning components. Furthermore, such thickened products are often put into packages with a closure that constricts the product to squeeze out in a narrow stream, for even more powerful and controllable product flow during application.
Consumer preferred products of this type therefore must have optimum flow properties under both dispensing and surface coating conditions. Products require ease of squeezing and projecting a fluid stream onto a surface. Products additionally require effectiveness of product coating and clinging to a surface. This optimization requires a balance. With too little thickening, the product will drain too quickly and result in insufficient perceived cling. With too much thickening, the product could result in dispensing problems or non-uniform coating.
A typical approach by those skilled in the art targets a higher product viscosity at low shear rates to ensure adequate cling, combined with a lower product viscosity at high shear rates to ensure ease of dispensing. A formulator might thus look for chemistries that result in sufficiently shear-thinning products to hit such viscosity ranges at both low and high shear rates.
Such systems are generally not difficult to formulate, and examples can be found on the market. However, the products that exhibit the most consumer preferred rheology for dispensing and coating are the non-bleach systems, for which thickening formulation approaches are much broader than for bleach-containing systems. Manufacturers have not been able to achieve the same optimum aesthetics with bleach-containing systems, which are commonly thickened with bleach stable surfactants, even though these formulations might be within the target viscosity ranges at low and high shear rates.
Formulators attempting to make improvements to product cling are most likely to make changes that increase the viscosity at low shear rate. This often has the effect of also increasing elasticity, and can actually negate any gains made to perceived cling by the increased viscosity. Alternatively, formulators may incorporate a component that forms weak interactions with the thickening system, which adds to the viscosity at low shear rates while having minimal impact at high shear rates. Aside from the added cost and formulation complexity, such additives may have a negative impact on the product aesthetics, e.g. forming an insoluble layer on the water surface in a toilet bowl or sticking to the hard surface to the point where it is difficult to rinse it away. Building the specified rheology with such a "filled" viscoelastic system is therefore not desirable.
Advantageously, the compositions of the invention are also suitable for the bleaching of different types of surfaces including hard-surfaces like floors, walls, tiles, glass, kitchen surfaces, bathrooms surfaces, toilet bowls and/or dishes and the like as well as fabrics. It is therefore an object of the present invention to provide a bleach-containing cleaning composition for use on a cleaning substrate that overcomes the disadvantages and shortcomings associated with prior art cleaning compositions for cleaning hard surfaces.
In accordance with the above objects and those that will be mentioned and will become apparent below, one aspect of the present invention comprises a cleaning system comprising:
In accordance with the above objects and those that will be mentioned and will become apparent below, another aspect of the present invention comprises a cleaning system comprising:
In accordance with the above objects and those that will be mentioned and will become apparent below, another aspect of the present invention comprises a cleaning composition comprising:
Further features and advantages of the present invention will become apparent to those of ordinary skill in the art in view of the detailed description of preferred embodiments below, when considered together with the attached claims.
Before describing the present invention in detail, it is to be understood that this invention is not limited to particularly exemplified systems or process parameters that may, of course, vary. It is also to be understood that the terminology used herein is for the purpose of describing particular embodiments of the invention only, and is not intended to limit the scope of the invention in any manner.
All publications, patents and patent applications cited herein, whether supra or infra, are hereby incorporated by reference in their entirety to the same extent as if each individual publication, patent or patent application was specifically and individually indicated to be incorporated by reference.
It must be noted that, as used in this specification and the appended claims, the singular forms "a," "an" and "the" include plural referents unless the content clearly dictates otherwise. Thus, for example, reference to a "surfactant" includes two or more such surfactants.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the invention pertains. Although a number of methods and materials similar or equivalent to those described herein can be used in the practice of the present invention, the preferred materials and methods are described herein.
The cleaning composition can be used as a disinfectant, sanitizer, and/or sterilizer. As used herein, the term "disinfect" shall mean the elimination of many or all pathogenic microorganisms on surfaces with the exception of bacterial endospores. As used herein, the term "sanitize" shall mean the reduction of contaminants in the inanimate environment to levels considered safe according to public health ordinance, or that reduces the bacterial population by significant numbers where public health requirements have not been established. An at least 99% reduction in bacterial population within a 24 hour time period is deemed "significant." As used herein, the term "sterilize" shall mean the complete elimination or destruction of all forms of microbial life and which is authorized under the applicable regulatory laws to make legal claims as a "Sterilant" or to have sterilizing properties or qualities.
In the application, effective amounts are generally those amounts listed as the ranges or levels of ingredients in the descriptions, which follow hereto. Unless otherwise stated, amounts listed in percentage ("%'s"): are in weight percent (based on 100% active) of the cleaning composition alone.
As used herein, the term "polymer" generally includes, but is not limited to, homopolymers, copolymers, such as for example, block, graft, random and alternating copolymers, terpolymers, etc. and blends and modifications thereof. Furthermore, unless otherwise specifically limited, the term "polymer" shall include all possible geometrical configurations of the molecule. These configurations include, but are not limited to isotactic, syndiotactic and random symmetries.
The term "cleaning composition", as used herein, is meant to mean and include a cleaning formulation having at least one surfactant.
The term "surfactant", as used herein, is meant to mean and include a substance or compound that reduces surface tension when dissolved in water or water solutions, or that reduces interfacial tension between two liquids, or between a liquid and a solid. The term "surfactant" thus includes anionic, nonionic and/or amphoteric agents.
It should be noted that as used herein the term "cleaning" refers generally to a chemical, physical or enzymatic treatment resulting in the reduction or removal of unwanted material, and "cleaning composition" specifically includes toilet bowl cleaners, drain openers, hard and soft surface cleaners and bleaching compositions. The cleaning composition may consist of a variety of chemically, physically or enzymatically reactive active ingredients, including solvents, acids, bases, oxidants, reducing agents, enzymes, detergents and thioorganic compounds.
The compositions of the invention may be in liquid aqueous form. They may comprise water in an amount of from 60% to 98% by weight, or from 80% to 97%, or from 85% to 97% by weight of the total aqueous liquid oxidant composition.
The current invention resolves the problem of achieving consumer preferred dispensing and cling by identifying an additional rheological property that significantly influences the consumer's perception of cling. Specifically, there are two components to good product cling: (1) an adequate value of viscosity at low shear rate, as already mentioned, and (2) a sufficiently high "liquification rate " of the product as it is applied to the surface. For embodiments of the invention that have a viscoelastic character, the liquification rate is inversely related to the material's relaxation time. Bleach-containing systems typically have an inadequate and lower liquification rate when formulated to satisfy condition (1), and thus will exhibit more elastic properties in the short time interval in which the product hits the surface and begins flowing to form a coating. These elastic properties can result in unevenness of the coating and a sense of inadequate product cling, even though the coating might be quite thick and slow draining in some places.
The current invention makes use of the surprising discovery that product cling can be enhanced without increasing the low shear viscosity, and can in fact accompany a decrease in low shear viscosity. This is accomplished by minimizing the elastic manifestations on product application, which leads to better coating efficiency and perceived cling.
The inventive cleaners can be Theologically characterized as viscoelastic, with fluid-like behavior at slow deformation rates, elastic behavior at high deformation rates, and an associated Relaxation constant that characterizes the boundary between the predominantly fluid and predominantly elastic regions. For embodiments of the invention that have a viscoelastic character, optimized cling can be achieved by formulating the material with a low Relaxation constant, for example less than 0.1 s and with a Zero-shear viscosity greater than 100 cP, or greater than 200 cP. Systems that meet these requirements will generally also be easy to dispense. Those skilled in the art can formulate such systems using the appropriate blend of bleach-stable surfactants, while accounting for the effects of other ingredients such as fragrance.
The compositions disclosed herein have elasticities and viscosities that are crucial rheological characterization parameters. Instruments capable of performing oscillatory or controlled stress creep measurements can be used to quantify elasticity. The rheology of the compositions disclosed herein was measured with a Stresstech rheometer at 25 � C. in the oscillatory mode and in the viscometry mode, using concentric cylinder geometry. A frequency sweep with a Stresstech rheometer produces oscillation data which shows the elastic and viscous moduli, G′ and G″, respectively, and the complex viscosity, as a function of frequency. For the viscoelastic compositions disclosed herein, G″ dominates G′ at low frequency, where the system is characterized by the Zero-shear viscosity, the plateau value of the complex viscosity with decreasing frequency. The elasticity increases in relative importance with increasing frequency, which can be seen by the faster growth of G′ vs. G″ and finally a "cross-over" to a region where G′ dominates G″ at higher frequency. The onset of elasticity in these systems is quantified as the frequency at which G′ crosses G″, or more conveniently, as the inverse of this quantity, called the Relaxation constant, which has units of time.
Embodiments disclosed herein have Zero-shear viscosities greater than 100 centipoise (cP) and Relaxation constants less than 0.1 seconds (s). Embodiments may also have Gel parameters less than 1.25. Liquids within the specified range of Zero-shear viscosity and having a Relaxation constant of less than 0.1 s will relax against the surface more quickly after being squirted, contributing to a more fluid perception and quicker, more efficient coating, thereby enhancing perceived cling. Liquids with a Zero-shear viscosity less than 100 cP will drain too quickly.
For most viscoelastic systems, the steady-state shear viscosity approaches a plateau as the shear rate is decreased, with a value that is reasonably close to the Zero-shear viscosity from the frequency sweep (Cox-Merz rule). Some products don't have a viscosity plateau with decreasing shear rate. In the "filled" systems, for example, the viscosity continues to climb with decreasing shear rate. In practice, this leads to somewhat gel-like behavior at low shear rate, rather than fluid-like as it would be if the viscosity were constant in this range. One consequence of this gel-like nature at low shear rate is that the product coating is harder to rinse off, for example, by flushing the toilet. Although the process of rinsing may be considered to be in a higher shear rate region where the existence of a low shear plateau seems irrelevant, it should be kept in mind that briefly flushing a coating that has been at rest is more a transient than steady-state process, and will thus reflect a considerable contribution from the low shear behavior. For this reason, materials with a viscosity that increases with decreasing shear rate beyond the break point (i.e., the point at which the curve can be expected to start flattening out with decreasing shear rate) are generally not desirable. A parameter that can be used to identify such systems is the ratio of shear viscosity at some defined rate below the break point to the Zero-shear viscosity from the frequency sweep. The Gel parameter is the ratio of steady-state shear viscosity at a shear rate of 2π/(100*RC) to Zero-shear viscosity (from frequency sweep). Liquids with gel parameters greater than 1.25 are generally harder to rinse.
Surfactants and Counterions
Where present the surfactant may be selected from anionic, nonionic, cationic, zwitterionic, amphoteric and mixtures thereof. In one embodiment of the present invention the surfactant is selected from amphoteric, zwitterionic and mixtures thereof. In another embodiment of the present invention, the surfactant is selected from amine oxide, betaine, sulphobetaine and mixtures thereof. In another embodiment of the present invention, the surfactant is selected from amine oxide, soap and mixtures thereof.
A suitable anionic surfactant is an alkali metal soap (alkyl carboxylates). The soaps utilized are typically formed in situ, by using the appropriate carboxylic acid (e.g., a C6-18 carboxylic acid, such as, without limitation, lauric, stearic, myristic acids, and unsaturated acids, such as coco fatty acid), and neutralizing with e.g., sodium hydroxide (NaOH). Other alkali metal hydroxides, such as potassium and lithium hydroxides, can be utilized. Commercial sources of these fatty acids include Henkel Corporation's Emery Division. The soap is present in an amount of about 0.1 to 10%. In one embodiment, the soap is present in an amount of about 0.5-1.5% by weight.
Suitable anionic surfactants for use herein include alkyl sulphates. Suitable alkyl sulphates for use herein include water-soluble salts or acids of the formula ROSO3M wherein R is a C6-C24 linear or branched, saturated or unsaturated alkyl group, preferably a C8-C20 alkyl group, more preferably a C8-C16 alkyl group and most preferably a C10-C14 alkyl group, and M is H or a cation or ammonium or substituted ammonium. As discussed above, where the surfactant is used as a means of thickening the composition, suitable alkyl sulphates include those having an alkyl chain length of greater than 10 carbon atoms, or from 12 to 20 carbon atoms, or from 12 to 18 carbon atoms. Examples of suitable sulphate surfactants include sodium dodecyl sulphate, sodium tetradecyl sulphate, sodium hexadecyl sulphate. Suitable anionic surfactants for use herein further include alkoxylated sulphate surfactants. Suitable alkoxylated sulphate surfactants for use herein are according to the formula RO(A)MSO3M wherein R is an unsubstituted C6-C24 alkyl, hydroxyalkyl or alkyl aryl group, having a linear or branched C6- C24 alkyl component, or a C12-C20 alkyl or hydroxyalkyl, or C 12 C18 alkyl or hydroxyalkyl, A is an ethoxy or propoxy or butoxy unit or a mixture thereof, m is greater than zero, typically between 0.5 and 6, or between 0.5 and 3, and M is H or a cation which can be, for example, a metal cation (e.g., sodium, potassium, lithium, calcium, magnesium, etc.), ammonium or substituted-ammonium cation. Alkyl ethoxylated sulphates, alkyl butoxylated sulphates as well as alkyl propoxylated sulphates are contemplated herein.
Where the surfactant is used as a means of thickening the composition, suitable alkoxylated sulphates include those having an alkyl chain length of greater than 12 carbon atoms, or from 14 to 20 carbon atoms, or from 14 to 16 carbon atoms and from 1 to 20 moles of alkoxy groups, or from 1 to 5 alkoxy groups, for example ethoxy groups. Suitable ethoxy sulphate surfactants include sodium dodecyl ethoxy sulphate (ethoxylation degree around 3), sodium tetradecyl ethoxy sulphate (ethoxylation degree around 3), sodium hexadecyl ethoxy sulphate (ethoxylation degree around 4).
Suitable anionic surfactants for use herein further include alkyl aryl sulphates. Suitable alkyl aryl sulphates for use herein include water-soluble salts or acids of the formula ROSO3M wherein R is an aryl, for example a benzyl, substituted by a C6-C24 linear or branched saturated or unsaturated alkyl group, or a C8-C20 alkyl group, or a C10-C16 alkyl group and M is H or a cation, or ammonium or substituted ammonium.
Suitable anionic surfactants for use herein further include alkyl sulphonates. Suitable alkyl sulphonates for use herein include water-soluble salts or acids of the formula RSO3M wherein R is a C6-C20 linear or branched, saturated or unsaturated alkyl group, or a C8-C18 alkyl group, or a C14-C17 alkyl group, and M is H or a cation, e.g., an alkali metal cation or ammonium or substituted ammonium.
Suitable anionic surfactants for use herein further include alkyl aryl sulphonates. Suitable alkyl aryl sulphonates for use herein include water-soluble salts or acids of the formula RSO3M wherein R is an aryl, preferably a benzyl, substituted by a C6-C20 linear or branched saturated or unsaturated alkyl group, for example a C8-C18 alkyl group, or a C9-C14 alkyl group, and M is H or a cation, or ammonium or substituted ammonium.
Suitable anionic surfactants for use herein further include alkoxylated sulphonate surfactants. Suitable alkoxylated sulphonate surfactants for use herein are according to the formula R(A)mSO3M wherein R is an unsubstituted C6-C20 alkyl, hydroxyalkyl or alkyl aryl group, having a linear or branched C6C20 alkyl component, or a C 12-C20 alkyl or hydroxyalkyl, or a C12-C 18 alkyl or hydroxyalkyl, A is an ethoxy or propoxy or butoxy unit, m is greater than zero, typically between 0.5 and 6, or between 0.5 and 3, and M is H or a cation, ammonium or substitutedammonium cation. Alkyl ethoxylated sulphonates, alkyl butoxylated sulphonates as well as alkyl propoxylated sulphonates are contemplated herein. Suitable anionic surfactants for use herein further include C6-C20 alkyl alkoxylated linear or branched diphenyl oxide disulphonate surfactants. Other suitable anionic surfactants for use herein include alkylcarboxylates.
Other anionic surfactants can include salts (including, for example, sodium, potassium, ammonium, and substituted ammonium salts such as mono-, di- and triethanolamine salts) of soap, C8-C24 olefinsulfonates, sulfonated polycarboxylic acids, acyl glycerol sulfonates, fatty oleyl glycerol sulfates, alkyl phenol ethylene oxide ether sulfates, alkyl phosphates, isethionates such as the acyl isethionates, N-acyl taurates, alkyl succinamates and sulfosuccinates, monoesters of sulfosuccinate (especially saturated and unsaturated C12- C 18 monoesters) diesters of sulfosuccinate (especially saturated and unsaturated C6-C14 diesters), acyl sarcosinates, sulfates of alkyl polysaccharides such as the sulfates of alkylpolyglucoside (the nonionic nonsulfated compounds being described below), branched primary alkyl sulfates, alkyl polyethoxy carboxylates such as those of the formula RO(CH2CH20)kCH2COO−M+wherein R is a C8-C 22 alkyl, k is an integer from 0 to 10, and M is a soluble salt-forming cation.
Resin acids and hydrogenated resin acids are also suitable, such as rosin, hydrogenated rosin, and resin acids and hydrogenated resin acids present in or derived from tall oil. Further examples are given in "Surface Active Agents and Detergents" (Vol. 1 and 11 by Schwartz, Perry and Berch). A variety of such surfactants are also generally disclosed in U.S. Pat. No. 3,929,678, issued Dec. 30, 1975 to Laughlin, et al. at Column 23, line 58 through Column 29, line 23.
Suitable nonionic surfactants for use herein are fatty alcohol ethoxylates and/or propoxylates, which are commercially available with a variety of fatty alcohol chain lengths and a variety of ethoxylation degrees. Indeed, the HLB values of such alkoxylated nonionic surfactants depend essentially on the chain length of the fatty alcohol, the nature of the alkoxylation and the degree of alkoxylation.
Surfactant catalogues are available which list a number of surfactants, including nonionics, together with their respective HLB values. The preferred nonionic surfactants are capped i.e. those where, instead of an H at the end of the chain there is an R group, preferably a methyl group. Such surfactants are for example marketed by BASF in the Plurafac range, for example Plurafac LF23 1.
Suitable amphoteric surfactants for use herein include amine oxides having the following formula R1R2R3NO wherein each of R1, R2 and R3 is independently a saturated substituted or unsubstituted, linear or branched hydrocarbon chains of from 1 to 30 carbon atoms. Suitable amine oxide surfactants to be used according to the present invention are amine oxides having the following formula R1R2R3NO wherein R1 is an hydrocarbon chain comprising from 1 to 30 carbon atoms, or from 6 to 20, or from 12 to 18, or from 14 to 16, and wherein R2 and R3 are independently substituted or unsubstituted, linear or branched hydrocarbon chains comprising from 1 to 4 carbon atoms, or from 1 to 3 carbon atoms, or are methyl groups. R1 may be a saturated substituted or unsubstituted linear or branched hydrocarbon chain. R1 is suitably a C16 alkyl group. Such amine oxides are commercially available from Hoechst and Clariant.
Suitable zwitterionic surfactants for use herein contain both cationic and anionic hydrophilic groups on the same molecule at a relatively wide range of pH's. The typical cationic group is a quaternary ammonium group, although other positively charged groups like phosphonium, imidazolium and sulfonium groups can be used. The typical anionic hydrophilic groups are carboxylates and sulfonates, although other groups like sulfates, phosphonates, and the like can be used. A generic formula for some zwitterionic surfactants to be used herein is R1 —N(R2)(R3)R4X− wherein R1 is a hydrophobic group; R2 and R3 are each C1-C4 alkyl, hydroxy alkyl or other substituted alkyl group which can also be joined to form ring structures with the N; R4 is a moiety joining the cationic nitrogen atom to the hydrophilic group and is typically an alkylene, hydroxy alkylene, or polyalkoxy group containing from 1 to 10 carbon atoms; and X is the hydrophilic group which is suitably a carboxylate or sulfonate group. Suitable hydrophobic groups R1 are alkyl groups containing from 1 to 24, or from 12 to 18, or from 14 to 16 carbon atoms. The hydrophobic group can contain unsaturation and/or substituents and/or linking groups such as aryl groups, amido groups, ester groups and the like. In general, the simple alkyl groups are suitable for cost and stability reasons.
Suitable zwitterionic surfactants include betaine and sulphobetaine surfactants, functionalized betaines such as acyl betaines, alkylamidoalkyldimethyl betaines, alkyl imidazoline alanine betaines, glycine betaines, derivatives thereof and mixtures thereof. Suitable betaine and sulphobetaine surfactants for use herein are the betaine/sulphobetaine and betaine-like detergents wherein the molecule contains both basic and acidic groups which form an inner salt giving the molecule both cationic and anionic hydrophilic groups over a broad range of pH values. Some common examples of these detergents are described in U. S. Pat. Nos. 2,082,275, 2,702,279, 2,255,082, and 5,252,245 incorporated herein by reference. Suitable betaine and sulphobetaine surfactants herein are according to the formula R2R1—N+—(CH2)n—Y—R3 wherein R1 is a hydrocarbon chain containing from 1 to 24 carbon atoms, or from 12 to 18, or from 14 to 16, wherein R2 and R3 are hydrocarbon chains containing from 1 to 3 carbon atoms, or 1 carbon atom, wherein n is an integer from 1 to 10, or from 1 to 6, or is 1, Y is selected from the group consisting of carboxyl and sulfonyl radicals and wherein the sum of R1, R2 and R3 hydrocarbon chains is from 14 to 24 carbon atoms, or mixtures thereof.
Examples of particularly suitable betaine surfactants include C12-C18 alkyl dimethyl betaine such as coconut-betaine and C10-C16 alkyl dimethyl betaine such as laurylbetaine. Coconutbetaine is commercially available from Seppic under the trade name of Amonyl 2659. Laurylbetaine is commercially available from Albright & Wilson under the trade name Empigen BB/L.
Other specific zwitterionic surfactants have the generic formulas: R1—C(O)—N (R2)—(C(R3)2)n—N(R2)2(+)—(C(R3) 2)n—SO3(−) or R1—C(O)—N (R2)—(C(R3)2)n—N(R2)2(+)—(C(R3)2)n—COO(−) wherein each R1 is a hydrocarbon, e.g. an alkyl group containing from 8 up to 20, or up to 18, or up to 16 carbon atoms, each R2 is either a hydrogen (when attached to the amido nitrogen), short chain alkyl or substituted alkyl containing from one to 4 carbon atoms, or groups selected from the group consisting of methyl, ethyl, propyl, hydroxy substituted ethyl or propyl and mixtures thereof, or methyl, each R3 is selected from the group consisting of hydrogen and hydroxy groups and each n is a number from 1 to 4, or from 2 to 3, or 3, with no more than one hydroxy group in any (C(R3)2) moiety. The R1 groups can be branched and/or unsaturated. The R2 groups can also be connected to form ring structures. A surfactant of this type is a C10-C14 fatty acylamidopropylene (hydroxypropylene) sulfobetaine that is available from the Sherex Company under the trade name "Varion CAS sulfobetaine".
A suitable composition contains a binary surfactant thickener comprising a betaine and anionic counterion. Examples of other suitable surfactants include amine oxides, sarcosinates, taurates and quaternary ammonium compounds.
Operative betaines include the C14-18 alkyl betaines and C14-18 alkyl sulfobetaines. Suitable is a cetyl dimethyl betaine (CEDB) such as Amphosol CDB (a trademarked product of the Stepan Company), which is about 95% or greater C16, less than 5% C12/14 and less than 1% C18. It is noted that when referring to carbon chain lengths of the betaine or any other compound herein, the commercial, polydisperse forms are contemplated (but not, required). Thus, a given chain length within the C14-18 range will be predominately, but not exclusively, the specified length. As used herein in reference to the betaine or sulfobetaine, the term "alkyl" includes both saturated and unsaturated groups. Fully saturated alkyl groups are suitable in the presence of hypochlorite. C10-18 alkylamido and alkylamino betaines, and sulfobetaines having C14-18 alkyl, or C10-18 alkylamino or alkylamido groups, are also suitable for use in the compositions of the present invention.
The betaine is added at levels, which, when combined with the counterion, are thickening effective. Generally about 0.1 to 10.0 weight percent of the betaine is utilized, or about 0.1 to 5.0% betaine, or about 0.15-2.0% betaine.
The counterion is an anionic organic counterion selected from the group consisting of C2-6 alkyl carboxylates, aryl carboxylates, C2-10 alkyl sulfonates, aryl sulfonates, sulfated C2-10 alkyl alcohols, sulfated aryl alcohols, and mixtures thereof. The aryl compounds are derived from benzene or napthalene and may be substituted or not. The alkyls may be branched or straight chain, or are those having two to eight carbon atoms. The counterions may be added in acid form and converted to the anionic form in situ, or may be added in anionic form. Suitable substituents for the alkyls or aryls are C1-4 alkyl or alkoxy groups, halogens, nitro groups, and mixtures thereof. Substituents such as hydroxy or amine groups are suitable for use with some non-hypochlorite cleaning actives, such as solvents, surfactants and enzymes. If present, a substituent may be in any position on the rings. If benzene is used, the para (4) and meta (3) positions are preferred. In some circumstances the cleaning active itself may be within the class of thickening-effective counterions. For example, some carboxylic acid cleaning actives may be present in both the acid and conjugate base forms, the latter which could serve as the counterion. The C2-6 alkyl carboxylates may act in this manner. The counterion is added in an amount sufficient to thicken and result in a viscoelastic rheology, suitably between about 0.01 to 10 weight percent. A suitable mole ratio of betaine to counterion depends on the chain length and concentration of the betaine, type of counterion, and the ionic strength of the solution, as well as whether the primary object of the composition is phase stability or viscosity. Using CEDB and sodium xylene sulfonate (SXS), a suitable mole ratio is about 10:1 to 1:3, or about 2:1 to 1:2. A suitable weight ratio of CEDB to SXS is about 15:1 to 1:2, or3:1 to 1:1.
Oxidants, when used, include, but are not limited to, peracids, hypohalite sources, hydrogen peroxide, and/or sources of hydrogen peroxide. An oxidant source may be selected from various hypochlorite-producing species, for example, halogen oxidants selected from the group consisting of the alkali metal and alkaline earth salts of hypohalite, haloamines, haloimines, haloimides and haloamides. All of these are believed to produce hypohalous oxidant species in situ. Hypochlorite and compounds producing hypochlorite in aqueous solution are suitable and hypobromite is also suitable. Representative hypochlorite-producing compounds include sodium, potassium, lithium and calcium hypochlorite, chlorinated trisodium phosphate dodecahydrate, potassium and sodium dicholoroisocyanurate and trichlorocyanuric acid. Organic oxidant sources suitable for use include heterocyclic N-bromo and N-chloro imides such as trichlorocyanuric and tribromo-cyanuric acid, dibromo- and dichlorocyanuric acid, and potassium and sodium salts thereof, N-brominated and N-chlorinated succinimide, malonimide, phthalimide and naphthalimide. Also suitable are hydantoins, such as dibromo and dichloro dimethyl-hydantoin, chlorobromodimethyl hydantoin, N-chlorosulfamide (haloamide) and chloramine (haloamine). Suitable in this invention is sodium hypochlorite having the chemical formula NaOCl, in an amount ranging from about 0.1 weight percent to about 15 weight percent, or about 0.2% to 10%, or about 2.0% to 6.0%. It may be necessary to add a buffer or other alkaline agent to increase the composition pH to above about 10.0, or about 12.0 to maintain the storage stability of the composition.
According to the present invention, the oxidizing agent may be an oxygen bleach, including a peroxygen, peroxyhydrate or active oxygen generating compound. Suitable peroxygen bleaches for use herein include hydrogen peroxide or sources thereof. As used herein a source of hydrogen peroxide refers to any compound which generates active oxygen when said compound is in contact with water. Suitable water-soluble sources of hydrogen peroxide for use herein include percarbonates, preformed percarboxylic acids, persilicates, persulphates, perborates, organic and inorganic peroxides and/or hydroperoxides.
In one embodiment, hydrogen peroxide is employed in the aqueous composition of the present invention. The compositions of the present invention that comprise a peroxygen bleach may further comprise a bleach activator or mixtures thereof. By "bleach activator", it is meant herein a compound which reacts with peroxygen bleach like hydrogen peroxide to form a peracid. The peracid thus formed constitutes the activated bleach. Suitable bleach activators to be used herein include those belonging to the class of esters, amides, imides, or anhydrides. Examples of suitable compounds of this type are disclosed in British Patent GB 1 586 769 and GB 2 143 231 and a method for their formation into a prilled form is described in European Published Patent Application EP-A-62 523. Suitable examples of such compounds to be used herein are tetracetyl ethylene diamine (TAED), sodium 3,5,5 trimethyl hexanoyloxybenzene sulphonate, diperoxy dodecanoic acid as described for instance in U.S. Pat. No. 4,818,425 and nonylamide of peroxyadipic acid as described for instance in U.S. Pat. No. 4,259,201 and n-nonanoyloxybenzenesulphonate (NOBS). Also suitable are N-acyl caprolactams selected from the group consisting of substituted or unsubstituted benzoyl caprolactam, octanoyl caprolactam, nonanoyl caprolactam, hexanoyl caprolactam, decanoyl caprolactam, undecenoyl caprolactam, formyl caprolactam, acetyl caprolactam, propanoyl caprolactam, butanoyl caprolactam pentanoyl caprolactam or mixtures thereof. A particular family of bleach activators of interest was disclosed in EP 624 154, and particularly preferred in that family is acetyl triethyl citrate (ATC). Acetyl triethyl citrate has the advantage that it is environmental-friendly as it eventually degrades into citric acid and alcohol. Furthermore, acetyl triethyl citrate has a good hydrolytical stability in the product upon storage and it is an efficient bleach activator. A particular family of bleach activators also of interest was disclosed in U.S. Pat. No.s 5,741,437, 6,010,994 and 6,046,150, generally described as n-alkyl alkyl ammonium acetonitrile activators, and particularly preferred in that family is n-methyl morpholinium acetonitrile (MA).
In addition, other classes of peroxides can be used as an alternative to hydrogen peroxide and sources thereof or in combination with hydrogen peroxide and sources thereof. Suitable classes include dialkylperoxides, diacylperoxide, performed percarboxylic acids, organic and inorganic peroxides and/or hydroperoxides. Suitable organic peroxides/hydroperoxides include diacyl and dialkyl peroxides/hydro-eroxides such as dibenzoyl peroxide, t-butyl hydroperoxide, dilauroyl peroxide, dicumyl peroxide, and mixtures thereof. Suitable preformed peroxyacids for use in the compositions according to the present invention include diperoxydodecandioic acid DPDA, magnesium perphthalic acid, perlauric acid, perbenzoic acid, diperoxyazelaic acid and mixtures thereof.
Persulfate salts, or mixtures thereof, are alternative sources of active oxygen that may be used in the compositions according to the present invention. In one embodiment, a persulfate salt can be used herein in the form of the monopersulfate triple salt. One example of monopersulfate salt commercially available is potassium monopersulfate commercialized by Peroxide Chemie GMBH under the trade name Curox�, by Degussa under the trade name Caroat and from Du Pont under the trade name Oxone. Other persulfate salts such as dipersulfate salts commercially available from Peroxide Chemie GMBH can be used in the compositions according to the present invention.
In embodiments employing a solid oxidizing agent and/or solid bleaching component, the material is preferably employed in the form of a finely divided particulate having a particle size, and/or average particle size distribution, that is sufficiently small to enable suspension in the aqueous composition with a minimum of settling or precipitation. In an alternative embodiment employing a particulate source of oxidizing agent, the agent is coated and/or encapsulated according to any known methods and materials in the art to prevent and/or retard dissolution of the agent in the aqueous compositions during storage, such encapsulation means and materials selected, however, so as to provide release of the oxidizing agent upon dilution of the compositions into a larger volume of water, such as for example, during dilution into a washing machine during use. In embodiments employing a plurality of oxidizing agents, or combinations of oxidizing agents, secondary oxidizing agents and/or oxidizing agents and/or activators, the materials may be present as separately dispersed particulate components, optionally coated and/or encapsulated, or alternatively present in the form of coated and/or encapsulated core agglomerate of the various agents, such coating or encapsulating material acting to prevent or retard water penetration into the core agglomerate under storage conditions, but providing release as described hereinbefore.
In a further embodiment, both a source of water soluble oxidizing agent and a particulate oxidizing agent are combined so as to provide a composition according to the present invention having immediate bleaching strength combined with a reserve bleaching strength when the compositions are diluted for use.
In yet further embodiments, only a low water solubility oxidizing agent, or alternatively a coated and/or encapsulated oxidizing agent, are employed in the inventive compositions so as to provide minimal or no bleaching effect, for example providing a composition that will not damage or over bleach a susceptible fabric or dye even upon (improper) direct application, such compositions however being capable of releasing the oxidizing agent when the composition is properly diluted for use, such as in a washing machine, where the diluted level of the oxidizing agent will not damage the fabric or dye.
Optional ingredients
The pH of the liquid compositions according to the present invention, as is, is typically from 4 to 14, or from 10 to 14, or from 12 to 14. The liquid compositions of the invention have a pH of from 7.5 to 13, or from 8 to 12, or from 8.5 to 11.5, when diluted into 1 to 500 times its weight of water. The pH range is suitably provided by the hypohalite bleach, which are alkalis and optionally by the pH buffering component if present. However, in addition to these components, a strong source of alkalinity may also optionally be used.
Suitable sources of alkalinity are the caustic alkalis such as sodium hydroxide, potassium hydroxide and/or lithium hydroxide, and/or the alkali metal oxides such as sodium and/or potassium oxide. A suitable strong source of alkalinity is a caustic alkali, for example sodium hydroxide and/or potassium hydroxide. Typical levels of such caustic alkalis, when present, are of from 0.1% to 1.5% by weight, or from 0.5% to 1.5% by weight of the composition.
The composition according to the invention may comprise other optional components such as pH buffering components, stabilizing agents, other oxidant-stable surfactants, builders, thickening agents, polymers, dyes, solvents, perfumes, brighteners, and mixtures thereof.
The compositions according to the present invention may optionally comprise a pH buffering component or mixture thereof. The pH buffering component ensures that the pH of the composition is buffered to a pH value ranging from 7.5 to 13, or from 8 to 12, or from 8.5 to 11.5 after the composition has been diluted into 1 to 500 times its weight of water. Suitable pH buffering components for use herein are selected from the group consisting of alkali metal salts of carbonates, polycarbonates, sesquicarbonates, silicates, polysilicates, boron salts, phosphates, stannates, alluminates and mixtures thereof. Suitable alkali metal salts for use herein are sodium and potassium.
Suitable boron salts or mixtures thereof for use herein include alkali metal salts of borates and alkyl borates and mixtures thereof. Examples of boron salts include boric acid, alkali metal salts of metaborate, tetraborate, octoborate, pentaborate, dodecaboron, borontrifluoride and alkyl borate containing from 1 to 12 carbon atoms, or from 1 to 4. Suitable alkyl borate includes methyl borate, ethyl borate and propyl borate. Suitable boron salts herein are the alkali metal salts of metaborate, such as sodium metaborate, potassium metaborate, and the alkali metal salts of borate, such as sodium borate, or mixtures thereof. Boron salts like sodium metaborate and sodium tetraborate are commercially available from Borax and Societa Chimica Larderello under the names sodium metaborate and Borax.
Suitable pH buffering components are selected from the group consisting of sodium carbonate, sodium silicate, sodium borate, sodium metaborate and mixtures thereof. The raw materials involved in the preparation of hypohalite bleaches usually contain by-products, e.g. calcium carbonate resulting in an amount of up to 0.4% by weight of by-product within the hypohalite composition. However, at such amount, the by-product will not have the buffering action defined above. Liquid oxidant compositions herein preferably contain an amount of pH buffering component of from 0.5% to 9% by weight, or from 0.5% to 5% by weight, or from 0.6% to 3% by weight of the composition.
Suitable radical scavengers for use herein include aromatic radical scavengers comprising an unsaturated ring system of from 3 to 20 carbon atoms, or from 3 to 18, or from 5 to 14 and having a double bond set comprising a total of 4n+2 electrons, wherein n is an integer of from 0 to 4, preferably of from 1 to 3. Indeed said aromatic radical scavengers include benzene derivatives, naphthalene derivatives, annulene derivatives, cyclopentadiene derivatives, cyclopropene derivatives and the like, especially aryl carboxylates and/or aryl sulfonates.
Viscosity of the compositions herein may be enhanced by including aliphatic and aromatic hydrocarbon oils such as hexadecane and dodecylbenzene.
The composition of the present invention can be formulated to include such components as fragrances, coloring agents, whiteners, solvents, soil release polymers, bacteriocidal agents, chelating agents and builders, which enhance performance, stability or aesthetic appeal of the composition. The composition of the present invention may contain from about 0.01% to about 0.5% of a fragrance such as those commercially available from International Flavors and Fragrance, Inc. Dyes and pigments may be included in small amounts. Ultramarine Blue (UMB) and copper phthalocyanines are examples of widely used pigments which may be incorporated in the composition of the present invention.
It should be briefly noted that the main ingredient of the oxidizing compositions disclosed herein is water, preferably softened, distilled or deionized water. Water provides the continuous liquid phase into which the other ingredients are added to be dissolved/dispersed. The amount of water present generally exceeds 30% and can be as high as 99.9%, although generally, it is present in a quantity sufficient (q.s.) to provide the appropriate rheology characteristics desired.
In the present invention, the composition can be used to treat surfaces. By "surfaces", it is meant herein any inanimate surface. These inanimate surfaces include, but are not limited to, hard-surfaces typically found in houses like kitchens, bathrooms, or in car interiors, e.g., tiles, walls, floors, chrome, glass, smooth vinyl, any plastic, plastified wood, table top, sinks, cooker tops, dishes, sanitary fittings such as sinks, showers, shower curtains, wash basins, toilets and the like, as well as fabrics including clothes, curtains, drapes, bed linens, bath linens, table cloths, sleeping bags, tents, upholstered furniture and the like, and carpets. Inanimate surfaces also include household appliances including, but not limited to, refrigerators, freezers, washing machines, automatic dryers, ovens, microwave ovens, dishwashers and so on.
Thus, the present invention also encompasses a process of treating (e.g. bleaching) a fabric, as the inanimate surface. In such a process a fabric is contacted with a composition according to the present invention. In another embodiment the present invention also encompasses a process of treating a hard surface, as the inanimate surface. In such a process a composition, as defined herein, is contacted with the hard surfaces to be treated. Thus, the present invention also encompasses a process of treating a hard-surface with a composition, as defined herein, wherein said process comprises the step of applying said composition to said hard surface, preferably only soiled portions thereof, and optionally rinsing said hard surface.
In the process of treating surfaces according to the present invention the composition, as defined herein, may be applied to the surface to be treated in its neat form or in its diluted form typically up to 200 times their weight of water, or 80 to 2 times their weight of water, or 60 to 2 times.
One example of containers suitable for use in the invention are those for manually cleaning the toilet bowl by delivering a cleaning fluid through a nozzle that is inclined to facilitate directing a fluid to surfaces within the toilet bowl, such as the sides. Other suitable containers can deliver the composition to a vertical hard surface. Such containers include one or more apertures through which the fluid is delivered as the flexible sides of the container are squeezed. Examples of suitable containers are described in U.S. Pat. No. 6,691,328 to Delfino, U.S. Pat. No. 6,583,103 to Klinkhamer, and U.S. Pat. No. 5,261,567 to Krall. U.S. Pat. No. 6,425,406 to Klinkhammer et al. describes a variety of toilet cleaning devices and methods. U.S. Pat. No. 6,234,412 to von Schuckmann describes suitable spray devices.
The invention may also include a system including the composition contained within a suitable container and instructions to apply the composition, for example to the sides of a toilet bowl or a vertical hard surface.
Inventive compositions were prepared as shown in Table I and tested with consumers against commercial manual toilet bowl cleaners in Table II. The rheology of the inventive compositions and comparative commercial compositions are given in Table III.
Composition A
Composition B
(% Actives)
(% Actives)
Coconut Fatty Acida
Potassium Iodide
Sodium hypochlorite
Balance Water
aEmery Coco Fatty Acid �
bAmmonyx MO �
cAmmonyx LO �
Lysol � Bleach
Manual Toilet
Bowl Cleaner
Composition A
Composition B
Overall rating
Easy to dispense
viscosity (cP)
constant (s)*
Oxidant compositions
Composition A
Composition B
Clorox � Bleach MTBC
Lysol � Bleach MTBC
Clorox � Cleanup Gel
Professional Strength
Liquid Plum'r �
Non-oxidant compositions
Clorox � MTBC
Lysol Cling � MTBC
Lime-a-way �
Easy-Off BAM �
*Relaxation constant is the inverse of frequency in Hz at cross-over of G′, G″
**Gel parameter is the ratio of steady-state shear viscosity at a shear rate of 2π/(100 * RC) to Zero-shear viscosity (from frequency sweep)
Without departing from the spirit and scope of this invention, one of ordinary skill can make various changes and modifications to the invention to adapt it to various usages and conditions. As such, these changes and modifications are properly, equitably, and intended to be, within the full range of equivalence of the following claims.
|Cited Patent
|Filing date
|Publication date
|Aug 11, 1972
|Dec 3, 1974
|Flow Pharma Inc
|Stable liquid detergent concentrates containing active oxygen
|Oct 2, 1975
|Oct 24, 1978
|Polytrol Chemical Corporation
|Amidobetaine containing detergent composition non-toxic to aquatic life
|Nov 17, 1978
|Jun 2, 1981
|Lever Brothers Company
|Pourable liquid compositions
|Nov 21, 1980
|Jun 29, 1982
|Lever Brothers Company
|Liquid, thickened chlorine bleaching composition
|Oct 19, 1981
|Mar 1, 1983
|Lever Brothers Company
|Viscous compositions containing amido betaines and salts
|Mar 23, 1982
|Jun 14, 1983
|The Drackett Company
|Thickened alkali metal hypochlorite compositions
|Sep 14, 1981
|Aug 2, 1983
|Lever Brothers Company
|Phosphate free liquid scouring composition
|Oct 28, 1982
|Oct 2, 1984
|Lever Brothers Company
|Colored aqueous alkalimetal hypochlorite compositions
|Mar 25, 1983
|Oct 23, 1984
|Ajinomoto Company Incorporated
|Detergent composition comprising a mixture of an N-acyllysine and anionic surface active agents, possessing unique properties in soft and hard water
|Nov 8, 1984
|Mar 18, 1986
|The Procter & Gamble Company
|Cleaning compositions
|Sep 28, 1984
|Jun 17, 1986
|Colgate-Palmolive Company
|High foaming nonionic surfacant based liquid detergent
|May 29, 1986
|Oct 13, 1987
|Ecolab, Inc.
|Aqueous acidic composition for cleaning fiberglass
|Sep 12, 1986
|May 10, 1988
|The Drackett Company
|Thickened acid cleaner compositions containing quaternary ammonium germicides and having improved thermal stability
|Aug 31, 1983
|Sep 13, 1988
|The Dow Chemical Company
|Shear stable antimisting formulations
|Nov 3, 1986
|Sep 20, 1988
|The Proctor & Gamble Company
|Shampoo containing mixtures of sulfate and/or sulfonate, sarcosinate and betaine surfactants
|Dec 23, 1985
|Sep 20, 1988
|Colgate-Palmolive Company
|Light duty liquid dishwashing composition containing abrasive
|May 23, 1986
|Nov 8, 1988
|The Procter & Gamble Company
|Cleaning compositions
|Dec 8, 1986
|Jan 24, 1989
|The Dow Chemical Company
|Aqueous bleach compositions thickened with a viscoelastic surfactant
|May 20, 1988
|Feb 13, 1990
|The Clorox Company
|Viscoelastic cleaning compositions with long relaxation times
|Sep 6, 1989
|Apr 30, 1991
|The Clorox Company
|Viscoelastic cleaning compositions and methods of use therefor
|Nov 17, 1987
|Oct 8, 1991
|The Clorox Company
|Viscoelastic cleaning compositions and methods of use therefor
|Dec 22, 1992
|Nov 16, 1993
|Owens-Illinois Plastic Products Inc.
|Squeeze package which can be inverted to dispense liquids
|Jul 15, 1991
|Aug 9, 1994
|Rader James E
|Phase stable viscoelastic cleaning compositions
|Jun 8, 1993
|Feb 14, 1995
|The Clorox Company
|Viscoelastic cleaning compositions with long relaxation times
|Mar 18, 1996
|Nov 18, 1997
|Reckitt & Colman Inc.
|Pigmented rheopectic cleaning compositions with thixotropic properties
|Aug 4, 1995
|Nov 10, 1998
|Rader; James E.
|Method for opening drains using phase stable viscoelastic cleaning compositions
|Dec 17, 1999
|Apr 24, 2001
|Henkel Kommanditgesellschaft Auf Aktien
|Viscoelastic bleaching and disinfecting compostions
|Sep 2, 1998
|May 22, 2001
|Alfred Von Schuckmann
|Spray pump capable of being actuated by a hand lever
|Sep 14, 1999
|Jul 30, 2002
|S. C. Johnson & Son, Inc.
|Toilet bowl cleaning method
|Jul 8, 1999
|Nov 12, 2002
|The Clorox Company
|Foaming drain cleaner
|Aug 9, 2002
|Jun 24, 2003
|S.C. Johnson & Son, Inc.
|Two part cleaning formula resulting in an effervescent liquid
|Oct 18, 2001
|Oct 28, 2003
|The Clorox Company
|Ternary foaming cleaner
|Dec 8, 2000
|Dec 9, 2003
|The Clorox Company
|Binary foaming drain cleaner
|Jul 15, 2002
|Feb 17, 2004
|Nicholas A. Delfino
|Fluid dispensing bottle having a refillable reservoir and a metering section
|May 19, 2003
|May 31, 2005
|The Clorox Company
|Binary foaming drain cleaner
|Oct 10, 2003
|Apr 14, 2005
|Stephen Chan
|Cleaning compositions with both viscous and elastic properties
|Apr 29, 2005
|Nov 2, 2006
|Kaaret Thomas W
|Oxidizing compositions and methods thereof
|Citing Patent
|Filing date
|Publication date
|Aug 21, 2007
|Sep 30, 2010
|Tokyo Electron Limited
|Etching method, etching apparatus, computer program and storage medium
|Aug 29, 2013
|Mar 13, 2014
|The Clorox Company
|Drain formulation for enhanced hair dissolution
|U.S. Classification
|510/191, 510/238, 510/380, 510/503, 510/481, 510/379, 510/372, 510/375, 510/433
|International Classification
|Cooperative Classification
|European Classification
|Dec 29, 2005
Owner name: CLOROX COMPANY, THE, CALIFORNIA
Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:MURTHY, GEETHA;FRITTER, DANIELA;REEL/FRAME:017150/0954
Effective date: 20051021
|Jun 6, 2006
Owner name: THE CLOROX COMPANY, CALIFORNIA
Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:ILIFF, ROBERT J.;SANCHEZ, PAULA ANN;REEL/FRAME:017758/0268
Effective date: 20060317
|Jun 13, 2011
|Fee payment
Year of fee payment: 4
|Jun 11, 2015
|Fee payment
Year of fee payment: 8


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Fine piping adds a polished note to a lightweight cotton oxford-cloth robe with a classic shawl collar and roomy patch pockets.
- 41" length (size Medium).
- Front tie closure.
- Cotton; machine wash.
- By Lauren Ralph Lauren; imported.
- Lingerie.
Short Shawl Collar Robe
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Close View Of A Mated Pair Of Common Loons Swimming In Tandem Stock PhotoAnimal,Animals In The Wild,Animals Mating,Aquatic,Close To,Color Image,Common Loon,Day,Female Animal,Full Length,Horizontal,Male Animal,Next To,No People,Outdoors,Photography,Pond,Side View,Swimming,Togetherness,Two Animals,WyomingPhotographer Michael S. QuintonCollection: National Geographic